EP0379431A1 - Glass-aluminium sealing process, in particular for a hybrid circuit box electrical feedthrough, corresponding composite article and glass composition - Google Patents
Glass-aluminium sealing process, in particular for a hybrid circuit box electrical feedthrough, corresponding composite article and glass composition Download PDFInfo
- Publication number
- EP0379431A1 EP0379431A1 EP90400134A EP90400134A EP0379431A1 EP 0379431 A1 EP0379431 A1 EP 0379431A1 EP 90400134 A EP90400134 A EP 90400134A EP 90400134 A EP90400134 A EP 90400134A EP 0379431 A1 EP0379431 A1 EP 0379431A1
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- European Patent Office
- Prior art keywords
- approximately
- vitreous
- taken
- combination
- object according
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims description 73
- 238000007789 sealing Methods 0.000 title claims description 32
- 239000011521 glass Substances 0.000 title claims description 20
- 239000000203 mixture Substances 0.000 title claims description 13
- 239000002131 composite material Substances 0.000 title claims description 6
- 239000004411 aluminium Substances 0.000 title abstract 2
- 239000000463 material Substances 0.000 claims abstract description 106
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 24
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract description 10
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000010304 firing Methods 0.000 claims abstract 3
- 229910052751 metal Inorganic materials 0.000 claims description 31
- 239000000843 powder Substances 0.000 claims description 29
- 229910044991 metal oxide Inorganic materials 0.000 claims description 27
- 150000004706 metal oxides Chemical class 0.000 claims description 26
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 22
- 239000003795 chemical substances by application Substances 0.000 claims description 21
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 20
- 239000011230 binding agent Substances 0.000 claims description 18
- 239000002184 metal Substances 0.000 claims description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 13
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 12
- 238000002425 crystallisation Methods 0.000 claims description 12
- 230000008025 crystallization Effects 0.000 claims description 12
- 238000005245 sintering Methods 0.000 claims description 12
- 238000010411 cooking Methods 0.000 claims description 11
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 229910000838 Al alloy Inorganic materials 0.000 claims description 9
- 239000000470 constituent Substances 0.000 claims description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- 229910019142 PO4 Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 239000010452 phosphate Substances 0.000 claims description 6
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 235000017550 sodium carbonate Nutrition 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 229910000952 Be alloy Inorganic materials 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000010397 one-hybrid screening Methods 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 238000003466 welding Methods 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 3
- 238000003754 machining Methods 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- FBEIPJNQGITEBL-UHFFFAOYSA-J tetrachloroplatinum Chemical compound Cl[Pt](Cl)(Cl)Cl FBEIPJNQGITEBL-UHFFFAOYSA-J 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 2
- 230000002093 peripheral effect Effects 0.000 claims description 2
- 229940057838 polyethylene glycol 4000 Drugs 0.000 claims description 2
- 238000010791 quenching Methods 0.000 claims description 2
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- 238000007493 shaping process Methods 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 229910052593 corundum Inorganic materials 0.000 claims 7
- 229910001845 yogo sapphire Inorganic materials 0.000 claims 7
- 239000000945 filler Substances 0.000 claims 3
- 230000008030 elimination Effects 0.000 claims 2
- 238000003379 elimination reaction Methods 0.000 claims 2
- 238000001354 calcination Methods 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 238000010025 steaming Methods 0.000 claims 1
- 239000005365 phosphate glass Substances 0.000 abstract description 7
- 238000002844 melting Methods 0.000 description 9
- 230000008018 melting Effects 0.000 description 9
- 229910000833 kovar Inorganic materials 0.000 description 8
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000011161 development Methods 0.000 description 4
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 3
- 125000004430 oxygen atom Chemical group O* 0.000 description 3
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
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- 238000002513 implantation Methods 0.000 description 2
- 235000019837 monoammonium phosphate Nutrition 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 239000005297 pyrex Substances 0.000 description 2
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 101150099374 PCF2 gene Proteins 0.000 description 1
- KGWWEXORQXHJJQ-UHFFFAOYSA-N [Fe].[Co].[Ni] Chemical compound [Fe].[Co].[Ni] KGWWEXORQXHJJQ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000003042 antagnostic effect Effects 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
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- 239000013078 crystal Substances 0.000 description 1
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- 239000003822 epoxy resin Substances 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000011872 intimate mixture Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/24—Manufacture or joining of vessels, leading-in conductors or bases
- H01J9/32—Sealing leading-in conductors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B17/00—Insulators or insulating bodies characterised by their form
- H01B17/26—Lead-in insulators; Lead-through insulators
- H01B17/30—Sealing
- H01B17/303—Sealing of leads to lead-through insulators
- H01B17/305—Sealing of leads to lead-through insulators by embedding in glass or ceramic material
Definitions
- the invention relates to the sealing of a glassy material on a material comprising aluminum.
- hybrid electronic circuits In addition to monolithic integrated circuits, hybrid electronic circuits are used, or more briefly "hybrid circuits". Their name comes from the fact that, on a ceramic substrate, they include monolithic integrated circuit chips, associated with discrete connections and components produced by metallic deposition on the ceramic.
- the hybrid circuits, used by group are combined in a hybrid box.
- a housing generally has a bottom, a cover and a plurality of electrical bushings located on at least one of these walls. In certain cases, it must be airtight both at the connection between the base and the cover and at the electrical bushings.
- Each electrical bushing includes a conductive pin, generally made of KOVAR, hermetically fixed in a passage of the wall by a glass-metal seal well known to those skilled in the art.
- the connection between the cover and the bottom is provided by a conventional electrical weld.
- a “macrohybrid” box is a large hybrid box and its production in KOVAR, according to the aforementioned technique, has two major drawbacks, in particular when such boxes are used inside computers on board an aircraft.
- the first of these drawbacks is linked to the density of the KOVAR which gives the macrohybrid housing a high mass which can become detrimental for the aforementioned use, the weight factor being particularly important in aeronautics.
- the second drawback is linked to the poor thermal conductivity of KOVAR. Due to its size, a macrohybrid box generally contains a very large number of hybrid circuits (or a very large hybrid circuit) which, in operation, release the heat energy usually evacuated by the body of the box. However, this poor thermal conductivity of KOVAR harms good heat dissipation and can therefore cause degraded operations, or even breakdowns.
- the main object of the present invention is therefore to provide a solution to this problem.
- An object of the invention is to allow direct sealing of a vitreous material on a material comprising aluminum.
- the invention relates to a composite part of the type comprising a wall and an insert mounted in a housing of said wall.
- the wall is composed of an aluminum-based material and the insert comprises, at least on the periphery, a vitreous material directly sealed on at least a portion of the internal surface of the housing. Wall.
- This part can for example be a macrohybrid box element or else a complete macrohybrid box, comprising a bottom hermetically closed by at least one cover.
- the insert may also include a metallic element directly sealed within the vitreous material.
- This metallic element may for example be a conductive pin passing right through the glassy material so as to form an electrical crossing through the wall.
- the insert In order to ensure good sealing performance, it is advantageous for the insert to comprise a first effective quantity of a first metal oxide located in the vicinity of the wall of the housing. Adjusting the thickness of this oxide layer also influences the hermeticity of the seal.
- the insert when it comprises a metallic element within it, it is advantageous that it also comprises a second effective quantity of a second metallic oxide located in the vicinity of this metallic element. This ensures better adhesion of this metallic element in the vitreous material and the adjustment of this quantity of oxide also influences the hermeticity of the seal.
- the invention also relates to a method of implanting at least one insert in at least one housing of a wall made of a material comprising aluminum.
- the dilatometric softening temperature of a vitreous material is a temperature for which this material has a viscosity of 1011 ⁇ 3 Poises.
- the notion of compatibility between the vitreous material and the material of the wall relates here, in particular, to the relationship between the dilatometric softening temperature of this vitreous material and the melting temperature of the material of the wall. It also relates, in particular, to the comparison of the respective expansion coefficients of these two materials.
- step b) comprises a sub-step b1), of forming the vitreous element of the insert from said powder, in the presence of a binder mixed with it; this sub-step b1) is followed by a sub-step of sintering this glassy element formed.
- the housing can be a passage passing through the wall and the insert can then comprise a metallic element such as a pin passing right through the insert, which makes it possible to obtain an electrical crossing.
- This wall can be an element of a macrohybrid housing.
- the method further comprises a step of laser welding of the cover of the housing on the bottom of the latter.
- the invention also relates to the composition of glass as that means capable of allowing the implementation of the implantation method according to the invention, this composition also being that of the glassy element of an insert of a composite part according to the invention.
- phosphate glass is used, that is to say phosphate-based, as opposed to certain other types of glass, in particular lead-based or silica-based (used in conventional glass sealing -KOVAR).
- a phosphate glass is not a "glass” in the strict sense, but in fact a partially crystalline ceramic glass. It will nevertheless be called here "glass-phosphate” in accordance with a dominant usage.
- a phosphate glass having the following composition: - between approximately 20% and approximately 50% in moles of sodium oxide (Na2O), - between approximately 5% and approximately 30% in moles of barium oxide (BaO), - between approximately 0.5% and approximately 3% by mole of alumina (Al2O3) - between approximately 40% and approximately 60% by moles of phosphoric anhydride (P2O5).
- the Applicant has found that it is preferable to add to the glass phosphate a crystallization modifying agent such as aluminum nitride (AlN) in an effective amount of less than approximately 7%. The reasons for this addition will be explained below.
- a crystallization modifying agent such as aluminum nitride (AlN)
- the glassy material must have a dilatometric softening temperature and an expansion coefficient compatible respectively with the melting temperature and the expansion coefficient of aluminum. It is therefore preferable to take a vitreous material having a dilatometric softening temperature comprised between approximately 300 ° C. and approximately 550 ° C. and a coefficient of expansion comprised between approximately 10 and approximately 25 ppm / ° C. (The notation ° C means degree Celsius and the notation ppm means part per millionth).
- the implantation of an insert in a housing of a wall requires, before sealing, a step a) of preparation of the housing and a step b) of preparation of the insert; these two steps can be carried out independently of each other in an order any.
- the insert comprises at the periphery a sintered vitreous element, obtained from a powder of a vitreous material of the type of those mentioned above.
- This powder can result, for example, from the grinding of a continuous body.
- Step b) of preparing such a vitreous element first consists in shaping it, in a sub-step b1), from the powder mixed with a binder. After removal of the binder, a sintering of the vitreous element is then carried out in a sub-step b2). The purpose of this sintering is to "stick" the glass grains to each other so as to obtain an insert whose consistency and consistency allow easy handling compatible with an industrial process.
- the sintered peripheral element of the insert is an FFR sheath.
- the powder P is obtained from a continuous body CC obtained in a sub-step 1 comprising the succession of operations illustrated in FIG. 2.
- An intimate mixture (operation 10) of various powders of base constituents CB is produced in order to obtain a base powder PB.
- a base powder PB For the production of this basic powder, 42.4 g of sodium carbonate (Na2CO3), 19.74 g of barium carbonate (BaCO3), 1.02 g of alumina (Al2O3), 112.73 g are used. of ammonium dihydrogen phosphate (NH4H2PO4), and 1.76 g of aluminum nitride (AlN).
- the basic powder thus obtained is placed in an alumina crucible (operation 11) then calcined at 300 ° for 12 hours (operation 12) to remove ammonia and water. Then a grinding (operation 13) of the calcined product is carried out, followed by a cooking of the BRO ground material (operation 14) in order to obtain a vitreous substance SV.
- This cooking 14 includes a rise in temperature of about one hour, at a rate of 750 ° C / hour, until reaching the temperature of 750 ° C, then a plateau at this temperature for 2 hours.
- the glassy substance is then subjected to thermal quenching by pouring onto a KOVAR or stainless steel plate at 200 ° C. (operation 15).
- the continuous body CC is then obtained containing approximately 38.35% in moles of Na2O, 9.59% in moles of BaO, 0.96% in moles of Al2O3, 46.98% in moles of P2O5, and 4.12% in moles of AlN.
- Such a vitreous material then has a dilatometric softening temperature of approximately 330 ° C, a coefficient of expansion of approximately 20 ppm / ° C, and its melting temperature is approximately 600 ° C.
- the powder P is then obtained from the continuous body CC in a sub-step 2 illustrated in detail in FIG. 3.
- a binder LI optionally comprising a polycarbon compound having a chain length at least equal to 1500 and at most equal to 6000.
- the polycarbon compound is polyethylene glycol 4000, therefore having by definition a chain length equal to 4000. Its quantity is 3% by weight.
- the mixture thus obtained is ground for approximately 5 minutes in a pestle mill (operation 21).
- the BROY ground material thus obtained is then sieved (operation 22) to obtain said powder P. By passing it through a sieve, this powder has a particle size between 75 and 106 micrometers.
- This particle size should generally be greater than about 5 micrometers. Its upper limit is chosen according to the desired size of the glassy element of the insert.
- the sub-step b1) of forming the sheath bears the reference 3, and is illustrated in detail in FIG. 4.
- Operation 30 consists in introducing into a pressing mold, having a shape combined with that of the sheath to be obtained, a quantity of powder chosen taking into account the geometry of the sheath.
- This mold comprises in particular a rod making it possible to produce a central channel in the sheath.
- an intermediate sheath FI is obtained. It should be noted here that it is important to use an organic binder having a chain length greater than 1500 to ensure good consistency of the intermediate sheath.
- This organic binder is then removed from the intermediate sheath by an oven 31, which in this embodiment is carried out at 200 ° C for 12 hours.
- the binder is thus evacuated from the inside of the intermediate sheath towards the outside.
- a scabbard formed FF is then obtained.
- step 2 for obtaining the powder P does not include any addition of binder, and that the latter only intervenes in step 3 of obtaining the sheath formed FF, prior to the pressing operation 30.
- the sintering sub-step b2) (reference 4) is generally carried out at a temperature located in the immediate vicinity of the dilatometric softening temperature of the glassy material, that is to say at a temperature where one begins to have softening of this material without deformation.
- the sintering of the sheath formed FF (reference 4) is carried out in a PYREX cup (registered trademark) according to a temperature gradient of 20 ° C / min until reaching the temperature of 335 ° C.
- Such a sintered sheath FF is shown in Figure 5. It consists of a cylinder with a length of about 1.9 mm, traversed longitudinally right through by a central channel CFF. The external diameter of this cylinder is approximately 1.3 mm while the diameter of the channel is approximately 0.6 mm.
- the housing intended to receive the insert may have various configurations depending on the applications envisaged.
- the housing is a passage through the wall. Step a) of preparation of this passage bears the reference 8 and is illustrated in FIG. 6. The passage obtained is illustrated in figure 7.
- machining 80 of the passage is carried out. This is then made up, from the internal face FAI of the wall to its external face FAE, of two bores AL1, AL2.
- the lengths of the bores AL1 and AL2 are respectively of the order of 0.50 mm and 2.50 mm. Their respective diameters are of the order of 1.2 mm and 1.35 mm.
- the material of the PAR wall is an aluminum alloy called "5086" according to the French standard. Its melting temperature is between 580 ° C and 640 ° C and its coefficient of expansion is 23.5 ppm / ° C. Its composition is as follows: - about 4% by weight of magnesium - about 0.5% by weight of manganese - about 95.5% by weight of aluminum.
- the wall is immersed in a bath of chromic acid in order to undergo an anodic chromic oxidation therein 81. It then deposits on the edges. of the passage NOT an alumina layer whose thickness is adjusted between approximately 1 micron and approximately 1.5 microns.
- the adjustment of the thickness of the layer of this first metal oxide OX1 is an important element for the characteristics of the sealing and we will return later to the usefulness of the deposition of such a layer.
- This PAS passage is intended to receive a conductive pin trice B, illustrated in FIG. 9, and the preparation step 9 of which is illustrated in FIG. 8.
- a spindle B is machined in the form of an elongated cylinder with a length of approximately 9.75 mm, one end of which is extended by a rounded truncated cone having an apex angle of approximately 30 °.
- Such a pin has a coefficient of expansion of 17.4 ppm / ° C and an electrical conductivity of 2.5.10 ⁇ 6 ohms.centimeter.
- metallic materials having a coefficient of expansion between about 15 and about 20 ppm per ° C and an electrical conductivity between about 2.10 ⁇ 6 and about 10.10 ⁇ 6 ohms.centimeter.
- This pin B will then undergo nickel plating 91 consisting of the deposition of a layer of nickel with a thickness of approximately 5 microns. This nickel plating is followed by air oxidation for 15 minutes in an oven at 490 ° C. Pin B is then found at the end of this oxidation step covered with nickel oxide OX2.
- nickel oxide OX2 The presence of this second metal oxide OX2 is also an important element for the good behavior of the spindle within the insert and its usefulness will be explained later.
- the assembly thus formed is brought into an oven in order to proceed to sealing 7 (FIG. 11) of the electrical bushing.
- the sealing step according to the invention is carried out under a neutral atmosphere, in particular of nitrogen, by raising the baking temperature above the dilatometric softening temperature of the vitreous material constituting the sintered sheath according to a chosen temperature profile.
- a temperature rise is first carried out with a gradian of 12 ° C. per minute (operation 700) and then a plateau at a cooking temperature equal to 450 ° C. for 50 minutes (operation 701). , then a temperature drop from this level with a gradian of 12 ° C per minute (operation 702).
- This cooking therefore takes place in the presence of the first oxide metal between the sintered sheath and the wall and in the presence of the second metal oxide between the sheath and the conductive pin.
- the presence of alumina between the sheath and the wall makes it possible to maintain the seal thus obtained by the interpenetration of the oxygen atoms of the alumina with the oxygen atoms belonging to the various oxides of the vitreous material.
- the adjustment of the thickness of the alumina layer which therefore induces a first effective amount of this first metal oxide, plays an important role, not only in the strength of the seal, but also in its hermeticity.
- a thickness of between approximately 1 and approximately 1.5 micrometers makes it possible in particular to obtain a vitreous material called "hermetically sealed".
- the hermeticity is then less than or equal to 10 ⁇ 9 cm3.s ⁇ 1 of Helium for a pressure difference of 1 atmosphere on either side of a seal having a unit area of 1 cm2.
- an effective amount of the first metal oxide is an amount which makes it possible to obtain a seal having a strength and hermeticity compatible with the intended application.
- an oxide thickness of less than approximately 0.5 microns does not make it possible to obtain mechanical strength of the glass on the aluminum.
- the maximum oxide thickness depends on the desired strength and hermeticity, it is preferable not to exceed 10 microns.
- the presence of nickel oxide in an effective amount, between the spindle and the glassy material contributes to ensuring good adhesion of these two bodies by interpenetration of the oxygen atoms of the nickel oxide with those of the various glass oxides.
- the 5 micron nickel layer deposited on the spindle leads, after oxidation, to a thickness of nickel oxide (about 3 microns) helping to ensure a hermetic seal.
- a thickness of nickel oxide of between approximately 2 and approximately 5 microns makes it possible to obtain the hermeticity indicated above.
- the sintered sheath conforms to the geometry of the passage, which makes it possible to obtain a direct simultaneous sealing, that is to say requiring no external material, from the spindle to the sheath and the scabbard on the wall.
- This hermetic and electrically insulating seal provides the required electrical crossing ( Figure 12).
- gilding 9 ′ For some applications, it may be necessary to perform on the pins, an additional treatment of gilding 9 ′, illustrated in FIG. 13.
- This gilding will make it possible to obtain a BD pin partially gilded, that is to say gilded only on its internal and external parts located outside the vitreous sealing material.
- the assembly In order to carry out such treatment, the assembly should be immersed in an electrolytic gilding bath (operation 90 ′).
- the Applicant has observed that the use of phosphate glass does not require protecting the seal before it is immersed in the gilding bath.
- vitreous material did not contain a crystallization modifying agent, it would be advisable to protect the seal, for example with a film of epoxy resin, before immersing the assembly in the gilding bath, because otherwise, the acid character of this bath would lead to a more or less significant degradation of the vitreous material of the seal.
- the sealing step 7 would comprise, after the cooking operation 70, annealing the sealing in order to ensure growth of the crystals. The gilding of the pins is then carried out after annealing.
- Figures 14A to 14C are arranged according to the conventional conventions of French industrial design, Figure 14B being more particularly section AA of Figure 14A, while Figure 14C partially includes section BB of Figure 14A.
- the BO case is substantially rectangular with a length of approximately 70 mm and a width of approximately 50 mm.
- This box comprises a bottom FD having two lateral edges BL1 and BL2 as well as a central part PCFD extending in the longitudinal direction of the housing between two lateral edges.
- An intermediate edge BIN is formed in a region of the central part PCFD. This edge BIN extends substantially perpendicularly to the lateral edge BL1 and is then folded back to square substantially parallel to the lateral edge BL2.
- the box BO is closed on the one hand by a first cover COUV1 extending between the intermediate edge BIN and the edges BL1 and BL2 forming an L. It is closed on the other hand by a second cover COUV2 disposed on the other side of the central part PCF2 between the lateral edges BL1 and BL2.
- a first cover COUV1 extending between the intermediate edge BIN and the edges BL1 and BL2 forming an L.
- a second cover COUV2 disposed on the other side of the central part PCF2 between the lateral edges BL1 and BL2.
- the material making up the bottom of the case comprises an aluminum alloy called "5086".
- the material constituting the two lids of the housing is an aluminum alloy known as "4047" according to French standard. It is made up of around 12% silicon and around 88% aluminum.
- the glassy material sealing each spindle to the wall consists of phosphate glass, the various components and their quantity ranges as well as the forks the dilatometric softening temperature and the expansion coefficient have been defined above.
- the glassy material comprises approximately 38.35% in moles of Na2O, 9.59% in moles of BaO, 0.96% in moles of Al2O3, 46.98% in moles of P2O5, and 4, 12 mole% AlN.
- It can also contain, as crystallization modifying agent, platinum in an effective amount and less than 0.5 mol%.
- the first metal oxide (alumina) located in the vicinity of the wall in an effective amount of between about 0.5% by weight and about 0.8% by weight.
- the sealed vitreous material comprises in the vicinity of the spindle (copper-beryllium alloy) the second metal oxide (nickel oxide) in an effective amount of between approximately 0.6% by weight and approximately 1.5% by weight.
- vitreous material directly sealed on aluminum will comprise an amount of alumina at least equal to 0.2% by weight.
- the maximum amount will preferably be of the order of 10% by weight.
- the parts of the spindle located outside the sealed vitreous material are golden.
- the different covers and the bottom are assembled using laser welding, thus ensuring airtightness required.
- the respective alloys of the bottom and the covers were chosen to allow such welding.
- two aluminum-based materials can be laser welded if each of them is free of copper and if at least one of the two contains silicon.
- a working temperature zone in which the glass has a viscosity allowing it to be deformed while retaining a certain consistency.
- the lower temperature of this working zone is the dilatometric softening temperature and the upper temperature is that for which the vitreous material has a viscosity of 104 poises.
- the phosphate glass comprises an agent modifying its working area which tends to increase the latter. Indeed, the larger this working area, the less critical are the details on the different temperatures used in the steps of the method according to the invention. This contributes in particular to further improving the reproducibility and consequently to an even easier industrialization of the process.
- This modifying agent for the working area is, for example, boron trioxide (B2O3) in an amount less than about 15 mol%.
- composition of such a glassy material is the next one : - 35% in moles of Na2O - 8.75% in moles of BaO - 0.87 mole% of Al2O3 - 42.88% in moles of P2O5 - 3.75% in moles of AlN - 8.75% in moles of B2O3.
- Such a vitreous material then has a dilatometric softening temperature of approximately 475 ° C. and a coefficient of expansion of approximately 16 ppm / ° C. Its working area is between around 475 ° C and 550 ° C and its melting temperature is around 700 ° C.
- the cooking of the BRO ground material (operation 14) making it possible to obtain the vitreous substance SV involves a rise in temperature of about one hour at a rate of 1100 ° C./hours then a level at 1100 ° C for 2 hours and finally a drop in temperature for about 30 minutes until reaching the temperature of about 850 ° C.
- the sintering step of the vitreous material (reference 4) is carried out in a PYREX dish according to a temperature gradient of 20 ° C / min until reaching the temperature of 470 ° C.
- the sealing step first includes a temperature rise with a gradient of 12 ° C per minute (operation 700) then a plateau at a cooking temperature equal to 525 ° C for 15 min (operation 701) then a descent in temperature from this level with a gradient of 12 ° C per minute (operation 702).
- the invention is not limited to the embodiments and embodiments described above, but embraces all variants, in particular the following: - It is conceivable that the spindle is replaced, in other applications, by another metallic element, at least; - the presence of the first and second metal oxides is only necessary at the level of the seal. Also, it is possible to envisage carrying out partial oxidations of the metallic element and of the housing only in the useful zones; - one could also conceive, in certain applications requiring only a direct sealing "spindle- glass "without good mechanical strength and airtightness being important factors, to perform this sealing without the presence of metal oxide between the spindle and the glassy material.
- step 3 it is possible, in step 3, to replace the rod of the pressing tool, used to shape the central channel of the sleeve, by the spindle itself.
- a composite insert is obtained at the periphery of the sleeve, and at the center of the spindle, which after removal of the binder and sintering becomes an element ready to be introduced into the passage of the wall.
- This variant makes it possible to limit the various centering and positioning tools used previously.
- the second metal oxide will have been deposited on the spindle before the formation of the single element.
- sheath of such an insert obtained after pressing, or, after removal of the binder, sintered at a temperature higher than the sintering temperature previously indicated so as to further increase its consistency.
Abstract
Description
L'invention concerne le scellement d'un matériau vitreux sur un matériau comportant de l'aluminium.The invention relates to the sealing of a glassy material on a material comprising aluminum.
Une application particulièrement intéressante de tels scellements réside dans la réalisation de boîtiers fonctionnels électriques contenant au moins un circuit électronique hybride, communément appelés "boîtiers hybrides". Cependant, l'invention n'est pas limitée à cette application particulière.A particularly interesting application of such seals resides in the production of electrical functional boxes containing at least one hybrid electronic circuit, commonly called "hybrid boxes". However, the invention is not limited to this particular application.
A côté des circuits intégrés monolithiques, on utilise des circuits électroniques hybrides, ou plus brièvement "circuits hybrides". Leur nom provient de ce que, sur un substrat de céramique, ils comportent des puces de circuits intégrés monolithiques, associées à des liaisons et composants discrets réalisés par dépôt métallique sur la céramique.In addition to monolithic integrated circuits, hybrid electronic circuits are used, or more briefly "hybrid circuits". Their name comes from the fact that, on a ceramic substrate, they include monolithic integrated circuit chips, associated with discrete connections and components produced by metallic deposition on the ceramic.
Pour certaines applications, les circuits hybrides, utilisés par groupe, sont réunis dans un boitier hybride. Un tel boîtier possède généralement un fond, un couvercle et une pluralité de traversées électriques situées sur au moins l'un de ces parois. Il doit être dans certains cas hermétique tant au niveau de la liaison entre le fond et le couvercle qu'au niveau des traversées électriques.For certain applications, the hybrid circuits, used by group, are combined in a hybrid box. Such a housing generally has a bottom, a cover and a plurality of electrical bushings located on at least one of these walls. In certain cases, it must be airtight both at the connection between the base and the cover and at the electrical bushings.
On connaît actuellement de tels boîtiers constitués en un matériau à base d'un alliage fer-nickel-cobalt connu notamment sous la marque KOVAR déposée par la société américaine WESTHINGHOUSE CORPORATION. Chaque traversée électrique comprend une broche conductrice, généralement en KOVAR, hermétiquement fixée dans un passage de la paroi par un scellement verre-métal bien connu de l'homme de l'art. La liaison entre le couvercle et le fond est assurée par une soudure électrique classique.Currently known such cases made of a material based on an iron-nickel-cobalt alloy known in particular under the brand KOVAR registered by the American company WESTHINGHOUSE CORPORATION. Each electrical bushing includes a conductive pin, generally made of KOVAR, hermetically fixed in a passage of the wall by a glass-metal seal well known to those skilled in the art. The connection between the cover and the bottom is provided by a conventional electrical weld.
Un boitier "macrohybride" est un boîtier hybride de grande taille et sa réalisation en KOVAR, selon la technique précitée, présente deux inconvénients majeurs, notamment lorsque de tels boîtiers sont utilisés à l'intérieur de calculateurs embarqués dans un aéronef.A "macrohybrid" box is a large hybrid box and its production in KOVAR, according to the aforementioned technique, has two major drawbacks, in particular when such boxes are used inside computers on board an aircraft.
Le premier de ces inconvénients est lié à la densité du KOVAR qui confère au boîtier macrohybride une masse élevée qui peut devenir pénalisante pour l'utilisation précitée, le facteur poids étant particulièrement important dans l'aéronautique.The first of these drawbacks is linked to the density of the KOVAR which gives the macrohybrid housing a high mass which can become detrimental for the aforementioned use, the weight factor being particularly important in aeronautics.
Le deuxième inconvénient est lié à la mauvaise conductibilité thermique du KOVAR. De par sa taille, un boîtier macrohybride contient généralement un très grand nombre de circuits hybrides (ou un circuit hybride de très grande taille) qui, en fonctionnement, libèrent de l'énergie calorifique habituellement évacuée par le corps du boîtier. Or, cette mauvaise conductibilité thermique du KOVAR nuit à une bonne dissipation thermique et peut donc engendrer des fonctionnements dégradés, voire des pannes.The second drawback is linked to the poor thermal conductivity of KOVAR. Due to its size, a macrohybrid box generally contains a very large number of hybrid circuits (or a very large hybrid circuit) which, in operation, release the heat energy usually evacuated by the body of the box. However, this poor thermal conductivity of KOVAR harms good heat dissipation and can therefore cause degraded operations, or even breakdowns.
Il s'avère que l'utilisation d'un matériau comportant de l'aluminium permet de pallier les deux inconvénients précités.It turns out that the use of a material comprising aluminum overcomes the two aforementioned drawbacks.
Cependant, cette utilisation soulève d'importants problèmes techniques quant à la réalisation d'un scellement verre-aluminium en raison, notamment, des propriétés physiques antagonistes (en particulier point de fusion et coefficient de dilatation) de ces deux matériaux. L'homme de l'art sait en effet que le point de fusion d'un verre classique est en général supérieur à 1000°C, alors que le point de fusion de l'aluminium est d'environ 550°C. Par ailleurs, le coefficient de dilatation de l'aluminium est généralement plus élevé que celui des verres classiques. L'importance de ces problèmes augmente encore pour l'obtention d'un scellement hermétique tel que celui habituellement requis pour les boitiers macrohybrides.However, this use raises important technical problems with regard to the production of a glass-aluminum seal due, in particular, to the antagonistic physical properties (in particular melting point and coefficient of expansion) of these two materials. Those skilled in the art know in fact that the melting point of a conventional glass is generally greater than 1000 ° C., while the melting point of aluminum is approximately 550 ° C. In addition, the coefficient of expansion of aluminum is generally higher than that of conventional glasses. The importance of these problems increases further for obtaining a hermetic seal such as that usually required for macrohybrid housings.
La présente invention a donc pour but principal d'apporter une solution à ce problème.The main object of the present invention is therefore to provide a solution to this problem.
Un but de l'invention est de permettre un scellement direct d'un matériau vitreux sur un matériau comportant de l'aluminium.An object of the invention is to allow direct sealing of a vitreous material on a material comprising aluminum.
L'invention vise une pièce composite du type comprenant une paroi et un insert monté dans un logement de ladite paroi.The invention relates to a composite part of the type comprising a wall and an insert mounted in a housing of said wall.
Selon une caractéristique générale de l'invention, la paroi est composée d'un matériau à base d'aluminium et l'insert comprend, au moins en périphérie, un matériau vitreux directement scellé sur une portion au moins de la surface interne du logement de la paroi.According to a general characteristic of the invention, the wall is composed of an aluminum-based material and the insert comprises, at least on the periphery, a vitreous material directly sealed on at least a portion of the internal surface of the housing. Wall.
Cette pièce peut être par exemple un élément de boîtier macrohybride ou bien un boitier macrohybride complet, comportant un fond hermétiquement fermé par au moins un couvercle.This part can for example be a macrohybrid box element or else a complete macrohybrid box, comprising a bottom hermetically closed by at least one cover.
L'insert peut comprendre également un élément métallique directement scellé au sein du matériau vitreux. Cet élément métallique peut être par exemple une broche conductrice traversant de part en part le matériau vitreux de façon à former une traversée électrique à travers la paroi.The insert may also include a metallic element directly sealed within the vitreous material. This metallic element may for example be a conductive pin passing right through the glassy material so as to form an electrical crossing through the wall.
Afin d'assurer la bonne tenue du scellement, il est avantageux que l'insert comprenne une première quantité efficace d'un premier oxyde métallique située au voisinage de la paroi du logement. L'ajustement de l'épaisseur de cette couche d'oxyde influe également sur l'herméticité du scellement.In order to ensure good sealing performance, it is advantageous for the insert to comprise a first effective quantity of a first metal oxide located in the vicinity of the wall of the housing. Adjusting the thickness of this oxide layer also influences the hermeticity of the seal.
De même, lorsque l'insert comprend un élément métallique en son sein, il est avantageux qu'il comprenne également une deuxième quantité efficace d'un deuxième oxyde métallique située au voisinage de cet élément métallique. On assure ainsi une meilleure adhérence de cet élément métallique dans le matériau vitreux et l'ajustement de cette quantité d'oxyde influe également sur l'herméticité du scellement.Likewise, when the insert comprises a metallic element within it, it is advantageous that it also comprises a second effective quantity of a second metallic oxide located in the vicinity of this metallic element. This ensures better adhesion of this metallic element in the vitreous material and the adjustment of this quantity of oxide also influences the hermeticity of the seal.
L'invention vise également un procédé d'implantation d'au moins un insert dans au moins un logement d'une paroi en un matériau comportant de l'aluminium.The invention also relates to a method of implanting at least one insert in at least one housing of a wall made of a material comprising aluminum.
Selon une caractéristique générale de l'invention, ce procédé comporte les étapes suivantes :
- a) préparer le logement dans la paroi ;
- b) préparer l'insert, lequel comporte au moins en périphérie un élément fritté, insérable dans ledit logement ; cet élément fritté est obtenu à partir d'une poudre d'un matériau vitreux compatible avec le matériau de la paroi ;
- c) introduire l'insert dans le logement ;
- d) élever l'insert à une température de cuisson supérieure à la température de ramollissement dilatométrique de ladite poudre en présence d'une première quantité efficace d'un premier oxyde métallique entre l'élément vitreux et la paroi.
- a) prepare the housing in the wall;
- b) preparing the insert, which comprises at least on the periphery a sintered element, insertable in said housing; this sintered element is obtained from a powder of a vitreous material compatible with the material of the wall;
- c) insert the insert into the housing;
- d) raise the insert to a higher cooking temperature at the dilatometric softening temperature of said powder in the presence of a first effective amount of a first metal oxide between the vitreous element and the wall.
On obtient ainsi un scellement direct de l'insert à la paroi.There is thus obtained a direct sealing of the insert to the wall.
On rappelle ici que la température de ramollissement dilatométrique d'un matériau vitreux est une température pour laquelle ce matériau présente une viscosité de 10¹¹ʼ³ Poises. Ainsi, la notion de compatibilité entre le matériau vitreux et le matériau de la paroi, concerne ici, notamment, la relation entre la température de ramollissement dilatométrique de ce matériau vitreux et la température de fusion du matériau de la paroi. Elle concerne également, notamment, la comparaison des coefficients de dilatation respectifs de ces deux matériaux.It is recalled here that the dilatometric softening temperature of a vitreous material is a temperature for which this material has a viscosity of 10¹¹ʼ³ Poises. Thus, the notion of compatibility between the vitreous material and the material of the wall, relates here, in particular, to the relationship between the dilatometric softening temperature of this vitreous material and the melting temperature of the material of the wall. It also relates, in particular, to the comparison of the respective expansion coefficients of these two materials.
Dans un mode de réalisation, l'étape b) comprend une sous-étape b1), de formation de l'élément vitreux de l'insert à partir de ladite poudre, en présence d'un liant mélangé à celle-ci ; cette sous-étape b1) est suivie par une sous-étape de frittage de cet élément vitreux formé.In one embodiment, step b) comprises a sub-step b1), of forming the vitreous element of the insert from said powder, in the presence of a binder mixed with it; this sub-step b1) is followed by a sub-step of sintering this glassy element formed.
Dans une application particulière, le logement peut être un passage traversant la paroi et l'insert peut comprendre alors un élément métallique tel qu'une broche traversant de part en part l'insert, ce qui permet d'obtenir une traversée électrique. Cette paroi peut être un élément d'un boîtier macrohybride. Dans ce cas, il est avantageux que le procédé comprenne en outre une étape de soudure au laser du couvercle du boîtier sur le fond de celui-ci.In a particular application, the housing can be a passage passing through the wall and the insert can then comprise a metallic element such as a pin passing right through the insert, which makes it possible to obtain an electrical crossing. This wall can be an element of a macrohybrid housing. In this case, it is advantageous that the method further comprises a step of laser welding of the cover of the housing on the bottom of the latter.
L'invention vise encore, la composition de verre en tant que moyen susceptible de permettre la mise en oeuvre du procédé d'implantation selon l'invention, cette composition étant également celle de l'élément vitreux d'un insert d'une pièce composite selon l'invention.The invention also relates to the composition of glass as that means capable of allowing the implementation of the implantation method according to the invention, this composition also being that of the glassy element of an insert of a composite part according to the invention.
D'autres avantages et caractéristiques de l'invention apparaîtront à l'examen de la description détaillée ci-après et les dessins annexés sur lesquels :
- - la figure 1 est un organigramme général d'un mode de mise en oeuvre du procédé selon l'invention permettant l'élaboration d'une traversée électrique ;
- - les figures 2 à 4 illustrent, de façon plus détaillée, différentes étapes de l'organigramme de la figure 1 ;
- - la figure 5 illustre de façon schématique un fourreau fritté obtenu par le procédé selon l'invention ;
- - la figure 6 illustre une étape de réalisation d'un passage ;
- - la figure 7 illustre un passage ainsi obtenu ;
- - la figure 8 illustre une étape de réalisation d'une broche ;
- - la figure 9 illustre une broche ainsi obtenue ;
- - la figure 10 illustre schématiquement une traversée électrique avant scellement ;
- - la figure 11 représente un organigramme d'une étape de scellement ;
- - la figure 12 représente de façon schématique une traversée électrique, après scellement ;
- - la figure 13 illustre une étape de traitement supplémentaire d'une broche ;
- - les figures 14A à 14C représentent un mode de réalisation d'un boîtier macrohybride.
- - Figure 1 is a general flowchart of an embodiment of the method according to the invention allowing the development of an electrical crossing;
- - Figures 2 to 4 illustrate, in more detail, different stages of the flow diagram of Figure 1;
- - Figure 5 schematically illustrates a sintered sheath obtained by the method according to the invention;
- - Figure 6 illustrates a step of making a passage;
- - Figure 7 illustrates a passage thus obtained;
- - Figure 8 illustrates a step of making a pin;
- - Figure 9 illustrates a pin thus obtained;
- - Figure 10 schematically illustrates an electrical crossing before sealing;
- - Figure 11 shows a flow diagram of a sealing step;
- - Figure 12 shows schematically an electrical crossing, after sealing;
- - Figure 13 illustrates an additional processing step of a spindle;
- - Figures 14A to 14C show an embodiment of a macrohybrid package.
Les dessins comportent, pour l'essentiel, des éléments de caractère certain, et font partie intégrante de la description. A ce titre, ils pourront non seulement servir à mieux faire comprendre la description détaillée ci-après, mais aussi contribuer, le cas échéant, à la définition de l'invention.The drawings essentially contain elements of a certain nature, and form an integral part of the description. As such, they can not only serve to better understand the detailed description below, but also contribute, if necessary, to the definition of the invention.
La réalisation d'un objet composite, comportant un matériau vitreux directement scellé sur une paroi à base d'aluminium, nécessite, entre autres conditions, un choix convenable de ce matériau vitreux. Pour un tel scellement, on utilise de préférence du verre phosphate c'est-à-dire à base de phosphate, par opposition à certains autres types de verre, notamment à base de plomb ou à base de silice (utilisé dans le scellement classique verre-KOVAR). Par ailleurs un verre-phosphate n'est pas un "verre" au sens strict mais en fait un verre-céramique partiellement cristallin. On l'appellera néanmoins ici "verre-phosphate" conformément à un usage dominant.The production of a composite object, comprising a vitreous material directly sealed on an aluminum-based wall, requires, among other conditions, a suitable choice of this vitreous material. For such sealing, phosphate glass is used, that is to say phosphate-based, as opposed to certain other types of glass, in particular lead-based or silica-based (used in conventional glass sealing -KOVAR). Furthermore, a phosphate glass is not a "glass" in the strict sense, but in fact a partially crystalline ceramic glass. It will nevertheless be called here "glass-phosphate" in accordance with a dominant usage.
Des familles de verre-phosphate sont décrites dans les brevets américains no 4 202 700 et no 4 455 384. Parmi celles-ci, toutes ne conviennent pas pour un scellement sur un alliage d'aluminium qui soit industriellement réalisable avec une bonne reproductibilité. Après de nombreux essais, la Demanderesse a constaté que l'on pouvait utiliser, notamment à cette fin, un verre-phosphate ayant la composition suivante :
- entre environ 20% et environ 50% en moles d'oxyde de sodium (Na₂O),
- entre environ 5% et environ 30% en moles d'oxyde de baryum (BaO),
- entre environ 0,5% et environ 3% en moles d'alumine (Al₂O₃)
- entre environ 40% et environ 60% en moles d'anhydride phosphorique (P₂O₅).Glass-phosphate family are described in US Patents No. 4,202,700 and No. 4 455 384. Of these, all are not suitable for sealing of an aluminum alloy that is industrially feasible with good reproducibility . After numerous tests, the Applicant has found that it is possible use, in particular for this purpose, a phosphate glass having the following composition:
- between approximately 20% and approximately 50% in moles of sodium oxide (Na₂O),
- between approximately 5% and approximately 30% in moles of barium oxide (BaO),
- between approximately 0.5% and approximately 3% by mole of alumina (Al₂O₃)
- between approximately 40% and approximately 60% by moles of phosphoric anhydride (P₂O₅).
La Demanderesse a constaté qu'il était préférable d'adjoindre au verre-phosphate un agent modificateur de cristallisation tel que du nitrure d'aluminium (AlN) en une quantité efficace inférieure à 7% environ. Les raisons de cette adjonction seront explicitées ci-après.The Applicant has found that it is preferable to add to the glass phosphate a crystallization modifying agent such as aluminum nitride (AlN) in an effective amount of less than approximately 7%. The reasons for this addition will be explained below.
Outre ces caractéristiques de composition, le matériau vitreux doit présenter une température de ramollissement dilatométrique et un coefficient de dilatation compatibles respectivement avec la température de fusion et le coefficient de dilatation de l'aluminium. On prendra donc de préférence un matériau vitreux ayant une température de ramollissement dilatométrique comprise entre environ 300°C et environ 550°C et un coefficient de dilatation compris entre environ 10 et environ 25 ppm/°C. (La notation °C signifie degré Celsius et la notation ppm signifie partie par millionième).In addition to these composition characteristics, the glassy material must have a dilatometric softening temperature and an expansion coefficient compatible respectively with the melting temperature and the expansion coefficient of aluminum. It is therefore preferable to take a vitreous material having a dilatometric softening temperature comprised between approximately 300 ° C. and approximately 550 ° C. and a coefficient of expansion comprised between approximately 10 and approximately 25 ppm / ° C. (The notation ° C means degree Celsius and the notation ppm means part per millionth).
D'une façon générale, l'implantation d'un insert dans un logement d'une paroi nécessite, avant le scellement, une étape a) de préparation du logement et une étape b) de préparation de l'insert ; ces deux étapes peuvent être effectuées indépendamment l'une de l'autre dans un ordre quelconque.In general, the implantation of an insert in a housing of a wall requires, before sealing, a step a) of preparation of the housing and a step b) of preparation of the insert; these two steps can be carried out independently of each other in an order any.
L'insert comporte en périphérie un élément vitreux fritté, obtenu à partir d'une poudre d'un matériau vitreux du type de ceux évoqués ci-avant. Cette poudre peut résulter par exemple du broyage d'un corps continu.The insert comprises at the periphery a sintered vitreous element, obtained from a powder of a vitreous material of the type of those mentioned above. This powder can result, for example, from the grinding of a continuous body.
L'étape b) de préparation d'un tel élément vitreux consiste d'abord à le mettre en forme, dans une sous-étape b1), à partir de la poudre mélangée à un liant. On effectue ensuite, après élimination du liant, un frittage de l'élément vitreux dans une sous-étape b2). Ce frittage a pour but de "coller" les grains de verre les uns aux autres de façon à obtenir un insert dont la consistance et la cohérence autorisent une manipulation aisée compatible avec un procédé industriel.Step b) of preparing such a vitreous element first consists in shaping it, in a sub-step b1), from the powder mixed with a binder. After removal of the binder, a sintering of the vitreous element is then carried out in a sub-step b2). The purpose of this sintering is to "stick" the glass grains to each other so as to obtain an insert whose consistency and consistency allow easy handling compatible with an industrial process.
Dans le cas de l'élaboration d'une traversée électrique, telle que définie sur la figure 1, l'élément périphérique fritté de l'insert est un fourreau FFR.In the case of the development of an electrical bushing, as defined in FIG. 1, the sintered peripheral element of the insert is an FFR sheath.
La poudre P est obtenue à partir d'un corps continu CC obtenu dans une sous-étape 1 comprenant la succession des opérations illustrées sur la figure 2.The powder P is obtained from a continuous body CC obtained in a sub-step 1 comprising the succession of operations illustrated in FIG. 2.
On réalise un mélange intime (opération 10) de diverses poudres de constituants de base CB pour obtenir une poudre de base PB. Pour la réalisation de cette poudre de base, on utilise 42,4 g de carbonate de sodium (Na₂CO₃), 19,74 g de carbonate de baryum (BaCO₃), 1,02 g d'alumine (Al₂O₃), 112,73 g de dihydrogénophosphate d'ammonium (NH₄H₂PO₄), et 1,76 g de nitrure d'aluminium (AlN).An intimate mixture (operation 10) of various powders of base constituents CB is produced in order to obtain a base powder PB. For the production of this basic powder, 42.4 g of sodium carbonate (Na₂CO₃), 19.74 g of barium carbonate (BaCO₃), 1.02 g of alumina (Al₂O₃), 112.73 g are used. of ammonium dihydrogen phosphate (NH₄H₂PO₄), and 1.76 g of aluminum nitride (AlN).
La poudre de base ainsi obtenue est mise dans un creuset en alumine (opération 11) puis calcinée à 300° pendant 12 heures (opération 12) afin d'éliminer l'ammoniac et l'eau. On effectue ensuite un broyage (opération 13) du produit calciné puis une cuisson du broyat BRO (opération 14) afin d'obtenir une substance vitreuse SV. Cette cuisson 14 comporte une montée en température d'une heure environ, à raison de 750°C/heure, jusqu'à atteindre la température de 750°C, puis un palier à cette température pendant 2 heures. La substance vitreuse subit ensuite une trempe thermique par coulage sur une plaque en KOVAR ou en acier inoxydable à 200°C (opération 15). On obtient alors le corps continu CC contenant environ 38,35% en moles de Na₂O, 9,59% en moles de BaO, 0,96% en moles de Al₂O₃, 46,98% en moles de P₂O₅, et 4,12% en moles de AlN.The basic powder thus obtained is placed in an alumina crucible (operation 11) then calcined at 300 ° for 12 hours (operation 12) to remove ammonia and water. Then a grinding (operation 13) of the calcined product is carried out, followed by a cooking of the BRO ground material (operation 14) in order to obtain a vitreous substance SV. This cooking 14 includes a rise in temperature of about one hour, at a rate of 750 ° C / hour, until reaching the temperature of 750 ° C, then a plateau at this temperature for 2 hours. The glassy substance is then subjected to thermal quenching by pouring onto a KOVAR or stainless steel plate at 200 ° C. (operation 15). The continuous body CC is then obtained containing approximately 38.35% in moles of Na₂O, 9.59% in moles of BaO, 0.96% in moles of Al₂O₃, 46.98% in moles of P₂O₅, and 4.12% in moles of AlN.
Un tel matériau vitreux a alors une température de ramollissement dilatométrique de 330°C environ, un coefficient de dilatation de 20 ppm/°C environ, et sa température de fusion est d'environ 600°C.Such a vitreous material then has a dilatometric softening temperature of approximately 330 ° C, a coefficient of expansion of approximately 20 ppm / ° C, and its melting temperature is approximately 600 ° C.
La poudre P est ensuite obtenue à partir du corps continu CC dans une sous-étape 2 illustrée en détail sur la figure 3.The powder P is then obtained from the continuous body CC in a sub-step 2 illustrated in detail in FIG. 3.
On ajoute au corps continu CC (opération 20) un liant LI comprenant éventuellement un composé polycarboné ayant une longueur de chaîne au moins égale à 1500 et au plus égale à 6000. Dans l'exemple décrit, le composé polycarboné est du polyéthylène glycol 4000, ayant donc par définition une longueur de chaine égale à 4000. Sa quantité est de 3% en poids. Le mélange ainsi obtenu est broyé pendant environ 5 minutes dans un broyeur à pilon (opération 21). Le broyat BROY ainsi obtenu est ensuite tamisé (opération 22) pour obtenir ladite poudre P. De par son passage dans un tamis, cette poudre a une granulométrie comprise entre 75 et 106 micromètres.Is added to the continuous body CC (operation 20) a binder LI optionally comprising a polycarbon compound having a chain length at least equal to 1500 and at most equal to 6000. In the example described, the polycarbon compound is polyethylene glycol 4000, therefore having by definition a chain length equal to 4000. Its quantity is 3% by weight. The mixture thus obtained is ground for approximately 5 minutes in a pestle mill (operation 21). The BROY ground material thus obtained is then sieved (operation 22) to obtain said powder P. By passing it through a sieve, this powder has a particle size between 75 and 106 micrometers.
Bien que l'opération de tamisage ne soit pas absolument nécessaire, l'obtention d'une poudre d'une granulométrie donnée facilite les étapes ultérieures du procédé. Il convient généralement que cette granulométrie soit supérieure à environ 5 micromètres. Sa limite supérieure est choisie en fonction de la taille désirée de l'élément vitreux de l'insert.Although the sieving operation is not absolutely necessary, obtaining a powder of a given particle size facilitates the later stages of the process. This particle size should generally be greater than about 5 micrometers. Its upper limit is chosen according to the desired size of the glassy element of the insert.
La sous-étape b1) de formation du fourreau, porte la référence 3, et est illustrée en détail sur la figure 4.The sub-step b1) of forming the sheath, bears the
L'opération 30 consiste à introduire dans un moule de pressage, ayant une forme conjuguée de celle du fourreau à obtenir, une quantité de poudre choisie compte tenu de la géométrie du fourreau. Ce moule comporte notamment une tige permettant de réaliser un canal central dans le fourreau.
Après pressage de cette poudre à une pression suffisante compte tenu de la densité désirée pour le fourreau, on obtient un fourreau intermédiaire FI. Il faut remarquer ici qu'il est important d'utiliser un liant organique ayant une longueur de chaine supérieure à 1500 pour assurer une bonne cohérence du fourreau intermédiaire.After pressing this powder at a sufficient pressure taking into account the density desired for the sheath, an intermediate sheath FI is obtained. It should be noted here that it is important to use an organic binder having a chain length greater than 1500 to ensure good consistency of the intermediate sheath.
Ce liant organique est ensuite éliminé du fourreau intermédiaire par un étuvage 31, qui dans ce mode de mise en oeuvre se réalise à 200°C pendant 12 heures. Le liant est ainsi évacué de l'intérieur du fourreau intermédiaire vers l'extérieur. Un fourreau formé FF est alors obtenu.This organic binder is then removed from the intermediate sheath by an
Il convient ici de remarquer qu'un liant polycarboné ayant une longueur de chaîne supérieure à 6000 serait très difficile à éliminer.It should be noted here that a polycarbonate binder having a chain length greater than 6000 would be very difficult to remove.
Dans une variante, on pourrait envisager que l'étape 2 d'obtention de la poudre P ne comprenne pas d'adjonction de liant, et que cette dernière n'intervienne que, dans l'étape 3 d'obtention du fourreau formé FF, antérieurement à l'opération 30 de pressage. Cependant, dans ce cas, il serait recommandé de broyer séparément le liant LI avant son incorporation à la poudre P.In a variant, it could be envisaged that
La sous-étape b2) de frittage (référence 4) s'effectue généralement à une température située au voisinage immédiat de la température de ramollissement dilatométrique du matériau vitreux, c'est-à-dire à une température où l'on commence à avoir un ramollissement de ce matériau sans déformation. Pour la composition de verre ci-dessus décrite, le frittage du fourreau formé FF (référence 4) est effectué dans une coupelle en PYREX (Marque déposée) selon un gradient de température de 20°C/mn jusqu'à atteindre la température de 335°C.The sintering sub-step b2) (reference 4) is generally carried out at a temperature located in the immediate vicinity of the dilatometric softening temperature of the glassy material, that is to say at a temperature where one begins to have softening of this material without deformation. For the glass composition described above, the sintering of the sheath formed FF (reference 4) is carried out in a PYREX cup (registered trademark) according to a temperature gradient of 20 ° C / min until reaching the temperature of 335 ° C.
Un tel fourreau fritté FF est représenté sur la figure 5. Il se compose d'un cylindre d'une longueur d'environ 1,9 mm, traversé longitudinalement de part en part par un canal central CFF. Le diamètre externe de ce cylindre est d'environ 1,3 mm tandis que le diamètre du canal est d'environ 0,6 mm.Such a sintered sheath FF is shown in Figure 5. It consists of a cylinder with a length of about 1.9 mm, traversed longitudinally right through by a central channel CFF. The external diameter of this cylinder is approximately 1.3 mm while the diameter of the channel is approximately 0.6 mm.
Bien entendu, les différentes cotes indiquées ici ainsi que celles indiquées ci-après ne le sont qu'à titre d'exemple non limitatif.Of course, the various dimensions indicated here as well as those indicated below are only by way of nonlimiting example.
Le logement destiné à recevoir l'insert peut présenter des configurations diverses selon les applications envisagées. Dans le cas présent de l'élaboration d'une traversée électrique, le logement est un passage traversant la paroi. L'étape a) de préparation de ce passage porte la référence 8 et est illustrée sur la figure 6. Le passage obtenu est illustré sur la figure 7.The housing intended to receive the insert may have various configurations depending on the applications envisaged. In the present case of the development of an electrical crossing, the housing is a passage through the wall. Step a) of preparation of this passage bears the reference 8 and is illustrated in FIG. 6. The passage obtained is illustrated in figure 7.
Dans la paroi PAR, on effectue un usinage 80 du passage. Celui-ci est alors constitué, depuis la face interne FAI de la paroi jusqu'à sa face externe FAE, de deux alésages AL1, AL2. Dans ce mode de mise en oeuvre, les longueurs des alésages AL1 et AL2 sont respectivement de l'ordre de 0,50 mm et 2,50 mm. Leurs diamètres respectifs sont de l'ordre de 1,2 mm et 1,35 mm.In the wall PAR, machining 80 of the passage is carried out. This is then made up, from the internal face FAI of the wall to its external face FAE, of two bores AL1, AL2. In this embodiment, the lengths of the bores AL1 and AL2 are respectively of the order of 0.50 mm and 2.50 mm. Their respective diameters are of the order of 1.2 mm and 1.35 mm.
Le matériau de la paroi PAR est un alliage d'aluminium dit "5086" selon la norme française. Sa température de fusion est comprise entre 580°C et 640°C et son coefficient de dilatation est de 23,5 ppm/°C. Sa composition est la suivante :
- environ 4% en poids de magnésium
- environ 0,5% en poids de manganèse
- environ 95,5% en poids d'aluminium.The material of the PAR wall is an aluminum alloy called "5086" according to the French standard. Its melting temperature is between 580 ° C and 640 ° C and its coefficient of expansion is 23.5 ppm / ° C. Its composition is as follows:
- about 4% by weight of magnesium
- about 0.5% by weight of manganese
- about 95.5% by weight of aluminum.
Il convient de noter ici que l'aluminium et tous ces alliages conviennent pour effectuer un scellement verre-métal conformément au procédé selon l'invention.It should be noted here that aluminum and all these alloys are suitable for effecting a glass-metal sealing in accordance with the method according to the invention.
Postérieurement à l'usinage du passage, la paroi est plongée dans un bain d'acide chromique pour y subir une oxydation anodique chromique 81. Il se dépose alors sur les bords. du passage PAS une couche d'alumine dont on ajuste l'épaisseur entre environ 1 micron et environ 1,5 micron. L'ajustement de l'épaisseur de la couche de ce premier oxyde métallique OX1 est un élément important pour les caractéristiques du scellement et l'on reviendra plus loin sur l'utilité du dépôt d'une telle couche.After the passage has been machined, the wall is immersed in a bath of chromic acid in order to undergo an anodic chromic oxidation therein 81. It then deposits on the edges. of the passage NOT an alumina layer whose thickness is adjusted between approximately 1 micron and approximately 1.5 microns. The adjustment of the thickness of the layer of this first metal oxide OX1 is an important element for the characteristics of the sealing and we will return later to the usefulness of the deposition of such a layer.
Ce passage PAS est destiné à recevoir une broche conduc trice B, illustrée sur la figure 9, et dont l'étape de préparation 9 est illustrée sur la figure 8.This PAS passage is intended to receive a conductive pin trice B, illustrated in FIG. 9, and the
A partir d'un alliage métallique de cuivre et de béryllium dont la composition est :
- Béryllium (Be) : entre environ 1,8% et environ 2% en poids
- Cobalt (Co) : entre environ 0,2% et environ 0,3% en poids
- Plomb (Pb) : entre environ 0,2% et environ 0,6% en poids
- Nickel (Ni) : environ 0,05% en poids
- Cuivre (Cu) : complément à 100% en poids,
on usine une broche B en forme d'un cylindre allongé d'une longueur de 9,75 mm environ, dont une extrémité se prolonge par un tronc de cône arrondi ayant un angle au sommet d'environ 30°. Une telle broche présente un coefficient de dilatation de 17,4 ppm/°C et une conductibilité électrique de 2,5.10⁻⁶ ohms.centimètre. D'une façon générale, on utilisera des matériaux métalliques présentant un coefficient de dilatation compris entre environ 15 et environ 20 ppm par °C et une conductibilité électrique comprise entre environ 2.10⁻⁶ et environ 10.10⁻⁶ ohms.centimètre.From a metallic alloy of copper and beryllium, the composition of which is:
- Beryllium (Be): between approximately 1.8% and approximately 2% by weight
- Cobalt (Co): between approximately 0.2% and approximately 0.3% by weight
- Lead (Pb): between approximately 0.2% and approximately 0.6% by weight
- Nickel (Ni): about 0.05% by weight
- Copper (Cu): complement to 100% by weight,
a spindle B is machined in the form of an elongated cylinder with a length of approximately 9.75 mm, one end of which is extended by a rounded truncated cone having an apex angle of approximately 30 °. Such a pin has a coefficient of expansion of 17.4 ppm / ° C and an electrical conductivity of 2.5.10⁻⁶ ohms.centimeter. In general, we will use metallic materials having a coefficient of expansion between about 15 and about 20 ppm per ° C and an electrical conductivity between about 2.10⁻⁶ and about 10.10⁻⁶ ohms.centimeter.
Cette broche B va ensuite subir un nickelage 91 consistant en le dépôt d'une couche de nickel d'une épaisseur d'environ 5 microns. Ce nickelage est suivi d'une oxydation à l'air pendant 15 minutes dans un four à 490°C. La broche B se trouve alors à l'issue de cette étape d'oxydation recouverte d'oxyde de nickel OX2. La présence de ce deuxième oxyde métallique OX2 est également un élément important pour la bonne tenue de la broche au sein de l'insert et son utilité sera expliquée plus loin.This pin B will then undergo nickel plating 91 consisting of the deposition of a layer of nickel with a thickness of approximately 5 microns. This nickel plating is followed by air oxidation for 15 minutes in an oven at 490 ° C. Pin B is then found at the end of this oxidation step covered with nickel oxide OX2. The presence of this second metal oxide OX2 is also an important element for the good behavior of the spindle within the insert and its usefulness will be explained later.
Tous les éléments constitutifs de la traversée étant maintenant réalisés, on peut procéder à l'insertion du fourreau fritté dans le passage, puis à l'insertion de la broche dans le fourreau. On obtient alors une traversée électrique TRA avant scellement représentée sur la figure 10. Le fourreau fritté FFR est situé dans l'alésage AL2 en appui contre l'alésage AL1. La broche B est maintenue à la distance choisie, dans le fourreau, par un outillage de centrage non représenté sur cette figure 10. Dans le mode de mise en oeuvre décrit, le bout arrondi de la broche est situé du côté de la face externe de la paroi PAR.All the constituent elements of the bushing now being produced, it is possible to insert the sintered sheath into the passage, then to insert the spindle into the sheath. An electrical crossing TRA is then obtained before sealing shown in FIG. 10. The sintered sleeve FFR is located in the bore AL2 bearing against the bore AL1. The spindle B is kept at the chosen distance, in the sheath, by a centering tool not shown in this figure 10. In the embodiment described, the rounded end of the spindle is located on the side of the external face of the PAR wall.
Bien que cet ordre d'insertion soit avantageux notamment pour le centrage de la broche, on pourrait envisager de l'inverser, c'est-à-dire d'insérer la broche dans le fourreau puis l'ensemble dans le passage.Although this order of insertion is advantageous in particular for centering the spindle, one could consider inverting it, that is to say inserting the spindle into the sheath and then the assembly into the passage.
L'ensemble ainsi constitué est amené dans un four afin de procéder au scellement 7 (figure 11) de la traversée électrique.The assembly thus formed is brought into an oven in order to proceed to sealing 7 (FIG. 11) of the electrical bushing.
L'étape de scellement selon l'invention s'effectue sous atmosphère neutre, en particulier d'azote, en élevant la température de cuisson au-dessus de la température de ramollissement dilatométrique du matériau vitreux constituant le fourreau fritté selon un profil de température choisi. Dans ce mode de mise en oeuvre, on effectue d'abord une montée en température avec un gradian de 12°C par minute (opération 700) puis un palier à une température de cuisson égale à 450°C pendant 50 mn (opération 701), puis une descente en température à partir de ce palier avec un gradian de 12°C par minute (opération 702).The sealing step according to the invention is carried out under a neutral atmosphere, in particular of nitrogen, by raising the baking temperature above the dilatometric softening temperature of the vitreous material constituting the sintered sheath according to a chosen temperature profile. . In this mode of implementation, a temperature rise is first carried out with a gradian of 12 ° C. per minute (operation 700) and then a plateau at a cooking temperature equal to 450 ° C. for 50 minutes (operation 701). , then a temperature drop from this level with a gradian of 12 ° C per minute (operation 702).
Cette cuisson s'effectue donc en présence du premier oxyde métallique entre le fourreau fritté et la paroi et en présence du deuxième oxyde métallique entre le fourreau et la broche conductrice.This cooking therefore takes place in the presence of the first oxide metal between the sintered sheath and the wall and in the presence of the second metal oxide between the sheath and the conductive pin.
La présence d'alumine entre le fourreau et la paroi permet d'assurer la tenue du scellement ainsi obtenu par l'interpénétration des atomes d'oxygène de l'alumine avec les atomes d'oxygène appartenant aux différents oxydes du matériau vitreux. L'ajustement de l'épaisseur de la couche d'alumine, qui induit donc une première quantité efficace de ce premier oxyde métallique, joue un rôle important, non seulement dans la tenue du scellement, mais aussi dans son herméticité. Une épaisseur comprise entre environ 1 et environ 1,5 micromètre permet notamment d'obtenir un matériaux vitreux dit "hermétiquement scellé". L'herméticité est alors inférieure ou égale à 10⁻⁹ cm³.s⁻¹ d'Hélium pour une différence de pression de 1 atmosphère de part et d'autre d'un scellement ayant une surface unitaire de 1 cm².The presence of alumina between the sheath and the wall makes it possible to maintain the seal thus obtained by the interpenetration of the oxygen atoms of the alumina with the oxygen atoms belonging to the various oxides of the vitreous material. The adjustment of the thickness of the alumina layer, which therefore induces a first effective amount of this first metal oxide, plays an important role, not only in the strength of the seal, but also in its hermeticity. A thickness of between approximately 1 and approximately 1.5 micrometers makes it possible in particular to obtain a vitreous material called "hermetically sealed". The hermeticity is then less than or equal to 10⁻⁹ cm³.s⁻¹ of Helium for a pressure difference of 1 atmosphere on either side of a seal having a unit area of 1 cm².
Si la couche d'alumine est plus épaisse, cette herméticité décroît jusqu'à éventuellement obtenir un scellement poreux au niveau de la paroi si cette couche est trop épaisse. On considère, d'une façon générale, qu'une quantité efficace du premier oxyde métallique est une quantité permettant d'obtenir un scellement ayant une tenue et une herméticité compatibles avec l'application envisagée.If the alumina layer is thicker, this hermeticity decreases until possibly obtaining a porous seal at the level of the wall if this layer is too thick. It is generally considered that an effective amount of the first metal oxide is an amount which makes it possible to obtain a seal having a strength and hermeticity compatible with the intended application.
Ainsi, quelle que soit l'application, la Demanderesse a observé qu'une épaisseur d'oxyde inférieure à 0,5 micron environ ne permet pas d'obtenir une tenue mécanique du verre sur l'aluminium. De même, bien que l'épaisseur maximale d'oxyde dépende de la tenue et de l'herméticité souhaitées, il est préférable de ne pas dépasser 10 microns.Thus, whatever the application, the Applicant has observed that an oxide thickness of less than approximately 0.5 microns does not make it possible to obtain mechanical strength of the glass on the aluminum. Similarly, although the maximum oxide thickness depends on the desired strength and hermeticity, it is preferable not to exceed 10 microns.
La présence de l'oxyde de nickel en une quantité efficace, entre la broche et le matériau vitreux contribue à assurer une bonne adhérence de ces deux corps par interpénétration des atomes d'oxygène de l'oxyde de nickel avec ceux des différents oxydes du verre. La couche de nickel de 5 microns déposée sur la broche conduit, après oxydation, à une épaisseur d'oxyde de nickel (environ 3 microns) contribuant à assurer un scellement hermétique. D'une façon générale, la Demanderesse a observé qu'une épaisseur d'oxyde de nickel comprise entre environ 2 et environ 5 microns, permet d'obtenir l'herméticité indiquée ci-avant.The presence of nickel oxide in an effective amount, between the spindle and the glassy material contributes to ensuring good adhesion of these two bodies by interpenetration of the oxygen atoms of the nickel oxide with those of the various glass oxides. The 5 micron nickel layer deposited on the spindle leads, after oxidation, to a thickness of nickel oxide (about 3 microns) helping to ensure a hermetic seal. In general, the Applicant has observed that a thickness of nickel oxide of between approximately 2 and approximately 5 microns makes it possible to obtain the hermeticity indicated above.
Lors du scellement, le fourreau fritté se conforme à la géométrie du passage ce qui permet d'obtenir un scellement simultané direct, c'est-à-dire ne nécessitant l'apport d'aucune matière externe, de la broche au fourreau et du fourreau à la paroi. Ce scellement hermétique et électriquement isolant permet d'obtenir la traversée électrique requise (figure 12).During sealing, the sintered sheath conforms to the geometry of the passage, which makes it possible to obtain a direct simultaneous sealing, that is to say requiring no external material, from the spindle to the sheath and the scabbard on the wall. This hermetic and electrically insulating seal provides the required electrical crossing (Figure 12).
Pour certaines applications, il peut être nécessaire d'effectuer sur les broches, un traitement supplémentaire de dorure 9′, illustré sur la figure 13. Cette dorure permettra d'obtenir une broche BD partiellement dorée, c'est-à-dire dorée uniquement sur ses parties internes et externes situées hors du matériau vitreux de scellement. Afin d'effectuer un tel traitement, il convient de plonger l'ensemble dans un bain électrolytique de dorure (opération 90′). La Demanderesse a observé que l'utilisation de verre-phosphate ne nécessitait pas de protéger le scellement avant son immersion dans le bain de dorure. Par contre si le matériau vitreux ne contenait pas d'agent modificateur de cristallisation, il conviendrait d'effectuer une protection du scellement, par exemple par un film de résine époxy, avant de plonger l'ensemble dans le bain de dorure, car sinon, le caractère acide de ce bain conduirait à une dégradation plus ou moins importante du matériau vitreux du scellement.For some applications, it may be necessary to perform on the pins, an additional treatment of
Cependant, cette raison n'est pas la seule qui motive une adjonction d'un agent modificateur de cristallisation. En effet, celui-ci confère notamment au scellement de meilleures propriétés mécaniques, une meilleure tenue aux conditions d'environnement et une meilleure longévité.However, this reason is not the only reason for the addition of a crystallization modifying agent. Indeed, it gives in particular better mechanical properties to sealing, better resistance to environmental conditions and better longevity.
Cependant, si la quantité de nitrure d'aluminium dépasse la quantité efficace de 7% en moles, on obtient une température de fusion de l'alliage d'aluminium inférieure à la température de ramollissement dilatométrique du matériau vitreux ce qui bien évidemment ne convient pas dans les applications selon l'invention.However, if the amount of aluminum nitride exceeds the effective amount of 7 mol%, a melting temperature of the aluminum alloy is obtained which is lower than the dilatometric softening temperature of the glassy material, which obviously is not suitable. in applications according to the invention.
On peut également choisir comme agent modificateur de cristallisation du platine (Pt) en une quantité efficace inférieure à 0,5% en moles. On ajoute alors dans ce cas, dans les constituants de base à la place du nitrure d'aluminium, du tétrachlorure de platine (PtCl₄). Dans ce cas, l'étape 7 de scellement comporterait après l'opération de cuisson 70 un recuit du scellement afin d'assurer une croissance des cristaux. Le traitement de dorure des broches s'effectue alors après le recuit.It is also possible to choose, as agent for modifying the crystallization of platinum (Pt) in an effective amount of less than 0.5 mol%. In this case, then, in the basic constituents, instead of aluminum nitride, platinum tetrachloride (PtCl₄) is added. In this case, the sealing
On va maintenant décrire ci-après, en se référant aux figures 12 et 14A à 14C, un mode de réalisation d'un boîtier macrohybride possédant une pluralité de traverses électriques. Les figures 14A à 14C sont disposées selon les conventions classiques du dessin industriel français, la figure 14B étant plus particulièrement la coupe AA de la figure 14A, tandis que la figure 14C comporte partiellement la coupe BB de la figure 14A.We will now describe below, with reference to FIGS. 12 and 14A to 14C, an embodiment of a macrohybrid box having a plurality of electrical sleepers. Figures 14A to 14C are arranged according to the conventional conventions of French industrial design, Figure 14B being more particularly section AA of Figure 14A, while Figure 14C partially includes section BB of Figure 14A.
Le boitier BO est sensiblement rectangulaire d'une longueur d'environ 70 mm et d'une largeur d'environ 50 mm. Ce boîtier comprend un fond FD possèdant deux bords latéraux BL1 et BL2 ainsi qu'une partie centrale PCFD s'étendant dans la direction longitudinale du boîtier entre deux bords latéraux. Un bord intermédiaire BIN est ménagé dans une région de la partie centrale PCFD. Ce bord BIN s'étend sensiblement perpendiculairement au bord latéral BL1 et est ensuite replié d'équerre sensiblement parallèlement au bord latéral BL2.The BO case is substantially rectangular with a length of approximately 70 mm and a width of approximately 50 mm. This box comprises a bottom FD having two lateral edges BL1 and BL2 as well as a central part PCFD extending in the longitudinal direction of the housing between two lateral edges. An intermediate edge BIN is formed in a region of the central part PCFD. This edge BIN extends substantially perpendicularly to the lateral edge BL1 and is then folded back to square substantially parallel to the lateral edge BL2.
Au travers de la partie centrale PCFD et du bord latéral BLD2 sont ménagées une pluralité de traversées électriques telles que celles représentées sur la figure 12. Le boîtier BO est fermé d'une part par un premier couvercle COUV1 s'étendant entre le bord intermédiaire BIN et les bords BL1 et BL2 en formant un L. Il est fermé d'autre part par un deuxième couvercle COUV2 disposé de l'autre côté de la partie centrale PCF2 entre les bords latéraux BL1 et BL2. Sont ainsi ménagés dans le boîtier B deux espaces situés de part et d'autre de la partie centrale PCFD du fond, propres à recevoir les composants hybrides.Through the central part PCFD and the lateral edge BLD2 are formed a plurality of electrical bushings such as those shown in FIG. 12. The box BO is closed on the one hand by a first cover COUV1 extending between the intermediate edge BIN and the edges BL1 and BL2 forming an L. It is closed on the other hand by a second cover COUV2 disposed on the other side of the central part PCF2 between the lateral edges BL1 and BL2. Are thus provided in the housing B two spaces located on either side of the central part PCFD of the bottom, suitable for receiving the hybrid components.
La face externe de la paroi représentée sur la figure 12 correspond ici effectivement à la face externe du boîtier. Les différentes broches dépassent ici de la face interne de la paroi d'une longueur égale à environ 1,5 mm. Ces broches sont destinées à assurer l'alimentation électrique des différents composants contenus dans le boîtier.The outer face of the wall shown in Figure 12 here effectively corresponds to the outer face of the housing. The different pins here protrude from the internal face of the wall by a length equal to about 1.5 mm. These pins are intended to supply electrical power to the various components contained in the housing.
Le matériau composant le fond du boitier comprend un alliage d'aluminium dit "5086". Le matériau constituant les deux couvercles du boîtier est par contre un alliage d'aluminium dit "4047" selon la norme française. Il se compose d'environ 12% de silicium et d'environ 88% d'aluminium.The material making up the bottom of the case comprises an aluminum alloy called "5086". The material constituting the two lids of the housing, on the other hand, is an aluminum alloy known as "4047" according to French standard. It is made up of around 12% silicon and around 88% aluminum.
Le matériau vitreux scellant chaque broche à la paroi est constitué de verre-phosphate dont les différents composants et leur fourchette de quantité ainsi que les fourchettes de la température de ramollissement dilatométrique et du coefficient de dilatation ont été définis ci-avant. Dans ce mode de réalisation, le matériau vitreux comprend environ 38,35% en moles de Na₂O, 9,59% en moles de BaO, 0,96% en moles de Al₂O₃, 46,98% en moles de P₂O₅, et 4,12% en moles de AlN.The glassy material sealing each spindle to the wall consists of phosphate glass, the various components and their quantity ranges as well as the forks the dilatometric softening temperature and the expansion coefficient have been defined above. In this embodiment, the glassy material comprises approximately 38.35% in moles of Na₂O, 9.59% in moles of BaO, 0.96% in moles of Al₂O₃, 46.98% in moles of P₂O₅, and 4, 12 mole% AlN.
Il peut également contenir, en tant qu'agent modificateur de cristallisation, du platine en une quantité efficace et inférieure à 0,5% en moles.It can also contain, as crystallization modifying agent, platinum in an effective amount and less than 0.5 mol%.
On trouve également dans ce matériau vitreux scellé le premier oxyde métallique (alumine) situé au voisinage de la paroi en une quantité efficace comprise entre environ 0,5% en poids et environ 0,8% en poids.Also found in this glassy sealed material is the first metal oxide (alumina) located in the vicinity of the wall in an effective amount of between about 0.5% by weight and about 0.8% by weight.
De même, le matériau vitreux scellé comporte au voisinage de la broche (alliage cuivre-béryllium) le deuxième oxyde métallique (oxyde de nickel) en une quantité efficace comprise entre environ 0,6% en poids et environ 1,5% en poids.Likewise, the sealed vitreous material comprises in the vicinity of the spindle (copper-beryllium alloy) the second metal oxide (nickel oxide) in an effective amount of between approximately 0.6% by weight and approximately 1.5% by weight.
Ces quantités efficaces d'oxydes métalliques permettent d'obtenir un scellement dit "hermétique". Cependant, d'une façon générale, un matériau vitreux directement scellé sur de l'aluminium comprendra une quantité d'alumine au moins égale à 0,2% en poids. La quantité maximale sera de préférence de l'ordre de 10% en poids.These effective amounts of metal oxides make it possible to obtain a so-called "hermetic" seal. However, in general, a vitreous material directly sealed on aluminum will comprise an amount of alumina at least equal to 0.2% by weight. The maximum amount will preferably be of the order of 10% by weight.
Afin d'assurer, notamment, une meilleure soudabilité à l'intérieur du boîtier et une meilleure tenue à la corrosion à l'extérieur du boitier, les parties de la broche situées à l'extérieur du matériau vitreux scellé, sont dorées. Les différents couvercles et le fond sont assemblés à l'aide d'une soudure au laser, assurant ainsi l'herméticité requise. Les alliages respectifs du fond et des couvercles ont été choisis pour autoriser une telle soudure. D'une façon générale, deux matériaux à base d'aluminium peuvent être soudés au laser si chacun d'eux est exempt de cuivre et si l'un au moins des deux contient du silicium.In order to ensure, in particular, better weldability inside the case and better resistance to corrosion outside the case, the parts of the spindle located outside the sealed vitreous material are golden. The different covers and the bottom are assembled using laser welding, thus ensuring airtightness required. The respective alloys of the bottom and the covers were chosen to allow such welding. In general, two aluminum-based materials can be laser welded if each of them is free of copper and if at least one of the two contains silicon.
Bien que l'invention trouve ses pleins avantages dans les modes de mise en oeuvre et de réalisation ci-dessus décrits, il s'est avéré encore meilleur pour certaines applications d'ajouter à la composition de verre utilisée un agent modificateur de la zone de travail du matériau vitreux.Although the invention finds its full advantages in the embodiments and embodiments described above, it has proved even better for certain applications to add to the glass composition used a modifying agent of the zone of glassy material work.
En effet, l'homme de l'art définit habituellement pour un matériau vitreux, une zone de températures de travail, dans laquelle le verre présente une viscosité lui permettant d'être déformé tout en conservant une certaine consistance. Ainsi, la température inférieure de cette zone de travail est la température de ramollissement dilatométrique et la température supérieure est celle pour laquelle le matériau vitreux présente une viscosité de 10⁴ poises.Indeed, those skilled in the art usually define for a vitreous material, a working temperature zone, in which the glass has a viscosity allowing it to be deformed while retaining a certain consistency. Thus, the lower temperature of this working zone is the dilatometric softening temperature and the upper temperature is that for which the vitreous material has a viscosity of 10⁴ poises.
Or il apparaît avantageux que le verre-phosphate comprenne un agent modificateur de sa zone de travail qui tende à augmenter cette dernière. En effet, plus vaste est cette zone de travail, moins critique sont les précisions sur les différentes températures utilisées dans les étapes du procédé selon l'invention. Ceci contribue notamment à encore améliorer la reproductibilité et par conséquent à une industrialisation encore plus aisée du procédé.However, it appears advantageous that the phosphate glass comprises an agent modifying its working area which tends to increase the latter. Indeed, the larger this working area, the less critical are the details on the different temperatures used in the steps of the method according to the invention. This contributes in particular to further improving the reproducibility and consequently to an even easier industrialization of the process.
Cet agent modificateur de la zone de travail est, par exemple, du trioxyde de bore (B₂O₃) en une quantité inférieure à environ 15% en moles.This modifying agent for the working area is, for example, boron trioxide (B₂O₃) in an amount less than about 15 mol%.
Un exemple de composition d'un tel matériau vitreux est la suivante :
- 35% en moles de Na₂O
- 8,75% en moles de BaO
- 0,87% en mole de Al₂O₃
- 42,88% en moles de P₂O₅
- 3,75% en moles de AlN
- 8,75% en moles de B₂O₃.An example of the composition of such a glassy material is the next one :
- 35% in moles of Na₂O
- 8.75% in moles of BaO
- 0.87 mole% of Al₂O₃
- 42.88% in moles of P₂O₅
- 3.75% in moles of AlN
- 8.75% in moles of B₂O₃.
Un tel matériau vitreux a alors une température de ramollissement dilatométrique de 475°C environ et un coefficient de dilatation de 16ppm/°C environ. Sa zone de travail est comprise entre 475°C environ et 550°C et sa température de fusion est d'environ 700°C.Such a vitreous material then has a dilatometric softening temperature of approximately 475 ° C. and a coefficient of expansion of approximately 16 ppm / ° C. Its working area is between around 475 ° C and 550 ° C and its melting temperature is around 700 ° C.
Les étapes du procédé de scellement verre-aluminium, utilisant ce matériau vitreux à base de trioxyde de bore sont analogues à celles décrites pour une composition de verre exempte de trioxyde de bore.The steps of the glass-aluminum sealing process using this glassy material based on boron trioxide are similar to those described for a glass composition free of boron trioxide.
Cependant des différences existent notamment quant aux températures auxquelles s'effectuent certaines étapes du procédé.However, differences exist in particular as to the temperatures at which certain stages of the process take place.
Dans la suite du texte, les références utilisées pour décrire ces étapes modifiées sont celles employées précédemment.In the rest of the text, the references used to describe these modified steps are those used previously.
Pour la réalisation de la poudre de base (opération 10) on utilise 42,4 g de carbonate de sodium (Na₂CO₃), 19,74 g de carbonate de baryum (BaCO₃), 1,02 g d'alumine (Al₂O₃), 112,73 g de dihydrogénophosphate d'ammonium (NH₄H₂PO₄), 6,96 g de trioxyde de bore (B₂O₃) et 1,76 g de nitrure d'aluminium (AlN).For the production of the base powder (operation 10), 42.4 g of sodium carbonate (Na₂CO₃), 19.74 g of barium carbonate (BaCO₃), 1.02 g of alumina (Al₂O₃) are used, 112 , 73 g of ammonium dihydrogen phosphate (NH₄H₂PO₄), 6.96 g of boron trioxide (B₂O₃) and 1.76 g of aluminum nitride (AlN).
Dans l'étape d'obtention du corps continu CC, la cuisson du broyat BRO (opération 14) permettant d'obtenir la substance vitreuse SV comporte une montée en température d'une heure environ à raison de 1100°C/heure puis un palier à 1100°C pendant 2 heures et enfin une descente en température pendant environ 30 minutes jusqu'à atteindre la température de 850°C environ.In the step of obtaining the continuous body CC, the cooking of the BRO ground material (operation 14) making it possible to obtain the vitreous substance SV involves a rise in temperature of about one hour at a rate of 1100 ° C./hours then a level at 1100 ° C for 2 hours and finally a drop in temperature for about 30 minutes until reaching the temperature of about 850 ° C.
L'étape de frittage du matériau vitreux (référence 4) est effectuée dans une coupelle en PYREX selon un gradient de température de 20°C/mn jusqu'à atteindre la température de 470°C.The sintering step of the vitreous material (reference 4) is carried out in a PYREX dish according to a temperature gradient of 20 ° C / min until reaching the temperature of 470 ° C.
L'étape de scellement comprend d'abord une montée en température avec un gradient de 12°C par minute (opération 700) puis un palier à une température de cuisson égale à 525°C pendant 15 mn (opération 701) puis une descente en température à partir de ce palier avec un gradient de 12°C par minute (opération 702).The sealing step first includes a temperature rise with a gradient of 12 ° C per minute (operation 700) then a plateau at a cooking temperature equal to 525 ° C for 15 min (operation 701) then a descent in temperature from this level with a gradient of 12 ° C per minute (operation 702).
L'invention n'est pas limitée aux modes de mise en oeuvre et de réalisation ci-dessus décrits mais en embrasse toutes les variantes, notamment les suivantes :
- on peut concevoir que la broche soit remplacée, dans d'autres applications, par un autre élément métallique, au moins ;
- la présence des premier et deuxième oxydes métalliques n'est nécessaire qu'au niveau du scellement. Aussi, on peut envisager d'effectuer des oxydations partielles des élément métallique et du logement uniquement dans les zones utiles ;
- on pourrait également concevoir, dans certaines applications nécessitant uniquement un scellement direct "broche- verre" sans que la bonne tenue mécanique et l'herméticité soient des facteurs importants, d'effectuer ce scellement sans présence d'oxyde métallique entre la broche et le matériau vitreux. La tenue de la broche serait alors simplement assurée par le rétreint du verre à la cuisson ;
- il est possible, dans l'étape 3, de remplacer la tige de l'outillage de pressage, servant à conformer le canal central du fourreau, par la broche elle-même. Ainsi, dans ce cas, après pressage, on obtient un insert composé en périphérie du fourreau, et au centre de la broche, qui après élimination du liant et frittage devient un élément prêt à être introduit dans le passage de la paroi. Cette variante permet de limiter les divers outillages de centrage et de positionnement utilisés précédemment. Bien entendu, le deuxième oxyde métallique aura été déposé sur la broche avant la formation de l'élément unique.The invention is not limited to the embodiments and embodiments described above, but embraces all variants, in particular the following:
- It is conceivable that the spindle is replaced, in other applications, by another metallic element, at least;
- the presence of the first and second metal oxides is only necessary at the level of the seal. Also, it is possible to envisage carrying out partial oxidations of the metallic element and of the housing only in the useful zones;
- one could also conceive, in certain applications requiring only a direct sealing "spindle- glass "without good mechanical strength and airtightness being important factors, to perform this sealing without the presence of metal oxide between the spindle and the glassy material. The holding of the spindle would then be simply ensured by the glass shrinking during cooking;
- It is possible, in
Il est également possible de concevoir que le fourreau d'un tel insert obtenu après pressage, soit, après élimination du liant, fritté à une température supérieure à la température de frittage précédemment indiquée de façon à augmenter encore sa cohérence.It is also possible to conceive that the sheath of such an insert obtained after pressing, or, after removal of the binder, sintered at a temperature higher than the sintering temperature previously indicated so as to further increase its consistency.
- On a décrit ci-avant l'étape de dorure des broches postérieurement à l'étape de scellement. Cependant, on pourrait envisager d'effectuer cette étape de dorure au moment de la préparation de la broche et donc avant d'effectuer le scellement. Cette dorure serait alors partielle et située sur les parties destinées à ne pas être scellées dans le passage. L'homme de l'art devrait alors utiliser un or résistant à la température de ramollissement dilatométrique du matériau vitreux. Une telle dorure partielle pourrait être effectuée, avant scellement, sur un insert fritté (fourreau et broche) tel qu'évoqué ci-avant ;
- on peut bien sûr ajouter au matériau vitreux à la fois l'un et l'autre des agents modificateurs de cristallisation évoqués ci-dessus.- We described above the step of gilding the pins after the sealing step. However, one could consider carrying out this gilding step at the time of the preparation of the pin and therefore before carrying out the sealing. This gilding would then be partial and located on the parts intended not to be sealed in the passage. Those skilled in the art should then use gold resistant to the dilatometric softening temperature of the glassy material. Such partial gilding could be carried out, before sealing, on a sintered insert (sheath and pin) as mentioned above;
- It is of course possible to add to the vitreous material both one and the other of the crystallization modifying agents mentioned above.
On a décrit, ci-avant, comme application particulière de l'invention, l'élaboration d'une traversée électrique à travers un élément de boîtier macrohybride. Cependant on pourrait utiliser ce scellement direct d'un matériau vitreux selon l'invention sur un matériau à base d'aluminium pour d'autres applications ou objets. On pourrait par exemple envisager que l'insert ne comprenne que du matériau vitreux.We have described above, as a particular application of the invention, the development of an electrical bushing through a macrohybrid housing element. However, this direct sealing of a vitreous material according to the invention could be used on an aluminum-based material for other applications or objects. One could for example consider that the insert comprises only glassy material.
Bien entendu, certains des moyens décrits ci-dessus peuvent être omis dans les variantes où ils ne servent pas. Ce peut être le cas par exemple des agents modificateurs de cristallisation et/ou de l'agent modificateur de la zone de travail.Of course, some of the means described above can be omitted in the variants where they are not used. This can be the case, for example, for modifying agents for crystallization and / or for modifying agents for the working area.
Claims (92)
ce qui permet d'obtenir un scellement direct de l'insert à la paroi.
which allows a direct sealing of the insert to the wall.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR8900709 | 1989-01-20 | ||
| FR8900709A FR2642257B1 (en) | 1989-01-20 | 1989-01-20 | GLASS-ALUMINUM SEALING PROCESS, PARTICULARLY FOR ELECTRICAL THROUGHING OF HYBRID CIRCUIT BOX, CORRESPONDING COMPOSITE OBJECT AND GLASS COMPOSITION |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0379431A1 true EP0379431A1 (en) | 1990-07-25 |
| EP0379431B1 EP0379431B1 (en) | 1994-10-05 |
Family
ID=9377940
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP90400134A Expired - Lifetime EP0379431B1 (en) | 1989-01-20 | 1990-01-17 | Glass-aluminium sealing process, in particular for a hybrid circuit box electrical feedthrough, corresponding composite article and glass composition |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US5538527A (en) |
| EP (1) | EP0379431B1 (en) |
| CA (1) | CA2008297C (en) |
| DE (1) | DE69013017D1 (en) |
| FR (1) | FR2642257B1 (en) |
| IL (1) | IL93101A (en) |
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| US6262477B1 (en) | 1993-03-19 | 2001-07-17 | Advanced Interconnect Technologies | Ball grid array electronic package |
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| US6274252B1 (en) * | 1994-08-04 | 2001-08-14 | Coors Ceramics Company | Hermetic glass-to-metal seal useful in headers for airbags |
| DE102006004036A1 (en) * | 2006-01-27 | 2007-08-09 | Schott Ag | Metal fixing material implementation and use of such a passage and airbag and belt tensioner with an ignition device |
| US8733250B2 (en) * | 2006-01-27 | 2014-05-27 | Schott Ag | Metal-sealing material-feedthrough and utilization of the metal-sealing material feedthrough with an airbag, a belt tensioning device, and an ignition device |
| JP4856025B2 (en) * | 2007-08-10 | 2012-01-18 | セイコーインスツル株式会社 | Airtight terminal manufacturing method and airtight terminal, piezoelectric vibrator manufacturing method and piezoelectric vibrator, oscillator, electronic device, radio timepiece |
| DE102010045641A1 (en) | 2010-09-17 | 2012-03-22 | Schott Ag | Process for producing a ring-shaped or plate-shaped element |
| US10684102B2 (en) | 2010-09-17 | 2020-06-16 | Schott Ag | Method for producing a ring-shaped or plate-like element |
| FR3036396B1 (en) | 2015-05-22 | 2020-02-28 | Axon Cable | GLASS COMPOSITION FOR SEALING MICRO-D CONNECTOR |
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| PATENT ABSTRACTS OF JAPAN vol. 9, no. 270 (E-353)(1993) 26 octobre 1985, & JP-A-60 116156 (FUJITSU K.K.) 22 juin 1985, * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6262477B1 (en) | 1993-03-19 | 2001-07-17 | Advanced Interconnect Technologies | Ball grid array electronic package |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2642257B1 (en) | 1996-05-24 |
| EP0379431B1 (en) | 1994-10-05 |
| IL93101A0 (en) | 1990-11-05 |
| US5538527A (en) | 1996-07-23 |
| CA2008297C (en) | 1995-08-01 |
| FR2642257A1 (en) | 1990-07-27 |
| DE69013017D1 (en) | 1994-11-10 |
| IL93101A (en) | 1994-07-31 |
| CA2008297A1 (en) | 1990-07-20 |
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