CN102924776B - PTC material composition and the overcurrent protection assembly be made up of it - Google Patents
PTC material composition and the overcurrent protection assembly be made up of it Download PDFInfo
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Abstract
PTC material composition and the overcurrent protection assembly be made up of it, this PTC material composition comprises: a positive temperature coefficient polymer unit; And a conductive filling, containing multiple titanium carbide granule.Described titanium carbide granule has based on its weight the residual oxygen level that is greater than 0.3wt%.The present invention also provides a kind of positive temperature coefficient overcurrent protection assembly.
Description
Technical field
The present invention relates to a kind of PTC material for the manufacture of overcurrent protection assembly composition and a kind of positive temperature coefficient overcurrent protection assembly, particularly relate to a kind of PTC material composition with titanium carbide granule.
Background technology
PTC conductive macromolecular component owing to having positive temperature coefficient effect, so can be used as overcurrent protection assembly.The positive and negative electrode that PTC conductive macromolecular component comprises a PTC conductive macromolecular material and is formed on two corresponding surfaces of this PTC conductive macromolecular material.The macromolecule matrix and one that this PTC conductive macromolecular material comprises a tool crystalline phase district and amorphous phase region is scattered in the amorphous phase region of this macromolecule matrix and forms the conductive particle weighting material in a continuous conduction path.Positive temperature coefficient effect refers to that, when the temperature of this macromolecule matrix is raised to its fusing point, this crystalline phase district starts melting and produces new amorphous phase region.When amorphous phase region is increased to a degree and combines with the former amorphous phase region deposited, the conductive path of this conductive particle weighting material can be made to form discontinuous shape, and cause the resistance of this PTC conductive macromolecular material to increase rapidly, and thus form power-off.
Simultaneously the main requirement of PTC conductive macromolecular component to have high positive temperature coefficient effect, high connductivity degree, high electric stability, high environmental stability.
The composition of existing PTC conductive macromolecular material generally includes a PTC conductive polymer unit and a carbon dust (carbon black) conductive filling.This PTC conductive polymer unit comprises a weight average molecular weight scope usually between 50,000g/mole to 300, the polyolefine [having the melt flow rate (under the condition of 190 DEG C/2.16Kg) between 0.01g/10min to 10g/10min] of 000g/mole and a selectively weight average molecular weight scope are between 50, the graft type polyolefine [there is the melt flow rate (under the condition of 190 DEG C/2.16Kg) between 0.5g/10min to 10g/10min] of 000g/mole to 200,000g/mole.The polyolefinic major function of this graft type is to increase PTC conductive polymer unit and interelectrode adherence.
Because the conductance of carbon dust conductive filling is low, be not therefore suitable for the current protection assembly that some need comparatively high connductivity degree (low resistance).In lifting conductance, although by increasing kenel (the such as metallic particles with the non-carbon class conductive particle weighting material of high conductivity, conductive ceramic particle and surface metalation particle etc.) increase the conductance (dropping to the volume specific resistance being less than 0.05ohm-cm from the volume specific resistance of 1.0ohm-cm or higher originally) of PTC conductive macromolecular component, but described non-carbon dust conductive filling and PTC conductive high molecular physical properties difference excessive, cause conductive filling that creep (creeping) easily occurs in electroconductive polymer matrix, cause the electric stability of electroconductive polymer positive temperature coefficient assembly and therefore reduce work-ing life.
Summary of the invention
The object of the present invention is to provide a kind of can improve electroconductive polymer positive temperature coefficient overcurrent assembly electric stability and the PTC material in work-ing life form.
So a kind of PTC material for the manufacture of overcurrent protection assembly of the present invention forms, and comprises: a positive temperature coefficient polymer unit; And a conductive filling, containing multiple titanium carbide granule.Described titanium carbide granule has one based on its weight and is not less than 0.5wt% and is less than the residual oxygen level of 1.0wt%.
The residual oxygen level of described titanium carbide granule is the oxygen level in the titanium carbide product that obtains of the mixture having titaniferous materials and carbonaceous material by carbonization one at 1700 DEG C ~ 2000 DEG C.
This titaniferous materials selects the combination from titanium dioxide, titanium tetrachloride, titanium hydride, arizonite, titanium and aforementioned substances.
Preferably, this titaniferous materials is titanium dioxide.
Preferably, this carbonaceous material is carbon black or graphite.
This positive temperature coefficient polymer unit comprises a polyolefin blend thing, and this polyolefin blend thing comprises high density polyethylene(HDPE) and unsaturated carboxylic acid graft type high density polyethylene(HDPE).And this positive temperature coefficient polymer unit accounts for the 10-30wt% of this PTC material composition, this conductive filling accounts for the 70-90wt% of this PTC material composition.
This conductive filling also comprises an electroconductive powder, this electroconductive powder selects certainly in zirconium carbide, vanadium carbide, niobium carbide, tantalum carbide, chromium carbide, molybdenum carbide, wolfram varbide, titanium nitride, zirconium nitride, vanadium nitride, niobium nitride, tantalum nitride, chromium nitride, titanium disilicide, zirconium disilicide, niobium disilicide, tungsten silicide, gold, silver, copper, aluminium, nickel, surface degree nickel glass sphere, plating nickel on surface graphite, titanium tantalum Solid solution, tungsten titanium tantalum chromium Solid solution, tungsten tantalum Solid solution, tungsten titanium tantalum niobium Solid solution, tungsten titanium tantalum Solid solution, tungsten titanium Solid solution, one combination of tantalum niobium Solid solution and aforementioned substances.
Preferably, this electroconductive powder is nickel powder.
Again, a kind of positive temperature coefficient overcurrent protection assembly of the present invention, comprises: a PTC material layer; And two electrodes, be located on this PTC material layer; This PTC material layer has a PTC material composition; this PTC material composition comprises a positive temperature coefficient polymer unit; and one containing the conductive filling of multiple titanium carbide granule, described titanium carbide granule has one based on its weight and is not less than 0.5wt% and is less than the residual oxygen level of 1.0wt%.
Beneficial effect of the present invention is: the electric stability that can improve positive temperature coefficient overcurrent assembly using the titanium carbide granule with the residual oxygen level being greater than 0.3wt% as a composition of conductive filling.
Accompanying drawing explanation
Fig. 1 is a schematic diagram, and the structure of a kind of positive temperature coefficient overcurrent protection assembly of a preferred embodiment of the present invention is described.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in detail.
Consult Fig. 1, a kind of positive temperature coefficient overcurrent protection assembly of the present invention comprises: a PTC material layer 2; And two electrodes 3, be arranged on this PTC material layer 2; This PTC material layer 2 has a PTC material composition.
This PTC material composition comprises: a positive temperature coefficient polymer unit; And a conductive filling, containing multiple titanium carbide granule.Described titanium carbide granule has based on its weight the residual oxygen level that is greater than 0.3wt%.The residual oxygen level of titanium carbide granule is defined as: a mixture with titaniferous materials (particulate state) and carbonaceous material (Powdered) at high temperature carries out oxygen amount contained in the titanium carbide granule product that carbonization (carbiding) obtains afterwards.Carbonization temperature is higher, and residual oxygen level is lower.When the residual oxygen level of titanium carbide granule is lower than 0.3wt%, the electric stability of PTC material has significant variation.
Under better, the residual oxygen level of described titanium carbide granule is for by carbonization (carbiding) at 1700 DEG C ~ 2000 DEG C, this has the mixture of titaniferous materials and carbonaceous material and the oxygen level in the titanium carbide granule product obtained.Under better, described titanium carbide granule has one based on its weight and is not less than (being namely more than or equal to) 0.5wt% and is less than the residual oxygen level of 1.0wt%.
Under better, the particle size range of described titanium carbide granule is preferably and is greater than 0.1 μm and is less than 200 μm.
Under better, this titaniferous materials selects the combination from titanium dioxide, titanium tetrachloride, titanium hydride, arizonite (Ferro titanium ore) or titanium particle and aforementioned substances.Under better, this titaniferous materials selects from titanium dioxide.
Under better, this carbonaceous material is carbon black (carbon black) or powdered graphite.
This positive temperature coefficient polymer unit can be the adulterant (polymer blend) of general existing positive temperature coefficient polymer or polymkeric substance.Under better, this positive temperature coefficient polymer unit comprises a polyolefin blend thing.Under better, this polyolefin blend thing comprises high density polyethylene(HDPE) and unsaturated carboxylic acid graft type high density polyethylene(HDPE).
Under better, this positive temperature coefficient polymer unit accounts for the 10-30wt% of this PTC material composition, and this conductive filling accounts for the 70-90wt% of this PTC material composition.
Under better, this conductive filling also comprises an electroconductive powder.This electroconductive powder selects certainly in zirconium carbide, vanadium carbide, niobium carbide, tantalum carbide, chromium carbide, molybdenum carbide, wolfram varbide, titanium nitride, zirconium nitride, vanadium nitride, niobium nitride, tantalum nitride, chromium nitride, titanium disilicide, zirconium disilicide, niobium disilicide, tungsten silicide, gold, silver, copper, aluminium, nickel, surface degree nickel glass sphere, plating nickel on surface graphite, titanium tantalum Solid solution, tungsten titanium tantalum chromium Solid solution, tungsten tantalum Solid solution, tungsten titanium tantalum niobium Solid solution, tungsten titanium tantalum Solid solution, tungsten titanium Solid solution, one combination of tantalum niobium Solid solution and aforementioned substances.Under better, this electroconductive powder is nickel powder.
Embodiment and effect of each object of the present invention will be described with embodiment and comparative example below.It is noted that, this embodiment is only and illustrates use, and should not be interpreted as restriction of the invention process.
Prepared by PTC conductive macromolecular component
< embodiment 1 (E1) >
By 10g high density polyethylene(HDPE) (marque: HDPE9002, purchased from Formosa plasticCorp., weight average molecular weight 150000g/mole, at 230 DEG C, M.F.I under 12.6kg is 45g/10min), 10g unsaturated carboxylic acid graft type high density polyethylene(HDPE) (marque: MB100D, purchased from Dupont, weight average molecular weight 80000g/mole, at 230 DEG C, M.F.I. under 12.6kg is 75g/10min), with 80g titanium carbide powder A (TiC-A, there is the residual oxygen level of 0.9wt%, the mixture that the preparation of titanium carbide powder A has titanium dioxide and carbon black by carbonization one at 1850 DEG C obtains) add in a Brabender mixing roll mixing.Melting temperature is 200 DEG C; Stirring velocity is 60rpm; Pressurization weight is 5kg; Mixing time is 10 minutes.The mixture of mixing rear gained is placed in a mould, then, with thermocompressor, hot pressing is carried out to blend sample, hot pressing temperature is 200 DEG C, hot pressing time is 4 minutes, hot pressing pressure is 80kg/cm
2, the sample after mixing being hot pressed into thickness is, after the thin slice of 0.12mm, respectively paste a slice nickel plating Copper Foil in thin slice both sides, then according to same hot pressing condition hot pressing, forms a sandwich structure, this sandwich structure is die-cut into the chip of 4.5mm × 3.2mm.Measure the resistance value (see table 1) of the PTC material obtained by embodiment 1.G-HDPE in table 1 represents graft type high density polyethylene(HDPE), and V-R represents volume resistance (ohm-cm).
Table 1
< embodiment 2 (E2) >
The preparation procedure of the sample of embodiment 2 is different with embodiment 1 from condition be in embodiment 2 are the titanium carbide powder A replacing embodiment 1 with titanium carbide powder B (TiC-B).Titanium carbide powder B has the residual oxygen level of 0.8wt%, and the mixture that its preparation has titanium hydride and carbon black by carbonization one at 1960 DEG C obtains.Measure the resistance value (see table 1) of the PTC material obtained by embodiment 2.
< embodiment 3 (E3) >
The preparation procedure of the sample of embodiment 3 is different with embodiment 1 from condition be in embodiment 3 are the titanium carbide powder A replacing embodiment 1 with titanium carbide powder C (TiC-C).Titanium carbide powder C has the residual oxygen level of 0.5wt%, and the mixture that its preparation has arizonite and graphite by carbonization one at 1780 DEG C obtains.Measure the resistance value (see table 1) of the PTC material obtained by embodiment 3.
< comparative example 1 (CE1) >
The preparation procedure of the sample of comparative example 1 is different with embodiment 1 from condition be in comparative example 1 be the titanium carbide powder A replacing embodiment 1 with titanium carbide powder D (TiC-D).Titanium carbide powder D has the residual oxygen level of 0.2wt%, and the mixture that its preparation has titanium dioxide and carbon black by carbonization one at 2200 DEG C obtains.Measure the resistance value (see table 1) of the PTC material obtained by comparative example 1.
< embodiment 4 (E4) >
The preparation procedure of the sample of embodiment 4 and be in embodiment 4 different from embodiment 1 of condition use the nickel powder of 60g titanium carbide powder A and 20g as conductive filler.Measure the resistance value (see table 2) of the PTC material obtained by embodiment 4.
Table 2
< embodiment 5 (E5) >
The preparation procedure of the sample of embodiment 5 and be in embodiment 5 different from embodiment 1 of condition use the nickel powder of 60g titanium carbide powder B and 20g as conductive filler.Measure the resistance value (see table 2) of the PTC material obtained by embodiment 5.
< embodiment 6 (E6) >
The preparation procedure of the sample of embodiment 6 and be in embodiment 6 different from embodiment 1 of condition use the nickel powder of 60g titanium carbide powder C and 20g as conductive filler.Measure the resistance value (see table 2) of the PTC material obtained by embodiment 6.
< comparative example 2 (CE2) >
The preparation procedure of the sample of comparative example 2 and be in comparative example 2 different from embodiment 1 of condition use the nickel powder of 80g as conductive filler.Measure the resistance value (see table 2) of the PTC material obtained by comparative example 2.
< comparative example 3 (CE3) >
The preparation procedure of the sample of comparative example 3 and be in comparative example 3 different from embodiment 1 of condition use the nickel powder of 60g titanium carbide powder D and 20g as conductive filler.Measure the resistance value (see table 2) of the PTC material obtained by comparative example 3.
Function test
Test chip prepared by embodiment 1-6 and comparative example 1-3 is carried out periodicity test and burn-in test.Periodically test is to carry out 720 loop cycle tests under 6Vdc and 50A (ampere) and energising power-off in the 60 seconds condition of 60 seconds, resistance (Ri) resistance (Rf) rear with test before measurement test.Burn-in test continues energising 504 hours with 6Vdc and 10A (ampere), resistance (Ri) resistance (Rf) rear with test before measurement test.The periodicity of embodiment 1-3 and comparative example 1 and ageing test result are as table 3 and table 4.The periodicity of embodiment 4-6 and comparative example 2-3 and ageing test result are as table 5 and table 6.
Table 3 (periodically test)
| Ri,avg,ohm | Rf,avg,ohm | Rf/Ri,avg,％ | Passratio,％ | |
| E1 | 0.008 | 0.0763 | 953.8％ | 100％ |
| E2 | 0.009 | 0.0565 | 627.8％ | 100％ |
| E3 | 0.009 | 0.0735 | 816.7％ | 100％ |
| CE1 | 0.008 | 13.763 | 172037.5％ | 92％ |
Table 4 (burn-in test)
| Ri,avg,ohm | Rf,avg,ohm | Rf/Ri,avg,％ | Passratio,％ | |
| E1 | 0.008 | 0.214 | 2675.0％ | 100％ |
| E2 | 0.009 | 0.195 | 2166.7％ | 100％ |
| E3 | 0.009 | 0.221 | 2455.6％ | 100％ |
| CE1 | 0.008 | 2.794 | 34925.0％ | 98％ |
Compare with ageing test result as can be seen from embodiment 1-3 with the periodicity of comparative example 1, when the residual oxygen level of titanium carbide is close to 0.2wt%, the electric stability of test chip is deteriorated.
Table 5 (periodically test)
| Ri,avg,ohm | Rf,avg,ohm | Rf/Ri,avg,％ | Passratio,％ | |
| E4 | 0.009 | 0.0185 | 205.6％ | 100％ |
| E5 | 0.009 | 0.0149 | 165.6％ | 100％ |
| E6 | 0.009 | 0.0204 | 226.7％ | 100％ |
| CE2 | 0.007 | 0.4496 | 6422.9％ | 70％ |
| CE3 | 0.008 | 35.97 | 449625.0％ | 92％ |
Table 6 (burn-in test)
As can be seen from the results contrast of embodiment 4-6 and comparative example 2-3, when the residual oxygen level of titanium carbide is close to 0.2wt% or when only using nickel powder (not containing titanium carbide), the electric stability of test chip is deteriorated.
In sum, by using the titanium carbide granule that is greater than the residual oxygen level of 0.3wt% can improve the electric stability of electroconductive polymer PTC material as a composition of conductive filling.
But the above, be only preferred embodiment of the present invention, when not limiting scope of the invention process with this, the simple equivalence namely generally done according to the present patent application the scope of the claims and invention description content changes and modifies, and all still remains within the scope of the patent.
Claims (10)
1. the PTC material for the manufacture of overcurrent protection assembly forms, and it is characterized in that it comprises:
One positive temperature coefficient polymer unit; And
One conductive filling, containing multiple titanium carbide granule;
Described titanium carbide granule has one based on its weight and is not less than 0.5wt% and is less than the residual oxygen level of 1.0wt%, and the residual oxygen level of described titanium carbide granule is the oxygen level in the titanium carbide product that obtains of the mixture having titaniferous materials and carbonaceous material by carbonization one at 1700 DEG C ~ 2000 DEG C.
2. PTC material composition according to claim 1, is characterized in that: this titaniferous materials selects the combination from titanium dioxide, titanium tetrachloride, titanium hydride, arizonite, titanium and aforementioned substances.
3. PTC material composition according to claim 2, is characterized in that: this titaniferous materials is titanium dioxide.
4. PTC material composition according to claim 1, is characterized in that: this carbonaceous material is carbon black or graphite.
5. PTC material composition according to claim 1, is characterized in that: this positive temperature coefficient polymer unit comprises a polyolefin blend thing.
6. PTC material composition according to claim 5, is characterized in that: this polyolefin blend thing comprises high density polyethylene(HDPE) and unsaturated carboxylic acid graft type high density polyethylene(HDPE).
7. PTC material composition according to claim 1, it is characterized in that: this positive temperature coefficient polymer unit accounts for the 10-30wt% of this PTC material composition, this conductive filling accounts for the 70-90wt% of this PTC material composition.
8. PTC material composition according to claim 1, it is characterized in that: this conductive filling also comprises an electroconductive powder, this electroconductive powder selects certainly in zirconium carbide, vanadium carbide, niobium carbide, tantalum carbide, chromium carbide, molybdenum carbide, wolfram varbide, titanium nitride, zirconium nitride, vanadium nitride, niobium nitride, tantalum nitride, chromium nitride, titanium disilicide, zirconium disilicide, niobium disilicide, tungsten silicide, gold, silver, copper, aluminium, nickel, surface degree nickel glass sphere, plating nickel on surface graphite, titanium tantalum Solid solution, tungsten titanium tantalum chromium Solid solution, tungsten tantalum Solid solution, tungsten titanium tantalum niobium Solid solution, tungsten titanium tantalum Solid solution, tungsten titanium Solid solution, one combination of tantalum niobium Solid solution and aforementioned substances.
9. PTC material composition according to claim 8, is characterized in that: this electroconductive powder is nickel powder.
10. a positive temperature coefficient overcurrent protection assembly, is characterized in that it comprises:
One PTC material layer; And
Two electrodes, are located on this PTC material layer;
This PTC material layer has a PTC material composition, and this PTC material composition comprises a positive temperature coefficient polymer unit, and one containing the conductive filling of multiple titanium carbide granule,
Described titanium carbide granule has one based on its weight and is not less than 0.5wt% and is less than the residual oxygen level of 1.0wt%, and the residual oxygen level of described titanium carbide granule is the oxygen level in the titanium carbide product that obtains of the mixture having titaniferous materials and carbonaceous material by carbonization one at 1700 DEG C ~ 2000 DEG C.
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| CN103333385A (en) * | 2013-05-29 | 2013-10-02 | 安徽荣玖光纤通信科技有限公司 | PTC polymer conductive material used for copper wires and preparation method thereof |
| TWI557756B (en) * | 2014-09-29 | 2016-11-11 | 聚鼎科技股份有限公司 | Positive temperature coefficient composition and over-current protection device containing the same |
| CN106298119B (en) * | 2015-05-13 | 2019-02-15 | 富致科技股份有限公司 | PTC circuit protection element |
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| GB898602A (en) * | 1957-05-01 | 1962-06-14 | British Aluminium Co Ltd | Improvements in or relating to electrolytic cells for the production of metals |
| US3900552A (en) * | 1972-02-01 | 1975-08-19 | Us Interior | Preparation of highly pure titanium tetrachloride from perovskite or titanite |
| US4732701A (en) * | 1985-12-03 | 1988-03-22 | Idemitsu Kosan Company Limited | Polymer composition having positive temperature coefficient characteristics |
| CN1909123A (en) * | 2005-08-05 | 2007-02-07 | 聚鼎科技股份有限公司 | Over current protection element |
| CN101763925A (en) * | 2009-12-25 | 2010-06-30 | 上海神沃电子有限公司 | Polymer positive temperature coefficient (PTC) chip and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP3413625B2 (en) * | 1995-06-07 | 2003-06-03 | 株式会社アライドマテリアル | Method for producing titanium carbonitride powder |
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| GB898602A (en) * | 1957-05-01 | 1962-06-14 | British Aluminium Co Ltd | Improvements in or relating to electrolytic cells for the production of metals |
| US3900552A (en) * | 1972-02-01 | 1975-08-19 | Us Interior | Preparation of highly pure titanium tetrachloride from perovskite or titanite |
| US4732701A (en) * | 1985-12-03 | 1988-03-22 | Idemitsu Kosan Company Limited | Polymer composition having positive temperature coefficient characteristics |
| CN1909123A (en) * | 2005-08-05 | 2007-02-07 | 聚鼎科技股份有限公司 | Over current protection element |
| CN101763925A (en) * | 2009-12-25 | 2010-06-30 | 上海神沃电子有限公司 | Polymer positive temperature coefficient (PTC) chip and application thereof |
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