CN104128897A - Method for preparing ceramic cBN abrasive disc through wet chemistry method forming and microwave sintering - Google Patents
Method for preparing ceramic cBN abrasive disc through wet chemistry method forming and microwave sintering Download PDFInfo
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- CN104128897A CN104128897A CN201410390060.9A CN201410390060A CN104128897A CN 104128897 A CN104128897 A CN 104128897A CN 201410390060 A CN201410390060 A CN 201410390060A CN 104128897 A CN104128897 A CN 104128897A
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Abstract
The invention belongs to the technical field of super-hard material preparation, and particularly relates to a method for preparing a ceramic cBN abrasive disc through wet chemistry method forming and microwave sintering. The method includes the steps that an aluminum, silicon and zirconium composite sol solution is prepared, a gel mixture is prepared by adding cBN abrasive material, diamond abrasive material, sintering additives, short carbon fiber, short glass fiber and dewatered sludge after sol curing is conducted, compression molding forming is conducted after pre-heating is conducted so that a cBN abrasive disc prefabricated block can be obtained, and then the ceramic cBN abrasive disc is obtained through microwave sintering. Compared with a high-temperature sintering method where traditional dry method mixed material compression molding forming is adopted, uniformity of raw material mixing can be obviously improved, stable pre-forming can be easily achieved, production programs are simple, production cost is reduced, and the method for preparing the cBN ceramic abrasive disc is capable of saving energy and efficient and can bring remarkable economic benefits and social benefits.
Description
Technical field
The invention belongs to superhard material preparing technical field, be specifically related to a kind of method that adopts wet chemical method moulding microwave sintering to prepare ceramic cBN emery wheel.
Background technology
Diamond is known the hardest material in the world up to now, and the hardness of cubic boron nitride is only second to diamond, and diamond and cubic boron nitride are referred to as superhard material.Superhard material is widely used in abrasive material, grinding tool and cutter material, and diamond high temperature is easily oxidized, particularly good with iron family element compatibility, is not suitable for the processing of iron family element ferrous metal.Cubic boron nitride (cBN) is compared and is had exclusive advantage with diamond, as high thermal stability, with iron family element chemical inertness.The main performance of cubic boron nitride is as follows: the microhardness of cBN is only second to diamond; The heat endurance of cBN is better than diamond, at high temperature still can keep sufficiently high mechanical property and hardness, has good red hardness; CBN Stability Analysis of Structures, have high oxidation resistance, chemical stability is good, compares with diamond, its special salient point be cBN at the temperature up to 1100～1300 ℃ also not with iron family element chemically reactive, so cBN is particularly suitable for processing ferrous metal; The thermal conductivity ratio diamond of cBN is little, but higher than carbide alloy, has good thermal conductivity; Bending strength is high; As grinding tool material, long service life, wearability are good.
So far, oarse-grained cBN single crystal preparation technology does not still break through.Short grained cBN monocrystalline is mainly as grinding tool material.CBN grinding tool is that the effect by means of bonding agent is bonded to cBN abrasive particle in the goods with certain geometrical shape, cBN grinding tool is as a kind of superhard material grinding tool, can be for the processing of iron, also can be for the processing of nonmetallic materials, range of application is wider than diamond abrasive tool, it is the super-hard abrasive tool that a class is had many uses, for high-speed and high-efficiency grinding and honing processing, can make grinding efficiency greatly improve, its grinding accuracy is high, wheel life is long, and grinding performance is good, has saved emery wheel and has changed many non-cutting times such as finishing, lathe adjustment and workpiece sensing.
The principal item of cBN grinding tool is emery wheel, the preparation method of general cBN vitrified abrasive is dry-press process, first vitrified bond is mixed to rear cold moudling with cBN abrasive material, the demoulding, high-temperature firing, machining and shaping is removed the unnecessary part in surface, obtains vitrified abrasive.The patent documentation of relevant cBN vitrified abrasive is a lot, as Chinese patent (CN101602188B, CN101353258B, CN102009391B).China's publication (CN103537993A), points out due to cold moudling, vitrified bond and abrasive material are not very fixing, and the demoulding easily causes emery wheel distortion or fracture damage, and yield rate is low.Chinese patent (CN102009393B) discloses a kind of high-speed grinding cBN grinding wheel preparation method, after various raw materials need to being mixed, through operations such as high temperature sintering, sub-cooled, fragmentation, oven dry, ball milling sieve, production process complexity, repetition are through high temperature melting sintering, energy consumption is large, cost is high, and properties of product are unstable.Generally, adopt conventional dry moulding to prepare cBN vitrified abrasive, there is following weak point, as: energy consumption is high, and operating process is many, complex procedures, and yield rate is low, and manufacturing cost is high.
Summary of the invention
The object of this invention is to provide a kind of method that adopts wet chemical method moulding microwave sintering to prepare ceramic cBN emery wheel, can overcome the defects such as the existing energy consumption of current dry-press process is high, complex procedures.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of method that adopts wet chemical method moulding microwave sintering to prepare ceramic cBN emery wheel, first prepare sial zirconium composite sol solution, after colloidal sol slaking, add abrasive material, sintering aid, reinforcing material, sintering pore former to prepare gel compound, preheat and process rear compression molding acquisition cBN emery wheel prefabricated section, microwave sintering obtains ceramic cBN emery wheel afterwards.
During preparation sial zirconium composite sol solution, by aluminum source compound, silicon-containing compound, zirconium-containing compound and catalyst being reacted in aqueous medium to acquisition, reaction temperature is 50～80 ℃.
Described aluminum source compound is selected from one or more the mixture in aluminium powder, aluminium isopropoxide, aluminum nitrate and aluminium chloride, and silicon-containing compound is ethyl orthosilicate, and described zirconium-containing compound is basic zirconium chloride, and catalyst is hydrochloric acid or acetic acid.
In aluminum source compound, silicon-containing compound, zirconium-containing compound three's quality summation, aluminum source compound accounts for 50～60%, and ethyl orthosilicate accounts for 35～40%, and surplus is basic zirconium chloride; The consumption of catalyst is for regulating pH value to 2～3.
Described sintering pore former is preferably the dewatered sludge that moisture content is less than 40%.
Described abrasive material is preferably cBN and diamond, and sintering aid is Graphene, and reinforcing material is chopped carbon fiber and short glass fiber.
Following material total amount is according to 100 parts of meters, and the mass parts adding is respectively 60～80 parts, cBN abrasive material, 5～16 parts of diamond abrasives, and 1～3 part of Graphene, 3～6 parts of chopped carbon fibers, 5～12 parts of short glass fibers, surplus is dewatered sludge.
Wherein, the length of chopped carbon fiber is 5～30mm, and short glass fiber length is 5～30mm.
The condition that preheats processing is 350～450 ℃ of temperature, 2～5 hours time.
800～1200 ℃ of microwave sintering temperature, sintered heat insulating time 20～40min.
Microwave power 20KW, microwave frequency 915 ± 50MHz.
The inventive method concrete steps are as follows:
1) aluminum source compound, silicon-containing compound, zirconium-containing compound and catalyst are reacted in aqueous medium and obtain transparent sial zirconium composite colloidal sol;
2) colloidal sol slaking step 1) being obtained, add cBN abrasive material, diamond abrasive, Graphene, chopped carbon fiber, short glass fiber, dewatered sludge, through being fully uniformly mixed, evaporation, obtain gel compound, preheat processing, the compressing cBN emery wheel prefabricated section that obtains of mold pressing;
3) step 2) emery wheel prefabricated section, adopt microwave to carry out heat-agglomerating, after microwave sintering, adopt nature cooling, through shaping processing, process and obtain cBN vitrified abrasive.
The multiple deficiency existing in order to overcome dry-press process, the invention provides a kind of method of wet chemistry moulding, in collosol and gel chemical reaction process, add cBN abrasive material, chopped carbon fiber, microwave sintering auxiliary agent Graphene that thermal conductivity is good, add pretreated dewatered sludge, after collosol and gel, through the pre-heat treatment, compression molding, adopt again Microwave Sintering Techniques, finally obtain light weight, hardness is high, thermal conductivity good, intensity is high and wearability is good cBN emery wheel sintered body, emery wheel product is processed in shaping.
Wherein, adopt wet chemical method synthesize ceramic grinding wheel bond, sol-gal process is prepared colloidal sol, and collosol stability, good fluidity are easy to infiltrate abrasive material and various filler, and the hold to abrasive material after abrasive wheel forming is strong, is suitable for regrinding application.In sol-gal process chemical reaction process, also add dewatered sludge to be used as high temperature sintering pore former.Because dehydrated sludge contains a large amount of organic matters, high temperature sintering pore-creating character is good, and after these organic matters burn, remaining inorganic matter main component is also to take silica as main aluminium oxide and the mixture of silica, the just main component of cBN vitrified abrasive bonding agent.Colloidal sol forms aluminium oxide, silica, zirconia blend after microwave high-temperature sintering, the main component of the bonding agent often using during the pre-compression molding of dry-press process emery wheel just.In addition, colloidal sol after high temperature sintering during dry method batch mixing chopped strand be difficult to evenly mix, wet moulding batch mixing is more even, the enhancing chopped carbon fiber especially adding and glass fibre are more easily evenly distributed in emery wheel, strengthen successful.Meanwhile, adopt microwave sintering, replace conventional heating by electric cooker, sintering time is short, little to the fire damage of abrasive material.Utilize the basic structure coupling of microwave special wave band and material-to-be-heated object and produce heat, microwave energy is converted into kinetic energy and the heat energy of molecule, the dielectric loss of material makes material monolithic heating, thereby there is homogeneous heating, and programming rate is fast, and the efficiency of heating surface is high, temperature retention time is short, many advantages such as energy consumption is low, simple to operate, and cost is low.
Compared with prior art, tool has the following advantages in the present invention:
The present invention compares with adopting conventional dry batch mixing compression molding high-temperature sintering process, can obviously improve the uniformity that raw material mixes, be easy to stablize preformed, production routine is simple, reduced production cost, be a kind of method of preparing cBN vitrified abrasive of efficient energy-saving, can bring significant economic benefit and social benefit.
The specific embodiment
With specific embodiment, technical scheme of the present invention is described below, but protection scope of the present invention is not limited to this:
Embodiment 1
Metering takes 3 moles of aluminum nitrates, 3 moles of aluminium isopropoxides, and 2 moles of ethyl orthosilicates, add 124 moles, water, and adding catalyst hydrochloric acid to adjust pH value is 2.8,65 ± 2
ounder the temperature conditions of C, react, polymerization obtains transparent colloidal sol; Colloidal sol is concentrated through ageing, then adds the following material after purified treatment: according to mass percent meter, cBN 60%, diadust 10%, Graphene 2%, chopped carbon fiber 5%, short glass fiber 7%, dewatered sludge 16%.Through being fully uniformly mixed, evaporation, obtain gel compound, at 350 ± 5 ℃, preheat 4 hours, mold pressing compressing cBN emery wheel prefabricated section.Compressing prefabricated section is by adopting microwave to carry out heat-agglomerating, microwave power 20KW; Microwave frequency 915 ± 50MHz; Far infrared temperature measurement, 1050 ± 20 ℃ of microwave sintering temperature; Sintered heat insulating time 36min.After microwave sintering, adopt nature cooling, through shaping processing, process and obtain cBN vitrified abrasive.
After tested, emery wheel sample microhardness is HV3500, and impact flexibility is 456 times, and three-point bending method test bending strength is 787 ± 56 MPa, and adopting standard JB/T3235-1999 wear tested ratio is 76220 ± 180.
Embodiment 2
Metering takes 3 moles of aluminum nitrates, 2 moles of basic zirconium chlorides, and 2 moles of ethyl orthosilicates, add 124 moles, water, and adding catalyst hydrochloric acid to adjust pH value is 2.8,65 ± 2
ounder the temperature conditions of C, react, polymerization obtains transparent colloidal sol; Colloidal sol is concentrated through ageing, then add the following material after purified treatment: according to mass percent meter, cBN 61.5%, diadust 13%, Graphene 2.5%, chopped carbon fiber 5%, short glass fiber 7%, dewatered sludge 11%, through being fully uniformly mixed, evaporation, obtain gel compound, at 350 ± 5 ℃, preheat 4 hours, mold pressing compressing cBN emery wheel prefabricated section.Compressing prefabricated section is by adopting microwave to carry out heat-agglomerating, microwave power 20KW; Microwave frequency 915 ± 50MHz; Far infrared temperature measurement, 1000 ± 20 ℃ of microwave sintering temperature; Sintered heat insulating time 40min.After microwave sintering, adopt nature cooling, through shaping processing, process and obtain cBN vitrified abrasive.
After tested, emery wheel sample microhardness is HV3429, and impact flexibility is 490 times, and three-point bending method test bending strength is 881 ± 71 MPa, and adopting standard JB/T3235-1999 wear tested ratio is 66205 ± 210.
Embodiment 3
Metering takes 3 moles of aluminum nitrates, 2 moles of basic zirconium chlorides, and 2 moles of ethyl orthosilicates, add 124 moles, water, and adding catalyst hydrochloric acid to adjust pH value is 2.8,65 ± 2
ounder the temperature conditions of C, react, polymerization obtains transparent colloidal sol; Colloidal sol is concentrated through ageing, then adds the following material after purified treatment: according to mass percent meter, and cBN66%, diadust 14%, Graphene 2%, chopped carbon fiber 4%, short glass fiber 8%, dewatered sludge 6%.Through being fully uniformly mixed, evaporation, obtain gel compound, at 4200 ± 5 ℃, preheat 3 hours, mold pressing compressing cBN emery wheel prefabricated section.Compressing prefabricated section is by adopting microwave to carry out heat-agglomerating, microwave power 20KW; Microwave frequency 915 ± 50MHz; Far infrared temperature measurement, 1000 ± 20 ℃ of microwave sintering temperature; Sintered heat insulating time 40min.After microwave sintering, adopt nature cooling, through shaping processing, process and obtain cBN vitrified abrasive.
After tested, emery wheel sample microhardness is HV4150, and impact flexibility is 437 times, and three-point bending method test bending strength is 723 ± 50 MPa, and adopting standard JB/T3235-1999 wear tested ratio is 77210 ± 190.
Embodiment 4
Metering takes 3 moles of aluminum nitrates, 2 moles of basic zirconium chlorides, and 2 moles of ethyl orthosilicates, add 124 moles, water, and adding catalyst hydrochloric acid to adjust pH value is 2.8,65 ± 2
ounder the temperature conditions of C, react, polymerization obtains transparent colloidal sol; Colloidal sol is concentrated through ageing, then add the following material after purified treatment: according to mass percent meter, cBN 70%, diadust 15%, Graphene 1%, chopped carbon fiber 4%, short glass fiber 9%, dewatered sludge 1%, through being fully uniformly mixed, evaporation, obtain gel compound, at 380 ± 5 ℃, preheat 4 hours, mold pressing compressing cBN emery wheel prefabricated section.Compressing prefabricated section is by adopting microwave to carry out heat-agglomerating, microwave power 20KW; Microwave frequency 915 ± 50MHz; Far infrared temperature measurement, 1000 ± 20 ℃ of microwave sintering temperature; Sintered heat insulating time 40min.After microwave sintering, adopt nature cooling, through shaping processing, process and obtain cBN vitrified abrasive.
After tested, emery wheel sample microhardness is HV3890, and impact flexibility is 651 times, and three-point bending method test bending strength is 812 ± 54 MPa, and adopting standard JB/T3235-1999 wear tested ratio is 71110 ± 185.
Embodiment 5
Metering takes 3 moles of aluminum nitrates, 2 moles of basic zirconium chlorides, and 2 moles of ethyl orthosilicates, add 124 moles, water, and adding catalyst hydrochloric acid to adjust pH value is 2.8,65 ± 2
ounder the temperature conditions of C, react, polymerization obtains transparent colloidal sol; Colloidal sol is concentrated through ageing, then add the following material after purified treatment: according to mass percent meter, cBN 75%, diadust 8%, Graphene 2%, chopped carbon fiber 5%, short glass fiber 5%, dewatered sludge 5%, through being fully uniformly mixed, evaporation, obtain gel compound, at 390 ± 5 ℃, preheat 4 hours, mold pressing compressing cBN emery wheel prefabricated section.Compressing prefabricated section is by adopting microwave to carry out heat-agglomerating, microwave power 20KW; Microwave frequency 915 ± 50MHz; Far infrared temperature measurement, 1100 ± 20 ℃ of microwave sintering temperature; Sintered heat insulating time 30min.After microwave sintering, adopt nature cooling, through shaping processing, process and obtain cBN vitrified abrasive.
After tested, emery wheel sample microhardness is HV3188, and impact flexibility is 651 times, and three-point bending method test bending strength is 682 ± 51MPa, and adopting standard JB/T3235-1999 wear tested ratio is 67227 ± 189.
Comparative example 1
Metering takes 3 moles of aluminum nitrates, 2 moles of basic zirconium chlorides, and 2 moles of ethyl orthosilicates, add 124 moles, water, and adding catalyst hydrochloric acid to adjust pH value is 2.8,65 ± 2
ounder the temperature conditions of C, react, polymerization obtains transparent colloidal sol; Colloidal sol is concentrated through ageing, then add the following material after purified treatment: according to mass percent meter, cBN 70%, diadust 10%, Graphene 2%, chopped carbon fiber 5%, short glass fiber 7%, dewatered sludge 6%, through being fully uniformly mixed, evaporation, obtain gel compound, at 350 ± 5 ℃, preheat 4 hours, mold pressing compressing cBN emery wheel prefabricated section.Compressing prefabricated section adopts Muffle furnace to carry out heat-agglomerating, 1000 ± 20 ℃ of sintering temperatures; Sintered heat insulating time 120min.After high temperature sintering, adopt nature cooling, through shaping processing, process and obtain cBN vitrified abrasive.
After tested, emery wheel sample microhardness is HV3266, and impact flexibility is 451 times, and three-point bending method test bending strength is 667 ± 53 MPa, and adopting standard JB/T3235-1999 wear tested ratio is 42206 ± 220.
Claims (10)
1. a method that adopts wet chemical method moulding microwave sintering to prepare ceramic cBN emery wheel, it is characterized in that, first prepare sial zirconium composite sol solution, after colloidal sol slaking, add abrasive material, sintering aid, reinforcing material, sintering pore former to prepare gel compound, preheat and process rear compression molding acquisition cBN emery wheel prefabricated section, microwave sintering obtains ceramic cBN emery wheel afterwards.
2. employing wet chemical method moulding microwave sintering as claimed in claim 1 is prepared the method for ceramic cBN emery wheel, it is characterized in that, described sintering pore former is the dewatered sludge that moisture content is less than 40%.
3. employing wet chemical method moulding microwave sintering as claimed in claim 2 is prepared the method for ceramic cBN emery wheel, it is characterized in that, described abrasive material is cBN and diamond, and sintering aid is Graphene, and reinforcing material is chopped carbon fiber and short glass fiber.
4. employing wet chemical method moulding microwave sintering as claimed in claim 3 is prepared the method for ceramic cBN emery wheel, it is characterized in that, following material total amount is according to 100 parts of meters, the mass parts adding is respectively 60～80 parts, cBN abrasive material, 5～16 parts of diamond abrasives, 1～3 part of Graphene, 3～6 parts of chopped carbon fibers, 5～12 parts of short glass fibers, surplus is dewatered sludge.
5. employing wet chemical method moulding microwave sintering as claimed in claim 4 is prepared the method for ceramic cBN emery wheel, it is characterized in that, the length of chopped carbon fiber is 5～30mm, and short glass fiber length is 5～30mm.
6. employing wet chemical method moulding microwave sintering as claimed in claim 3 is prepared the method for ceramic cBN emery wheel, it is characterized in that, the condition that preheats processing is 350～450 ℃ of temperature, 2～5 hours time.
7. employing wet chemical method moulding microwave sintering as claimed in claim 3 is prepared the method for ceramic cBN emery wheel, it is characterized in that 800～1200 ℃ of microwave sintering temperature, sintered heat insulating time 20～40min.
8. employing wet chemical method moulding microwave sintering as claimed in claim 7 is prepared the method for ceramic cBN emery wheel, it is characterized in that microwave power 20KW, microwave frequency 915 ± 50MHz.
9. employing wet chemical method moulding microwave sintering as claimed in claim 3 is prepared the method for ceramic cBN emery wheel, it is characterized in that, during preparation sial zirconium composite sol solution, by aluminum source compound, silicon-containing compound, zirconium-containing compound and catalyst being reacted in aqueous medium to acquisition, reaction temperature is 50～80 ℃.
10. employing wet chemical method moulding microwave sintering as claimed in claim 9 is prepared the method for ceramic cBN emery wheel, it is characterized in that, described aluminum source compound is selected from one or more the mixture in aluminium powder, aluminium isopropoxide, aluminum nitrate and aluminium chloride, silicon-containing compound is ethyl orthosilicate, described zirconium-containing compound is basic zirconium chloride, and catalyst is hydrochloric acid or acetic acid; In aluminum source compound, silicon-containing compound, zirconium-containing compound three's quality summation, aluminum source compound accounts for 50～60%, and ethyl orthosilicate accounts for 35～40%, and surplus is basic zirconium chloride; The consumption of catalyst is for regulating pH value to 2～3.
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| CN105583742A (en) * | 2016-02-03 | 2016-05-18 | 浙江工业大学 | Production method of fixed abrasive particle grinding disc |
| CN106425897A (en) * | 2016-08-30 | 2017-02-22 | 湖北东方玉扬电子科技有限公司 | Polishing piece for brake pad grinder and preparation method for polishing piece |
| CN106994652A (en) * | 2016-01-25 | 2017-08-01 | 江苏华东砂轮有限公司 | Fibre reinforced high porosity ceramic bonding agent CBN grinding wheel preparation methods |
| CN108321260A (en) * | 2017-12-30 | 2018-07-24 | 苏州赛尔科技有限公司 | Led epitaxial wafer grinding wheel and preparation method thereof |
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| CN106994652A (en) * | 2016-01-25 | 2017-08-01 | 江苏华东砂轮有限公司 | Fibre reinforced high porosity ceramic bonding agent CBN grinding wheel preparation methods |
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| CN108321260A (en) * | 2017-12-30 | 2018-07-24 | 苏州赛尔科技有限公司 | Led epitaxial wafer grinding wheel and preparation method thereof |
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