CN108276003A - A method of preparing boron carbide complex phase ceramic using sapphire grinding dead meal - Google Patents
A method of preparing boron carbide complex phase ceramic using sapphire grinding dead meal Download PDFInfo
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- CN108276003A CN108276003A CN201810150135.4A CN201810150135A CN108276003A CN 108276003 A CN108276003 A CN 108276003A CN 201810150135 A CN201810150135 A CN 201810150135A CN 108276003 A CN108276003 A CN 108276003A
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- boron carbide
- dead meal
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/563—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on boron carbide
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62695—Granulation or pelletising
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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Abstract
The present invention relates to a kind of methods preparing boron carbide complex phase ceramic using sapphire grinding dead meal, belong to boron carbide ceramics technical field.The designed method for preparing boron carbide complex phase ceramic using sapphire grinding dead meal of the present invention; this method is raw material using the dead meal that sapphire grinding and polishing process generates; B4C complex phase ceramics are prepared in conjunction with normal atmosphere sintering method; this method cost is relatively low, environmentally protective, and can be with large-scale production.Using grinding and polishing sapphire dead meal as ceramic product raw material, production cost can be not only reduced, but also environmental pollution can be reduced, there are significant economic results in society.In addition, the method and process for preparing boron carbide complex phase ceramic using sapphire grinding dead meal is simple, cost is relatively low, it can be achieved that industrialization large-scale production, is suitble to promote the use of.
Description
Technical field
The present invention relates to a kind of methods preparing boron carbide complex phase ceramic using sapphire grinding dead meal, belong to boron carbide
Ceramic field.
Background technology
B4C is the high hard material for being only second to diamond and cubic boron nitride, has low-density, high-modulus and excellent high temperature
Performance, fine and close B4C ceramics then mainly apply its superior mechanical performance to be used as mechanical part and Protective armor.Additionally, due to B element
With very high neutron absorption cross-section, B4C can be as nuclear reactor deceleration component or the radiation protection component of nuclear reactor.B4C
It is the very strong compound of covalent bond, covalent bond is close to 94%, and B4The plasticity of C is poor, and crystal boundary moving resistance is very big, table when solid-state
Face tension very little, these intrinsic characteristics determine B4C is a kind of ceramic material of extremely difficult sintering, sintering temperature under usual conditions
It is higher, therefore manufacturing cost is high, affects B also more seriously4C ceramics low-coat scale preparations and engineering are answered
With.In order to reduce B4The sintering temperature of C ceramics, and its sintered density and performance are not influenced, generally use hot pressing sintering method
And lqiuid phase sintering method.Hot pressing sintering method refers to that certain pressure is loaded in sintering process, promotes B4C sintering densifications.But
Hot pressing sintering method low output, it is of high cost, it is difficult to obtain the product of complicated shape while can not large-scale production.Lqiuid phase sintering method is
Refer in B4Appropriate Y is added in C2O3、Al2O3、La2O3Equal low melting point rare earths mixture, forms eutectic point, in sintering process,
Partial Liquid Phase is generated come acceleration of sintering using low melting point.Lqiuid phase sintering method generally in atmospheric conditions, can prepare complexity
The ceramic product of shape and can be with large-scale production.
In sapphire（Main component Al2O3）Grinding and polishing in, need to use a large amount of abrasive media powder, it is main
Ingredient is B4C.After sapphire grinding and polishing, this kind of powder will certainly introduce a large amount of Al2O3Impurity, thus it is discarded as grinding
Material, but these dead meals can be used as ceramic raw material, and Al2O3B can be used as4One of C ceramic post sintering auxiliary agents, no
It needs that such sintering aid is additionally added.Using grinding and polishing dead meal as ceramic product raw material, it can not only reduce and be produced into
This, and environmental pollution cost can be reduced, significant economic results in society can be generated.
Invention content
The present invention is raw material using the dead meal that sapphire grinding and polishing process generates, and is prepared in conjunction with normal atmosphere sintering method
B4C complex phase ceramics, this method cost is relatively low, environmentally protective, and can be with large-scale production.The technical solution adopted in the present invention
It is：A method of boron carbide complex phase ceramic being prepared using sapphire grinding dead meal, wherein sapphire grinds dead meal ingredient
Include boron carbide, further includes one or more in aluminium oxide, silicon carbide and graphite, profit in sapphire grinding dead meal ingredient
Included the following steps with the method that sapphire grinding dead meal prepares boron carbide complex phase ceramic：
（1）Raw material cleans, and sapphire grinding dead meal powder is impregnated 10 hours or more with dilute hydrochloric acid solution and removes ferrous contaminants；
Then it is rinsed 5 minutes or more with clear water, filter and dries or dry that obtain material powder within 1 hour standby in 105 DEG C of baking oven
With；
（2）Raw material weighing uses step（1）The material powder and phenolic resin of preparation are by weight 100:5~30 ratio weighs
It is good；
（3）Slurry is prepared, using water or alcohol as solvent, by the mixture of load weighted material powder and phenolic resin in step 2
It is 40~60wt% to be made into solid content（Weight percent）Slurry, with B4Slurry is uniformly mixed by C balls as mill ball；
（4）Prepared by powder, by step（3）In prepared slurry drying, crushing, sieving, or through powder made from mist projection granulating
Body, wherein the average grain diameter of control mist projection granulating is less than 100 microns；
（5）Unsticking is sintered, by step（4）In powder obtained after dry-pressing and/or isostatic pressing, through unsticking, then in argon
It is sintered under gas atmosphere protection, that is, prepares boron carbide complex phase ceramic.
The preferred step（1）The grain size of middle material powder is 0.1~5 micron.
The preferred step（2）The Residual carbon of middle phenolic resin is 10~60wt%（Weight percent）.
The preferred step（3）In mill ball B4C ball dosages are 1~5 times of material powder weight, the mixing of slurry
Time is 24 hours.
The preferred step（4）Middle drying temperature is 60~80 DEG C, and sieving process selects the sieve of 100 mesh.
The preferred step（4）The outlet temperature of middle mist projection granulating is 60~80 DEG C.
The preferred step（5）Middle dry-pressing pressure is 20 ~ 100 megapascal, and hydrostatic pressure is 150 ~ 300 megapascal.
The preferred step（5）Middle sintering temperature is 2200-2300 DEG C, and the sintered heat insulating time is 30-90 minutes.
The present invention devises a kind of method preparing boron carbide complex phase ceramic using sapphire grinding dead meal, this method profit
The dead meal generated with sapphire grinding and polishing process is raw material, and B is prepared in conjunction with normal atmosphere sintering method4C complex phase ceramics, this method
Cost is relatively low, environmentally protective, and can be with large-scale production.Using grinding and polishing sapphire dead meal as ceramic product raw material,
Production cost can be not only reduced, but also environmental pollution can be reduced, there are significant economic results in society.In addition, the utilization
The method and process that sapphire grinding dead meal prepares boron carbide complex phase ceramic is simple, and cost is relatively low, it can be achieved that industrialization is extensive
Production, is suitble to promote the use of.
Specific implementation mode
Specific embodiment one, a method of boron carbide complex phase ceramic being prepared using sapphire grinding dead meal, wherein blue
Gem grinding dead meal ingredient includes boron carbide 88%（Weight percent）With aluminium oxide 12%（Weight percent）, utilize blue treasured
The method that stone grinding dead meal prepares boron carbide complex phase ceramic includes the following steps：
（1）Raw material cleans, and sapphire grinding dead meal powder dilute hydrochloric acid solution is impregnated 11 hours, ferrous contaminants are removed；It connects
It and is rinsed 6 minutes with clear water, filtered and dry to obtain material powder and is spare；
（2）Raw material weighing weighs step（1）100 grams of the material powder of preparation weighs 5 grams of phenolic resin；
（3）Slurry is prepared, using water as solvent, the mixture of load weighted material powder and phenolic resin in step 2 is made into solid
Content is 45wt%（Weight percent）Slurry, with B4Slurry is uniformly mixed by C balls as mill ball；
（4）Prepared by powder, by step（3）In prepared slurry drying, crushing, sieving；
（5）Unsticking is sintered, by step（4）In powder obtained after dry-pressing formed, through unsticking, then argon gas atmosphere protection under
Sintering, that is, prepare boron carbide complex phase ceramic, and obtained boron carbide complex phase ceramic density is 2.49gcm-3, bending strength is
320MPa, hardness 26.7GPa.
The step（1）The grain size of middle material powder is 0.1~5 micron, the step（2）The Residual carbon of middle phenolic resin
For 10~30wt%（Weight percent）, the step（3）In mill ball B4C ball dosages are 450 grams, the incorporation time of slurry
It is 24 hours, the step（4）Middle drying temperature is 70 DEG C, and sieving process selects the sieve of 100 mesh, the step（5）In do
Pressure pressure is 25 megapascal, and hydrostatic pressure is 150 megapascal, the step（5）Middle sintering temperature is 2200 DEG C, the sintered heat insulating
Time is 90 minutes.
Specific embodiment two, a method of boron carbide complex phase ceramic being prepared using sapphire grinding dead meal, wherein blue
Gem grinding dead meal ingredient includes boron carbide 76.8%（Weight percent）, aluminium oxide 21.2%（Weight percent）And graphite
2%（Weight percent）, included the following steps using the method that sapphire grinding dead meal prepares boron carbide complex phase ceramic：
（1）Raw material cleans, and sapphire grinding dead meal powder is impregnated 12 hours with dilute hydrochloric acid solution and removes ferrous contaminants；Then
It is rinsed 10 minutes with clear water, dries that obtain material powder within 1 hour spare in 105 DEG C of baking oven；
（2）Raw material weighing weighs step（1）100 grams of the material powder of preparation weighs 10 grams of phenolic resin；
（3）Slurry is prepared to be made into the mixture of load weighted material powder and phenolic resin in step 2 using alcohol as solvent
Solid content is 60wt%（Weight percent）Slurry, with B4Slurry is uniformly mixed by C balls as mill ball；
（4）Prepared by powder, by step（3）In prepared slurry through powder made from mist projection granulating, wherein controlling mist projection granulating
Average grain diameter be less than 100 microns；
（5）Unsticking is sintered, by step（4）In powder obtained after dry-pressing and isostatic pressing, through unsticking, then in argon gas gas
The lower sintering of atmosphere protection, that is, prepare boron carbide complex phase ceramic, obtained boron carbide complex phase ceramic density is 2.62gcm-3, bending resistance is strong
Degree is 330MPa, hardness 24.6GPa.
The step（1）The grain size of middle material powder is 1~5 micron, the step（2）The Residual carbon of middle phenolic resin is
10~60wt%（Weight percent）, the step（3）In mill ball B4C ball dosages are 350 grams, and the incorporation time of slurry is
24 hours, the step（4）The outlet temperature of middle mist projection granulating is 65 DEG C, the step（5）Middle dry-pressing pressure is 50 megapascal, etc.
Static pressure pressure is 200 megapascal, the step（5）Middle sintering temperature is 2250 DEG C, and the sintered heat insulating time is 60 minutes.
Specific embodiment three, a method of boron carbide complex phase ceramic being prepared using sapphire grinding dead meal, wherein blue
Gem grinding dead meal ingredient includes boron carbide 32%（Weight percent）, aluminium oxide 14%（Weight percent）And silicon carbide
54%（Weight percent）, included the following steps using the method that sapphire grinding dead meal prepares boron carbide complex phase ceramic：
（1）Raw material cleans, and sapphire grinding dead meal powder is impregnated 12 hours with dilute hydrochloric acid solution and removes ferrous contaminants；Then
It is rinsed 8 minutes with clear water, dries that obtain material powder within 1 hour spare in 105 DEG C of baking oven；
（2）Raw material weighing weighs step（1）100 grams of the material powder of preparation weighs 10 grams of phenolic resin；
（3）Slurry is prepared to be made into the mixture of load weighted material powder and phenolic resin in step 2 using alcohol as solvent
Solid content is 60wt%（Weight percent）Slurry, with B4Slurry is uniformly mixed by C balls as mill ball；
（4）Prepared by powder, by step（3）In prepared slurry through powder made from mist projection granulating, wherein controlling mist projection granulating
Average grain diameter be less than 100 microns；
（5）Unsticking is sintered, by step（4）In powder obtained after dry-pressing and isostatic pressing, through unsticking, then in argon gas gas
The lower sintering of atmosphere protection, that is, prepare boron carbide complex phase ceramic, obtained boron carbide complex phase ceramic density is 2.88gcm-3, bending resistance is strong
Degree is 350MPa, hardness 25.4GPa.
The step（1）The grain size of middle material powder is 2~4 microns, the step（2）The Residual carbon of middle phenolic resin is
30~60wt%（Weight percent）, the step（3）In mill ball B4C ball dosages are 450 grams, and the incorporation time of slurry is
24 hours, the step（4）The outlet temperature of middle mist projection granulating is 65 DEG C, the step（5）Middle dry-pressing pressure is 50 megapascal, etc.
Static pressure pressure is 200 megapascal, the step（5）Middle sintering temperature is 2250 DEG C, and the sintered heat insulating time is 60 minutes.
The present invention devises a kind of method preparing boron carbide complex phase ceramic using sapphire grinding dead meal, this method profit
The dead meal generated with sapphire grinding and polishing process is raw material, and B4C complex phase ceramics, this method are prepared in conjunction with normal atmosphere sintering method
Cost is relatively low, environmentally protective, and can be with large-scale production.Using grinding and polishing sapphire dead meal as ceramic product raw material,
Production cost can be not only reduced, but also environmental pollution can be reduced, there are significant economic results in society.In addition, the utilization
The method and process that sapphire grinding dead meal prepares boron carbide complex phase ceramic is simple, and cost is relatively low, it can be achieved that industrialization is extensive
Production, is suitble to promote the use of.
The present invention devises a kind of method preparing boron carbide complex phase ceramic using sapphire grinding dead meal, this method profit
The dead meal generated with sapphire grinding and polishing process is raw material, and B4C complex phase ceramics, this method are prepared in conjunction with normal atmosphere sintering method
Cost is relatively low, environmentally protective, and can be with large-scale production.Using grinding and polishing sapphire dead meal as ceramic product raw material,
Production cost can be not only reduced, but also environmental pollution can be reduced, there are significant economic results in society.In addition, the utilization
The method and process that sapphire grinding dead meal prepares boron carbide complex phase ceramic is simple, and cost is relatively low, it can be achieved that industrialization is extensive
Production, is suitble to promote the use of.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (8)
1. a kind of using the sapphire grinding dead meal method for preparing boron carbide complex phase ceramic, wherein sapphire grinding dead meal at
Point include boron carbide, sapphire grind in dead meal ingredient further include it is one or more in aluminium oxide, silicon carbide and graphite,
Included the following steps using the method that sapphire grinding dead meal prepares boron carbide complex phase ceramic：
（1）Raw material cleans, and sapphire grinding dead meal powder is impregnated 10 hours or more with dilute hydrochloric acid solution and removes ferrous contaminants；
Then it is rinsed 5 minutes or more with clear water, filter and dries or dry that obtain material powder within 1 hour standby in 105 DEG C of baking oven
With；
（2）Raw material weighing uses step（1）The material powder and phenolic resin of preparation are by weight 100:5~30 ratio weighs
It is good；
（3）Slurry is prepared, using water or alcohol as solvent, by the mixture of load weighted material powder and phenolic resin in step 2
It is 40~60wt% to be made into solid content（Weight percent）Slurry, with B4Slurry is uniformly mixed by C balls as mill ball；
（4）Prepared by powder, by step（3）In prepared slurry drying, crushing, sieving, or through powder made from mist projection granulating
Body, wherein the average grain diameter of control mist projection granulating is less than 100 microns；
（5）Unsticking is sintered, by step（4）In powder obtained after dry-pressing and/or isostatic pressing, through unsticking, then in argon
It is sintered under gas atmosphere protection, that is, prepares boron carbide complex phase ceramic.
2. a kind of method preparing boron carbide complex phase ceramic using sapphire grinding dead meal according to claim 1,
It is characterized in that, the step（1）The grain size of middle material powder is 0.1~5 micron.
3. a kind of method preparing boron carbide complex phase ceramic using sapphire grinding dead meal according to claim 1,
It is characterized in that, the step（2）The Residual carbon of middle phenolic resin is 10~60wt%（Weight percent）.
4. a kind of method preparing boron carbide complex phase ceramic using sapphire grinding dead meal according to claim 1,
It is characterized in that, the step（3）In mill ball B4C ball dosages are 1~5 times of material powder weight, the incorporation time of slurry
It is 24 hours.
5. a kind of method preparing boron carbide complex phase ceramic using sapphire grinding dead meal according to claim 1,
It is characterized in that, the step（4）Middle drying temperature is 60~80 DEG C, and sieving process selects the sieve of 100 mesh.
6. a kind of method preparing boron carbide complex phase ceramic using sapphire grinding dead meal according to claim 1,
It is characterized in that, the step（4）The outlet temperature of middle mist projection granulating is 60~80 DEG C.
7. a kind of method preparing boron carbide complex phase ceramic using sapphire grinding dead meal according to claim 1,
It is characterized in that, the step（5）Middle dry-pressing pressure is 20 ~ 100 megapascal, and hydrostatic pressure is 150 ~ 300 megapascal.
8. a kind of method preparing boron carbide complex phase ceramic using sapphire grinding dead meal according to claim 1,
It is characterized in that, the step（5）Middle sintering temperature is 2200-2300 DEG C, and the sintered heat insulating time is 30-90 minutes.
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Cited By (1)
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| CN113024256A (en) * | 2021-03-19 | 2021-06-25 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Production method for preparing boron carbide-silicon carbide composite ceramic by using silicon carbide crystal grinding waste liquid |
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Application publication date: 20180713 |