CN116041063A - Preparation method of diamond boron carbide composite ceramic - Google Patents
Preparation method of diamond boron carbide composite ceramic Download PDFInfo
- Publication number
- CN116041063A CN116041063A CN202211667812.2A CN202211667812A CN116041063A CN 116041063 A CN116041063 A CN 116041063A CN 202211667812 A CN202211667812 A CN 202211667812A CN 116041063 A CN116041063 A CN 116041063A
- Authority
- CN
- China
- Prior art keywords
- diamond
- boron carbide
- carbide composite
- composite ceramic
- powder
- 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.)
- Granted
Links
- 229910052580 B4C Inorganic materials 0.000 title claims abstract description 65
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 57
- 239000010432 diamond Substances 0.000 title claims abstract description 57
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 239000000919 ceramic Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 34
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000005011 phenolic resin Substances 0.000 claims abstract description 20
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000005238 degreasing Methods 0.000 claims abstract description 15
- 230000008014 freezing Effects 0.000 claims abstract description 11
- 238000007710 freezing Methods 0.000 claims abstract description 11
- 238000000465 moulding Methods 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000005271 boronizing Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000007921 spray Substances 0.000 claims abstract description 9
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 7
- 239000010439 graphite Substances 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 7
- 238000005469 granulation Methods 0.000 claims abstract description 3
- 230000003179 granulation Effects 0.000 claims abstract description 3
- 238000007873 sieving Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 23
- 238000003825 pressing Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 abstract description 4
- 239000010703 silicon Substances 0.000 abstract description 4
- 229910010271 silicon carbide Inorganic materials 0.000 abstract description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 4
- 238000013001 point bending Methods 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 238000005507 spraying Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 description 12
- 238000004321 preservation Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 238000005475 siliconizing Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/52—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 carbon, e.g. graphite
- C04B35/528—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 carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—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 carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/52—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 carbon, e.g. graphite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/626—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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3821—Boron carbides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/425—Graphite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/427—Diamond
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Abstract
The invention discloses a preparation method of diamond boron carbide composite ceramic, which comprises the following steps: mixing diamond powder with boron carbide, graphite and absolute ethyl alcohol for phenolic resin uniformly; preparing into particles by adopting a freezing spray granulation mode or a manual crushing and sieving mode; hot press molding; degreasing the pressed blank; and performing boronizing sintering on the obtained porous preform. The diamond-boron carbide composite material prepared by the invention reduces impurities such as silicon carbide, residual silicon and the like possibly generated in a sample, so that the performance of the sample is more excellent; according to the invention, larger-particle diamond is selected for freezing, spraying and granulating, so that phenolic resin is more uniformly wrapped on the surface of the diamond, and the surface of the diamond is carbonized at high temperature, and reacts with boron powder to generate boron carbide in situ, so that the inside of a sample is more compact; the hardness and three-point bending strength of the diamond-boron carbide composite material prepared by the invention are greatly improved, and the diamond-boron carbide composite material is completely suitable for the requirements of bulletproof ceramics.
Description
Technical Field
The invention relates to the technical field of composite ceramics, in particular to a preparation method of diamond boron carbide composite ceramics.
Background
Diamond is currently the most hard material known in the world, while boron carbide (B 4 C) The hardness of the ceramic is only that of the secondary diamond and the cubic boron nitride, is the third hard substance in nature, and has the characteristics of low density, high modulus, high wear resistance and the like. If the combination of diamond and boron carbide can be realized, more ideal armored ceramic can be prepared. In the last 70 th century, the reaction sintering boron carbide ceramic composite material is prepared for the first time in the United states by an infiltration method, so that the preparation cost of the boron carbide material is greatly reduced, and the method is widely focused and researched by students at home and abroad. At the beginning of the 21 st century, the united states, israel and other countries have applied reactive sintering boron carbide materials to the protection field of armored vehicles and military engines, but the research of reactive sintering boron carbide composite materials in China still has a great gap from developed countries, and the application degree is far from reaching. Therefore, the development of the boron carbide material and the high protection and light weight development of the weaponry in China have important practical and theoretical significance. The currently known preparation method of the diamond and boron carbide composite ceramic is that boron carbide powder, diamond, phenolic resin and simple substance silicon powder are adopted to jointly react to generate the diamond and boron carbide composite ceramic. However, by adopting the method, simple substance silicon and silicon carbide are easy to remain in the composite ceramic, and the simple substance silicon and the silicon carbide can greatly reduce the hardness reduction caused by the performance of the diamond and boron carbide composite ceramic.
Disclosure of Invention
Aiming at the defects in the background technology, the invention provides a preparation method of diamond boron carbide composite ceramic, which solves the problem of lower hardness of the diamond and boron carbide composite ceramic in the prior art.
The technical scheme of the invention is realized as follows:
the preparation method of the diamond boron carbide composite ceramic comprises the following steps:
(1) Mixing diamond powder with boron carbide, graphite and absolute ethyl alcohol for phenolic resin uniformly;
(2) Preparing into particles by adopting a freezing spray granulation mode or a manual crushing and sieving mode;
(3) Hot press molding;
(4) Degreasing the pressed blank;
(5) And (3) performing boronizing sintering on the porous preform obtained in the step (4).
Further, the diamond powder has a particle size of more than 50 μm.
Further, the volume percentage of the diamond powder, the boron carbide, the graphite and the phenolic resin is 30-75%:0-45%:5-15%:15-25%.
Further, the purity of the diamond powder and graphite is more than or equal to 99.99 percent.
Further, the diamond powder includes single crystal diamond and polycrystalline diamond.
Further, the hot press molding in the step (3) is performed at a temperature range of: 130-150 ℃; the pressing pressure is 150Mp, and the pressure is maintained for 10-20min.
Further, the degreasing treatment in the step (4) is carried out at the degreasing temperature of 1000-1100 ℃ and the degreasing speed of 1-3 ℃/min; preserving heat at the highest temperature point for 90-120 min.
Further, the boronizing sintering in the step (5) is performed, and the vacuum degree in the boronizing process is between 0.1pa and 320 pa.
Further, in the boronizing process, the heating rate is 8-15 ℃ per minute before the melting temperature of the boron powder is 2200 ℃, and the temperature is kept for 30min at a temperature slightly higher than the melting temperature of the boron powder.
Further, the purity of the boron powder is more than or equal to 99.99 percent.
The invention has the beneficial effects that:
1. compared with a general siliconizing method, the diamond-boron carbide composite material prepared by the invention reduces impurities such as silicon carbide, residual silicon and the like possibly generated in the sample, so that the performance of the sample is more excellent, and particularly the hardness is more outstanding;
2. the diamond-boron carbide composite material prepared by the invention selects larger-particle diamond for freezing, spraying and granulating, so that phenolic resin is more uniformly wrapped on the surface of the diamond, and carbonization is carried out on the surface of the diamond at high temperature, thus boron carbide is generated in situ by reacting with boron powder, the inside of a sample is more compact, and gaps are reduced;
3. the hardness and the three-point bending strength of the finally obtained sample of the diamond-boron carbide composite material prepared by the invention are greatly improved, and the diamond-boron carbide composite material is completely suitable for the requirements of bulletproof ceramics.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without any inventive effort, are intended to be within the scope of the invention.
Example 1
The novel diamond-boron carbide composite ceramic is prepared from the following raw materials in percentage by volume: 50% of diamond powder, 15% of boron carbide, 10% of graphite powder and 25% of phenolic resin.
Weighing the required raw materials according to the proportion, uniformly mixing diamond powder (100 mu m), boron carbide (30 mu m-50 mu m), graphite powder (30 mu m-50 mu m) and absolute ethyl alcohol for phenolic resin, and granulating by adopting freezing spray; then carrying out hot press molding, wherein the pressing temperature is 130 ℃, the pressing pressure is 150Mp, the pressure is maintained for 10min, degreasing treatment is carried out on a pressed sample, the heating rate is 1 ℃/min, the highest temperature is 1100 ℃, and the temperature is kept for 120min; and then carrying out high Wen Shenpeng treatment on the porous preform, wherein the highest temperature is 2200 ℃, the vacuum degree is 10Pa, and the heat preservation is carried out for 30min, so that the required diamond-boron carbide composite ceramic is finally obtained.
Example 2
The novel diamond-boron carbide composite ceramic is prepared from the following raw materials in percentage by volume: 65% of diamond powder, 0% of boron carbide powder, 15% of graphite powder and 25% of phenolic resin.
Weighing the required raw materials according to the proportion, uniformly mixing diamond powder (120 mu m), boron carbide powder (30 mu m-50 mu m), graphite powder (30 mu m-50 mu m) and absolute ethyl alcohol for phenolic resin, and granulating by adopting freezing spray; then carrying out hot press molding, wherein the pressing temperature is 150 ℃, the pressing pressure is 150Mp, the pressure is maintained for 15min, degreasing treatment is carried out on a pressed sample, the heating rate is 3 ℃/min, the highest temperature is 1100 ℃, and the heat is preserved for 100min; and then carrying out high Wen Shenpeng on the porous preform, wherein the highest temperature is 2200 ℃, the vacuum degree is 300Pa, and the heat preservation is carried out for 30min, so that the required diamond-boron carbide composite ceramic is finally obtained.
Example 3
The novel diamond-boron carbide composite ceramic is prepared from the following raw materials in percentage by volume: 40% of diamond powder, 30% of boron carbide powder, 5% of graphite powder and 25% of phenolic resin.
Weighing the required raw materials according to the proportion, uniformly mixing diamond powder (50 mu m), boron carbide powder (30 mu m-50 mu m), graphite powder (30 mu m-50 mu m) and absolute ethyl alcohol for phenolic resin, and granulating by adopting freezing spray; then carrying out hot press molding, wherein the pressing temperature is 130 ℃, the pressing pressure is 150Mp, the pressure is maintained for 10min, degreasing treatment is carried out on a pressed sample, the heating rate is 2 ℃/min, the highest temperature is 1000 ℃, and the temperature is kept for 90min; and then carrying out high Wen Shenpeng on the porous preform, wherein the highest temperature is 2200 ℃, the vacuum degree is 50Pa, and the heat preservation is carried out for 30min, so that the required diamond-boron carbide composite ceramic is finally obtained.
Example 4
The novel diamond-boron carbide composite ceramic is prepared from the following raw materials in percentage by volume: 30% of diamond powder, 45% of boron carbide powder, 5% of graphite powder and 25% of phenolic resin.
Weighing the required raw materials according to the proportion, uniformly mixing diamond powder (100 mu m), boron carbide powder (30 mu m-50 mu m), graphite powder (30 mu m-50 mu m) and absolute ethyl alcohol for phenolic resin, and granulating by adopting freezing spray; then carrying out hot press molding, wherein the pressing temperature is 150 ℃, the pressing pressure is 150Mp, the pressure is maintained for 20min, degreasing treatment is carried out on a pressed sample, the heating rate is 3 ℃/min, the highest temperature is 1000 ℃, and the temperature is kept for 120min; and then carrying out high Wen Shenpeng on the porous preform, wherein the highest temperature is 2200 ℃, the vacuum degree is 3Pa, and the heat preservation is carried out for 30min, thus finally obtaining the required diamond-boron carbide composite ceramic.
Example 5
The novel diamond-boron carbide composite ceramic is prepared from the following raw materials in percentage by volume: 75% of diamond powder, 0% of boron carbide powder, 10% of graphite powder and 15% of phenolic resin.
Weighing the required raw materials according to the proportion, uniformly mixing diamond powder (80 mu m), boron carbide powder (30 mu m-50 mu m), graphite powder (30 mu m-50 mu m) and absolute ethyl alcohol for phenolic resin, and granulating by adopting freezing spray; then carrying out hot press molding, wherein the pressing temperature is 130 ℃, the pressing pressure is 150Mp, the pressure is maintained for 20min, degreasing treatment is carried out on a pressed sample, the heating rate is 1 ℃/min, the highest temperature is 1100 ℃, and the heat preservation is carried out for 90min; and then carrying out high Wen Shenpeng on the porous preform, wherein the highest temperature is 2200 ℃, the vacuum degree is 100Pa, and the heat preservation is carried out for 30min, so that the required diamond-boron carbide composite ceramic is finally obtained.
Comparative example
The diamond-boron carbide composite ceramic is prepared from the following raw materials in percentage by volume: 55% of diamond powder, 20% of boron carbide powder and 25% of phenolic resin.
Weighing the required raw materials according to the proportion, uniformly mixing diamond powder (50 mu m), boron carbide powder (30 mu m-50 mu m) and absolute ethyl alcohol for phenolic resin, and granulating by adopting freezing spray; then carrying out hot press molding, wherein the pressing pressure is 150Mp, the pressure is maintained for 10min, degreasing treatment is carried out on a pressed sample, the heating rate is 1 ℃/min, the highest temperature is 1000 ℃, and the temperature is kept for 120min; and then siliconizing the porous preform at the high temperature of 1600 ℃, and preserving the heat for 30min to finally obtain the required diamond-boron carbide composite ceramic.
Three-point flexural strength and hardness tests were now performed on examples 1, 2, 3, 4 and 5 and comparative examples, with the test results being given in the following table:
| group of | Vickers hardness GPa | Three-point bending strength MPa |
| Example 1 | 35 | 455 |
| Example 2 | 36 | 431 |
| Example 3 | 36 | 442 |
| Example 4 | 33 | 465 |
| Example 5 | 39 | 423 |
| Comparative example | 27 | 345 |
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (10)
1. A preparation method of diamond boron carbide composite ceramic is characterized in that: the method comprises the following steps:
(1) Mixing diamond powder with boron carbide, graphite and absolute ethyl alcohol for phenolic resin uniformly;
(2) Preparing into particles by adopting a freezing spray granulation mode or a manual crushing and sieving mode;
(3) Hot press molding;
(4) Degreasing the pressed blank;
(5) And (3) performing boronizing sintering on the porous preform obtained in the step (4).
2. The method for preparing the diamond boron carbide composite ceramic according to claim 1, wherein the method comprises the following steps: the diamond powder has a particle size of more than 50 mu m.
3. The method for preparing the diamond boron carbide composite ceramic according to claim 1 or 2, wherein: the volume percentage of the diamond powder, the boron carbide, the graphite and the phenolic resin is 30-75 percent: 0-45%:5-15%:15-25%.
4. A method for preparing a diamond boron carbide composite ceramic according to claim 3, wherein: the purity of the diamond powder and graphite is more than or equal to 99.99 percent.
5. The method for preparing the diamond boron carbide composite ceramic according to claim 1, 2 or 4, wherein the method comprises the following steps: the diamond powder comprises monocrystalline diamond and polycrystalline diamond.
6. The method for preparing the diamond boron carbide composite ceramic according to claim 1, 2 or 4, wherein the method comprises the following steps: and (3) hot press forming, wherein the temperature range of the hot press is as follows: 130-150 ℃; the pressing pressure is 150Mp, and the pressure is maintained for 10-20min.
7. The method for preparing the diamond boron carbide composite ceramic according to claim 6, wherein the method comprises the following steps: degreasing treatment is carried out in the step (4), wherein the degreasing temperature is 1000-1100 ℃, and the degreasing rate is 1-3 ℃/min; preserving heat at the highest temperature point for 90-120 min.
8. The method for preparing the diamond boron carbide composite ceramic according to claim 1 or 2 or 4 or 7, wherein the method comprises the following steps: and (3) boronizing and sintering, wherein the vacuum degree in the boronizing process is between 0.1pa and 320 pa.
9. The method for preparing the diamond boron carbide composite ceramic according to claim 8, wherein: in the boronizing process, the heating rate is 8-15 ℃ per minute before the melting temperature of the boron powder is 2200 ℃, and the temperature is kept for 30min at a temperature slightly higher than the melting temperature of the boron powder.
10. The method for preparing the diamond boron carbide composite ceramic according to claim 9, wherein: the purity of the boron powder is more than or equal to 99.99 percent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211667812.2A CN116041063B (en) | 2022-12-24 | 2022-12-24 | Preparation method of diamond boron carbide composite ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211667812.2A CN116041063B (en) | 2022-12-24 | 2022-12-24 | Preparation method of diamond boron carbide composite ceramic |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116041063A true CN116041063A (en) | 2023-05-02 |
| CN116041063B CN116041063B (en) | 2024-04-30 |
Family
ID=86119436
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211667812.2A Active CN116041063B (en) | 2022-12-24 | 2022-12-24 | Preparation method of diamond boron carbide composite ceramic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116041063B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102046564A (en) * | 2008-05-16 | 2011-05-04 | 六号元素（产品）（控股）公司 | Boron carbide composite materials |
| CN104591783A (en) * | 2015-01-29 | 2015-05-06 | 吉林大学 | Method for plating boron carbide on diamond surface |
| CN108658602A (en) * | 2017-12-25 | 2018-10-16 | 成都晋阳科技有限公司 | A kind of preparation method of diamond boron carbide composite material |
| JP2019006662A (en) * | 2017-06-28 | 2019-01-17 | 博 石塚 | Diamond-based composite material using boron-based binder, production method therefor, and tool constituent using the same |
| CN115010496A (en) * | 2022-07-04 | 2022-09-06 | 东北大学 | Controllable B of performance 4 Preparation method of C-diamond composite material |
-
2022
- 2022-12-24 CN CN202211667812.2A patent/CN116041063B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102046564A (en) * | 2008-05-16 | 2011-05-04 | 六号元素（产品）（控股）公司 | Boron carbide composite materials |
| CN104591783A (en) * | 2015-01-29 | 2015-05-06 | 吉林大学 | Method for plating boron carbide on diamond surface |
| JP2019006662A (en) * | 2017-06-28 | 2019-01-17 | 博 石塚 | Diamond-based composite material using boron-based binder, production method therefor, and tool constituent using the same |
| CN108658602A (en) * | 2017-12-25 | 2018-10-16 | 成都晋阳科技有限公司 | A kind of preparation method of diamond boron carbide composite material |
| CN115010496A (en) * | 2022-07-04 | 2022-09-06 | 东北大学 | Controllable B of performance 4 Preparation method of C-diamond composite material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116041063B (en) | 2024-04-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109553419B (en) | Pneumatic solid-phase sintered boron carbide complex-phase ceramic and preparation method thereof | |
| CN102219536B (en) | B4C/SiC whisker/SiC multiphase ceramic matrix composite and preparation method thereof | |
| CN103030396A (en) | Boron carbide silicon carbide composite ceramic and preparation method thereof | |
| CN100396650C (en) | Method for preparing Ti2AlC ceramic material | |
| CN113121237B (en) | Boron carbide-based composite ceramic and preparation process thereof | |
| CN113149686B (en) | Carbon/carbon composite material crucible with composite ceramic layer and preparation method thereof | |
| CN113698222B (en) | Engine piston C f /C-SiC composite material and preparation method thereof | |
| CN111004036A (en) | High-density hexagonal boron nitride-based solid lubricating composite material and preparation method thereof | |
| CN112194492B (en) | Silicon nitride ceramic material, preparation method and application thereof, and bulletproof flashboard | |
| CN110903091A (en) | SiC-Ti3SiC2Composite material and preparation method thereof | |
| CN113121242A (en) | Short carbon fiber toughened silicon carbide composite material and preparation method thereof | |
| CN110304933B (en) | Preparation method of surface modified silicon carbide whisker toughening reaction sintered silicon carbide ceramic | |
| CN111848170A (en) | Boron carbide-based composite ceramic material and preparation method thereof | |
| CN113416075B (en) | Method for preparing Diamond/SiC composite material | |
| CN116041063B (en) | Preparation method of diamond boron carbide composite ceramic | |
| CN107746282A (en) | A kind of in-situ carburization silica fibre enhancing liquid phase sintering silicon carbide ceramic and manufacture method | |
| CN107540411B (en) | Method for reducing residual silicon content in carbon fiber reinforced ceramic matrix composite | |
| CN111606711B (en) | Polycrystal B 4 C-SiC double-layer composite material and preparation method thereof | |
| CN111825461A (en) | Graphene modified silicon carbide ceramic material, preparation method thereof and bulletproof armor | |
| CN111825462A (en) | Diamond graphene modified silicon carbide ceramic material, preparation method thereof and bulletproof armor | |
| CN108585907B (en) | Cr (chromium)2Preparation method of AlC modified self-healing silicon carbide ceramic matrix composite | |
| CN110981443A (en) | Preparation method of alumina ceramic | |
| CN115010496A (en) | Controllable B of performance 4 Preparation method of C-diamond composite material | |
| CN1478757A (en) | Method of preparing high pruity block titanium aluminium carbon material using discharge plasma sintering | |
| CN101955357B (en) | Processable complex-phase ceramic material and preparation method thereof as well as secondary hardening heat treatment method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant |