CN114409406A - B12(C,Si,B)3Preparation method of-SiC two-phase ceramic - Google Patents
B12(C,Si,B)3Preparation method of-SiC two-phase ceramic Download PDFInfo
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 40
- 239000000919 ceramic Substances 0.000 title claims abstract description 39
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title abstract description 13
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 39
- 239000000843 powder Substances 0.000 claims abstract description 34
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000126 substance Substances 0.000 claims abstract description 20
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 238000005049 combustion synthesis Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 16
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- 230000001939 inductive effect Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 238000003825 pressing Methods 0.000 abstract description 6
- 239000012071 phase Substances 0.000 description 18
- 239000010703 silicon Substances 0.000 description 6
- 238000002289 liquid silicon infiltration Methods 0.000 description 5
- 238000005470 impregnation Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 239000011184 SiC–SiC matrix composite Substances 0.000 description 1
- 229910021431 alpha silicon carbide Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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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
- C04B35/565—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 silicon carbide
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- C—CHEMISTRY; METALLURGY
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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
- C04B35/64—Burning or sintering processes
- C04B35/65—Reaction sintering of free metal- or free silicon-containing compositions
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- 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
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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
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/428—Silicon
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
The invention introduces a preparation B12(C,Si,B)3The method of the-SiC two-phase ceramic can improve the toughness of the SiC ceramic with poor toughness. Namely, the invention takes silicon powder, boron carbide powder and silicon carbide powder as raw materials, and prepares the B by a low-cost short-period chemical furnace combustion synthesis method12(C,Si,B)3-SiC two-phase ceramics. Mixing silicon powder, boron carbide powder and silicon carbide powder, pressing into a blank, embedding the blank into chemical furnace powder, igniting the chemical furnace powder, and then burning to synthesize B12(C,Si,B)3The compactness of the ceramic can reach more than 95 percent, and the maximum fracture toughness can reach 5.8MPa/m1/2。
Description
Technical Field
The invention relates to the field of SiC-based composite materialsDomains, especially involving B12(C,Si,B)3Preparation of-SiC two-phase ceramics.
Background
The silicon carbide (SiC) ceramic is an advanced engineering material with excellent physical and mechanical properties, and has the characteristics of high hardness, high strength, low density, good chemical stability and the like. However, natural low fracture toughness and poor sinterability (sintering temperature)>2000 c) limits their applications and typically high pressure equipment such as SPS and autoclave must be used. The Liquid Silicon Infiltration (LSI) process is a rapid and direct method, and can prepare large-size compact SiC ceramics with complex shapes at a high temperature of 1600 ℃. In addition, the boron carbide particles are doped to reinforce the silicon carbide ceramic, and a ternary boron carbide-based compound B is found on the surface of the silicon carbide ceramic12(B，C，Si)3The ternary phase has toughening effect relative to SiC ceramic.
Mengyong Sun et al prepared B by impregnating liquid silicon12(C,Si,B)3the-SiC two-phase ceramic adopts alpha-SiC powder with the grain size of 1 mu m and B4Taking the powder C as an initial raw material, carrying out wet mixing and ball milling for 24h, forming, removing the organic solvent at low temperature, sintering for 1h at 1300 ℃, and permeating liquid silicon for 1h at 1550 ℃ under vacuum to obtain a ceramic material with the porosity of 35%; however, the impregnation with the molten silicon requires a long time of high temperature heating to melt Si, and the preparation period and cost are still high.
Liujianggong et al prepare Si-B-C modified C/C-SiC composite material by liquid silicon infiltration method, wherein B is prepared first12(C,Si, B)3B4C powder having a particle size of 1.5 μm and Si powder having a particle size of 45 μm were mixed, ball-milled, dried, molded, and sintered in an argon atmosphere. In the preparation process of the reactive sintering method, the heat preservation is carried out at the temperature of 1300 ℃ and 1500 ℃, the energy consumption is high, and the cost is high.
CN106431452 mentions that vacuum-pressure impregnation is adopted to introduce phenolic resin mixed with B4C powder into a porous SiC/SiC composite material, then solidification, cracking, heat treatment are carried out, short-time liquid silicon infiltration is carried out under vacuum condition, and molten silicon reacts with cracking C and B4C to generate ternary B12(C,Si,B)3And SiC. Although the method adopts short-time liquid silicon infiltration, the preparation process is complex, organic matters exist, and the flow is weekLong period and is not beneficial to industrial production.
Disclosure of Invention
In order to solve the technical problems, the invention seeks a rapid and low-cost process for preparing B12(C,Si,B)3The SiC two-phase ceramic can achieve the effect of toughening the SiC ceramic.
The technical scheme adopted by the invention is as follows:
b12(C,Si,B)3-SiC two-phase ceramic, characterized in that B is present in the two-phase ceramic12(C,Si,B)3The mass ratio of phase to SiC phase is 1.375y (100-x-0.875y), where x: 0.15 to 0.35; y: 0.01 to 0.5.
B12(C,Si,B)3The preparation method of the-SiC two-phase ceramic is characterized by comprising the following steps of:
(1) powder mixing: silicon powder, boron carbide powder and silicon carbide powder are used as initial raw materials, and according to mass fraction, 15-35 wt% of silicon powder, 1-50 wt% of boron carbide powder and 15-84 wt% of silicon carbide powder are uniformly mixed by a wet method or a dry method and dried to obtain mixed powder;
(2) forming a ceramic blank: forming the mixed powder under the pressure of 50-80 MPa and the pressure maintaining for 60-90 s to obtain a reaction blank;
(3) setting a chemical furnace: embedding the reaction green body into the powder of the chemical furnace by adopting the chemical furnace;
(4) combustion synthesis: igniting a chemical furnace under the vacuum condition, inducing the reaction blank to burn and synthesize to obtain B with the density of 95-99 percent12(C,Si,B)3-SiC constitutes a two-phase ceramic.
Furthermore, the particle size of the silicon powder is in the range of 0.1-15 μm, and more preferably 1-10 μm.
Further, the particle size range of the boron carbide powder is 0.1-40 μm, and more preferably 10-20 μm.
Furthermore, the particle size range of the silicon carbide powder is 0.1-10 μm, and more preferably 0.1-2 μm.
Further, the porosity of the reaction blank in the step (2) is 50-80%.
Further, the chemical furnace in the step (3) is composed of 70-85% of Ti + C powder and 15-30% of Al + Fe2O3 powder by mass, wherein the molar ratio of Ti to C is 1:1, and the molar ratio of Al to Fe2O3 is 1: 1.
Further, B is12(C,Si,B)3The compactness of the-SiC two-phase ceramic is more than 97 percent.
In general, in order to make Si melt at high temperature to fill the pores as much as possible to reduce the porosity, the two-phase ceramic may contain a part of unreacted Si, usually more than 10%, and XRD can see that the two-phase ceramic contains a part of Si, which is equivalent to Si in the silicon melt impregnation process for increasing the compactness.
The invention has the beneficial effect that the combustion synthesis method is adopted to prepare the B12(C,Si,B)3the-SiC two-phase ceramic avoids high-temperature liquid phase silicon penetration, the synthesized two-phase ceramic has good dimensional stability and no defect in appearance, the measured compactness is more than 95%, and the fracture toughness is 3.2-5.8 MPa/m1/2。
Drawings
The invention will be described in more detail hereinafter on the basis of embodiments and with reference to the accompanying drawings. Wherein:
FIG. 1 shows B prepared according to the present invention12(C,Si,B)3-XRD spectrum of SiC two-phase ceramic.
Detailed Description
The technical solutions in 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 obvious that the embodiments described are only some representative embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
Example 1
Uniformly mixing 30g of silicon powder with the particle size of 2 microns, 40g of boron carbide powder with the particle size of 20 microns and 40g of silicon carbide with the particle size of 1 micron to obtain mixed powder, and carrying out dry pressing molding on the mixed powder in a one-way hydraulic press under the pressure of 80MPa for 90s to obtain a blank body with the porosity of 65%; setting a chemical furnace comprising 80 mass percent of Ti + C powder (the molar ratio of Ti to C is 1:1) and 20 mass percent of Al + Fe2O3Powder (Al, Fe)2O3The molar ratio is 1: 1); the blank is combusted and synthesized in a chemical furnace under the vacuum condition to induce the blank to react to obtain B12(C,Si,B)3-SiC two-phase ceramic; the synthesized product was found to be typical of B by XRD12(C, Si,B)3The density of the product is 97.3 percent, and the fracture toughness is 4.7MPa/m1/2。
Example 2:
as in example 1, except for the same reaction conditions, 25g of silicon powder having a particle size of 1 μm, 20g of boron carbide powder having a particle size of 15 μm, and 55g of silicon carbide having a particle size of 0.1 μm were used; adopting dry pressing molding pressure of 50Mpa to obtain blank porosity of 63%; setting a chemical furnace to perform combustion synthesis reaction under vacuum condition to obtain B12(C,Si,B)3The density of the product is 98.6 percent, and the fracture toughness is 5.3MPa/m1/2。
Example 3:
as in example 1, 20g of silicon powder having a particle size of 1 μm, 15g of boron carbide powder having a particle size of 15 μm, and 65g of silicon carbide having a particle size of 0.5 μm were used, except that the reaction conditions were the same; adopting dry pressing molding pressure of 60Mpa to obtain blank with porosity of 50%; setting a chemical furnace to perform combustion synthesis reaction under vacuum condition to obtain B12(C,Si,B)3The density of the product is 98.9 percent, and the fracture toughness is 5.8MPa/m1/2。
Example 4:
as in example 1, 35g of silicon powder having a particle size of 15 μm, 50g of boron carbide powder having a particle size of 0.1 μm, and 15g of silicon carbide having a particle size of 2 μm were used, except that the reaction conditions were the same; the dry pressing forming pressure is 80Mpa, and the porosity of the obtained blank is 65%; setting a chemical furnace comprising 70 mass percent of Ti + C powder (the molar ratio of Ti to C is 1:1) and 30 mass percent of Al + Fe2O3Powder (Al, Fe)2O3The molar ratio is 1: 1); combustion synthesis reaction under vacuum condition to obtain B12(C,Si,B)3The density of the product is 95.6 percent, and the fracture toughness is 3.2MPa/m1/2。
Example 5:
as in example 1, 15g of silicon powder having a particle size of 0.1 μm, 1g of boron carbide powder having a particle size of 40 μm, and 84g of silicon carbide having a particle size of 10 μm were used, except that the reaction conditions were the same; the dry pressing forming pressure is 80Mpa, and the porosity of the obtained blank is 67%; setting a chemical furnace comprising 85 mass percent of Ti + C powder (the molar ratio of Ti to C is 1:1) and 15 mass percent of Al + Fe2O3Powder (Al, Fe)2O3The molar ratio is 1: 1); combustion synthesis reaction under vacuum condition to obtain B12(C,Si,B)3The density of the product is 97.9 percent, and the fracture toughness is 4.2MPa/m1/2。
Table 1.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. B12(C,Si,B)3-SiC two-phase ceramic, characterized in that B is present in the two-phase ceramic12(C,Si,B)3The mass ratio of phase to SiC phase is 1.375y (100-x-0.875y), where x: 0.15 to 0.35; y: 0.01 to 0.5.
2. B as claimed in claim 112(C,Si,B)3The preparation method of the-SiC two-phase ceramic is characterized by comprising the following steps of:
(1) powder mixing: silicon powder, boron carbide powder and silicon carbide powder are used as initial raw materials, and according to the mass fraction, 15-35 wt% of silicon powder, 1-50 wt% of boron carbide powder and 15-84 wt% of silicon carbide powder are uniformly mixed and dried to obtain mixed powder;
(2) forming a ceramic blank: forming the mixed powder under the pressure of 50-80 MPa and the pressure maintaining for 60-90 s to obtain a reaction blank;
(3) setting a chemical furnace: embedding the reaction green body into the powder of the chemical furnace by adopting the chemical furnace;
(4) combustion synthesis: igniting a chemical furnace under the vacuum condition, inducing the reaction blank to burn and synthesize to obtain B with the density of 95-99 percent12(C,Si,B)3-SiC constitutes a two-phase ceramic.
3. B as claimed in claim 212(C,Si,B)3The preparation method of the-SiC two-phase ceramic is characterized in that the particle size range of the silicon powder is 0.1-15 mu m, and more preferably 1-10 mu m.
4. B as claimed in claim 212(C,Si,B)3The preparation method of the-SiC two-phase ceramic is characterized in that the particle size range of the boron carbide powder is 0.1-40 mu m, and more preferably 10-20 mu m.
5. B as claimed in claim 212(C,Si,B)3The preparation method of the-SiC two-phase ceramic is characterized in that the particle size range of the silicon carbide powder is 0.1-10 mu m, and more preferably 0.1-2 mu m.
6. B as claimed in claims 2 to 512(C,Si,B)3The preparation method of the-SiC two-phase ceramic is characterized in that the porosity of the reaction blank in the step (2) is 50-80%.
7. B as claimed in claims 2 to 512(C,Si,B)3The preparation method of the-SiC two-phase ceramic is characterized in that the chemical furnace in the step (3) adopts 70-85% of Ti + C powder and 15-30% of Al + Fe powder by mass fraction2O3Powder composition, wherein the molar ratio of Ti to C is 1:1, and Al and Fe2O3The molar ratio is 1: 1.
8. B as claimed in claim 212(C,Si,B)3-SiC two-phase ceramics, characterized in that B is12(C,Si,B)3The compactness of the-SiC two-phase ceramic is more than 97 percent.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1198780A (en) * | 1995-10-02 | 1998-11-11 | 陶氏化学公司 | Singal step synthesis and densification of ceramic-ceramic and ceramic-metal composite materials |
| CN101372073A (en) * | 2008-08-18 | 2009-02-25 | 江阴东大新材料研究院 | Aluminothermy overlaying welding and rolling technique |
| CN101456737A (en) * | 2009-01-05 | 2009-06-17 | 西安交通大学 | Boron carbide base composite ceramic and preparation method thereof |
| CN101775517A (en) * | 2009-09-18 | 2010-07-14 | 江阴东大新材料研究院 | Method for preparing TiC/Al2O3/Fe composite ceramic matrix composite material |
| JP2012031499A (en) * | 2010-07-29 | 2012-02-16 | Kunio Matsunaga | Method for recovering gold, silver, platinum or rare metal from waste by use of thermite melting method |
| CN105622102A (en) * | 2015-12-18 | 2016-06-01 | 中国科学院上海硅酸盐研究所 | Pseudo-boron carbide phase-silicon carbide or pseudo-boron carbide phase-silicon carbide-boron carbide complex-phase ceramic material and preparation method thereof |
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- 2020-10-28 CN CN202011168636.9A patent/CN114409406A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1198780A (en) * | 1995-10-02 | 1998-11-11 | 陶氏化学公司 | Singal step synthesis and densification of ceramic-ceramic and ceramic-metal composite materials |
| CN101372073A (en) * | 2008-08-18 | 2009-02-25 | 江阴东大新材料研究院 | Aluminothermy overlaying welding and rolling technique |
| CN101456737A (en) * | 2009-01-05 | 2009-06-17 | 西安交通大学 | Boron carbide base composite ceramic and preparation method thereof |
| CN101775517A (en) * | 2009-09-18 | 2010-07-14 | 江阴东大新材料研究院 | Method for preparing TiC/Al2O3/Fe composite ceramic matrix composite material |
| JP2012031499A (en) * | 2010-07-29 | 2012-02-16 | Kunio Matsunaga | Method for recovering gold, silver, platinum or rare metal from waste by use of thermite melting method |
| CN105622102A (en) * | 2015-12-18 | 2016-06-01 | 中国科学院上海硅酸盐研究所 | Pseudo-boron carbide phase-silicon carbide or pseudo-boron carbide phase-silicon carbide-boron carbide complex-phase ceramic material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| MENGYONG SUN ET AL.: ""In situ toughened two-phase Bi2(C,Si, B)3-SiC ceramics fabricated via liquid silicon infiltration"", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 * |
| 李沐山: "《八十年代世界硬质合金技术进展》", 31 August 1992 * |
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