CN110590373A - MoSi prepared by Flashing method2Method for preparing-MoB-SiC three-phase composite material - Google Patents
MoSi prepared by Flashing method2Method for preparing-MoB-SiC three-phase composite material Download PDFInfo
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- CN110590373A CN110590373A CN201911031916.2A CN201911031916A CN110590373A CN 110590373 A CN110590373 A CN 110590373A CN 201911031916 A CN201911031916 A CN 201911031916A CN 110590373 A CN110590373 A CN 110590373A
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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
- C04B35/58—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/58085—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicides
- C04B35/58092—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicides based on refractory metal silicides
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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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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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
- C04B2235/3804—Borides
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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
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
Abstract
The invention provides a method for preparing MoSi by using a flash method2Method for producing a three-phase composite material of-MoB-SiC, with MoSi2、B4C. Si, C and phenolic resin are used as raw materials, the raw materials are uniformly stirred, pressed into sheets and solidified, a current and voltage are applied to a sample through a conductive adhesive to carry out low-temperature short-time sintering by a flash method, and MoSi is obtained2-MoB-SiC three-phase composite material. The method greatly reduces the time and temperature required by ceramic-making, and has obvious energy-saving, cheaper equipment and wider environmental benefits. The method can obtain MoSi with any phase composition2the-MoB-SiC three-phase composite material realizes low-temperature short-time sintering, and is environment-friendly and energy-saving.
Description
Technical Field
The invention relates to the field of preparation of three-phase high-temperature structure composite materials, in particular to a method for preparing MoSi by using a Flashing method2-a method for preparing a MoB-SiC three-phase composite material.
Background
Flash Sintering (FS) was discovered in 2010 by crorona et al, university of colorado, brodif, usa, in a laboratory directed by professor R Raij. Flash sintering belongs to a broad class of Field Assisted Sintering Techniques (FAST) and more specifically to the current assisted sintering (ECAS) process. At a particular starting combination of electric field furnace temperatures, the material densifies in a very short time, typically ranging from a few seconds to several minutes.
The background of the first flash sintering experiment was essentially constituted by an earlier study by godson et al published in 2009 showing the interaction between the application of a small dc electric field and grain coarsening in 3 YSZ.
Flash sintering is essentially characterized by very rapid densification (about 1 minute or less) that occurs in a so-called Flash Event (FE). Therefore, flash sintering can be defined as an electric field assisted sintering technology, and is characterized in that: rapid densification; a sudden drop in conductivity and a strong bright light emission.
Flash sintering has many advantages over conventional sintering processes. One of the most obvious reasons is obviously linked to the considerable reduction in time and temperature required for ceramization, which means significant energy savings, cheaper equipment, and broader environmental benefits. The consolidation time is generally reduced from 1 to 3 orders, and is shortened from several hours in the traditional process to several minutes in flash sintering; the consolidation temperature is also significantly reduced (sometimes by about 1000 c). Another advantage of flash sintering is that it is an unbalanced process, which is associated with extremely high heating rates and extremely short processing times. Thus, it is possible to sinter the metastable material or to avoid unnecessary phase changes.
Disclosure of Invention
The invention provides a method for preparing MoSi by using a Flashing method2Method for producing a three-phase composite material of MoB-SiC using MoSi2、B4C. Si, C, phenolic resin, conductive adhesive and the like are taken as raw materials, the mixture is pressed into tablets within the range of 500-1200 ℃, and low-temperature short-time sintering is carried out by a flash method to obtain MoSi2-MoB-SiC IIIThe control of the non-oxidizing atmosphere is one of the key factors for the flash sintering of the three-phase composite material.
The technical scheme for realizing the invention is as follows:
MoSi prepared by Flashing method2Method for producing a three-phase composite material of-MoB-SiC, with MoSi2、B4C. Si, C and phenolic resin are used as raw materials, the raw materials are uniformly stirred, pressed into sheets and solidified, a current and voltage are applied to a sample through a conductive adhesive to carry out low-temperature short-time sintering by a flash method, and MoSi is obtained2-MoB-SiC three-phase composite material.
The weight parts of all the materials in the raw materials are as follows: MoSi245-50 parts of B40.5-1.5 parts of C, 0.3-1.5 parts of Si, 1-2 parts of C and 10-15 parts of phenolic resin.
The preparation of MoSi by the Flashing method2The method for preparing the MoB-SiC three-phase composite material comprises the following specific steps:
(1) mixing MoSi2、B4C. Stirring Si, C and phenolic resin uniformly, and pressing into tablets;
(2) brushing conductive adhesive on the surface or the side of the pressed sheet in the step (1), bonding a lead, and heating and fixing;
(3) heating to 500-1200 ℃ in a non-oxidizing atmosphere, and applying current and voltage to the conducting wire;
(4) flash firing is carried out on the pressed sheet to obtain MoSi2-MoB-SiC three-phase composite material.
The current applied in the step (3) is 0.1-60A, and the flash time in the step (4) is 0.1-10 min.
The conductive adhesive is prepared from silicon carbide, phenolic resin and graphite conductive adhesive in a mass ratio of (0.5-1): (0.5-0.7): (0.3-1), mixing uniformly and grinding into paste.
The invention has the beneficial effects that: the method greatly reduces the time and temperature required by ceramic-making, and has obvious energy-saving, cheaper equipment and wider environmental benefits. The method can obtain MoSi with any phase composition2the-MoB-SiC three-phase composite material realizes low-temperature short-time sintering, and is environment-friendly and energy-saving.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
MoSi prepared by Flashing method2-MoB-SiC three-phase composite material, comprising the following steps:
47.76g of MoSi2Powder, 0.63g B4Uniformly mixing C powder, 1.15g C powder and 0.46g of Si powder, adding 12g of phenolic resin, uniformly stirring, pressing into a wafer with the diameter of 12mm, and curing at 110 ℃.
And brushing carbon conductive adhesive on the edge of the wafer, and fixing the platinum wire on the edge. Then the sample is put into a tube furnace with the furnace temperature of 800 ℃ and argon is introduced for protection. A current of 50A was applied to the sample and after 2 minutes, the sample was sintered completely.
Example 2
MoSi prepared by Flashing method2-MoB-SiC three-phase composite material, comprising the following steps:
45.0g of MoSi2Powder, 1.5g B4Mixing C powder, 2g C powder, and 1.5g Si powder, adding 10g phenolic resin, stirring, pressing into long strips with diameter of 50 × 4 × 1mm, and curing at 110 deg.C.
And brushing carbon conductive adhesive on the edge of the pressing strip, and fixing the platinum wire on the edge. The sample was then placed in a tube furnace at 798 ℃ and argon was passed through the furnace for protection. A current of 40A was applied to the sample and after 2 minutes, the sample was sintered completely.
Example 3
MoSi prepared by Flashing method2-MoB-SiC three-phase composite material, comprising the following steps:
45.0g of MoSi2Powder, 1.5g B4C powder, 2g C powder, 1.5g Si powderMixing, adding 10g of phenolic resin, stirring, pressing into strips with diameter of 50X 4X 1mm, and curing at 110 deg.C.
And brushing a mixture of silicon carbide and phenolic resin on the edge of the pressing strip, and fixing the platinum wire on the edge. The sample was then placed in a tube furnace at 798 ℃ and argon was passed through the furnace for protection. A current of 60A was applied to the sample and after 2 minutes, the sample was sintered completely.
Example 4
MoSi prepared by Flashing method2-MoB-SiC three-phase composite material, comprising the following steps:
50g of MoSi2Powder, 1.0g B4Mixing C powder, 1.0g C powder, 2g Si powder, adding 15g phenolic resin, stirring, pressing into strips with diameter of 50 × 4 × 1mm, and curing at 110 deg.C.
And brushing a mixture of silicon carbide and phenolic resin on the edge of the pressing strip, and fixing the platinum wire on the edge. Then the sample is put into a tube furnace with the furnace temperature of 500 ℃ and argon is introduced for protection. A current of 0.1A was applied to the sample, and after 10min, the sample was sintered.
Example 5
MoSi prepared by Flashing method2-MoB-SiC three-phase composite material, comprising the following steps:
48g of MoSi2Powder, 0.5g B4Mixing C powder, 0.3g C powder, and 1g Si powder, adding 13g phenolic resin, stirring, pressing into long strips with diameter of 50 × 4 × 1mm, and curing at 110 deg.C.
And brushing a mixture of silicon carbide and phenolic resin on the edge of the pressing strip, and fixing the platinum wire on the edge. Then the sample is put into a tube furnace with the furnace temperature of 1200 ℃, and argon is introduced for protection. A current of 30A was applied to the sample, and after 0.1min, the sample was sintered.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. MoSi prepared by Flashing method2-method of MoB-SiC three-phase composite material, characterized in that: with MoSi2、B4C. Si, C and phenolic resin are used as raw materials, the raw materials are uniformly stirred, pressed into sheets and solidified, a current and voltage are applied to a sample through a conductive adhesive to carry out low-temperature short-time sintering by a flash method, and MoSi is obtained2-MoB-SiC three-phase composite material.
2. Preparation of MoSi by the Flashing process according to claim 12-method of MoB-SiC three-phase composite material, characterized in that: the weight parts of all the materials in the raw materials are as follows: MoSi245-50 parts of B40.5-1.5 parts of C, 0.3-1.5 parts of Si, 1-2 parts of C and 10-15 parts of phenolic resin.
3. The method of producing MoSi according to claim 1 or 2 by the Flashing method2The method for preparing the MoB-SiC three-phase composite material is characterized by comprising the following specific steps of:
(1) mixing MoSi2、B4C. Stirring Si, C and phenolic resin uniformly, and pressing into tablets;
(2) brushing conductive adhesive on the surface or the side of the pressed sheet in the step (1), bonding a lead, and heating and fixing;
(3) heating to 500-1200 ℃ in a non-oxidizing atmosphere, and applying current and voltage to the conducting wire;
(4) flash firing is carried out on the pressed sheet to obtain MoSi2-MoB-SiC three-phase composite material.
4. Preparation of MoSi by the Flashing process according to claim 32-method of MoB-SiC three-phase composite material, characterized in that: the current applied in the step (3) is 0.1-60A, and the flash time in the step (4) is 0.1-10 min.
5. Preparation of MoSi by the Flashing process according to claim 12-method of MoB-SiC three-phase composite material, characterized in that: the conductive adhesive takes silicon carbide, phenolic resin and graphite conductive adhesive as raw materials according to massThe ratio is (0.5-1): (0.5-0.7): (0.3-1), mixing uniformly and grinding into paste.
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Citations (7)
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|---|---|---|---|---|
| JPH09132460A (en) * | 1995-11-09 | 1997-05-20 | Riken Corp | Tungsten solid solution type molybdenum disilicide composite ceramics and its production |
| EP1348984A1 (en) * | 2002-03-27 | 2003-10-01 | Carl Zeiss Semiconductor Manufacturing Technologies Ag | Optical broad band element and process for its production |
| CN105565816A (en) * | 2015-12-12 | 2016-05-11 | 中原工学院 | Preparation method of MoSi2/MoB/SiC three-phase ceramic |
| CN106630974A (en) * | 2016-11-25 | 2017-05-10 | 中国工程物理研究院材料研究所 | Flash sintering method of low-temperature flash sintering ceramic and obtained ceramic and device thereof |
| CN109437974A (en) * | 2018-11-20 | 2019-03-08 | 北京航空航天大学 | A kind of C/SiC composite material and preparation method with Mo-Si-B-O high-temperature oxidation resistant coating |
| CN109638276A (en) * | 2018-12-29 | 2019-04-16 | 中原工学院 | A kind of complete densification LLZO series solid state battery material and preparation method thereof |
| CN109704772A (en) * | 2019-03-06 | 2019-05-03 | 东北大学 | A kind of boron-carbide-based ceramic composite material and preparation method of original position toughening |
-
2019
- 2019-10-28 CN CN201911031916.2A patent/CN110590373A/en active Pending
Patent Citations (7)
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| JPH09132460A (en) * | 1995-11-09 | 1997-05-20 | Riken Corp | Tungsten solid solution type molybdenum disilicide composite ceramics and its production |
| EP1348984A1 (en) * | 2002-03-27 | 2003-10-01 | Carl Zeiss Semiconductor Manufacturing Technologies Ag | Optical broad band element and process for its production |
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| CN106630974A (en) * | 2016-11-25 | 2017-05-10 | 中国工程物理研究院材料研究所 | Flash sintering method of low-temperature flash sintering ceramic and obtained ceramic and device thereof |
| CN109437974A (en) * | 2018-11-20 | 2019-03-08 | 北京航空航天大学 | A kind of C/SiC composite material and preparation method with Mo-Si-B-O high-temperature oxidation resistant coating |
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Non-Patent Citations (2)
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| XIAOLI ZHANG等: "The preparation of in-situ MoSi2-SiC-MoB three-phase composite completely eliminating the PEST phenomena", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
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