CN110590374A - MoSi prepared by Flashing method2Method for producing-SiC composite material - Google Patents
MoSi prepared by Flashing method2Method for producing-SiC composite material Download PDFInfo
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- CN110590374A CN110590374A CN201911033183.6A CN201911033183A CN110590374A CN 110590374 A CN110590374 A CN 110590374A CN 201911033183 A CN201911033183 A CN 201911033183A CN 110590374 A CN110590374 A CN 110590374A
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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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- C04B35/65—Reaction sintering of free metal- or free silicon-containing compositions
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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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
- C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
Abstract
The invention provides a method for preparing MoSi by using a flash method2Method for producing-SiC composite materials from Mo and/or MoSi2C, Si and/or SiO2The mixture is pressed into tablets at the temperature of 500-1200 ℃ by using phenolic resin as a raw material, and low-temperature short-time sintering is carried out by using a flash method to obtain MoSi2-a SiC composite material. FS is associated with a substantial reduction in the time and temperature required for ceramming compared to conventional sintering processes, which means significant energy savings, cheaper equipment, and broader environmental benefits. The present invention and method may also be applied to the preparation of carbide ceramics, nitride ceramics, oxide ceramics and composite systems thereof, where controlling the non-oxidizing atmosphere is one of the key factors of the composite system FS.
Description
Technical Field
The invention relates to MoSi2The field of preparation of-SiC composite materials, in particular to a method for preparing MoSi by using a Flashing method2-SiC composite material.
Background
Flashing, FS for short, was discovered in 2010 in the laboratory guided by professor R Raij by Colonna et al, university of Colorado, Border, Calif. FS typically at a particular starting combination of e-furnace temperatures, the material densifies in a very short time, typically ranging from seconds to minutes.
FS is essentially characterized by very rapid densification (approximately less than one minute or less) that occurs in a 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 and bright light emission.
FS has many advantages over traditional 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 of magnitude, from several hours in the traditional process to several seconds in flash sintering; the consolidation temperature is also significantly reduced (sometimes by about 1000 c). Another advantage of FS 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-SiC composite material using Mo, MoSi2、Si、C、SiO2The mixture is pressed into tablets at the temperature of 500-1200 ℃ and sintered at low temperature for short time by an FS method to obtain MoSi2-SiC composite material, the control of the non-oxidizing atmosphere being one of the key factors for the flash sintering of the composite material.
The technical scheme for realizing the invention is as follows:
MoSi prepared by Flashing method2Method for producing-SiC composite materials from Mo and/or MoSi2C, Si and/or SiO2Uniformly stirring phenolic resin serving as a raw material, tabletting and solidifying, applying current and voltage to a sample through conductive adhesive to perform low-temperature short-time sintering by a flash method to obtain MoSi2-a SiC composite material.
The weight parts of all the materials in the raw materials are respectively as follows: mo and/or MoSi224-45 parts of Si and/or SiO21.5-11.2 parts, C2-4.8 parts and phenolic resin 10-12 parts.
The preparation of MoSi by the Flashing method2The method for preparing the-SiC composite material comprises the following specific steps:
(1) mixing Mo and/or MoSi2Si and/or SiO2C, mixing with 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 curing at 110 ℃;
(3) heating to 500-1200 ℃ in a non-oxidizing atmosphere, and applying an electric field to the conducting wire;
(4) flash firing is carried out on the pressed sheet to obtain MoSi2-a SiC composite material.
The electric field current 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 invention can obtain MoSi with any phase composition2The SiC composite material realizes low-temperature short-time sintering, and is environment-friendly and energy-saving; the FS method can also be used for sintering nitride ceramics, carbide ceramics, oxide ceramic composite materials thereof and the like. The method greatly reduces the time and temperature required by ceramic formation, and has obvious energy-saving, cheaper equipment and wider environmental benefits.
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
Preparation of MoSi by Flashing method2-SiC composite material, comprising the following steps:
32 g of MoSi2Powder, 2.4 g C powder, 5.0g Si powder, the balance being 0.6g SiO2The powder is evenly mixed, then 12g of phenolic resin is added, after even stirring, the mixture is pressed into a wafer with the diameter of 12mm, and the wafer is solidified at 110 ℃.
The conductive adhesive is prepared from silicon carbide, phenolic resin and graphite conductive adhesive in a mass ratio of 0.5: 0.5: 0.3, mixing uniformly and grinding into paste.
Brushing self-made 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 790 ℃, 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
Preparation of MoSi by Flashing method2-SiC composite material, comprising the following steps:
24 g of MoSi2The powder, 4.8 g C powder, 11.2g Si powder, were mixed homogeneously, then 10g phenolic resin was added, after stirring homogeneously, pressed into long strips with a diameter of 50 x 4 x 1mm and cured at 110 ℃.
The conductive adhesive is prepared from silicon carbide, phenolic resin and graphite conductive adhesive in a mass ratio of 1: 0.7: 1, mixing uniformly and grinding into paste.
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 0.1A was applied to the sample and after 10 minutes, the sample was sintered completely.
Example 3
Preparation of MoSi by Flashing method2-SThe method for preparing the iC composite material comprises the following steps:
45.0g of MoSi2The powder, 2g C powder and 1.5g Si powder were mixed uniformly, then 10g phenolic resin was added, after stirring uniformly, pressed into long pieces with a diameter of 50 x 4 x 1mm and cured at 110 ℃.
The conductive adhesive is prepared from silicon carbide, phenolic resin and graphite conductive adhesive in a mass ratio of 0.8: 0.6: 0.6, mixing evenly and grinding into paste.
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 780 ℃ and argon is introduced for protection. The sample was subjected to a current of 60A and after 0.1 minute, the sample was completely sintered.
Example 4
Preparation of MoSi by Flashing method2-SiC composite material, comprising the following steps:
the preparation was carried out as in example 1, except that the sintering temperature was 500 ℃.
Example 5
Preparation of MoSi by Flashing method2-SiC composite material, comprising the following steps:
the preparation was carried out as in example 1, except that the sintering temperature was 1200 ℃.
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-SiC composite material, characterized in that: with Mo and/or MoSi2C, Si and/or SiO2Uniformly stirring phenolic resin serving as a raw material, tabletting and solidifying, applying current and voltage to a sample through conductive adhesive to perform low-temperature short-time sintering by a flash method to obtain MoSi2-a SiC composite material.
2. Preparation of MoSi by the Flashing process according to claim 12-SiA method of making a C composite, characterized by: the weight parts of all the materials in the raw materials are respectively as follows: mo and/or MoSi224-45 parts of Si and/or SiO21.5-11.2 parts, C2-4.8 parts and phenolic resin 10-12 parts.
3. Preparation of MoSi according to the Flashing process according to any of claims 1 to 22-a method for producing a SiC composite material, characterized in that the specific steps are as follows:
(1) mixing Mo and/or MoSi2Si and/or SiO2C, mixing with 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 curing at 110 ℃;
(3) heating to 500-1200 ℃ in a non-oxidizing atmosphere, and applying an electric field to the conducting wire;
(4) flash firing is carried out on the pressed sheet to obtain MoSi2-a SiC composite material.
4. Preparation of MoSi by the Flashing process according to claim 32-SiC composite material, characterized in that: the electric field current 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 32-SiC composite material, characterized in that: 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.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN116547253A (en) * | 2020-10-20 | 2023-08-04 | 赛峰集团陶瓷 | Method for producing hollow parts from short-fiber-reinforced metal matrix or ceramic matrix composite materials |
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EP0463180A1 (en) * | 1990-01-19 | 1992-01-02 | Kabushiki Kaisha Kouransha | Material generating heat by absorbing microwaves |
CN101157556A (en) * | 2007-09-26 | 2008-04-09 | 中南大学 | Method for preparing nano SiC particle reinforced MoSi2 radical composite material by polymer cracking-reaction hot-pressing |
CN102515770A (en) * | 2011-11-25 | 2012-06-27 | 中原工学院 | Method for preparing nano SiC reinforced MoSi2 composite material |
CN105565816A (en) * | 2015-12-12 | 2016-05-11 | 中原工学院 | Preparation method of MoSi2/MoB/SiC three-phase ceramic |
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2019
- 2019-10-28 CN CN201911033183.6A patent/CN110590374A/en active Pending
Patent Citations (6)
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EP0463180A1 (en) * | 1990-01-19 | 1992-01-02 | Kabushiki Kaisha Kouransha | Material generating heat by absorbing microwaves |
CN101157556A (en) * | 2007-09-26 | 2008-04-09 | 中南大学 | Method for preparing nano SiC particle reinforced MoSi2 radical composite material by polymer cracking-reaction hot-pressing |
CN102515770A (en) * | 2011-11-25 | 2012-06-27 | 中原工学院 | Method for preparing nano SiC reinforced MoSi2 composite material |
EP3138829A1 (en) * | 2015-08-28 | 2017-03-08 | Rolls-Royce High Temperature Composites Inc | Ceramic matrix composite including silicon carbide fibers in a ceramic matrix comprising a max phase compound |
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Non-Patent Citations (2)
Title |
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XIAOLI ZHANG等: "Electrical resistivity and microstructure of pressureless reactive sintered MoSi2–SiC composite", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116547253A (en) * | 2020-10-20 | 2023-08-04 | 赛峰集团陶瓷 | Method for producing hollow parts from short-fiber-reinforced metal matrix or ceramic matrix composite materials |
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