CN101423395B - Method for preparing Ti3SiC2 material by melting infiltration sintering - Google Patents

Method for preparing Ti3SiC2 material by melting infiltration sintering Download PDF

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CN101423395B
CN101423395B CN2008102323806A CN200810232380A CN101423395B CN 101423395 B CN101423395 B CN 101423395B CN 2008102323806 A CN2008102323806 A CN 2008102323806A CN 200810232380 A CN200810232380 A CN 200810232380A CN 101423395 B CN101423395 B CN 101423395B
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powder
particle diameter
sic
sintering
temperature
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CN101423395A (en
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吕振林
邢志国
李开雄
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Xian University of Technology
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Xian University of Technology
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Abstract

The invention discloses a method for preparing a Ti3SiC2 material through infiltration sintering, which comprises the following steps: using one or two of Ti powder, Si powder and TiC powder or C powder as raw materials; preparing a diluted binder from the binder and ethanol; sufficiently mixing the raw materials and the diluted binder to prepare a blank, and drying the blank to obtain a prefabricated part; and covering the Si powder on the surface of the prefabricated part, sintering the prefabricated part into a hydrogen atmosphere protected sintering furnace, raising the temperature in the protected furnace to between 1,000 and 1,100 DEG C at a speed of 10 DEG C per minute and keeping the temperature for 30 to 40 minutes, then continuously raising the temperature to between 1,300 and 1,400 DEG C at the speed of 10 DEG C per minute and keeping the temperature for 30 to 40 minutes, and raising the temperature to between 1,500 and 1,600 DEG C at a speed of 5 DEG C per minute and keeping the temperature for 60 to 70 minutes so as to obtain the Ti3SiC2 material. The Ti3SiC2 material prepared by the method has the advantages of less impurity phase content, low air porosity and good density.

Description

A kind of melting infiltration sintering prepares Ti 3SiC 2The method of material
Technical field
The invention belongs to technical field of material, be specifically related to a kind of melting infiltration sintering and prepare Ti 3SiC 2The method of material.
Background technology
Ti 3SiC 2As M N+1AX nTypical case's representative in the ternary compound; Be to study the most comprehensive ternary layered compound up to now; Performance with following excellence: under the normal temperature; As metal good heat conductivility and conductivity, lower Vickers' hardness, higher modulus of elasticity and shearing modulus are arranged, can carry out mechanical workout as metal and graphite, and have high-temp plastic; Simultaneously, have the performance of stupalith again, higher yield strength, good thermostability, excellent antioxidant property and heat-shock resistance are arranged; What have more application value is that it has the graphite of being superior to and MoS 2Self-lubricating property.Therefore, Ti 3SiC 2Application prospect boundless, can be used as: 1) high-temperature structural material, 2) substitute workability pottery, 3) kiln furnitures, 4) anticorrosive resist, 5) heat exchanger, 6) can be used as contact material, 7) material such as low-friction coefficient material uses.Ti 3SiC 2Because of its many excellent properties that have metal and pottery concurrently, make it be with a wide range of applications in fields such as electromechanics, instrument, metallurgy, chemical industry, automobile, boats and ships, petrochemical industry, space flight, national defence.
From 1967, utilize TiH 2, Si and graphite mixed powder be raw material, under 2000 ℃ temperature, make Ti first 3SiC 2Since the material, up to the present, the investigator prepares Ti with multiple compound method 3SiC 2Material.Present Ti 3SiC 2Compound method mainly contain: the auxiliary synthesis method (MA) of chemical vapor deposition (CVD) method, self propagating high temperature synthesis method (SHS), physical chemistry synthesis method, discharge plasma sintering method (SHS), liquid-solid reaction method, mechanical alloying, hot pressed sintering (HP) method, hot isostatic pressing (HIP) method, solid state reaction sintering process etc.But existing preparation Ti 3SiC 2The method of material, as hot pressed sintering, though void content is very low, density can reach 90%, and not only complex process is very high to the conditional request of equipment, and the preparation material shape is required extremely strict; The Ti for preparing with reaction sintering 3SiC 2Though material technology is simple, not high to equipment requirements, the preparation process is not strict with material shape, wherein contains impurity phases such as a large amount of TiC, SiC or silicide, causes Ti yet 3SiC 2The purity of material is lower, and pore is many, and density is relatively poor, only has 60%～70%, has a strong impact on Ti 3SiC 2The performance of material.
Summary of the invention
The purpose of this invention is to provide a kind of melting infiltration sintering and prepare Ti 3SiC 2The method of material, the Ti that adopts this method to make 3SiC 2Purity is high, pore is few, compactness good, and technology is simple, and is lower to the requirement of producing apparatus.
The technical scheme that the present invention adopted is that a kind of melting infiltration sintering prepares Ti 3SiC 2The method of material is a raw material with in Ti powder, Si powder and TiC powder or the C powder one or both, uniform mixing and process precast body after, through infiltration, sintering, the Ti that preparation purity is high, pore is few, density is high 3SiC 2Material, this method is carried out according to the following steps:
Step 1: mix powder
By mole per-cent; Si powder 5%～25% and the particle diameter of getting particle diameter respectively and be 50 μ m～Ti powder 45%～65% of 75 μ m, particle diameter and be 65 μ m～85 μ m are the TiC powder 15%～35% of 45 μ m～100 μ m, each component total amount 100%, uniform mixing; Obtain mixed powder
Or by a mole per-cent, Si powder 5%～25% and the particle diameter of getting particle diameter respectively and be 50 μ m～Ti powder 45%～65% of 75 μ m, particle diameter and be 65 μ m～85 μ m are the C powder 15%～35% of 60 μ m～80 μ m; Each component total amount 100%; Uniform mixing obtains mixed powder
Or; By mole per-cent; TiC powder 15%～35% and the particle diameter of getting particle diameter respectively and be 50 μ m～Ti powder 45%～65% of 75 μ m, particle diameter and be 65 μ m～Si powder 5%～25% of 85 μ m, particle diameter and be 45 μ m～100 μ m are the C powder 5%～15% of 60 μ m～80 μ m; Each component total amount 100%, uniform mixing obtains mixed powder;
Step 2: the sticker of preparation dilution
Per-cent is by volume got sticker 30%～40% and ethanol 60%～70% respectively, and each component total amount 100% mixes, and makes the sticker after the dilution;
Step 3: preparation precast body
By mass percentage, get the sticker 10%～20% after the dilution that mixed powder 80%～90% that step 1 makes and step 2 make respectively, each component total amount 100% behind the thorough mixing, is processed blank, and oven dry makes precast body;
Step 4: melting infiltration sintering
The precast body surface coverage Si powder that made in the last step then, is put into hydrogen atmosphere protection sintering oven sintering; The heat-up rate of controlling in this protection stove is 10 ℃/min, slowly is warming up to 1000 ℃～1100 ℃, is incubated 30～40 minutes; It is 1300 ℃～1400 ℃ that continuation is warming up to temperature with the heat-up rate of 10 ℃/min, is incubated 30～40 minutes, afterwards; Continue slowly to be warmed up to that temperature is 1450 ℃～1650 ℃ in the protection stove with the heat-up rate of 5 ℃/min, be incubated 60～70 minutes, promptly make Ti 3SiC 2Material.
The inventive method adopts infiltration, sintering to make highly purified Ti 3SiC 2Material reduces Ti significantly through infiltration Si 3SiC 2The void content of material improves its density.Through detecting the Ti that makes 3SiC 2Ti in the material 3SiC 2Weight percentage reach more than the 92.3wt%, void content is lower, density has reached 85%～95%.
Description of drawings
Fig. 1 is that the inventive method employing Ti/Si/TiC/C is the Ti that raw material makes 3SiC 2The profile scanning electromicroscopic photograph of material;
Fig. 2 is that the inventive method employing Ti/Si/TiC/C is the Ti that raw material makes 3SiC 2The local magnified sweep electromicroscopic photograph of pore in the material;
Fig. 3 is that prior art employing Ti/Si/TiC/C is the Ti that raw material makes 3SiC 2The end face stereoscan photograph of material;
Fig. 4 is that prior art employing Ti/Si/TiC/C is the Ti that raw material makes 3SiC 2The local magnified sweep electromicroscopic photograph of pore in the material;
Fig. 5 is that the inventive method employing Ti/Si/TiC is the Ti that raw material makes 3SiC 2The profile scanning electromicroscopic photograph of material;
Fig. 6 is that the inventive method employing Ti/Si/C is the Ti that raw material makes 3SiC 2The profile scanning electromicroscopic photograph of material.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated.
The inventive method is a raw material with in Ti powder, Si powder and TiC powder or the C powder one or both, uniform mixing and process precast body after, through infiltration, sintering, the Ti that preparation purity is high, pore is few, density is high 3SiC 2Material.This method is carried out according to the following steps:
Step 1: mix powder
By mole per-cent; Si powder 5%～25% and the particle diameter of getting particle diameter respectively and be 50 μ m～Ti powder 45%～65% of 75 μ m, particle diameter and be 65 μ m～85 μ m are the TiC powder 15%～35% of 45 μ m～100 μ m, each component total amount 100%, uniform mixing; Obtain mixed powder
Or by a mole per-cent, Si powder 5%～25% and the particle diameter of getting particle diameter respectively and be 50 μ m～Ti powder 45%～65% of 75 μ m, particle diameter and be 65 μ m～85 μ m are the C powder 15%～35% of 60 μ m～80 μ m; Each component total amount 100%; Uniform mixing obtains mixed powder
Or; By mole per-cent; TiC powder 15%～35% and the particle diameter of getting particle diameter respectively and be 50 μ m～Ti powder 45%～65% of 75 μ m, particle diameter and be 65 μ m～Si powder 5%～25% of 85 μ m, particle diameter and be 45 μ m～100 μ m are the C powder 5%～15% of 60 μ m～80 μ m; Each component total amount 100%, uniform mixing obtains mixed powder;
Step 2: the sticker of preparation dilution
Per-cent is by volume got sticker 30%～40% and ethanol 60%～70% respectively, and each component total amount 100% mixes, and makes the sticker after the dilution;
Sticker is selected a kind of in resol, epoxy resin or the urethane for use.
Step 3: preparation precast body
By mass percentage, get the sticker 10%～20% after the dilution that mixed powder 80%～90% that step 1 makes and step 2 make respectively, each component total amount 100% behind the thorough mixing, is processed blank, and oven dry makes precast body;
Step 4: melting infiltration sintering
Get the precast body that makes of step and, then, put into hydrogen atmosphere protection sintering oven sintering at its surface coverage one deck Si powder; The heat-up rate of controlling in this protection stove is 10 ℃/min, slowly is warming up to 1000 ℃～1100 ℃, is incubated 30～40 minutes; It is 1300 ℃～1400 ℃ that continuation is warming up to temperature with the heat-up rate of 10 ℃/min, is incubated 30～40 minutes, afterwards; Continue slowly to be warmed up to that temperature is 1450 ℃～1650 ℃ in the protection stove with the heat-up rate of 5 ℃/min; Be incubated 60～70 minutes, take out, promptly make Ti 3SiC 2Material.
The inventive method as the guiding phase, helps Ti at an amount of Si of the surface coverage of precast body 3SiC 2Generation.Precast body is when 1300 ℃ sintering temperature, and the sintering neck between the TiC/Ti/Si powder forms, and its combination begins to change Chemical bond into by mechanical bond, and in the place that Si is arranged, sintering neck place begins to have a spot of Ti 3SiC 2Generate; The Ti that has generated 3SiC 2And chemically combined TiC/Ti forms the porous skeleton structure.Temperature is higher than 1300 ℃, and when the infiltration of Si did not take place, the content of simple substance Ti was higher than the content of Si in the precast body, preferentially generates Ti at the enrichment region of Ti 5Si 3, along with temperature continues to raise, few part Ti 5Si 3And β-Ti fusion earlier forms the Ti-Si liquid phase; When temperature arrives 1410 ℃; The Si powder fusion of precast body surface coverage under the effect of this fused Si powder capillary vessel power that pore produces in forming the porous skeleton structure, is infiltrated precast body through this pore; Along with the infiltration and the flow expansion of liquid Si, liquid Si and remaining Ti 5Si 3Form a large amount of Ti-Si liquid phases, the TiC in the precast body is coated, generate a large amount of Ti through liquid phase reaction 3SiC 2
Ti 3SiC 2Pore in the material, the Ti that mainly generates by reaction 3SiC 2And the hole that produces owing to the volatilization of sticker in gap in the material between the sintering neck of remaining TiC metallurgical binding and the sintering process constitutes.Because sintering generates Ti 3SiC 2The reaction of material makes precast body volumetric shrinkage occur, generates Ti so the inventive method through an amount of Si of infiltration, makes the volume of the Si that infiltrates precast body equal the precast body complete reaction 3SiC 2The volatilization of caking agent in the volume shrinkage mass that produces and the precast body and both sums of the hole volume that produces, so reduced Ti 3SiC 2The void content of material is prepared purity height, pore is few, density is high Ti 3SiC 2Material.
Embodiment 1
By mole per-cent; TiC powder 35% and the particle diameter of getting particle diameter respectively and be 50 μ m～Ti powder 45% of 75 μ m, particle diameter and be 65 μ m～Si powder 5% of 85 μ m, particle diameter and be 45 μ m～100 μ m are the C powder 15% of 60 μ m～80 μ m; Mix, make mixed powder; Per-cent is by volume got resol 30% and ethanol 70% respectively, and mixing and stirring makes the phenolic resin adhesive after the dilution; By mass percentage, get the phenolic resin adhesive 20% of mixed powder 80% that makes and the dilution that makes respectively, behind the thorough mixing, process blank,, obtain precast body this blank oven dry; At this precast body surface coverage one deck Si powder, then, put into hydrogen atmosphere protection sintering oven and carry out sintering, control this protection sintering oven and slowly heat up with the heat-up rate of 10 ℃/min; To temperature be 1000 ℃, be incubated 40 minutes, continue with 10 ℃/min heat-up rate, the temperature in the protection stove is risen to 1300 ℃; Be incubated 40 minutes, afterwards, slowly heat up with the heat-up rate of 5 ℃/min, temperature is 1450 ℃ to the stove; Be incubated 70 minutes and carry out sintering, take out, make Ti 3SiC 2Material.
Fig. 1 and Fig. 2 are respectively this Ti 3SiC 2The local magnified sweep electromicroscopic photograph of pore in the profile scanning electromicroscopic photograph of material and the material as can be seen from the figure, infiltrates the Si of precast body and the TiC and the Ti complete reaction on precast body top layer, and pore is filled obstruction gradually, and void content is very low, the Ti of generation 3SiC 2Material is very fine and close, records Ti 3SiC 2The density of material reaches 91.83%.
The Ti that adopts the existing method of identical component and content utilization to make 3SiC 2The local magnified sweep electromicroscopic photograph of pore is respectively like Fig. 3, shown in Figure 4 in the profile scanning electromicroscopic photograph of material and the material, as can be seen from the figure, and Ti 3SiC 2The material intermediate section is furnished with a lot of holes, and void content is very high, and through detecting, its density is 68.61%.
Embodiment 2
By mole per-cent; TiC powder 15% and the particle diameter of getting particle diameter respectively and be 50 μ m～Ti powder 65% of 75 μ m, particle diameter and be 65 μ m～Si powder 15% of 85 μ m, particle diameter and be 45 μ m～100 μ m are the C powder 5% of 60 μ m～80 μ m; Mix, make mixed powder; Per-cent by volume, extracting epoxy resin 40% and ethanol 60% respectively, mixing and stirring makes the epoxy adhesive after the dilution; By mass percentage, get the epoxy adhesive 10% of mixed powder 90% that makes and the dilution that makes respectively, behind the thorough mixing, process blank,, obtain precast body this blank oven dry; At surface coverage one deck Si of this precast body powder, and put into hydrogen atmosphere protection sintering oven and carry out sintering, control this protection sintering oven and slowly heat up with the heat-up rate of 10 ℃/min, to temperature be 1100 ℃; Be incubated 30 minutes, continue heat-up rate, the temperature in the protection stove is risen to 1400 ℃, be incubated 30 minutes with 10 ℃/min; Afterwards, slowly heat up with the heat-up rate of 5 ℃/min, temperature is 1650 ℃ to the stove; Be incubated 60 minutes and carry out sintering, take out, make Ti 3SiC 2Material.
Through detecting this Ti 3SiC 2Material density reaches 91.32%.And the Ti that adopts identical component and content to utilize prior art for preparing to obtain 3SiC 2The material void content obviously increases, and testing its density only has 66.32%
Embodiment 3
By mole per-cent; TiC powder 15% and the particle diameter of getting particle diameter respectively and be 50 μ m～Ti powder 50% of 75 μ m, particle diameter and be 65 μ m～Si powder 25% of 85 μ m, particle diameter and be 45 μ m～100 μ m are the C powder 10% of 60 μ m～80 μ m; Mix, make mixed powder; Per-cent is by volume got urethane 35% and ethanol 65% respectively, mixes, and makes the polyurethane adhesive after the dilution; By mass percentage, get the polyurethane adhesive 15% after the mixed powder that makes 85% and the dilution that makes respectively, behind the thorough mixing, process blank,, obtain precast body this blank oven dry; At this precast body surface coverage one deck Si powder, then, put into hydrogen atmosphere protection sintering oven and carry out sintering, control this protection stove and slowly heat up with the heat-up rate of 10 ℃/min; To temperature be 1050 ℃, be incubated 35 minutes, continue heat-up rate with 10 ℃/min, the temperature in the protection stove is risen to 1350 ℃; Be incubated 35 minutes, afterwards, slowly heat up with the heat-up rate of 5 ℃/min, temperature is 1550 ℃ to the stove; Be incubated 65 minutes and carry out sintering, take out, make Ti 3SiC 2Material.
Through detecting this Ti 3SiC 2The density of material reaches 92.21%.
Embodiment 4
By mole per-cent; TiC powder 25% and the particle diameter of getting particle diameter respectively and be 50 μ m～Ti powder 55% of 75 μ m, particle diameter and be 65 μ m～Si powder 10% of 85 μ m, particle diameter and be 45 μ m～100 μ m are the C powder 10% of 60 μ m～80 μ m; Mix, make mixed powder; Per-cent is by volume got urethane 32% and ethanol 68% respectively, mixes, and makes the polyurethane adhesive after the dilution; By mass percentage, get the polyurethane adhesive 12% after the mixed powder that makes 88% and the dilution that makes respectively, behind the thorough mixing, process blank,, obtain precast body this blank oven dry; At this precast body surface coverage one deck Si powder, then, put into hydrogen atmosphere protection sintering oven and carry out sintering, control this protection stove and slowly heat up with the heat-up rate of 10 ℃/min; To temperature be 1025 ℃, be incubated 32 minutes, continue heat-up rate with 10 ℃/min, the temperature in the protection stove is risen to 1375 ℃; Be incubated 32 minutes, afterwards, slowly heat up with the heat-up rate of 5 ℃/min, temperature is 1500 ℃ to the stove; Be incubated 62 minutes and carry out sintering, take out, make Ti 3SiC 2Material.
Through detecting this Ti 3SiC 2The density of material reaches 92.21%.
Embodiment 5
By mole per-cent, getting particle diameter respectively is that 50 μ m～Ti powder 45% of 75 μ m, particle diameter are that 65 μ m～Si powder 20% of 85 μ m, particle diameter are the TiC powder 35% of 45 μ m～100 μ m, mixes, and makes mixed powder; Then, method and the step according to embodiment 1 prepares Ti 3SiC 2Material.
This Ti 3SiC 2The end face stereoscan photograph of material, as shown in Figure 5, show among the figure that the pore in the material is less, density is high, through detecting this Ti 3SiC 2The density of material is 91.57%.
Embodiment 6
By mole per-cent, getting particle diameter respectively is that 50 μ m～Ti powder 65% of 75 μ m, particle diameter are that 65 μ m～Si powder 5% of 85 μ m, particle diameter are the TiC powder 30% of 45 μ m～100 μ m, mixes, and makes mixed powder; Then, method and the step according to embodiment 2 prepares Ti 3SiC 2Material.
Through detecting this Ti 3SiC 2The density of material is 93.23%.
Embodiment 7
By mole per-cent, getting particle diameter respectively is that 50 μ m～Ti powder 60% of 75 μ m, particle diameter are that 65 μ m～Si powder 25% of 85 μ m, particle diameter are the TiC powder 15% of 45 μ m～100 μ m, mixes, and makes mixed powder; Then, method and the step according to embodiment 3 prepares Ti 3SiC 2Material.
Through detecting this Ti 3SiC 2The density of material is 92.18%.
Embodiment 8
By mole per-cent, getting particle diameter respectively is that 50 μ m～Ti powder 45% of 75 μ m, particle diameter are that 65 μ m～Si powder 20% of 85 μ m, particle diameter are the C powder 35% of 60 μ m～80 μ m, mixes, and makes mixed powder; Then, method and the step according to embodiment 1 prepares Ti 3SiC 2Material.
This Ti 3SiC 2The end face stereoscan photograph of material, as shown in Figure 6, from figure, can find out that the pore of this material is less, material is fine and close, through detecting this Ti 3SiC 2The density of material is 92.43%.
Embodiment 9
By mole per-cent, getting particle diameter respectively is that 50 μ m～Ti powder 65% of 75 μ m, particle diameter are that 65 μ m～Si powder 5% of 85 μ m, particle diameter are the C powder 30% of 60 μ m～80 μ m, mixes, and makes mixed powder; Then, method and the step according to embodiment 2 prepares Ti 3SiC 2Material.
Through detecting this Ti 3SiC 2The density of material is 95%.
Embodiment 10
By mole per-cent, getting particle diameter respectively is that 50 μ m～Ti powder 60% of 75 μ m, particle diameter are that 65 μ m～Si powder 25% of 85 μ m, particle diameter are the C powder 15% of 60 μ m～80 μ m, mixes, and makes mixed powder; Then, method and the step according to embodiment 3 prepares Ti 3SiC 2Material.
Through detecting this Ti 3SiC 2The density of material is 90.36%.
The inventive method at first forms the porous skeleton structure through sintering; Continue to heat up and make the fusion of Si powder; Under the effect of the capillary vessel power that pore in porous skeleton structure produces, the melt of si powder infiltrates the pore in the porous skeleton structure, and forms the Ti-Si liquid phase with Ti in the skeleton structure; TiC in the skeleton structure is coated, and then generate Ti with the TiC reaction 3SiC 2Material, not only this Ti 3SiC 2The material void content is very low, and density has reached 85%～95%, and technology is simple, to preparing the less demanding of equipment.

Claims (2)

1. a melting infiltration sintering prepares Ti 3SiC 2The method of material is a raw material with in Ti powder, Si powder and TiC powder or the C powder one or both, uniform mixing and process precast body after, through infiltration, sintering, the Ti that preparation purity is high, pore is few, density is high 3SiC 2Material is characterized in that, this method is carried out according to the following steps:
Step 1: mix powder
By mole per-cent; Si powder 5%～25% and the particle diameter of getting particle diameter respectively and be 50 μ m～Ti powder 45%～65% of 75 μ m, particle diameter and be 65 μ m～85 μ m are the TiC powder 15%～35% of 45 μ m～100 μ m, each component total amount 100%, uniform mixing; Obtain mixed powder
Or by a mole per-cent, Si powder 5%～25% and the particle diameter of getting particle diameter respectively and be 50 μ m～Ti powder 45%～65% of 75 μ m, particle diameter and be 65 μ m～85 μ m are the C powder 15%～35% of 60 μ m～80 μ m; Each component total amount 100%; Uniform mixing obtains mixed powder
Or; By mole per-cent; TiC powder 15%～35% and the particle diameter of getting particle diameter respectively and be 50 μ m～Ti powder 45%～65% of 75 μ m, particle diameter and be 65 μ m～Si powder 5%～25% of 85 μ m, particle diameter and be 45 μ m～100 μ m are the C powder 5%～15% of 60 μ m～80 μ m; Each component total amount 100%, uniform mixing obtains mixed powder;
Step 2: the sticker of preparation dilution
Per-cent is by volume got sticker 30%～40% and ethanol 60%～70% respectively, and each component total amount 100% mixes, and makes the sticker after the dilution;
Step 3: preparation precast body
By mass percentage, get the sticker 10%～20% after the dilution that mixed powder 80%～90% that step 1 makes and step 2 make respectively, each component total amount 100% behind the thorough mixing, is processed blank, and oven dry makes precast body;
Step 4: melting infiltration sintering
The precast body surface coverage Si powder that made in the last step then, is put into hydrogen atmosphere protection sintering oven sintering; The heat-up rate of controlling in this protection sintering oven is 10 ℃/min, slowly is warming up to 1000 ℃～1100 ℃, is incubated 30～40 minutes; It is 1300 ℃～1400 ℃ that continuation is warming up to temperature with the heat-up rate of 10 ℃/min; Be incubated 30～40 minutes, afterwards, continue slowly to be warmed up to that temperature is 1450 ℃～1650 ℃ in the protection sintering oven with the heat-up rate of 5 ℃/min; Be incubated 60～70 minutes, promptly make Ti 3SiC 2Material.
2. method according to claim 1 is characterized in that, described sticker is selected a kind of in resol, epoxy resin or the urethane for use.
CN2008102323806A 2008-11-21 2008-11-21 Method for preparing Ti3SiC2 material by melting infiltration sintering Expired - Fee Related CN101423395B (en)

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CN102206079B (en) * 2011-03-29 2013-01-02 西北有色金属研究院 Method for preparing large-size Ti3SiC2 ceramic material
CN104018155B (en) * 2014-06-06 2016-03-30 江苏大学 The method of Ti-Si-C coating is prepared in surface of metal titanium
CN105149597B (en) * 2015-08-11 2018-09-11 利宝地工程有限公司 The reparation of metal or alloy component or connecting method and component that is repaired or being coupled
JP6763699B2 (en) * 2016-06-06 2020-09-30 イビデン株式会社 Manufacturing method of honeycomb structure
CN108358205B (en) * 2018-03-07 2020-03-10 中南大学 Ti3SiC2Powder synthesis method
CN108794013B (en) * 2018-07-26 2021-05-04 北京理工大学 B4C ceramic block and rapid preparation method thereof
CN109487110B (en) * 2018-12-20 2020-02-18 河南科技大学 In-situ self-generated Al2O3Prefabricated body for particle reinforced steel-based surface composite material, preparation method and application
CN111646799B (en) * 2020-05-10 2022-05-27 华北理工大学 Combustion method for preparing Tin+1ACnMethod of producing a material

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