CN116639998B - Porous silicon carbide ceramic material and preparation method thereof - Google Patents
Porous silicon carbide ceramic material and preparation method thereof Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910021426 porous silicon Inorganic materials 0.000 title claims abstract description 32
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title description 7
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical class O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000005245 sintering Methods 0.000 claims abstract description 33
- 239000000440 bentonite Substances 0.000 claims abstract description 18
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims abstract description 14
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 12
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims abstract description 12
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims abstract description 12
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 239000002270 dispersing agent Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 15
- 239000000919 ceramic Substances 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229920002125 Sokalan® Polymers 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000004584 polyacrylic acid Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 240000004808 Saccharomyces cerevisiae Species 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 239000011148 porous material Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000047 product Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000002277 temperature effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
The invention provides a porous silicon carbide ceramic material which is prepared from the following raw materials in parts by weight: 50-100 parts of silicon carbide powder, 10-35 parts of aluminum hydroxide powder, 1-8 parts of sintering aid, 0.1-5 parts of pore-forming agent, 0.1-5 parts of dispersing agent and 20-100 parts of deionized water; the sintering aid is modified bentonite. According to the porous silicon carbide ceramic material, modified bentonite is used as a sintering aid, sodium lignin sulfonate and bentonite are connected in a net manner through sodium carboxymethyl cellulose, so that the bonding strength and the bonding efficiency of the sintering aid and silicon carbide powder are improved, and the porosity and the mechanical property of the ceramic material are improved after sintering.
Description
Technical Field
The invention belongs to the field of aviation, and particularly relates to a porous silicon carbide ceramic material and a preparation method thereof.
Background
The porous silicon carbide ceramic has the advantages of good chemical stability, high mechanical strength, acid and alkali resistance, high temperature resistance and the like, and can be widely applied to various aspects such as aerospace, biomedical science, energy chemical industry, electronic devices and the like.
The pore-forming agent method commonly used for the porous silicon carbide ceramic material is to add an organic or inorganic pore-forming agent into the raw material, and the pore-forming agent leaves the green body under the high temperature effect through sintering, so that pores are formed in the green body, and the porous ceramic is obtained. As a traditional process, the method of adding the pore-forming agent has the advantages of mature process, simple flow, low operation difficulty, conventional required equipment and the like, and is widely used for large-scale production of porous silicon carbide ceramic materials. However, the porous silicon carbide ceramic prepared by the method has lower porosity, and if the porosity is improved by increasing the consumption of the pore-forming agent, the pore size distribution and the pore size of pores cannot be well controlled by the method, so that the internal defects of the material are also sharply increased while the pores are increased, the mechanical properties of the finally obtained material are poor, and the use of the material is affected.
Disclosure of Invention
In view of the above, the present invention aims to overcome the defects in the prior art, and provides a porous silicon carbide ceramic material and a preparation method thereof.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
the porous silicon carbide ceramic material is prepared from the following raw materials in parts by weight:
50-100 parts of silicon carbide powder,
10-35 parts of aluminum hydroxide powder,
1-8 parts of a sintering aid,
0.1-5 parts of pore-forming agent,
0.1-5 parts of dispersing agent,
20-100 parts of deionized water;
the sintering aid is modified bentonite.
Preferably, the porous silicon carbide ceramic is prepared from the following raw materials in parts by weight:
60-80 parts of silicon carbide powder,
20-35 parts of aluminum hydroxide powder,
1-8 parts of a sintering aid,
0.1-3 parts of pore-forming agent,
0.1-3 parts of dispersing agent,
40-80 parts of deionized water.
Further, the silicon carbide powder consists of silicon carbide fine powder and silicon carbide coarse powder in the mass ratio of 1:5-20, wherein the granularity of the silicon carbide fine powder is D 50 =0.5-2 μm, the silicon carbide coarse powder has a particle size of D 50 =3-10μm。
Preferably, the silicon carbide powder consists of silicon carbide fine powder and silicon carbide coarse powder in the mass ratio of 1:5-12.
Further, the modified bentonite is prepared by a method comprising the following steps: uniformly mixing sodium carboxymethyl cellulose with bentonite, and then ball-milling and blending with sodium lignin sulfonate to obtain the modified bentonite.
Further, the mass ratio of the sodium lignin sulfonate, the sodium carboxymethylcellulose and the bentonite is 1-10:0.1-5:100; the particle size of the bentonite is 0.1-1 mu m; the ball milling step is carried out for 10-60 minutes.
Preferably, the mass ratio of the sodium lignin sulfonate, the sodium carboxymethylcellulose and the bentonite is 1-6:0.1-2:100.
further, the dispersing agent is at least one of sodium hydroxide, tetramethyl ammonium hydroxide, polyacrylic acid or polyethylene glycol.
Further, the pore-forming agent is at least one of carbon powder, graphite powder or yeast powder.
The preparation method of the porous silicon carbide ceramic material comprises the following steps:
step 1, ball-milling and mixing silicon carbide powder, aluminum hydroxide powder, a sintering aid and deionized water, adding a dispersing agent and a pore-forming agent into the mixture, and uniformly stirring the mixture to obtain ceramic slurry;
and 2, injecting the ceramic slurry into a non-water-absorbing mold, standing, demolding, drying the obtained green body, and sintering at a high temperature to obtain the porous silicon carbide ceramic material.
Further, the time of the ball milling step in the step 1 is 1.5-3 hours.
Further, the temperature of the high-temperature sintering step in the step 2 is 1200-2000 ℃.
Compared with the prior art, the invention has the following advantages:
according to the porous silicon carbide ceramic material, modified bentonite is used as a sintering aid, sodium lignin sulfonate and bentonite are connected in a net manner through sodium carboxymethyl cellulose, so that the bonding strength and the bonding efficiency of the sintering aid and silicon carbide powder are improved, and the porosity and the mechanical property of the ceramic material are improved after sintering.
The porous silicon carbide ceramic material adopts silicon carbide fine powder and silicon carbide coarse powder to be matched with modified bentonite for preparing the porous material, and the silicon carbide powder and sintering auxiliary agent are fully combined according to the proportion of different particle sizes.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention pertains. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to examples.
Example 1
The porous silicon carbide ceramic material is prepared from the following raw materials in parts by weight: 72 parts of silicon carbide powder, 26 parts of aluminum hydroxide powder, 3 parts of sintering aid, 1.2 parts of graphite powder, 1.2 parts of polyacrylic acid and 60 parts of deionized water.
The silicon carbide powder consists of silicon carbide fine powder and silicon carbide coarse powder in the mass ratio of 1:8, and the granularity of the silicon carbide fine powder is D 50 =1.2 μm, the silicon carbide coarse powder has a particle size D 50 =8.0μm。
The sintering aid is modified bentonite, and the modified bentonite is prepared by a method comprising the following steps: uniformly mixing sodium carboxymethyl cellulose with bentonite, and then ball milling and blending with sodium lignin sulfonate for 40 minutes to obtain the modified bentonite. The mass ratio of the sodium lignin sulfonate, the sodium carboxymethylcellulose and the bentonite is 5:0.5:100.
the preparation method of the porous silicon carbide ceramic material comprises the following steps:
step 1, performing ball milling and mixing on silicon carbide powder, aluminum hydroxide powder, a sintering aid and deionized water for 2 hours, then adding a dispersing agent and a pore-forming agent into the mixture, and uniformly stirring to obtain ceramic slurry;
and 2, injecting the ceramic slurry into a non-water-absorbing mold, standing, demolding, drying the obtained green body, and sintering at a high temperature of 1500 ℃ to obtain the porous silicon carbide ceramic material.
Example 2
The porous silicon carbide ceramic material is prepared from the following raw materials in parts by weight: 72 parts of silicon carbide powder, 26 parts of aluminum hydroxide powder, 3 parts of sintering aid, 1.2 parts of graphite powder, 1.2 parts of polyacrylic acid and 60 parts of deionized water.
The silicon carbide powder consists of silicon carbide fine powder and silicon carbide coarse powder in the mass ratio of 1:10, and the granularity of the silicon carbide fine powder is D 50 =1.2 μm, the silicon carbide coarse powder has a particle size D 50 =8.0μm。
The sintering aid is modified bentonite, and the modified bentonite is prepared by a method comprising the following steps: uniformly mixing sodium carboxymethyl cellulose with bentonite, and then ball milling and blending with sodium lignin sulfonate for 40 minutes to obtain the modified bentonite. The mass ratio of the sodium lignin sulfonate, the sodium carboxymethylcellulose and the bentonite is 10:1:100.
the preparation method of the porous silicon carbide ceramic material comprises the following steps:
step 1, performing ball milling and mixing on silicon carbide powder, aluminum hydroxide powder, a sintering aid and deionized water for 2 hours, then adding a dispersing agent and a pore-forming agent into the mixture, and uniformly stirring to obtain ceramic slurry;
and 2, injecting the ceramic slurry into a non-water-absorbing mold, standing, demolding, drying the obtained green body, and sintering at a high temperature of 1500 ℃ to obtain the porous silicon carbide ceramic material.
Comparative example 1
Compared with example 1, the only difference is that: the modified bentonite is prepared by a method comprising the following steps: ball milling and blending bentonite and sodium lignin sulfonate for 40 minutes to obtain modified bentonite. The mass ratio of the sodium lignin sulfonate to the bentonite is 5:100.
comparative example 2
Compared with example 1, the only difference is that: the sintering aid is bentonite.
Comparative example 3
Compared with example 1, the only difference is that: the sintering aid is calcium oxide.
Comparative example 4
Compared with example 1, the only difference is that: the silicon carbide powder consists of silicon carbide fine powder and silicon carbide coarse powder in the mass ratio of 1:1. The granularity of the silicon carbide fine powder is D 50 =1.2 μm, the silicon carbide coarse powder has a particle size D 50 =8.0μm。
Comparative example 5
Compared with example 1, the only difference is that: the granularity of the silicon carbide powder is D 50 =8.0μm。
The porous silicon carbide ceramic products prepared in examples 1-2 and comparative examples 1-5 were subjected to performance test, and the results are shown in Table 1.
TABLE 1 results data
As shown in Table 1, the ceramic materials obtained in examples 1-2 have uniform and ordered porous structures, the sintering aid is prepared by directly using bentonite and sodium lignin sulfonate in comparative example 1, the bonding effect of sodium carboxymethylcellulose is avoided, the pore forming effect of the ceramic materials is affected, the bentonite is directly used as the sintering aid in comparative example 2, the pores of the final product are mostly closed pores, the pore size is larger, the conventional sintering aid is directly used in comparative example 3, the pore structure of the product is not ideal, excessive silicon carbide fine powder is added in comparative example 4, the pores of the product are also affected to a certain extent, and the pore forming effect of the product is also affected by silicon carbide powder with single particle size.
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 (7)
1. A porous silicon carbide ceramic material, characterized by: the porous silicon carbide ceramic is prepared from the following raw materials in parts by weight:
50-100 parts of silicon carbide powder,
10-35 parts of aluminum hydroxide powder,
1-8 parts of a sintering aid,
0.1-5 parts of pore-forming agent,
0.1-5 parts of dispersing agent,
20-100 parts of deionized water;
the sintering aid is modified bentonite;
the silicon carbide powder consists of silicon carbide fine powder and silicon carbide coarse powder with the mass ratio of 1:5-20, and the granularity of the silicon carbide fine powder is D 50 =0.5-2 μm, the silicon carbide coarse powder has a particle size of D 50 =3-10μm;
The modified bentonite is prepared by a method comprising the following steps: uniformly mixing sodium carboxymethylcellulose with bentonite, and then ball-milling and blending with sodium lignin sulfonate to obtain the modified bentonite;
the mass ratio of the sodium lignin sulfonate, the sodium carboxymethylcellulose and the bentonite is 1-10:0.1-5:100.
2. the porous silicon carbide ceramic material of claim 1, wherein: the particle size of the bentonite is 0.1-1 mu m; the ball milling step is carried out for 10-60 minutes.
3. The porous silicon carbide ceramic material of claim 1, wherein: the dispersing agent is at least one of sodium hydroxide, tetramethyl ammonium hydroxide, polyacrylic acid or polyethylene glycol.
4. The porous silicon carbide ceramic material of claim 1, wherein: the pore-forming agent is at least one of carbon powder, graphite powder or yeast powder.
5. A method for preparing a porous silicon carbide ceramic material according to any of claims 1 to 4, wherein: the method comprises the following steps:
step 1, ball-milling and mixing silicon carbide powder, aluminum hydroxide powder, a sintering aid and deionized water, adding a dispersing agent and a pore-forming agent into the mixture, and uniformly stirring the mixture to obtain ceramic slurry;
and 2, injecting the ceramic slurry into a non-water-absorbing mold, standing, demolding, drying the obtained green body, and sintering at a high temperature to obtain the porous silicon carbide ceramic material.
6. The method for preparing a porous silicon carbide ceramic material according to claim 5, wherein: the ball milling step in the step 1 is carried out for 1.5-3 hours.
7. The method for preparing a porous silicon carbide ceramic material according to claim 5, wherein: the temperature of the high-temperature sintering step in the step 2 is 1200-2000 ℃.
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