CN115231926B - 一种微波制备莫来石结合碳化硅陶瓷的方法 - Google Patents
一种微波制备莫来石结合碳化硅陶瓷的方法 Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 63
- 239000000919 ceramic Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 21
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 title abstract description 28
- 229910052863 mullite Inorganic materials 0.000 title abstract description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000000465 moulding Methods 0.000 claims abstract description 12
- 238000009768 microwave sintering Methods 0.000 claims abstract description 10
- 239000012298 atmosphere Substances 0.000 claims abstract description 9
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 16
- 239000011812 mixed powder Substances 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 7
- 239000006004 Quartz sand Substances 0.000 claims description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 2
- 238000005056 compaction Methods 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 16
- 229910052782 aluminium Inorganic materials 0.000 abstract description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 14
- 239000010703 silicon Substances 0.000 abstract description 14
- 229910052710 silicon Inorganic materials 0.000 abstract description 14
- 238000005245 sintering Methods 0.000 abstract description 14
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 11
- 239000000377 silicon dioxide Substances 0.000 abstract description 9
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 9
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 238000004321 preservation Methods 0.000 abstract description 4
- 239000002002 slurry Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 8
- 239000003570 air Substances 0.000 description 7
- 238000000498 ball milling Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
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- 229910052786 argon Inorganic materials 0.000 description 2
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- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 description 2
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- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000000614 phase inversion technique Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
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- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 description 1
- 229910018540 Si C Inorganic materials 0.000 description 1
- 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 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 229910003465 moissanite Inorganic materials 0.000 description 1
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- 239000000843 powder Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供了一种微波制备莫来石结合碳化硅陶瓷的方法，按照二氧化硅、氧化铝和碳化硅的摩尔比为2:3:5～100称取硅源、铝源和碳化硅，将其均匀混合后按照一定的成型方法制得坯体；将成型后的坯体置于微波烧结炉中，在烧结气氛保护下，以0.1～3KW/min的速度提升输入功率，升温至900～1300℃后，保温0～1h，得到莫来石结合碳化硅陶瓷。本发明借助微波烧结时碳化硅自身的发热实现烧结，莫来石在高温下可提高制品的抗氧化性能；加热过程能耗低，莫来石产生迅速，结合均匀度好，烧成温度低，保温时间短；制备的莫来石结合碳化硅制品强度高，市场前景广阔。
Description
技术领域
本发明属于陶瓷材料技术领域，具体涉及一种微波制备莫来石结合碳化硅陶瓷的方法。
背景技术
SiC陶瓷由于具有热膨胀系数低，耐磨性能高，硬度高，化学稳定性好，热导率高，在高温下仍具有良好力学性能和抗氧化性能等特点，被广泛应用于制造保险柜，密封环，运钞车的防护等相关领域；是极有发展前景的结构陶瓷。
然而，Si-C的共价性质键是极强的，因此SiC的烧结需升高至2000℃以上，造成了极大的能源消耗。
为了降低烧成温度，研究人员尝试加入烧结助剂进行SiC陶瓷的烧成，其中，莫来石具有良好的抗氧化性，高温稳定性，其热膨胀系数(5.3×10-6/K在0～1000℃)与SiC(4.7×10-6/K在0～1000℃)相近；但是，目前莫来石结合碳化硅的烧成温度普遍在1500℃以上，且保温时间一般在3h以上，不仅增加能耗，且制品在传统加热方式的作用下，材料受热不均匀，难以制备出力学性能优异的莫来石结合SiC陶瓷。
发明内容
针对现有技术存在的问题，本发明提出一种微波制备莫来石结合碳化硅陶瓷的方法，采用微波加热，以SiC为热源，借助SiC的吸波特性使材料升温，加热硅源和铝源，实现均匀莫来石化反应。无需借助外界热源，加热过程能耗低，莫来石产生迅速，结合均匀度好，烧成温度低(900℃～1200℃)，保温时间短(<20min)，制备的莫来石结合碳化硅制品强度高。
本发明具体是通过以下技术方案来实现的，依据本发明提出的一种微波制备莫来石结合碳化硅陶瓷的方法，具体包括以下步骤：(1)将硅源、铝源和碳化硅粉体均匀混合后成型制得坯体；(2)将成型后的坯体置于微波烧结炉中，借助碳化硅粉体的吸波特性使材料升温，硅源和铝源发生原位莫来石化反应，实现莫来石结合碳化硅陶瓷的烧成。
进一步地，所述的硅源为二氧化硅粉体、二氧化硅溶胶、石英砂、硅粉、硅溶胶、白炭黑、正硅酸乙酯、稻壳中的一种或多种。
进一步地，所述的铝源为氧化铝，氢氧化铝，铝溶胶，聚合氯化铝，磷酸二氢铝等中的一种或多种。
进一步地，所述的莫来石结合碳化硅陶瓷为致密陶瓷或多孔陶瓷。
进一步地，所述的硅源、铝源、碳化硅粉体中的二氧化硅、氧化铝和碳化硅的摩尔比为2:3:5～100，即莫来石与碳化硅的摩尔比为1:1～1:20。
进一步地，所述的粉体成型方式包括干压，等静压，凝胶成型，挤出成型等。
进一步地，所述的莫来石结合碳化硅陶瓷若为多孔陶瓷，造孔方式采用包括发泡法，乳状液模板法、固态造孔剂法、有机泡沫浸渍法、相转化法等。
进一步地，所述的微波烧结制度为以0.1～3KW/min的速度提升输入功率，直至升温至900～1300℃后，保温0～1h，烧成气氛包括但不限于空气，氮气和氩气。
与现有技术相比，本发明具有以下有益效果：
(1)本发明采用微波加热的方式，借助SiC的吸波特性，以碳化硅自身为热源，加热硅源和铝源，实现均匀莫来石化反应，省去了巨大的能耗，反应效率高，速率快；烧成温度低，保温时间短，能源利用率高。
(2)本发明加入的烧结助剂为莫来石，莫来石具有良好的高温稳定性和抗氧化性，其膨胀系数也与碳化硅相近，制成的莫来石结合碳化硅制品强度高，其抗折强度最高可达108MPa。
附图说明
图1是本发明实施例2所得莫来石结合碳化硅陶瓷的扫描电镜图。
图2是本发明实施例2所得莫来石结合碳化硅陶瓷的XRD图。
图3是本发明实施例3所得莫来石结合碳化硅陶瓷的扫描电镜图。
图4是本发明实施例3所得莫来石结合碳化硅陶瓷的XRD图。
具体实施方式
为了更好地理解本发明的内容，下面将结合具体实施例和附图来进一步阐述本发明。以下实施例以本发明的技术为基础实施，给出了详细的实施方式和操作步骤，但本发明的保护范围不限于下述实施例。
本发明提出的一种微波制备莫来石结合碳化硅陶瓷的方法，具体包括以下步骤：
(1)按照二氧化硅、氧化铝和碳化硅的摩尔比为2:3:5～100称取硅源、铝源和碳化硅(即莫来石与碳化硅的摩尔比为1:1～1:20)，将其均匀混合后按照一定的成型方法制得坯体；
(2)将成型后的坯体置于微波烧结炉中，在烧结气氛保护下，以0.1～3KW/min的速度提升输入功率，升温至900～1300℃后，保温0～1h，得到莫来石结合碳化硅陶瓷。本发明借助碳化硅粉体的吸波特性使材料升温，硅源和铝源发生原位莫来石化反应，实现莫来石结合碳化硅陶瓷的烧成。
进一步地，所述的硅源选自二氧化硅粉体、二氧化硅溶胶、石英砂、硅粉、硅溶胶、白炭黑、正硅酸乙酯、稻壳中的一种或多种。
进一步地，所述的铝源铝源选自氧化铝，氢氧化铝，铝溶胶，聚合氯化铝，磷酸二氢铝中的一种或多种。
进一步地，所制备的莫来石结合碳化硅陶瓷为致密或多孔陶瓷。当制备多孔陶瓷时，采用的造孔方式可以选用发泡法，乳状液模板法、固态造孔剂法、有机泡沫浸渍法、相转化法等。
进一步地，所述的成型方式可以选用干压成型，等静压成型，凝胶成型，挤出成型等。
进一步地，所述的烧结气氛至少包括空气、氮气、氩气中的一种或多种。
下面以具体实施例对本发明进行详细说明：
实施例1：
按照二氧化硅、氧化铝和碳化硅的摩尔比为2:3:30的比例称取石英砂、氢氧化铝和碳化硅粉体混合均匀形成混合粉体，加入固含量为3％的且占混合粉体质量5％的聚乙烯醇作为结合剂进行混料，困料24h后在干压成型机上以70MPa的压力成型，最后置于微波烧结炉中，在氮气气氛下，以0.2KW/min速率提升微波输入功率，升温至950℃保温20min后制得莫来石结合碳化硅陶瓷，其抗折强度可达76.5MPa。
实施例2：
按照二氧化硅、氧化铝和碳化硅的摩尔比为2:3:60的比例称取固含量30％的二氧化硅溶胶、氧化铝和碳化硅粉体，球磨混料2h后制得陶瓷浆料，将陶瓷浆料置于搅拌桶中，搅拌的同时加入浓度为30％且占混合粉体质量0.5％的氯化铵溶液作为固化剂，继续搅拌20min后将浆料浇注于模具中，经空气气氛干燥3d后脱模，并在110℃下烘烤12h，最后置于微波烧结炉中，在空气气氛下，以0.5KW/min速率提升微波输入功率，升温至1100℃保温10min后制得莫来石结合碳化硅陶瓷，其抗折强度可达93MPa。
图1是本实施例所制备的莫来石结合碳化硅陶瓷的扫描电镜图，从图中可知碳化硅颗粒接触部位烧结良好，可见明显的烧结颈。
图2是本实施例所制备的莫来石结合碳化硅陶瓷的XRD图，从图中可知材料烧后由莫来石和碳化硅两相组成，莫来石相特征峰明显。
实施例3：
按照二氧化硅、氧化铝和碳化硅的摩尔比为2:3:50的比例称取二氧化硅粉体、氧化铝和碳化硅粉体，将硅源、铝源和碳化硅形成的混合物置于球磨罐中，在球磨罐中同时加入占混合物质量50％的水，占混合物质量3％的丙烯酰胺，占混合物质量0.3％的N，N'-亚甲基双丙烯酰胺，占混合物质量2％的十二烷基硫酸钠，其中丙烯酰胺和N，N'-亚甲基双丙烯酰胺为凝胶剂，十二烷基硫酸钠为发泡剂，进行球磨混料2h后制得陶瓷浆料，将陶瓷浆料置于搅拌桶中，搅拌的同时加入浓度为30％且占混合物为0.5％的过硫酸铵溶液(作为引发剂)和占混合物0.1％的N，N，N'，N'-四甲基乙二胺(作为催化剂)，继续搅拌10min后将浆料浇注于模具中，经空气气氛干燥3d后脱模，并在110℃下烘烤24h，最后置于微波烧结炉中，在氩气气氛下，以0.1KW/min速率提升微波输入功率，升温至1200℃保温20min后制得多孔莫来石结合碳化硅陶瓷，其抗折强度可达45MPa。
图3是本实施例所制备的多孔莫来石结合碳化硅陶瓷的扫描电镜图，从图中可知材料呈多孔结构，孔壁烧结致密。
图4是本实施例所制备的莫来石结合碳化硅陶瓷的XRD图，从图中可知材料烧后由莫来石和碳化硅两相组成，莫来石相特征峰明显。
实施例4：
按照二氧化硅、氧化铝和碳化硅的摩尔比为2:3:70的比例称取石英砂、氢氧化铝和碳化硅粉体形成混合粉体，加入固含量为3％的且占混合粉体质量5％聚乙烯醇作为结合剂进行混料，困料24h后在等静压成型机上以30MPa的压力成型，最后置于微波烧结炉中，在空气气氛下，以1KW/min速率提升微波输入功率，升温至1000℃保温20min后制得莫来石结合碳化硅陶瓷，其抗折强度可达108MPa。
实施例5：
按照二氧化硅、氧化铝和碳化硅的摩尔比为2:3:20的比例称取稻壳，氧化铝和碳化硅粉体形成混合粉体，加入固含量为2％的且占混合粉体质量3％羧甲基纤维素钠作为结合剂进行混料，困料24h后在干压成型机上以50MPa的压力成型，最后置于微波烧结炉中，在空气气氛下，以0.2KW/min速率提升微波输入功率，升温至1100℃保温10min后制得多孔莫来石结合碳化硅陶瓷，其抗折强度可达62MPa。
本发明可以根据以上制备方法具有其它形式的实施例，不再一一列举。因此，任何熟悉本专业的技术人员，在不脱离本发明技术方案范围内，依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰，均仍属于本发明技术方案的范围内。
Claims (1)
1.一种微波制备莫来石结合碳化硅陶瓷的方法，其特征在于具体包括以下步骤：
按照二氧化硅、氧化铝和碳化硅的摩尔比为2:3:70称取石英砂、氢氧化铝和碳化硅，将其混合形成混合粉体，在混合粉体中加入固含量为3％且占混合粉体质量5％的聚乙烯醇作为结合剂进行混料，困料24h后在等静压成型机上以30MPa的压力成型制得坯体，将坯体置于微波烧结炉中，在空气气氛保护下，以1KW/min的速度提升输入功率，升温至1000℃后，保温20min，得到莫来石结合碳化硅陶瓷，其抗折强度为108MPa。
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