CN115368138B - 一种微波制备Si2N2O结合碳化硅陶瓷的方法 - Google Patents
一种微波制备Si2N2O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 67
- 239000000919 ceramic Substances 0.000 title claims abstract description 54
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 26
- 229910002790 Si2N2O Inorganic materials 0.000 title description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 44
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 238000009768 microwave sintering Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000012298 atmosphere Substances 0.000 claims abstract description 11
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 11
- 238000005303 weighing Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims description 18
- 239000002002 slurry Substances 0.000 claims description 17
- 239000011863 silicon-based powder Substances 0.000 claims description 13
- 238000000498 ball milling Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 239000006004 Quartz sand Substances 0.000 claims description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 9
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 5
- 229920000877 Melamine resin Polymers 0.000 claims description 4
- 238000000462 isostatic pressing Methods 0.000 claims description 4
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 4
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 3
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 239000003999 initiator Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 3
- 229910021426 porous silicon Inorganic materials 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 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 description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 2
- 229920000053 polysorbate 80 Polymers 0.000 claims description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 2
- 239000002699 waste material Substances 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 38
- 229910052710 silicon Inorganic materials 0.000 abstract description 21
- 239000010703 silicon Substances 0.000 abstract description 21
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 20
- 239000000463 material Substances 0.000 abstract description 10
- 238000005245 sintering Methods 0.000 abstract description 9
- 238000000465 moulding Methods 0.000 abstract description 6
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- 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
- 239000000839 emulsion Substances 0.000 description 3
- 238000005187 foaming Methods 0.000 description 3
- 239000011819 refractory material Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 2
- 239000007767 bonding agent Substances 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 238000000614 phase inversion technique Methods 0.000 description 2
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- 229910021487 silica fume Inorganic materials 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
本发明提供了一种微波制备Si2N2O结合碳化硅陶瓷的方法，按照二氧化硅和碳化硅的摩尔比为1:1～20称取硅源和碳化硅，氮源以混料或烧结气氛的形式添加；将其均匀混合后，按照一定的成型方法制得坯体；将坯体置于微波烧结炉中，在氮气或真空的气氛保护下，以0.1～3KW/min的速度提升输入功率，升温至900～1200℃后，保温0～30min，硅源和氮源反应生成Si2N2O，实现Si2N2O结合碳化硅陶瓷的烧成。本发明借助微波烧结时碳化硅自身的发热实现烧结，Si2N2O的热震稳定性和抗氧化性能良好；加热过程减少热能损耗，能源利用率高，Si2N2O受热结合均匀度好，制备的Si2N2O结合碳化硅制品强度高，抗腐蚀性好，具有广阔的应用前景。
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Si2N2O结合碳化硅陶瓷的方法。
背景技术
氮化硅结合碳化硅材料由于具有强度高(普通耐火材料的4～8倍)、热膨胀系数低(高铝材料的一半)，热震稳定性好、荷重软化点高、导热性能好、电阻阻值高、抗侵蚀性能优异等性能，在炼铝、铜、锌，炼钢及轧钢，炼铁，金属热处理，环境保护等领域有广泛的应用前景。
Si2N2O与Si3N4材料相比，有相似的热学和力学性能，但其热震稳定性、抗氧化性能及化学稳定性要优于Si3N4，所以Si2N2O结合SiC陶瓷在耐火材料、发动机的耐热组件、高温绝缘材料等方面有着更为广阔的应用前景。
然而，目前Si2N2O结合SiC陶瓷的烧成温度普遍在1400℃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Si2N2O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Si2N2O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，加热相邻的硅源和氮源，实现Si2N2O的均匀合成。无需借助外界热源，加热过程能源利用率高，硅源和氮源受热结合均匀度好，制备的Si2N2O结合碳化硅陶瓷制品强度高，抗腐蚀性好。
发明提供了一种微波制备Si2N2O结合碳化硅陶瓷的方法，具体包括以下步骤：(1)将硅源、氮源和碳化硅粉体均匀混合后成型制得坯体，或者将硅源和碳化硅粉体均匀混合后成型制得坯体并在后续的微波烧结工序采用氮气气氛(氮气此时作为氮源)；(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，硅源和氮源反应生成Si2N2O，实现Si2N2O结合碳化硅陶瓷的烧成。
进一步地，所述的硅源包括但不限于二氧化硅粉体，石英砂，硅粉，硅微粉，硅溶胶，白炭黑，正硅酸乙酯等中的一种或多种。
进一步地，所述的氮源包括但不限于氮化硅，氮气，三聚氰胺，尿素等。
进一步地，所述的Si2N2O结合碳化硅陶瓷为致密陶瓷或多孔陶瓷。
进一步地，所述的硅源中硅与碳化硅粉体的摩尔比为1:1～20。
进一步地，所述的粉体成型方式包括但不限于干压，等静压，凝胶成型，挤出成型等。
进一步地，所述的Si2N2O结合碳化硅陶瓷若为多孔陶瓷，造孔方式采用包括但不限于发泡法，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900～1200℃后，保温0～30min，烧结气氛为氮气或真空。
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，实现硅源和氮源受热均匀，加快反应速率，省去了巨大的能耗，烧成温度低(900℃～1200℃)，保温时间短(<30min)，能源利用率高，抗腐蚀性好。
(2)本发明加入的烧结助剂为Si2N2O，Si2N2O具有良好的热震稳定性和抗氧化性，制成的Si2N2O结合碳化硅制品强度高；Si2N2O结合碳化硅陶瓷在耐火材料、发动机的耐热组件、高温绝缘材料等方面有着广阔的应用前景。
附图说明
图1为本发明实施例4所得Si2N2O结合碳化硅陶瓷的扫描电镜图。
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。
本发明提供了一种微波制备Si2N2O结合碳化硅陶瓷的方法，具体包括以下步骤：(1)将硅源、氮源和碳化硅粉体均匀混合后成型制得坯体，或者将硅源和碳化硅粉体均匀混合后成型制得坯体并在后续的微波烧结工序采用氮气气氛(氮气此时作为氮源)；(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，硅源和氮源反应生成Si2N2O，实现Si2N2O结合碳化硅陶瓷的烧成。
进一步地，所述的硅源包括但不限于二氧化硅粉体，石英砂，硅粉，硅微粉，硅溶胶，白炭黑，正硅酸乙酯等中的一种或多种。
进一步地，所述的氮源包括但不限于氮化硅，氮气，三聚氰胺，尿素等。
进一步地，所述的Si2N2O结合碳化硅陶瓷为致密陶瓷或多孔陶瓷。
进一步地，所述的硅源中硅与碳化硅粉体的摩尔比为1:1～20。
进一步地，所述的粉体成型方式包括但不限于干压，等静压，凝胶成型，挤出成型等。
进一步地，所述的Si2N2O结合碳化硅陶瓷若为多孔陶瓷，造孔方式采用包括但不限于发泡法，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900～1200℃后，保温0～30min，烧结气氛为氮气或真空。
下面以具体实施例对本发明进行详细说明：
实施例1：
按照硅和碳化硅的摩尔比为1:10的比例称取，石英砂、氮化硅(占石英砂质量的20％)和碳化硅粉体，加入占粉体质量6％纸浆废液为结合剂进行混料，然后后在干压成型机上以100MPa的压力成型，最后置于微波烧结炉中，在真空气氛下，以0.6KW/min速率提升微波输入功率，升温至1200℃保温20min后制得Si2N2O结合碳化硅陶瓷，其抗折强度可达65MPa。
实施例2：
按照硅和碳化硅的摩尔比为1:12的比例称取，硅粉、硅溶胶(硅粉和硅溶胶质量比为1:2)和碳化硅粉体，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10％且占粉体质量为0.6％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2d后脱模，并在110℃下烘烤24h，最后置于微波烧结炉中，在氮气气氛下，以0.3KW/min速率提升微波输入功率，升温至900℃保温10min后制得Si2N2O结合碳化硅陶瓷，其抗折强度可达62MPa。
实施例3：
按照硅和碳化硅的摩尔比为1:15的比例称取，硅粉、二氧化硅(硅粉和二氧化硅质量比为1:2)和碳化硅粉体置于球磨罐中，在球磨罐中同时加入占粉体质量50％的水，3％的丙烯酰胺(作为凝胶单体)，0.3％的N，N'-亚甲基双丙烯酰胺(作为交联剂)，2％的十二烷基硫酸钠(作为发泡剂)，进行球磨混料2h后制得陶瓷浆料(发泡法造孔方式制备多孔陶瓷)，将陶瓷浆料置于搅拌桶中，搅拌的同时加入浓度为30％且占粉体质量为0.5％的过硫酸铵溶液(作为引发剂)和占粉体质量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，在氮气气氛下，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Si2N2O结合碳化硅陶瓷，其抗折强度可达34MPa。
实施例4：
按照硅和碳化硅的摩尔比为1:18的比例称取，硅粉、二氧化硅(硅粉和二氧化硅质量比为1:2)和碳化硅粉体置于球磨罐中，在球磨罐中同时加入占粉体质量50％的水，3％的丙烯酰胺(作为凝胶单体)，0.3％的N，N'-亚甲基双丙烯酰胺(作为交联剂)，与水体积比为1:1的正辛烷(作为造孔剂)，占水质量2％的吐温80(作为乳化剂)，进行球磨混料2h后制得陶瓷浆料(乳液法造孔制备多孔陶瓷，乳液法制备的孔径较小)，将陶瓷浆料置于搅拌桶中，搅拌的同时加入浓度20％且占粉体质量为0.3％的过硫酸铵溶液(作为引发剂)和占粉体质量0.2％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，在氮气气氛下，以0.3KW/min速率提升微波输入功率，升温至1100℃保温20min后制得多孔Si2N2O结合碳化硅陶瓷，其抗折强度可达38MPa。
图1是本实施例所制得的Si2N2O结合碳化硅陶瓷的扫描电镜图，从图中可知碳化硅颗粒间生长了晶粒发育良好的具有片状结构的Si2N2O，且利用乳液法制备出了孔径小于20μm的多孔Si2N2O结合碳化硅陶瓷。
实施例5：
按照硅和碳化硅的摩尔比为1:5的比例称取，石英砂、三聚氰胺(占石英砂质量的10％)和碳化硅粉体，加入固含量为3％的且占粉体质量5％羧甲基纤维素钠作为结合剂进行混料，困料24h后在等静压成型机上以20MPa的压力成型，最后置于微波烧结炉中，在氮气气氛下，以0.4KW/min速率提升微波输入功率，升温至1000℃保温20min后制得Si2N2O结合碳化硅陶瓷，其抗折强度可达78MPa。
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 (4)
1.一种微波制备Si2N2O结合碳化硅陶瓷的方法，其特征在于具体包括以下步骤：按照硅和碳化硅的摩尔比为1:18称取硅粉、二氧化硅和碳化硅粉体置于球磨罐中，二氧化硅与硅粉的质量比为2:1，在球磨罐中加入占粉体质量50%的水、3%的丙烯酰胺、0.3%的N，N'-亚甲基双丙烯酰胺、与水体积比为1:1的正辛烷、占水质量2%的吐温80，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20%且占粉体质量为0.3%的过硫酸铵溶液作为引发剂、占粉体质量0.2%的N，N，N'，N'-四甲基乙二胺作为催化剂，搅拌10 min后将浆料浇注于模具中，经空气气氛干燥3 d后脱模，并在110 ℃烘烤24 h得到坯体，将坯体置于微波烧结炉中，在氮气气氛下，以0.3 KW/min速率提升微波输入功率，升温至1100 ℃保温20 min后得到多孔Si2N2O结合碳化硅陶瓷。
2.一种微波制备Si2N2O结合碳化硅陶瓷的方法，其特征在于具体包括以下步骤：按照硅和碳化硅的摩尔比为1:10称取石英砂和碳化硅粉体，称取占石英砂质量20%的氮化硅，加入占粉体质量6%纸浆废液进行均匀混料，在干压成型机上以100 MPa的压力成型制得坯体，将坯体置于微波烧结炉中，在真空条件下，以0.6 KW/min速率提升微波输入功率，升温至1200℃保温20 min后得到Si2N2O结合碳化硅陶瓷。
3.一种微波制备Si2N2O结合碳化硅陶瓷的方法，其特征在于具体包括以下步骤：按照硅和碳化硅的摩尔比为1:12称取硅粉、硅溶胶和碳化硅粉体，硅粉和硅溶胶质量比为1:2，放入球磨机均匀混料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10%且占粉体质量为0.6%的氯化铵溶液，搅拌20 min后将浆料浇注于模具中，经空气气氛干燥2 d后脱模，并在110 ℃烘烤24 h得到坯体，将坯体置于微波烧结炉中，在氮气气氛下，以0.3 KW/min速率提升微波输入功率，升温至900 ℃保温10 min后得到Si2N2O结合碳化硅陶瓷。
4.一种微波制备Si2N2O结合碳化硅陶瓷的方法，其特征在于具体包括以下步骤：按照硅和碳化硅的摩尔比为1:5的比例称取石英砂和碳化硅粉体，加入占石英砂质量10%的三聚氰胺，并加入固含量为3%的且占粉体质量5%羧甲基纤维素钠进行混料，困料24 h后在等静压成型机上以20 MPa的压力成型，最后置于微波烧结炉中，在氮气气氛下，以0.4 KW/min速率提升微波输入功率，升温至1000 ℃保温20 min后制得Si2N2O结合碳化硅陶瓷。
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