CN112573927A - 一种氮化硅陶瓷粉体及其制备工艺 - Google Patents
一种氮化硅陶瓷粉体及其制备工艺 Download PDFInfo
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 55
- 239000000919 ceramic Substances 0.000 title claims abstract description 51
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000000843 powder Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 46
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 40
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000007789 gas Substances 0.000 claims abstract description 23
- 239000006229 carbon black Substances 0.000 claims abstract description 21
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 21
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 20
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 229910052786 argon Inorganic materials 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 6
- 239000004005 microsphere Substances 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 229920000609 methyl cellulose Polymers 0.000 claims description 7
- 239000001923 methylcellulose Substances 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- 238000001694 spray drying Methods 0.000 claims description 6
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 5
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 5
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 5
- 239000000395 magnesium oxide Substances 0.000 claims description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 5
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- PLUHAVSIMCXBEX-UHFFFAOYSA-N azane;dodecyl benzenesulfonate Chemical compound N.CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 PLUHAVSIMCXBEX-UHFFFAOYSA-N 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 3
- 239000005751 Copper oxide Substances 0.000 claims description 3
- 241000872198 Serjania polyphylla Species 0.000 claims description 3
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 3
- 229910000431 copper oxide Inorganic materials 0.000 claims description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 3
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- 229920000193 polymethacrylate Polymers 0.000 claims description 3
- VKFFEYLSKIYTSJ-UHFFFAOYSA-N tetraazanium;phosphonato phosphate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[O-]P([O-])(=O)OP([O-])([O-])=O VKFFEYLSKIYTSJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 3
- 229940075624 ytterbium oxide Drugs 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 230000017525 heat dissipation Effects 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract 1
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
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- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
本发明涉及一种氮化硅陶瓷粉体及其制备工艺，通过水煤气和催化剂作用下制备氮化硅粉体、高导热陶瓷的制备工艺,氮化硅陶瓷粉体由以下重量配比的原料制成：纳米气相二氧化硅6%～11%，白炭黑80%～89%，分散剂1%～3%，氧化物4%～6%，氮化硅陶瓷粉体的制备工艺。本发明的氮化硅陶瓷粉体以金属氧氮化物作为烧结助剂，可实现低温快速氮化，同时提前加入可以免除后期酸洗过程，简化操作工艺；旋转炉的使用可以实现快速散热；水煤气便宜易得，还原性好；将氮气和氩气混合气体代替氮气制取氮化硅粉，可大大加快反应速度，解决了现有技术中制备周期长、工艺复杂且制备的氮化硅陶瓷粉体纯度不高，进而导致的氮化硅陶瓷致密性不高，导热系数低的技术问题。
Description
技术领域
本发明涉及陶瓷材料领域，特别是指一种氮化硅陶瓷粉体及其制备工艺。
背景技术
随着绿色能源的发展，我国对高导热氮化硅陶瓷的需求日益增多，国内在高导热氮化硅方面的研究相对落后，现有的产品绝大多数依赖进口，亟待研究及实现产品化。
目前氮化硅陶瓷高热导率的获得通常需要在高温、高氮压环境下长时间烧结以促进晶内和晶间的纯化，这对设备要求极高的同时也带来了生产效率低生产成本高昂的缺点。同时，高性能氮化硅陶瓷材料的制备对氮化硅粉体的品质提出了更高的要求，这就要求氮化硅粉体有较高的纯度以保证制品的性能，较高的α相、较小的粒径及规则的形貌以获得好的烧结活性。有鉴于此，针对氮化硅陶瓷材料的技术弱点，想要突破其广泛应用的瓶颈，就要从根本上解决其技术问题。
发明内容
本发明提供一种氮化硅陶瓷粉体及其制备工艺，以克服上述现有技术存在的缺点。
本发明采用如下技术方案：
一种氮化硅陶瓷粉体，上述氮化硅陶瓷粉体由以下重量配比的原料制成：纳米气相二氧化硅6%～11%，白炭黑80%～89%，分散剂1%～3%，氧化物4%～6%。
进一步改进地，上述纳米气相二氧化硅的规格为10～30nm，优选纳米气相二氧化硅的规格为20nm。
进一步改进地，上述白炭黑的规格为325～1000目，优选白炭黑的规格为500目。
进一步改进地，上述分散剂为焦磷酸铵、聚丙烯酸铵、甲基纤维素、聚甲基丙烯酸铵、十二烷基苯磺酸铵、聚乙二醇中的一种或多种，优选的分散剂为甲基纤维素。
进一步改进地，上述的氧化物为氧化镁、氧化钙、氧化钴、氧化钇、氧化镱、氧化铜、氧化铝、氧化铈、氧化铬中的一种或多种。
一种氮化硅陶瓷粉体的制备工艺，上述制备工艺包括以下步骤：
步骤S1：将不同颗粒度的纳米气相二氧化硅和白炭黑混合，然后加入合适的分散剂、水、氧化物、微球，球料比1:（5～10），优选的球料比1：5，球磨10～20小时，优选的球磨时间为15小时，然后经过喷雾干燥得到分散性良好的混合粉体；
步骤S2：旋转炉中抽真空，在1000～1400℃通入水煤气1～15小时后，再将氮气和氩气的混合气体通入炉体，反应3～24小时得到掺杂a-氮化硅陶瓷粉体，优选的反应温度为1350℃，反应时间为4小时；
步骤S3：在1600～1800℃，氮气压力为1～10Mpa的环境中烧结2～24小时，得到导热系数为68～90w/m.k的高导热陶瓷，陶瓷烧结温度为1740℃。
进一步改进地，上述微球为氧化铝、氧化锆或氮化硅微球中的一种或多种，优选的微球为氧化铝微球。
进一步改进地，上述微球的直径为0.1～2mm，优选直径为2mm。
进一步改进地，上述纳米气相二氧化硅、白炭黑、分散剂和氧化物的总质量与水的质量之比为1：（1～2），优选纳米气相二氧化硅、白炭黑、分散剂和氧化物的总质量与水的质量之比为1：1。
进一步改进地，上述混合气体的氮气与氩气的体积之比为（80～95）：（20～5），优选氮气与氩气的体积之比为80:20。
由上述对本发明的描述可知，和现有技术相比，本发明具有如下优点：本发明的氮化硅陶瓷粉体选择二氧化硅为原料，水和碳的反应产物水煤气为反应介质，金属氧氮化物或微球为烧结助剂，旋转炉为反应容器，于水煤气下还原，然后在混合气体下氮化，得到掺杂a-氮化硅陶瓷粉体，氮气气氛下压力烧结，得到导热系数较高的陶瓷材料。其制备工艺为：将两种不同颗粒度的二氧化硅混合，然后加入合适的分散剂、水、氧化物、微球，球料比1:5～10，球磨10～20小时，然后经过喷雾干燥得到分散性良好的混合粉体；旋转炉中抽真空，在1000～1400℃通入水煤气1～15小时后，再将氮气和氩气混合气体通入炉体，烧结3～24小时，得到掺杂a-氮化硅陶瓷粉体，最后在1600～1800℃下，1～10Mpa氮气压力下烧结2～24小时，得到导热系数为68～90w/m.k的高导热陶瓷。
本发明提供的氮化硅粉体、高导热陶瓷的制备工艺，以金属氧氮化物得还原物活性金属为烧结助剂，可实现低温快速氮化，同时免除后期酸洗过程，简化操作工艺；旋转炉的使用可实现快速散热；水煤气便宜易得，还原性好；氮气和氩气混合气体代替氮气制取氮化硅粉，可有效控制a-氮化硅向β-氮化硅转化，解决了现有技术中制备周期长、工艺复杂且制备的氮化硅陶瓷粉体纯度不高，进而导致的氮化硅陶瓷致密性不高，导热系数低的技术问题，以达到高导热氮化硅陶瓷低温制备的目的。
具体实施方式
实施方式一：
一种氮化硅陶瓷粉体，上述氮化硅陶瓷粉体由以下重量配比的原料制成：纳米气相二氧化硅8%，白炭黑85%，十二烷基苯磺酸铵2%，氧化镁5%。
上述纳米气相二氧化硅的规格为10～30nm，优选纳米气相二氧化硅的规格为20nm。
上述白炭黑的规格为325～1000目，优选白炭黑的规格为500目。
上述分散剂为焦磷酸铵、聚丙烯酸铵、甲基纤维素、聚甲基丙烯酸铵、十二烷基苯磺酸铵、聚乙二醇中的一种或多种，优选的分散剂为甲基纤维素。
上述的氧化物为氧化镁、氧化钙、氧化钴、氧化钇、氧化镱、氧化铜、氧化铝、氧化铈、氧化铬中的一种或多种。
一种氮化硅陶瓷粉体的制备工艺，上述制备工艺包括以下步骤：
步骤S1：将不同颗粒度的纳米气相二氧化硅8g和白炭黑85g混合，然后加入合适的十二烷基苯磺酸钠2g、水100ml、氧化镁5g、直径为2.0mm的氧化铝微球40g，球料比1:（5～10），优选的球料比1：5，球磨10小时，然后经过喷雾干燥得到分散性良好的混合粉体；
步骤S2：氧化铝管旋转炉中抽真空，在1300℃通入水煤气5小时后，再将氮气和氩气的混合气体通入炉体，氮气与氩气的体积之比为80:20，反应3～24小时得到掺杂a-氮化硅陶瓷粉体，优选的反应温度为1350℃，反应时间为4小时；
步骤S3：在1700℃，氮气压力为4Mpa的环境中烧结24小时，得到导热系数为89w/m.k的高导热陶瓷。
上述纳米气相二氧化硅、白炭黑、分散剂和氧化物的总质量与水的质量之比为1：（1～2），优选纳米气相二氧化硅、白炭黑、分散剂和氧化物的总质量与水的质量之比为1：1。
实施方式二：
一种氮化硅陶瓷粉体，上述氮化硅陶瓷粉体由以下重量配比的原料制成：纳米气相二氧化硅10%，白炭黑82%，甲基纤维素2%，氧化铈2%，氧化铝4%。
一种氮化硅陶瓷粉体的制备工艺，上述制备工艺包括以下步骤：
步骤S1：将10g纳米气相二氧化硅与82g白炭黑进行混合，然后加入2g甲基纤维素，100ml水，2g氧化铈，4克氧化铝，40g直径为1.8mm的氧化铝微球，球磨15小时后，经过喷雾干燥后得到分散性好的混合粉体；
步骤S2：将氧化铝管旋转炉抽真空，在1270℃通入水煤气4小时后，再将体积比为80：20的氮气和氩气的混合气体通入炉体，反应6小时，得到掺杂a-氮化硅陶瓷粉体；
步骤S3：最后1720℃压力烧结，2Mpa压力下烧结15小时，得到导热系数为76w/m.k的高导热陶瓷。
实施方式三：
一种氮化硅陶瓷粉体，上述氮化硅陶瓷粉体由以下重量配比的原料制成：纳米气相二氧化硅9%，白炭黑85%，聚乙二醇1%，氧化钴5%。
一种氮化硅陶瓷粉体的制备工艺，上述制备工艺包括以下步骤：
步骤S1：将9g纳米气相二氧化硅与85g白炭黑进行混合，然后加入1g聚丙烯酸钠，100ml水，5g氧化钴，40g直径为1.5mm的氧化铝微球，球磨20小时后，经过喷雾干燥后得到分散性好的混合粉体；
步骤S2：将金属钨旋转炉抽真空，在1200℃通入水煤气2小时后，将体积比为90：10的氮气和氩气的混合气体通入炉体，1350℃下反应8小时，得到掺杂a-氮化硅陶瓷粉体；
步骤S3：最后1750℃，5Mpa压力氮气环境下烧结10小时得到导热系数为81w/m.k的高导热陶瓷。
上述仅为本发明的具体实施方式，但本发明的设计构思并不局限于此，凡利用此构思对本发明进行非实质性的改动，均应属于侵犯本发明保护范围的行为。
Claims (10)
1.一种氮化硅陶瓷粉体，其特征在于，所述氮化硅陶瓷粉体由以下重量配比的原料制成：纳米气相二氧化硅6%～11%，白炭黑80%～89%，分散剂1%～3%，氧化物4%～6%。
2.如权利要求1所述的一种氮化硅陶瓷粉体，其特征在于：所述纳米气相二氧化硅的规格为10～30nm。
3.如权利要求1所述的一种氮化硅陶瓷粉体，其特征在于：所述白炭黑的规格为325～1000目。
4.如权利要求1所述的一种氮化硅陶瓷粉体，其特征在于：所述分散剂为焦磷酸铵、聚丙烯酸铵、甲基纤维素、聚甲基丙烯酸铵、十二烷基苯磺酸铵、聚乙二醇中的一种或多种。
5.如权利要求1所述的一种氮化硅陶瓷粉体，其特征在于：所述的氧化物为氧化镁、氧化钙、氧化钴、氧化钇、氧化镱、氧化铜、氧化铝、氧化铈、氧化铬中的一种或多种。
6.如权利要求1至5任一项所述的一种氮化硅陶瓷粉体的制备工艺，其特征在于，所述制备工艺包括以下步骤：
步骤S1：将不同颗粒度的纳米气相二氧化硅和白炭黑混合，然后加入合适的分散剂、水、氧化物、微球，球料比1:（5～10），球磨10～20小时，然后经过喷雾干燥得到分散性良好的混合粉体；
步骤S2：旋转炉中抽真空，在1000～1400℃通入水煤气1～15小时后，再将氮气和氩气的混合气体通入炉体，反应3～24小时得到掺杂a-氮化硅陶瓷粉体；
步骤S3：在1600～1800℃，氮气压力为1～10Mpa的环境中烧结2～24小时，得到导热系数为68～90w/m.k的高导热陶瓷。
7.如权利要求6所述的一种氮化硅陶瓷粉体的制备工艺，其特征在于：所述微球为氧化铝、氧化锆或氮化硅微球中的一种或多种。
8.如权利要求6所述的一种氮化硅陶瓷粉体的制备工艺，其特征在于：所述微球的直径为0.1～2mm。
9.如权利要求6所述的一种氮化硅陶瓷粉体的制备工艺，其特征在于：所述纳米气相二氧化硅、白炭黑、分散剂和氧化物的总质量与水的质量之比为1：（1～2）。
10.如权利要求6所述的一种氮化硅陶瓷粉体的制备工艺，其特征在于：所述混合气体的氮气与氩气的体积之比为（80～95）：（20～5）。
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