CN113816753A - 一种原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法 - Google Patents
一种原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法 Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 46
- 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 claims abstract description 43
- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 43
- 239000011819 refractory material Substances 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 14
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000008187 granular material Substances 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 27
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000000227 grinding Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001570 bauxite Inorganic materials 0.000 claims abstract description 11
- 239000004927 clay Substances 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 11
- 229910052851 sillimanite Inorganic materials 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229920001353 Dextrin Polymers 0.000 claims abstract description 9
- 239000004375 Dextrin Substances 0.000 claims abstract description 9
- 235000019425 dextrin Nutrition 0.000 claims abstract description 9
- 230000032683 aging Effects 0.000 claims abstract description 8
- 238000003483 aging Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims description 9
- 238000000748 compression moulding Methods 0.000 claims description 5
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical group F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000009423 ventilation Methods 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 11
- 230000007246 mechanism Effects 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 238000003825 pressing Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 12
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 229910004291 O3.2SiO2 Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
本发明公开了一种原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法，包括以下步骤：将催化剂、氧化铝粉、高铝矾土粉、软质粘土、干糊精球粉磨预混后加水搅拌形成泥浆；将泥浆、烧结莫来石颗粒料和碳化硅颗粒料放入行星式强制混合机中搅拌，使泥浆均匀包裹在颗粒料的表面，通风干燥；干燥后的颗粒包裹料放入混合机中加入硅溶胶搅拌，把碳化硅粉、细硅线石、金属硅粉加入混合机中进行混碾，混好的原料困料后机压成型；高温烧成得成品。本发明通过加入催化剂的手段影响莫来石晶体的生长，使其晶核通过气固反应而沿C轴快速生长，形成莫来石晶须，莫来石晶须通过晶须拔出、晶须桥联、裂纹偏转等作用机制显著提高莫来石结合碳化硅材料的力学性能。
Description
技术领域
本发明属于耐火材料领域，具体涉及一种原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法。
背景技术
目前新型的氮化硅结合碳化硅材料因其优异的性能，已成为干熄焦斜道区主流耐火材料；但它的生产工艺要求十分严格，且在生产过程中还会发生氮化不透的问题。从使用条件来说，斜道区耐火材料需要在900℃左右的高温下具有足够的强度、低膨胀和较好的热震稳定性。传统的斜道区使用的耐火材料是莫来石- 碳化硅材料，该材料具有良好的抗氧化性、较好的热震稳定性、耐磨损和抗侵蚀性能；莫来石(化学式3Al2O3.2SiO2)是铝硅酸盐二元体系中最稳定的化合物。由于其晶体结构沿C轴结晶方向具有较高的生长速率，从而导致莫来石晶体的高度各向异性。在高温烧结的过程中，莫来石晶粒不断生长，会使莫来石的强度与韧性降低，同时由于线膨胀方向的不同，当温度快速下降时，晶相之间会产生应力破坏烧结体，导致莫来石室温下的力学性能较差。碳化硅属于脆性材料，其本身韧性差，与莫来石相形成的复合材料其韧性不会得到明显改善。
发明内容
发明目的：本发明目的是提供一种原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法。
技术方案：本发明公开的原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法，包括以下步骤：
S1、将催化剂、氧化铝粉、高铝矾土粉、软质粘土、干糊精球粉磨预混后加水搅拌形成泥浆；有利于莫来石晶相的形成和晶体沿特定方向生长；干糊精能使泥浆在烘干后具有一定的强度，不易被破坏，还可以为莫来石晶须的生长提供一定的空间；
S2、将泥浆、烧结莫来石颗粒料和碳化硅颗粒料放入行星式强制混合机中搅拌，使泥浆均匀包裹在颗粒料的表面，放入干燥箱干燥，得到干燥后的颗粒包裹料；把泥浆包裹在颗粒料的表面能使颗粒物更加圆整，实现更加紧密的堆积，降低气孔率；能使颗粒在坯体中的分布更加均匀，颗粒与颗粒之间由于充满基质料，所以在合理烧结制度下结合得更加牢固；
S3、干燥后的颗粒包裹料放入混合机中加入硅溶胶搅拌均匀，然后把碳化硅粉、细硅线石、金属硅粉加入混合机中进行混碾，混好的原料困料后机压成型；
S4、高温烧成得到成品。
其中，采用以下质量份数的原料：催化剂3-7份，氧化铝粉8-15份，高铝矾土粉10-15份，软质粘土5-8份，干糊精粉1-1.5份，烧结莫来石15-25份，碳化硅40-50份，细硅线石4-6份，金属硅粉1-2份。
进一步的，S1中，球磨预混后按质量比1：0.5-1加水。
进一步的，S2中，碳化硅颗粒料占碳化硅总量的70-80％。
进一步的，S2中，在100-120℃下通风干燥8-10h。
进一步的，S3中，硅溶胶加入量为干燥后的颗粒包裹料总质量的3-3.5％。
进一步的，S3中，混碾10-15min，困料22-26h。
进一步的，S4中，高温烧成制度为以5℃/min升温至400℃保温30min，以 7℃/min升温至700℃保温1h，再以相同的速率升温到980℃保温30min，作为等温处理，随后以4℃/min升温至1480℃保温5h，然后随炉冷却。
进一步的，催化剂为AlF3。
有益效果：本发明相对于现有技术：通过加入催化剂并以新的工艺的手段影响莫来石晶体的生长，使其晶核通过气固反应而沿C轴快速生长，形成莫来石晶须，莫来石晶须通过晶须拔出、晶须桥联、裂纹偏转等作用机制显著提高莫来石结合碳化硅材料的力学性能
具体实施方式
下面结合实施例对本发明做进一步描述。
实施例1
一种原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法，包括以下步骤：
准备以下质量份的原料：催化剂(AlF3)3份，氧化铝粉8份，高铝矾土粉 10份，软质粘土5份，干糊精粉1份，烧结莫来石15份，碳化硅40份，细硅线石4份，金属硅粉1份。
S1、将催化剂、氧化铝粉、高铝矾土粉、软质粘土、干糊精球粉磨预混后按质量比1：0.5加水搅拌形成泥浆；
S2、将泥浆、烧结莫来石颗粒料和碳化硅颗粒料(碳化硅颗粒料占碳化硅总量的70％)放入行星式强制混合机中搅拌，使泥浆均匀包裹在颗粒料的表面，放入干燥箱干燥，100℃下干燥8h，得到干燥后的颗粒包裹料；
S3、干燥后的颗粒包裹料放入混合机中加入颗粒包裹料总质量3％硅溶胶搅拌均匀，然后把碳化硅粉、细硅线石、金属硅粉加入混合机中进行混碾10min，混好的原料困料22h后机压成型；
S4、高温烧成，以5℃/min升温至400℃保温30min，以7℃/min升温至700℃保温1h，再以相同的速率升温到980℃保温30min，作为等温处理，随后以4℃/min 升温至1480℃保温5h，然后随炉冷却，得到成品。
成品性能：
显气孔率(％)：<13
体积密度(g/cm3)：>2.58
常温抗折强度(MPa)：>35
常温耐压强度(MPa)：>180
吸水率(％)：<4.5
高温抗折强度(MPa)：>22
荷重软化温度(℃)：>1700
实施例2
一种原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法，包括以下步骤：
准备以下质量份的原料：催化剂(AlF3)5份，氧化铝粉12份，高铝矾土粉13份，软质粘土6份，干糊精粉1.2份，烧结莫来石20份，碳化硅45份，细硅线石5份，金属硅粉1.5份。
S1、将催化剂、氧化铝粉、高铝矾土粉、软质粘土、干糊精球粉磨预混后按质量比1：0.8加水搅拌形成泥浆；
S2、将泥浆、烧结莫来石颗粒料和碳化硅颗粒料(碳化硅颗粒料占碳化硅总量的75％)放入行星式强制混合机中搅拌，使泥浆均匀包裹在颗粒料的表面，放入干燥箱干燥，110℃下通风干燥9h，得到干燥后的颗粒包裹料；
S3、干燥后的颗粒包裹料放入混合机中加入颗粒包裹料总质量3.3％硅溶胶搅拌均匀，然后把碳化硅粉、细硅线石、金属硅粉加入混合机中进行混碾13min，混好的原料困料24h后机压成型；
S4、高温烧成，以5℃/min升温至400℃保温30min，以7℃/min升温至700℃保温1h，再以相同的速率升温到980℃保温30min，作为等温处理，随后以4℃/min 升温至1480℃保温5h，然后随炉冷却，得到成品。
成品性能：
显气孔率(％)：<11
体积密度(g/cm3)：>2.61
常温抗折强度(MPa)：>40
常温耐压强度(MPa)：>195
吸水率(％)：<3.6
高温抗折强度(MPa)：>22
荷重软化温度(℃)：>1700
实施例3
一种原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法，包括以下步骤：
准备以下质量份的原料：催化剂(AlF3)7份，氧化铝粉15份，高铝矾土粉15份，软质粘土8份，干糊精粉1.5份，烧结莫来石25份，碳化硅50份，细硅线石6份，金属硅粉2份。
S1、将催化剂、氧化铝粉、高铝矾土粉、软质粘土、干糊精球粉磨预混后按质量比1：1加水搅拌形成泥浆；
S2、将泥浆、烧结莫来石颗粒料和碳化硅颗粒料(碳化硅颗粒料占碳化硅总量的80％)放入行星式强制混合机中搅拌，使泥浆均匀包裹在颗粒料的表面，放入干燥箱干燥，120℃下通风干燥10h，得到干燥后的颗粒包裹料；
S3、干燥后的颗粒包裹料放入混合机中加入颗粒包裹料总质量3.5％硅溶胶搅拌均匀，然后把碳化硅粉、细硅线石、金属硅粉加入混合机中进行混碾15min，混好的原料困料26h后机压成型；
S4、高温烧成，以5℃/min升温至400℃保温30min，以7℃/min升温至700℃保温1h，再以相同的速率升温到980℃保温30min，作为等温处理，随后以4℃/min 升温至1480℃保温5h，然后随炉冷却，得到成品。
成品性能：
显气孔率(％)：<11.5
体积密度(g/cm3：>2.59
常温抗折强度(MPa)：>38
常温耐压强度(MPa)：>185
吸水率(％)：<4.1
高温抗折强度(MPa)：>22
荷重软化温度(℃)：>1700。
Claims (9)
1.一种原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法，其特征在于，包括以下步骤：
S1、将催化剂、氧化铝粉、高铝矾土粉、软质粘土、干糊精球粉磨预混后加水搅拌形成泥浆；
S2、将泥浆、烧结莫来石颗粒料和碳化硅颗粒料放入行星式强制混合机中搅拌，使泥浆均匀包裹在颗粒料的表面，放入干燥箱干燥，得到干燥后的颗粒包裹料；
S3、干燥后的颗粒包裹料放入混合机中加入硅溶胶搅拌均匀，然后把碳化硅粉、细硅线石、金属硅粉加入混合机中进行混碾，混好的原料困料后机压成型；
S4、高温烧成得到成品。
2.根据权利要求1所述的原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法，其特征在于，采用以下质量份数的原料：催化剂3-7份，氧化铝粉8-15份，高铝矾土粉10-15份，软质粘土5-8份，干糊精粉1-1.5份，烧结莫来石15-25份，碳化硅40-50份，细硅线石4-6份，金属硅粉1-2份。
3.根据权利要求1所述的原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法，其特征在于：S1中，球磨预混后按质量比1∶0.5-1加水。
4.根据权利要求1所述的原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法，其特征在于：S2中，碳化硅颗粒料占碳化硅总量的70-80％。
5.根据权利要求1所述的原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法，其特征在于：S2中，在100-120℃下通风干燥8-10h。
6.根据权利要求1所述的原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法，其特征在于：S3中，硅溶胶加入量为干燥后的颗粒包裹料总质量的3-3.5％。
7.根据权利要求1所述的原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法，其特征在于：S3中，混碾10-15min，困料22-26h。
8.根据权利要求1所述的原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法，其特征在于：S4中，高温烧成制度为以5℃/min升温至400℃保温30min，以7℃/min升温至700℃保温1h，再以相同的速率升温到980℃保温30min，作为等温处理，随后以4℃/min升温至1480℃保温5h，然后随炉冷却。
9.根据权利要求1所述的原位反应生成莫来石晶须包裹碳化硅耐火材料的制备方法，其特征在于：催化剂为AlF3。
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