CN113072383A - 耐腐蚀碳化硅陶瓷制备方法及其应用 - Google Patents
耐腐蚀碳化硅陶瓷制备方法及其应用 Download PDFInfo
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 48
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000000919 ceramic Substances 0.000 title claims abstract description 35
- 230000007797 corrosion Effects 0.000 title claims abstract description 23
- 238000005260 corrosion Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 26
- 238000000227 grinding Methods 0.000 claims abstract description 20
- 239000002002 slurry Substances 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 229910021431 alpha silicon carbide Inorganic materials 0.000 claims abstract description 12
- 238000000498 ball milling Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000005469 granulation Methods 0.000 claims abstract description 9
- 230000003179 granulation Effects 0.000 claims abstract description 9
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000011230 binding agent Substances 0.000 claims abstract description 6
- 239000002270 dispersing agent Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 6
- 238000001694 spray drying Methods 0.000 claims abstract description 6
- 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 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 6
- 239000005751 Copper oxide Substances 0.000 claims description 6
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 6
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 6
- 229910000431 copper oxide Inorganic materials 0.000 claims description 6
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229920002125 Sokalan® Polymers 0.000 claims description 4
- 239000004584 polyacrylic acid Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 claims description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 238000001272 pressureless sintering Methods 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229910052682 stishovite Inorganic materials 0.000 claims description 3
- 229910052905 tridymite Inorganic materials 0.000 claims description 3
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 239000002912 waste gas Substances 0.000 abstract description 4
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- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
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- 238000000462 isostatic pressing Methods 0.000 description 6
- 239000007921 spray Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
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- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229920001778 nylon Polymers 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
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Abstract
本发明公开了一种耐腐蚀碳化硅陶瓷制备方法及其应用,旨在解决目前氧化铝生产中耐腐蚀碳化硅陶瓷烧结工艺复杂、成本高的技术问题的技术问题。本发明的制备方法为:取α‑SiC微粉85~90份、β‑SiC微粉5~9份、烧结助剂1~1.2份、分散剂3.5~5份、粘结剂0.3~0.5份,混合得研磨混合料;将所述研磨混合料球磨得浆料;将所述浆料喷雾干燥,造粒;将所述造粒所得的粉料无压烧结;并将所述的耐腐蚀碳化硅陶瓷制备方法制得的材料在氧化铝生产中应用。本发明的制备方法成本低、操作简单;不产生二次污染,无废气、废液及废气排放,对环境友好,适合大规模生产。
Description
技术领域
本发明涉及碳化硅陶瓷制备技术领域,具体涉及一种耐腐蚀碳化硅陶瓷制备方法及其应用。
背景技术
腐蚀磨损是引起摩擦材料损伤的主要形式之一。在氧化铝生产过程中,生产系统中有部分机械密封件长期工作于腐蚀性环境,不耐腐蚀的装置或部件会引起密封性能的变化,导致机械密封件使用寿命短,使得生产成本大大提高。
碳化硅陶瓷具有良好的化学稳定性,可以应用于各种腐蚀性强的酸碱性介质中。然而,由于碳化硅化学键特性,其陶瓷烧结条件较为苛刻,必须借助添加剂或外部压力或反应才能实现致密化,碳化硅陶瓷的难烧结性使高性能碳化硅陶瓷的成本居高不下,严重阻碍了其应用。
碳化硅陶瓷烧结制备方法多样,组成结构复杂,产品性能也有明显不同。常压烧结的热压烧结碳化硅陶瓷耐腐蚀性较强,热压烧结碳化硅陶瓷在高温下扔可具有良好的化学稳定性。但是,目前的烧结制备方法工艺复杂,成本高,烧结条件严苛,对操作工的要求高。
因此,开发一种工艺简单、成本低的耐腐蚀碳化硅的制备方法,是当前氧化铝生产中迫切需要解决的技术问题之一。
发明内容
本发明要解决的技术问题是提供一种耐腐蚀碳化硅陶瓷制备方法及其应用。旨在解决现有烧结工艺复杂、成本高的技术问题。
为解决上述技术问题,本发明采用如下技术方案:
提供一种耐腐蚀碳化硅陶瓷制备方法,包括以下步骤:
(1)以质量份数计,取α-SiC微粉85~90份、β-SiC微粉5~9份、烧结助剂1~1.2份、分散剂3.5~5份、粘结剂0.3~0.5份,混合得研磨混合料;
(2)将所述研磨混合料以料、水、球质量比为1::0.8~1:1.5~1.8的比例加入研磨球;以400~450r/min转速球磨3~5h,过250~300目筛,得浆料;
(3)将所述浆料喷雾干燥,造粒;
(4)将所述造粒所得的粉料送入模具中,压制得素胚,在氩气的保护下进行无压烧结,烧结温度为1600~1650℃,保温3~3.5小时后缓慢降温到1400~1450℃,冷却即成。
优选的,所述α-SiC微粉由0.027%的SiO2、0.018%的Fe2O3、0.026%的K2O、0.08%的Na2O、99.85%的SiC组成。
优选的,所述烧结助剂为氧化铬、氧化铜、氧化铝、氧化锰中的至少一种。
优选的,所述烧结助剂由以下质量份数的原料组成:氧化铬0.03份、氧化铜0.02份、氧化铝0.15份、氧化锰0.8份。
优选的,所述分散剂为聚丙烯酸或聚丙烯酸铵。
优选的,所述粘结剂为四甲基氢氧化铵、聚乙烯吡咯烷酮、氨基乙醇、顺丁烯二酸酐中的至少一种。
进一步的,将所述的耐腐蚀碳化硅陶瓷制备方法制得的材料在氧化铝生产中应用。
与现有技术相比,本发明采用无压烧结方式,成本低、操作简单;不产生二次污染,无废气、废液及废气排放,对环境友好;可以制备出形状、大小复杂的耐腐蚀碳化硅陶瓷部件,适合大规模生产。
具体实施方式
下面结合实施例来说明本发明的具体实施方式,但以下实施例只是用来详细说明本发明,并不以任何方式限制本发明的范围。
在以下实施例中所涉及的仪器设备如无特别说明,均为常规仪器设备;所涉及的工业原料如无特别说明,均为市售常规工业原料;所涉及的试验方法,如无特别说明,均为常规方法。所涉及的“份”,均代表重量份。
实施例1:耐腐蚀碳化硅陶瓷制备方法
(1)取α-SiC微粉、β-SiC微粉(纯度99.99%,购自湖州源沁新材料有限公司)、烧结助剂、分散剂、成型剂和粘结剂,其中α-SiC微粉的粒度为50nm,β-SiC微粉的粒度为30-100nm。
α-SiC微粉的化学成分如表1所示:
表1 α-SiC化学成分
成分 | SiO<sub>2</sub> | Fe<sub>2</sub>O<sub>3</sub> | K<sub>2</sub>O | Na<sub>2</sub>O | SiC |
含量/% | 0.027 | 0.018 | 0.026 | 0.08 | 99.85 |
(2)研磨料
取α-SiC微粉86.5份、β-SiC微粉7份、氧化铬0.03份、氧化铜0.02份、氧化铝0.15份、氧化锰0.8份、聚丙烯酸5份、四甲基氢氧化铵0.5份。将配置好的研磨混合料置于尼龙球磨罐中,以料:水:球为1:1:1.5的质量比入碳化硅陶瓷球作为研磨球,将盖拧紧。将球磨罐置于滚筒式球磨机上以400r/min转速球磨5h将研磨球过300筛筛除,即可得到各组分均匀分散的浆料。
(3)造粒
将浆料转移到喷雾造粒塔中进行造粒,使用LGZ-8高速离心式喷雾干燥机对浆料进行喷雾干燥,采用的技术参数为:热风进口温度为260℃,出口温度为100℃,冷却收集造粒料,过100目筛。
(4)烧结
将造粒粉料送入等静压成型模具中,采用湿袋等静压成型机300-800/250成型得素胚,置于石墨坩埚内,再将该素胚放入无压真空烧结炉HYTVHS12-320中,在氩气的保护下进行烧结,烧结温度为1600℃,保温3.5小时后缓慢降温到1400℃,随炉冷却。
(5)对烧结的陶瓷毛坯进行轻磨加工,保证产品的精度和表面光洁度。
实施例2:耐腐蚀碳化硅陶瓷制备方法
(1)取α-SiC微粉、β-SiC微粉同实施例1;
(2)研磨料
取α-SiC微粉88.9份、β-SiC微粉6份、氧化铬0.05份、氧化铝0.3份、氧化锰0.65份、聚丙烯酸铵3.8份、聚乙烯吡咯烷酮0.3份。将配置好的研磨混合料置于尼龙球磨罐中,以料:水:球为1:0.9:1.8的质量比入碳化硅陶瓷球作为研磨球,将盖拧紧。将球磨罐置于滚筒式球磨机上以450r/min转速球磨4h将研磨球过300筛筛除,即可得到各组分均匀分散的浆料。
(3)造粒
将浆料转移到喷雾造粒塔中进行造粒,使用LGZ-8高速离心式喷雾干燥机对浆料进行喷雾干燥,采用的技术参数为:热风进口温度为260℃,出口温度为100℃,冷却收集造粒料,过100目筛。
(4)烧结
将造粒粉料送入等静压成型模具中,采用湿袋等静压成型机300-800/250成型得素胚,置于石墨坩埚内,再将该素胚放入无压真空烧结炉HYTVHS12-320中,在氩气的保护下进行烧结,烧结温度为1650℃,保温3小时后缓慢降温到1450℃,随炉冷却。
(5)对烧结的陶瓷毛坯进行轻磨加工,保证产品的精度和表面光洁度。
实施例3:耐腐蚀碳化硅陶瓷制备方法
(1)取α-SiC微粉、β-SiC微粉同实施例1;
(2)研磨料
取α-SiC微粉96.37份、β-SiC微粉8份、氧化铜0.03份、氧化铝0.1份、氧化锰1份、聚丙烯酸4份、氨基乙醇0.5份。将配置好的研磨混合料置于尼龙球磨罐中,以料:水:球为1:0.8:1.5的质量比入碳化硅陶瓷球作为研磨球,将盖拧紧。将球磨罐置于滚筒式球磨机上以400r/min转速球磨5h将研磨球过300筛筛除,即可得到各组分均匀分散的浆料。
(3)造粒
将浆料转移到喷雾造粒塔中进行造粒,使用LGZ-8高速离心式喷雾干燥机对浆料进行喷雾干燥,采用的技术参数为:热风进口温度为260℃,出口温度为100℃,冷却收集造粒料,过100目筛。
(4)烧结
将造粒粉料送入等静压成型模具中,采用湿袋等静压成型机300-800/250成型得素胚,置于石墨坩埚内,再将该素胚放入无压真空烧结炉HYTVHS12-320中,在氩气的保护下进行烧结,烧结温度为1600℃,保温3.5小时后缓慢降温到1400℃,随炉冷却。
(5)对烧结的陶瓷毛坯进行轻磨加工,保证产品的精度和表面光洁度。
试验例:
取实施例1、2和3制备的碳化硅陶瓷产品,依据耐酸性与耐碱性根据JC/T2138-2012《精细陶瓷耐酸碱腐蚀性能试验方法》测其耐腐蚀性能,结果如下:
表1 耐腐蚀性能检测
性能 | 耐酸性(%) | 耐碱性(%) |
实施例1 | 99.7 | 98.6 |
实施例2 | 98.3 | 97.4 |
实施例3 | 99.1 | 98.9 |
上面结合实施例对本发明作了详细的说明,但是,所属技术领域的技术人员能够理解,在不脱离本发明宗旨的前提下,还可以对上述实施例中的各个具体参数进行变更,形成多个具体的实施例,均为本发明的常见变化范围,在此不再一一详述。
Claims (7)
1.一种耐腐蚀碳化硅陶瓷制备方法,其特征在于:包括以下步骤:
(1)以质量份数计,取α-SiC微粉85~90份、β-SiC微粉5~9份、烧结助剂1~1.2份、分散剂3.5~5份、粘结剂0.3~0.5份,混合得研磨混合料;
(2)将所述研磨混合料以料、水、球质量比为1::0.8~1:1.5~1.8的比例加入研磨球;以400~450r/min转速球磨3~5h,过250~300目筛,得浆料;
(3)将所述浆料喷雾干燥,造粒;
(4)将所述造粒所得的粉料送入模具中,压制得素胚,在氩气的保护下进行无压烧结,烧结温度为1600~1650℃,保温3~3.5小时后缓慢降温到1400~1450℃,冷却即成。
2.依据权利要求1所述的耐腐蚀碳化硅陶瓷制备方法,其特征在于,所述α-SiC微粉由0.027%的SiO2、0.018%的Fe2O3、0.026%的K2O、0.08%的Na2O、99.85%的SiC组成。
3.依据权利要求1所述的耐腐蚀碳化硅陶瓷制备方法,其特征在于,所述烧结助剂为氧化铬、氧化铜、氧化铝、氧化锰中的至少一种。
4.依据权利要求3所述的耐腐蚀碳化硅陶瓷制备方法,其特征在于,所述烧结助剂由以下质量份数的原料组成:氧化铬0.03份、氧化铜0.02份、氧化铝0.15份、氧化锰0.8份。
5.依据权利要求1所述的耐腐蚀碳化硅陶瓷制备方法,其特征在于,所述分散剂为聚丙烯酸或聚丙烯酸铵。
6.依据权利要求1所述的耐腐蚀碳化硅陶瓷制备方法,其特征在于,所述粘结剂为四甲基氢氧化铵、聚乙烯吡咯烷酮、氨基乙醇、顺丁烯二酸酐中的至少一种。
7.权利要求1所述的耐腐蚀碳化硅陶瓷制备方法制得的材料在氧化铝生产中的应用。
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