CN109231991A - 一种氧氮化硅结合碳化硅蜂窝陶瓷及其制备方法 - Google Patents
一种氧氮化硅结合碳化硅蜂窝陶瓷及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种氧氮化硅结合碳化硅蜂窝陶瓷及其制备方法,制备方法为:以硅晶圆切割尾料为原料,采用挤出成型工艺进行成型、通过反应烧结工艺在氮气环境下将尾料中的Si粉氮化生成氧氮化硅,进而制备出氧氮化硅结合碳化硅蜂窝陶瓷。本发明减少了蜂窝陶瓷生产成本,同时有效降低了环境污染;此外,本发明制备的氧氮化硅结合碳化硅蜂窝陶瓷,抗压强度>50.4MPa,热导率达到20.9Wm‑1K‑1,抗热冲击温度达到800℃以上,相关性能完全符合蜂窝陶瓷国家标准。
Description
技术领域
本发明涉及一种氧氮化硅(Si2N2O)结合碳化硅(SiC)蜂窝陶瓷及其制备方法,具体涉及种以硅晶圆切割尾料为原料制备氧氮化硅结合碳化硅蜂窝陶瓷的方法,属于蜂窝陶瓷技术领域。
背景技术
蜂窝陶瓷是一种多功能环境材料,由于其比表面积高、化学性质稳定、耐腐蚀性好,一直受到人们的青睐。但是,被应用的最多的堇青石质蜂窝陶瓷存在如力学性能差、热导率低、热膨胀高等特点,严重阻碍了蜂窝陶瓷的应用。目前,SiC蜂窝陶瓷是最理想的蜂窝陶制备材料之一,但有于其成型难、烧结温度高、成本高等缺点,导致其很难推广。所以制备一种成本低、性能好的SiC质蜂窝陶瓷有着可观的应用价值和市场前景。
近些年来,随着光伏产业和电子行业的飞速发展,人们对晶体硅的需求越来越高,同时硅晶圆大量生产导致的后续问题也随之而来。大量的硅元切割后产生的尾料的存储和排放,不但增加了硅片的生产成本,而且对环境造成严重的污染,所以尾料妥善的处理就成了一个至关重要的问题。
发明内容
本发明提供了一种氧氮化硅(Si2N2O)结合碳化硅(SiC)蜂窝陶瓷及其制备方法,以硅晶圆切割尾料为原料,采用挤出成型工艺进行成型、通过反应烧结工艺在氮气环境下将尾料中的Si粉氮化生成氧氮化硅,进而制备出氧氮化硅结合碳化硅蜂窝陶瓷。本发明减少了蜂窝陶瓷生产成本,同时有效降低了环境污染;此外,本发明制备的氧氮化硅结合碳化硅蜂窝陶瓷,抗压强度>51.4MPa,热导率达到11.3-24.6Wm-1K-1,抗热冲击温度达到800℃以上,相关性能完全符合蜂窝陶瓷国家标准。本发明获得的氧氮化硅结合碳化硅蜂窝陶瓷具有成本低、力学性能好、耐腐蚀性好、抗热震性好、热导高等特点。本发明的技术方案如下:
一种氧氮化硅结合碳化硅蜂窝陶瓷的其制备方法,具体步骤如下:
(1)将硅晶圆切割尾料经纯净水洗1-3次,每次用2倍体积的纯净水,加入纯净水后经搅拌、沉淀,然后去除上清液,将处理后尾料于80-100℃条件下烘干;
(2)向步骤(1)烘干后的尾料中加入氧化物,然后经球磨机混料10-18小时,获得粉料;氧化物的加入的百分比为2-10%,氧化物为Y2O3(三氧化钇)或ZrO2(二氧化锆)中的至少一种物质;
(3)向步骤(2)获得的粉料加入纯净水、桐油及羟丙基甲基纤维素,加入的百分比分别为30-50%、20-30%及10-40%,然后经混料机混料2-6小时,再经真空练泥机在真空条件下练泥1-3次后密封,密封后在温度为20-25℃条件下陈化2-3天,再次练泥3-4次,获得泥料;
(4)将步骤(3)获得的泥料经真空挤出机挤出成型,蜂窝体尺寸为边长40-500mm的正方体,蜂窝体壁厚为0.1-1mm,挤出后获得坯体;
(5)将步骤(4)获得的坯体在通风、避光、25℃恒温处风干2-3天,再置于80-150℃的恒温干燥箱中干燥1-3天;
(6)将步骤(5)获得的生坯置于空气炉中,在400-800℃保温4-5小时排胶,随炉冷却至室温;
(7)经步骤(6)排胶处理过的生坯放入氮气炉中经氮气洗气,在氮气环境中常压烧结,温度经5-10℃/min的升温速度升至1300-1600℃,然后保温3-12个小时后随炉冷却至室温,即得蜂窝陶瓷成品。
进一步的,所述步骤(1)中将硅晶圆切割尾料经纯净水洗3次,每次用2倍体积的纯净水,加入纯净水后经搅拌、沉淀,然后去除上清液,将处理后尾料于90℃条件下烘干;所述步骤(2)中向步骤(1)烘干后的尾料中加入氧化物,然后经球磨机混料15小时,获得粉料;Y2O3的加入量为3%、ZrO2的加入量为5%;所述(3)中向步骤(2)获得的粉料加入纯净水、桐油及羟丙基甲基纤维素,加入的百分比分别为40%、25%及30%,然后经混料机混料6小时,再经真空练泥机在真空条件下练泥3次后密封,密封后在温度为20℃条件下陈化2天,再次练泥4次,获得泥料;所述(4)中将步骤(3)获得的泥料经真空挤出机挤出成型,蜂窝体尺寸为边长200mm的正方体,蜂窝体壁厚为0.5mm,挤出后获得坯体;所述(5)中将步骤(4)获得的坯体在通风、避光、25℃恒温处风干2天,再置于100℃的恒温干燥箱中干燥2天;所述(6)中将步骤(5)获得的生坯置于空气炉中,在500℃保温5小时排胶,随炉冷却至室温;所述(7)中经步骤(6)排胶处理过的生坯放入氮气炉中经氮气洗气,在氮气环境中常压烧结,温度经8℃/min的升温速度升至1600℃,然后保温8个小时后随炉冷却至室温,即得蜂窝陶瓷成品。
本发明还包括上述制备方法获得的氧氮化硅结合碳化硅蜂窝陶瓷。
本发明中,“%”均为质量百分数。
本发明与现有技术相比具有以下优点:
本发明利用尾料制备Si2N2O结合SiC质蜂窝陶瓷可有效的提高SiC质蜂窝陶瓷的性能,同时可以减少生产成本;本发明对硅晶圆切割尾料利用的开发可有效的降低环境污染,实现可循环发展;本发明制备的氧氮化硅结合碳化硅蜂窝陶瓷,抗压强度>50.4MPa,热导率最高达到20.9Wm-1K-1,抗热冲击温度达到800℃以上,相关性能完全符合蜂窝陶瓷国家标准。
附图说明
为更清楚地说明背景技术或本发明的技术方案,下面对现有技术或具体实施方式中结合使用的附图作简单地介绍;显而易见地,以下结合具体实施方式的附图仅是用于方便理解本发明实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图;
图1为材料烧结后样品X射线衍射分析图谱;
图2为Si2N2O结合SiC蜂窝陶瓷烧结后微观形貌图。
具体实施方式
下面结合具体实施例来进一步描述本发明,本发明的优点和特点将会随着描述而更为清楚。但实施例仅是范例性的,并不对本发明的范围构成任何限制。本领域技术人员应该理解的是,在不偏离本发明的精神和范围下可以对本发明技术方案的细节和形式进行修改或替换,但这些修改和替换均落入本发明的保护范围内。
实施例1一种氧氮化硅结合碳化硅蜂窝陶瓷的其制备方法
(1)将硅晶圆切割尾料经2倍体积的纯净水洗3次,经搅拌、沉淀后去除上清液,将处理完成的尾料于90℃下烘干;
(2)向步骤(1)烘干后的尾料中加入氧化物,然后经球磨机混料10小时,获得粉料;Y2O3的加入量为3%、ZrO2的加入量为5%;
(3)向步骤(2)获得的粉料加入纯净水、桐油及羟丙基甲基纤维素,加入的百分比分别为40%、25%及30%,然后经混料机混料6小时,再经真空练泥机在真空条件下练泥3次后密封,密封后在温度为20℃条件下陈化2天,再次练泥4次,获得泥料;
(4)将步骤(3)获得的泥料经真空挤出机挤出成型,蜂窝体尺寸为边长200mm的正方体,蜂窝体壁厚为0.5mm,挤出后获得坯体;
(5)将步骤(4)获得的坯体在通风、避光、25℃恒温处风干2天,再置于100℃的恒温干燥箱中干燥2天;
(6)将步骤(5)获得的生坯置于空气炉中,在500℃保温5小时排胶,随炉冷却至室温;
(7)经步骤(6)排胶处理过的生坯放入氮气炉中经氮气洗气,在氮气环境中常压烧结,温度经8℃/min的升温速度升至1600℃,然后保温8个小时后随炉冷却至室温,即得蜂窝陶瓷成品。
实施例2一种氧氮化硅结合碳化硅蜂窝陶瓷的其制备方法
(1)将硅晶圆切割尾料经纯净水洗2次,每次用2倍体积的纯净水,经搅拌、沉淀后去除上清液,将处理完成的尾料于100℃下烘干;
(2)向步骤(1)烘干后的尾料中加入氧化物,然后经球磨机混料10小时,获得粉料;Y2O3的加入量为5%、ZrO2的加入量为4%;
(3)向步骤(2)获得的粉料加入纯净水、桐油及羟丙基甲基纤维素,加入的百分比分别为40%、25%及10%,然后经混料机混料4小时,再经真空练泥机在真空条件下练泥1次后密封,密封后在温度为25℃条件下陈化2天,再次练泥4次,获得泥料;
(4)将步骤(3)获得的泥料经真空挤出机挤出成型,蜂窝体尺寸为边长40mm的正方体,蜂窝体壁厚为0.1mm,挤出后获得坯体;
(5)将步骤(4)获得的坯体在通风、避光、25℃恒温处风干3天,再置于150℃的恒温干燥箱中干燥3天;
(6)将步骤(5)获得的生坯置于空气炉中,在800℃保温5小时排胶,随炉冷却至室温;
(7)经步骤(6)排胶处理过的生坯放入氮气炉中经氮气洗气,在氮气环境中常压烧结,温度经10℃/min的升温速度升至1400℃,然后保温6个小时后随炉冷却至室温,即得蜂窝陶瓷成品。
实施例3一种氧氮化硅结合碳化硅蜂窝陶瓷的其制备方法
(1)将硅晶圆切割尾料经纯净水洗3次,每次用2倍体积的纯净水,经搅拌、沉淀后去除上清液,将处理完成的尾料于100℃下烘干;
(2)将步骤(1)烘干后的尾料中加入氧化物,然后经球磨机混料14小时,获得粉料;Y2O3的加入量为2%、ZrO2的加入量为6%;
(3)向步骤(2)获得的粉料加入纯净水、桐油及羟丙基甲基纤维素,加入的百分比分别为50%、30%及30%,然后经混料机混料6小时,再经真空练泥机在真空条件下练泥2次后密封,密封后在温度为25℃条件下陈化3天,再次练泥4次,获得泥料;
(4)将步骤(3)获得的泥料经真空挤出机挤出成型,蜂窝体尺寸为边长500mm的正方体,蜂窝体壁厚为1mm,挤出后获得坯体;
(5)将步骤(4)获得的坯体在通风、避光、25℃恒温处风干3天,再置于120℃的恒温干燥箱中干燥3天;
(6)将步骤(5)获得的生坯置于空气炉中,在400℃保温5小时排胶,随炉冷却至室温;
(7)经步骤(6)排胶处理过的生坯放入氮气炉中经氮气洗气,在氮气环境中常压烧结,温度经10℃/min的升温速度升至1500℃,然后保温12个小时后随炉冷却至室温,即得蜂窝陶瓷成品。
实施例4一种氧氮化硅结合碳化硅蜂窝陶瓷的其制备方法
(1)将硅晶圆切割尾料经2倍体积的纯净水洗1次,经搅拌、沉淀后去除上清液,将处理完成的尾料于100℃下烘干;
(2)向步骤(1)烘干后的尾料中加入氧化物,然后经球磨机混料10小时,获得粉料;Y2O3的加入量为3%、ZrO2的加入量为4%;
(3)向步骤(2)获得的粉料加入纯净水、桐油及羟丙基甲基纤维素,加入的百分比分别为30%、20%及40%,然后经混料机混料4小时,再经真空练泥机在真空条件下练泥1次后密封,密封后在温度为25℃条件下陈化3天,再次练泥4次,获得泥料;
(4)将步骤(3)获得的泥料经真空挤出机挤出成型,蜂窝体尺寸为边长40mm的正方体,蜂窝体壁厚为0.5mm,挤出后获得坯体;
(5)将步骤(4)获得的坯体在通风、避光、25℃恒温处风干3天,再置于150℃的恒温干燥箱中干燥1天;
(6)将步骤(5)获得的生坯置于空气炉中,在800℃保温5小时排胶,随炉冷却至室温;
(7)经步骤(6)排胶处理过的生坯放入氮气炉中经氮气洗气,在氮气环境中常压烧结,温度经10℃/min的升温速度升至1600℃,然后保温8个小时后随炉冷却至室温,即得蜂窝陶瓷成品。
实施例5一种氧氮化硅结合碳化硅蜂窝陶瓷的其制备方法
(1)将硅晶圆切割尾料经纯净水洗2次,每次用2倍体积的纯净水,经搅拌、沉淀后去除上清液,将处理完成的尾料于100℃下烘干;
(2)将步骤(1)烘干后的尾料中加入氧化物,然后经球磨机混料18小时,获得粉料;Y2O3的加入量为8%、ZrO2的加入量为2%;
(3)向步骤(2)获得的粉料加入纯净水、桐油及羟丙基甲基纤维素,加入的百分比分别为40%、25%及10%,然后经混料机混料6小时,再经真空练泥机在真空条件下练泥2次后密封,密封后在温度为20℃条件下陈化2天,再次练泥3次,获得泥料;
(4)将步骤(3)获得的泥料经真空挤出机挤出成型,蜂窝体尺寸为边长200mm的正方体,蜂窝体壁厚为0.5mm,挤出后获得坯体;
(5)将步骤(4)获得的坯体在通风、避光、25℃恒温处风干3天,再置于150℃的恒温干燥箱中干燥3天;
(6)将步骤(5)获得的生坯置于空气炉中,在800℃保温4小时排胶,随炉冷却至室温;
(7)经步骤(6)排胶处理过的生坯放入氮气炉中经氮气洗气,在氮气环境中常压烧结,温度经5℃/min的升温速度升至1300℃,然后保温8个小时后随炉冷却至室温,即得蜂窝陶瓷成品。
实施例6一种氧氮化硅结合碳化硅蜂窝陶瓷的其制备方法
(1)将硅晶圆切割尾料经纯净水洗2次,每次用2倍体积的纯净水,经搅拌、沉淀后去除上清液,将处理完成的尾料于80℃下烘干;
(2)将步骤(1)烘干后的尾料中加入氧化物,然后经球磨机混料14小时,获得粉料;Y2O3的加入量为7%、ZrO2的加入量为2%;
(3)向步骤(2)获得的粉料加入纯净水、桐油及羟丙基甲基纤维素,加入的百分比分别为40%、25%及40%,然后经混料机混料6小时,再经真空练泥机在真空条件下练泥2次后密封,密封后在温度为20℃条件下陈化2天,再次练泥4次,获得泥料;
(4)将步骤(3)获得的泥料经真空挤出机挤出成型,蜂窝体尺寸为边长200mm的正方体,蜂窝体壁厚为1mm,挤出后获得坯体;
(5)将步骤(4)获得的坯体在通风、避光、25℃恒温处风干3天,再置于150℃的恒温干燥箱中干燥3天;
(6)将步骤(5)获得的生坯置于空气炉中,在800℃保温4小时排胶,随炉冷却至室温;
(7)经步骤(6)排胶处理过的生坯放入氮气炉中经氮气洗气,在氮气环境中常压烧结,温度经5℃/min的升温速度升至1600℃,然后保温3个小时后随炉冷却至室温,即得蜂窝陶瓷成品。
试验例1对本发明获得的蜂窝陶瓷进行性能检测
取本发明样品进行力学性能、耐腐蚀性、抗热震性、以及热导率的测试,实验结果如表1所示。实验发现本发明力学性能好、抗热震性好、热导率高、有较大的比热容,且耐腐蚀性好。对除氢氟酸外的其他无机酸具有较好的耐受性。材料性能完全满足蜂窝陶瓷使用性能。
表1蜂窝陶瓷性质表
试验例2取本发明实施例1获得的样品,材料烧结后样品X射线衍射分析图谱如图1所示;Si2N2O结合SiC蜂窝陶瓷烧结后微观形貌如图2所示,本发明颗粒大小及分布均匀;且经检测本发明蜂窝陶瓷沿挤出方向定向排列的径向尺寸在1-10μm,轴向尺寸在30-100μm气孔,这一结构对于热导,热膨胀,抗压强度均有促进作用。
Claims (10)
1.一种氧氮化硅结合碳化硅蜂窝陶瓷的制备方法,其特征在于,制备方法如下:
以硅晶圆切割尾料为原料,采用挤出成型工艺进行成型、通过反应烧结工艺在氮气环境下将尾料中的Si粉氮化生成氧氮化硅,进而制备出氧氮化硅结合碳化硅蜂窝陶瓷。
2.根据权利要求1所述的制备方法,其特征在于,具体步骤如下:
(1)将硅晶圆切割尾料经纯净水洗1-3次,每次用2倍体积的纯净水,加入纯净水后经搅拌、沉淀,然后去除上清液,将处理后尾料于80-100℃条件下烘干;
(2)向步骤(1)烘干后的尾料中加入氧化物,然后经球磨机混料10-18小时,获得粉料;氧化物的加入的百分比为2-10%,氧化物为Y2O3(三氧化钇)或ZrO2(二氧化锆)中的至少一种物质;
(3)向步骤(2)获得的粉料加入纯净水、桐油及羟丙基甲基纤维素,加入的百分比分别为30-50%、20-30%及10-40%,然后经混料机混料2-6小时,再经真空练泥机在真空条件下练泥1-3次后密封,密封后在温度为20-25℃条件下陈化2-3天,再次练泥3-4次,获得泥料;
(4)将步骤(3)获得的泥料经真空挤出机挤出成型,蜂窝体尺寸为边长40-500mm的正方体,蜂窝体壁厚为0.1-1mm,挤出后获得坯体;
(5)将步骤(4)获得的坯体在通风、避光、25℃恒温处风干2-3天,再置于80-150℃的恒温干燥箱中干燥1-3天;
(6)将步骤(5)获得的生坯置于空气炉中,在400-800℃保温4-5小时排胶,随炉冷却至室温;
(7)经步骤(6)排胶处理过的生坯放入氮气炉中经氮气洗气,在氮气环境中常压烧结,温度经5-10℃/min的升温速度升至1300-1600℃,然后保温3-12个小时后随炉冷却至室温,即得蜂窝陶瓷成品。
3.根据权利要求2所述的制备方法,其特征在于,所述步骤(1)中将硅晶圆切割尾料经纯净水洗3次,每次用2倍体积的纯净水,加入纯净水后经搅拌、沉淀,然后去除上清液,将处理后尾料于90℃条件下烘干。
4.根据权利要求2所述的制备方法,其特征在于,所述步骤(2)中向步骤(1)烘干后的尾料中加入氧化物,然后经球磨机混料15小时,获得粉料;Y2O3的加入量为3%、ZrO2的加入量为5%。
5.根据权利要求2所述的制备方法,其特征在于,所述(3)中向步骤(2)获得的粉料加入纯净水、桐油及羟丙基甲基纤维素,加入的百分比分别为40%、25%及30%,然后经混料机混料6小时,再经真空练泥机在真空条件下练泥3次后密封,密封后在温度为20℃条件下陈化2天,再次练泥4次,获得泥料。
6.根据权利要求2所述的制备方法,其特征在于,所述(4)中将步骤(3)获得的泥料经真空挤出机挤出成型,蜂窝体尺寸为边长200mm的正方体,蜂窝体壁厚为0.5mm,挤出后获得坯体。
7.根据权利要求2所述的制备方法,其特征在于,所述(5)中将步骤(4)获得的坯体在通风、避光、25℃恒温处风干2天,再置于100℃的恒温干燥箱中干燥2天。
8.根据权利要求2所述的制备方法,其特征在于,所述(6)中将步骤(5)获得的生坯置于空气炉中,在500℃保温5小时排胶,随炉冷却至室温。
9.根据权利要求2所述的制备方法,其特征在于,所述(7)中经步骤(6)排胶处理过的生坯放入氮气炉中经氮气洗气,在氮气环境中常压烧结,温度经8℃/min的升温速度升至1600℃,然后保温8个小时后随炉冷却至室温,即得蜂窝陶瓷成品。
10.如权利要求1-9任一项所述的制备方法获得的氧氮化硅结合碳化硅蜂窝陶瓷。
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1849276A (zh) * | 2003-09-09 | 2006-10-18 | 日本碍子株式会社 | 氮化硅结合SiC耐火材料及其制造方法 |
CN101708402A (zh) * | 2009-12-24 | 2010-05-19 | 中钢集团洛阳耐火材料研究院有限公司 | 一种复相氮化物结合碳化硅泡沫陶瓷过滤器及其制备方法 |
CN102275925A (zh) * | 2011-06-09 | 2011-12-14 | 东北大学 | 一种晶体硅切割废料氮化反应烧结碳化硅的方法 |
JP2012153596A (ja) * | 2011-01-07 | 2012-08-16 | National Institute Of Advanced Industrial Science & Technology | 1次元構造体を配置した無機多孔質体の製造方法、該無機多孔質体およびそれを使用した部材 |
CN103764357A (zh) * | 2011-08-26 | 2014-04-30 | 陶氏环球技术有限责任公司 | 制备陶瓷体的改进方法 |
CN107973604A (zh) * | 2016-10-24 | 2018-05-01 | 日本碍子株式会社 | 多孔质材料、蜂窝结构体及多孔质材料的制造方法 |
-
2018
- 2018-08-30 CN CN201811001118.0A patent/CN109231991A/zh active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1849276A (zh) * | 2003-09-09 | 2006-10-18 | 日本碍子株式会社 | 氮化硅结合SiC耐火材料及其制造方法 |
CN101708402A (zh) * | 2009-12-24 | 2010-05-19 | 中钢集团洛阳耐火材料研究院有限公司 | 一种复相氮化物结合碳化硅泡沫陶瓷过滤器及其制备方法 |
JP2012153596A (ja) * | 2011-01-07 | 2012-08-16 | National Institute Of Advanced Industrial Science & Technology | 1次元構造体を配置した無機多孔質体の製造方法、該無機多孔質体およびそれを使用した部材 |
CN102275925A (zh) * | 2011-06-09 | 2011-12-14 | 东北大学 | 一种晶体硅切割废料氮化反应烧结碳化硅的方法 |
CN103764357A (zh) * | 2011-08-26 | 2014-04-30 | 陶氏环球技术有限责任公司 | 制备陶瓷体的改进方法 |
CN107973604A (zh) * | 2016-10-24 | 2018-05-01 | 日本碍子株式会社 | 多孔质材料、蜂窝结构体及多孔质材料的制造方法 |
Non-Patent Citations (2)
Title |
---|
YANJUN LIA ET AL: "Fabrication of Si2N2O ceramic with silicon kerf waste as raw material", 《CERAMICS INTERNATIONAL》 * |
罗民华: "《多孔陶瓷实用技术》", 31 March 2006, 中国建材工业出版社 * |
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