CN114560703B - 一种凝胶注模反应烧结碳化硅陶瓷工艺 - Google Patents

一种凝胶注模反应烧结碳化硅陶瓷工艺 Download PDF

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CN114560703B
CN114560703B CN202210299871.2A CN202210299871A CN114560703B CN 114560703 B CN114560703 B CN 114560703B CN 202210299871 A CN202210299871 A CN 202210299871A CN 114560703 B CN114560703 B CN 114560703B
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刘欢
李文杰
朱晓雪
栾秀静
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Shandong Baichuan Intelligent Technology Co ltd
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Abstract

本发明公开了一种反应烧结碳化硅陶瓷凝胶注模工艺,属于陶瓷制备技术领域,所述碳化硅陶瓷的原料包括碳化硅微粉、氮化硼、石油焦、异丁烯马来酸酐共聚物、羧甲基纤维素钠、酚醛树脂、改性分散剂、乙醇胺、蔗糖脂肪酸酯、去离子水30‑35份;所述工艺包括搅浆,陈腐,浇筑成型,干燥,坯体改性,烧结;本发明的工艺具有投资小,无毒害,低成本,净尺寸,操作简单,可实现结构复杂、超大、超薄件产品一次性净尺寸成型,该工艺生产的产品具有热导率高,耐腐蚀,耐高温,抗热震性好,热膨胀系数低,高弹性模量,可广泛用于冶金、电力、化工、水泥等行业的耐腐蚀、耐磨损领域。

Description

一种凝胶注模反应烧结碳化硅陶瓷工艺
技术领域
本发明涉及一种凝胶注模反应烧结碳化硅陶瓷工艺,属于陶瓷制备技术领域。
背景技术
目前,碳化硅陶瓷行业中反应烧结碳化硅制品的主流生产工艺有浇筑成型和冷压成型两种。浇筑成型主要问题是模具制造繁琐、产品尺寸精度不高、浇筑产品操作繁琐,生产环境差。冷压工艺前期设备投资高昂,只能压制简单形状的产品,无法实现结构复杂产品、超大型件、超薄件的一次性成型。原先凝胶注模工艺受制于气候、温度、湿度、原料高毒性、可操作性差等原因一直停留在实验阶段,无法实现规模化生产。为此,寻找一种可兼顾复杂结构件净尺寸生产、低投资成本、无毒害又具有生产大尺寸超薄件综合浇筑和冷压两种工艺优点的工艺就显得尤为必要了。
发明内容
针对现在工艺的不足,本发明提供一种凝胶注模反应烧结碳化硅陶瓷工艺,该工艺具有投资小,无毒害,低成本,净尺寸,操作简单,可实现结构复杂、超大、超薄件产品一次性净尺寸成型,该工艺生产的产品具有热导率高,耐腐蚀,耐高温,抗热震性好,热膨胀系数低,高弹性模量,可广泛用于冶金、电力、化工、水泥等行业的耐腐蚀、耐磨损领域。
为解决以上技术问题,本发明采取的技术方案如下:
一种凝胶注模反应烧结碳化硅陶瓷工艺,所述碳化硅陶瓷的原料,按重量份计,包括:碳化硅微粉78.5-80份、氮化硼1.5-2份、石油焦3-4份、异丁烯马来酸酐共聚物2-2.5份、羧甲基纤维素钠1-1.5份、酚醛树脂3-3.5份、改性分散剂2-2.5份、乙醇胺3-4份、蔗糖脂肪酸酯1-1.2份、去离子水30-35份;
所述改性分散剂的制备方法,将纳米氮化硼,纳米石墨烯,硫代硫酸钠,N,N-亚甲基双丙烯酰胺,二乙烯三胺,丙烯酸月桂酯,去离子水混合均匀后置于50-60℃下静置30-40min得到初混物,将初混物加入真空均质机中进行真空均质,控制真空均质时的真空度为0.04-0.06Mpa,转速为2000-2600rpm,均质时间为15-25min,均质结束后进行真空喷雾干燥,控制真空度为0.06-0.07MPa,雾化压力为0.4-0.5MPa,进风温度为100-110℃,出风温度为40-50℃,喷雾干燥结束得到改性分散剂;
所述纳米氮化硼的粒径为60-80nm;
所述纳米石墨烯的粒径为120-150nm;
其中,纳米氮化硼,纳米石墨烯,硫代硫酸钠,N,N-亚甲基双丙烯酰胺,二乙烯三胺,丙烯酸月桂酯,去离子水的质量比为20-25:30-35:2-3:4-5:3-4:1-2:50-55。
一种凝胶注模反应烧结碳化硅陶瓷工艺,包括搅浆,陈腐,浇筑成型,干燥,坯体改性,烧结。
所述搅浆,将碳化硅微粉、氮化硼、石油焦、异丁烯马来酸酐共聚物、羧甲基纤维素钠、酚醛树脂、改性分散剂、乙醇胺、蔗糖脂肪酸酯、去离子水混合后,控制搅拌速度为800-1000rpm,搅拌3-4h后,得到浆料;
所述陈腐,将浆料在相对湿度为45-50%,温度为25-30℃下静止存放24-26h,得到陈腐后的浆料;
所述浇筑成型,将陈腐后的浆料通过3kg管道压力浇筑到模具中,凝固40-50min后得陶瓷坯体;
所述干燥,将陶瓷坯体放入真空烘箱内,控制真空度为0.07-0.08MPa,以5-5.5℃/min的升温速度升至80-85℃后烘干8-8.5h,得到烘干后的坯体;
所述坯体改性,采用UV紫外灯管对烘干后的坯体进行臭氧处理,控制UV紫外灯管的发射波长为185nm,UV紫外灯管的照射时间为35-45min,臭氧处理结束得到改性后的坯体;
所述烧结,将改性后的坯体置于真空度为10-30Pa的真空状态下,然后进行升温,首先以7-7.5℃/min的升温速度升温至300-320℃;待升温至300-320℃,通入氮气作为保护气体,并控制气体压力为0.5-0.6MPa,同时将升温速度调整为5-5.5℃/min;待升温至1400-1420℃,保温20-25min,然后继续升温,将升温速度调整为3-3.5℃/min;待升温至1680-1700℃,保温60-65min,然后自然降温,得到碳化硅陶瓷。
与现有技术相比,本发明的有益效果为:
(1)本发明的凝胶注模反应烧结碳化硅陶瓷工艺,采用碳化硅微粉为制备原料,配以氮化硼、石油焦、石墨、粘合剂、有机溶剂,通过搅浆、陈腐、浇筑成型、干燥、烧结,制得的碳化硅陶瓷,生产成本低,工艺简单稳定,可以连续化生产;
(2)本发明的反应烧结碳化硅陶瓷凝胶注模工艺,采用碳化硅微粉作为制备原料,选用搅拌机混料,浇筑即可自行固化,可得净尺寸坯体,适合连续生产,制得的碳化硅陶瓷,密度、硬度、强度、热导率等性能均匀统一,制备的碳化硅陶瓷的体积密度为3.020-3.028g/cm3,维氏硬度为19-22GPa,抗弯强度328-350MPa,耐磨、耐腐蚀性能好;
(3)本发明的反应烧结碳化硅陶瓷凝胶注模工艺,工艺中使用的均匀分散的石油焦、石墨为产品反应烧结提供主要碳源,有机溶剂起到均匀分散原料,防止团聚、沉淀、凝结,有利于促进粉体融合的作用,粘结剂能够在粘结物料的同时在烧结过程中为产品反应烧结提供辅助碳源,氮化硼的引入能有效增加浆料流动性和填充浆料气孔降低金属硅在产品中出现斑点聚合使产品组织结构更加均匀;
(4)本发明的反应烧结碳化硅陶瓷凝胶注模工艺,制备的碳化硅陶瓷的热导率能够达到100-108 W·m-2·K-1,热膨胀系数能够降至(3.6-4.0)*10-6/℃,弹性模量能够达到350-355GPa,能够耐1380-1420℃的高温。
具体实施方式
为了对本发明的技术特征、目的和效果有更加清楚的理解,现说明本发明的具体实施方式。
实施例1
一种凝胶注模反应烧结碳化硅陶瓷工艺,所述碳化硅陶瓷的原料,按重量份计,包括:碳化硅微粉78.5份、氮化硼1.5份、石油焦3份、异丁烯马来酸酐共聚物2份、羧甲基纤维素钠1份、酚醛树脂3份、改性分散剂2份、乙醇胺3份、蔗糖脂肪酸酯1份、去离子水30份;
所述改性分散剂的制备方法,具体为:将纳米氮化硼,纳米石墨烯,硫代硫酸钠,N,N-亚甲基双丙烯酰胺,二乙烯三胺,丙烯酸月桂酯,去离子水混合均匀后置于50℃下静置30min得到初混物,将初混物加入真空均质机中进行真空均质,控制真空均质时的真空度为0.04Mpa,转速为2000rpm,均质时间为15min,均质结束后进行真空喷雾干燥,控制真空度为0.06MPa,雾化压力为0.4MPa,进风温度为100℃,出风温度为40℃,喷雾干燥结束得到改性分散剂;
所述纳米氮化硼的粒径为60nm;
所述纳米石墨烯的粒径为120nm;
其中,纳米氮化硼,纳米石墨烯,硫代硫酸钠,N,N-亚甲基双丙烯酰胺,二乙烯三胺,丙烯酸月桂酯,去离子水的质量比为20:30:2:4:3:1:50。
一种凝胶注模反应烧结碳化硅陶瓷工艺,具体为:
1.搅浆:将碳化硅微粉、氮化硼、石油焦、异丁烯马来酸酐共聚物、羧甲基纤维素钠、酚醛树脂、改性分散剂、乙醇胺、蔗糖脂肪酸酯、去离子水混合后,控制搅拌速度为800rpm,搅拌3h后,得到浆料;
2.陈腐:将浆料在相对湿度为45%,温度为25℃下静止存放24h,得到陈腐后的浆料;
3.浇筑成型:将陈腐后的浆料通过3kg管道压力浇筑到模具中,凝固40min后得陶瓷坯体;
4.干燥:将陶瓷坯体放入真空烘箱内,控制真空度为0.07MPa,以5℃/min的升温速度升至80℃后烘干8h,得到烘干后的坯体;
5.坯体改性:采用UV紫外灯管对烘干后的坯体进行臭氧处理,控制UV紫外灯管的发射波长为185nm,UV紫外灯管的照射时间为35min,臭氧处理结束得到改性后的坯体;
6.烧结:将改性后的坯体置于真空度为10Pa的真空状态下,然后进行升温,首先以7℃/min的升温速度升温至300℃;待升温至300℃,通入氮气作为保护气体,并控制气体压力为0.5MPa,同时将升温速度调整为5℃/min;待升温至1400℃,保温20min,然后继续升温,将升温速度调整为3℃/min;待升温至1680℃,保温60min,然后自然降温,得到碳化硅陶瓷。
经检测,制备出的碳化硅陶瓷的体积密度为3.020g/cm3,维氏硬度为19GPa,抗弯强度为328MPa,热导率为100 W·m-2·K-1,热膨胀系数为3.6*10-6/℃,弹性模量为350GPa,能够耐1380℃的高温。
实施例2
一种凝胶注模反应烧结碳化硅陶瓷工艺,所述碳化硅陶瓷的原料,按重量份计,包括:碳化硅微粉79份、氮化硼1.7份、石油焦3.5份、异丁烯马来酸酐共聚物2.2份、羧甲基纤维素钠1.2份、酚醛树脂3.2份、改性分散剂2.2份、乙醇胺3.5份、蔗糖脂肪酸酯1.1份、去离子水32份。
所述改性分散剂的制备方法,具体为:将纳米氮化硼,纳米石墨烯,硫代硫酸钠,N,N-亚甲基双丙烯酰胺,二乙烯三胺,丙烯酸月桂酯,去离子水混合均匀后置于55℃下静置35min得到初混物,将初混物加入真空均质机中进行真空均质,控制真空均质时的真空度为0.05Mpa,转速为2500rpm,均质时间为20min,均质结束后进行真空喷雾干燥,控制真空度为0.06MPa,雾化压力为0.4MPa,进风温度为105℃,出风温度为45℃,喷雾干燥结束得到改性分散剂;
所述纳米氮化硼的粒径为70nm;
所述纳米石墨烯的粒径为140nm;
其中,纳米氮化硼,纳米石墨烯,硫代硫酸钠,N,N-亚甲基双丙烯酰胺,二乙烯三胺,丙烯酸月桂酯,去离子水的质量比为22:32:2.5:4.5:3.5:1.5:52。
一种凝胶注模反应烧结碳化硅陶瓷工艺,具体为:
1.搅浆:将碳化硅微粉、氮化硼、石油焦、异丁烯马来酸酐共聚物、羧甲基纤维素钠、酚醛树脂、改性分散剂、乙醇胺、蔗糖脂肪酸酯、去离子水混合后,控制搅拌速度为900rpm,搅拌3.5h后,得到浆料;
2.陈腐:将浆料在相对湿度为47%,温度为27℃下静止存放25h,得到陈腐后的浆料;
3.浇筑成型:将陈腐后的浆料通过3.5kg管道压力浇筑到模具中,凝固45min后得陶瓷坯体;
4.干燥:将陶瓷坯体放入真空烘箱内,控制真空度为0.07MPa,以5.2℃/min的升温速度升至82℃后烘干8.2h,得到烘干后的坯体;
5.坯体改性:采用UV紫外灯管对烘干后的坯体进行臭氧处理,控制UV紫外灯管的发射波长为185nm,UV紫外灯管的照射时间为40min,臭氧处理结束得到改性后的坯体;
6.烧结:将改性后的坯体置于真空度为20Pa的真空状态下,然后进行升温,首先以7.2℃/min的升温速度升温至310℃;待升温至310℃,通入氮气作为保护气体,并控制气体压力为0.5MPa,同时将升温速度调整为5.2℃/min;待升温至1410℃,保温22min,然后继续升温,将升温速度调整为3.2℃/min;待升温至1690℃,保温62min,然后自然降温,得到碳化硅陶瓷。
经检测,制备出的碳化硅陶瓷的体积密度为3.025g/cm3,维氏硬度为20GPa,抗弯强度为330MPa,热导率为105 W·m-2·K-1,热膨胀系数为3.7*10-6/℃,弹性模量为352GPa,能够耐1400℃的高温。
实施例3
一种凝胶注模反应烧结碳化硅陶瓷工艺,所述碳化硅陶瓷的原料,按重量份计,包括:碳化硅微粉80份、氮化硼2份、石油焦4份、异丁烯马来酸酐共聚物2.5份、羧甲基纤维素钠1.5份、酚醛树脂3.5份、改性分散剂2.5份、乙醇胺4份、蔗糖脂肪酸酯1.2份、去离子水35份。
所述改性分散剂的制备方法,具体为:将纳米氮化硼,纳米石墨烯,硫代硫酸钠,N,N-亚甲基双丙烯酰胺,二乙烯三胺,丙烯酸月桂酯,去离子水混合均匀后置于60℃下静置40min得到初混物,将初混物加入真空均质机中进行真空均质,控制真空均质时的真空度为0.06Mpa,转速为2600rpm,均质时间为25min,均质结束后进行真空喷雾干燥,控制真空度为0.07MPa,雾化压力为0.5MPa,进风温度为110℃,出风温度为50℃,喷雾干燥结束得到改性分散剂;
所述纳米氮化硼的粒径为80nm;
所述纳米石墨烯的粒径为150nm;
其中,纳米氮化硼,纳米石墨烯,硫代硫酸钠,N,N-亚甲基双丙烯酰胺,二乙烯三胺,丙烯酸月桂酯,去离子水的质量比为25:35:3:5:4:2:55。
一种凝胶注模反应烧结碳化硅陶瓷工艺,具体为:
1.搅浆:将碳化硅微粉、氮化硼、石油焦、异丁烯马来酸酐共聚物、羧甲基纤维素钠、酚醛树脂、改性分散剂、乙醇胺、蔗糖脂肪酸酯、去离子水混合后,控制搅拌速度为1000rpm,搅拌4h后,得到浆料;
2.陈腐:将浆料在相对湿度为50%,温度为30℃下静止存放26h,得到陈腐后的浆料;
3.浇筑成型:将陈腐后的浆料通过4kg管道压力浇筑到模具中,凝固50min后得陶瓷坯体;
4.干燥:将陶瓷坯体放入真空烘箱内,控制真空度为0.08MPa,以5.5℃/min的升温速度升至85℃后烘干8.5h,得到烘干后的坯体;
5.坯体改性:采用UV紫外灯管对烘干后的坯体进行臭氧处理,控制UV紫外灯管的发射波长为185nm,UV紫外灯管的照射时间为45min,臭氧处理结束得到改性后的坯体;
6.烧结:将改性后的坯体置于真空度为30Pa的真空状态下,然后进行升温,首先以7.5℃/min的升温速度升温至320℃;待升温至320℃,通入氮气作为保护气体,并控制气体压力为0.6MPa,同时将升温速度调整为5.5℃/min;待升温至1420℃,保温25min,然后继续升温,将升温速度调整为3.5℃/min;待升温至1700℃,保温65min,然后自然降温,得到碳化硅陶瓷。
经检测,制备出的碳化硅陶瓷的体积密度为3.028g/cm3,维氏硬度为22GPa,抗弯强度为350MPa,热导率为108 W·m-2·K-1,热膨胀系数为4.0*10-6/℃,弹性模量为355GPa,能够耐1420℃的高温。
除非另有说明,本发明中所采用的百分数均为质量百分数。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。

Claims (4)

1.一种凝胶注模反应烧结碳化硅陶瓷工艺,其特征在于,所述碳化硅陶瓷的原料,按重量份计,包括:碳化硅微粉78.5-80份、氮化硼1.5-2份、石油焦3-4份、异丁烯马来酸酐共聚物2-2.5份、羧甲基纤维素钠1-1.5份、酚醛树脂3-3.5份、改性分散剂2-2.5份、乙醇胺3-4份、蔗糖脂肪酸酯1-1.2份、去离子水30-35份;
所述改性分散剂的制备方法,将纳米氮化硼,纳米石墨烯,硫代硫酸钠,N,N-亚甲基双丙烯酰胺,二乙烯三胺,丙烯酸月桂酯,去离子水混合均匀后置于50-60℃下静置30-40min得到初混物,将初混物加入真空均质机中进行真空均质,控制真空均质时的真空度为0.04-0.06Mpa,转速为2000-2600rpm,均质时间为15-25min,均质结束后进行真空喷雾干燥,控制真空度为0.06-0.07MPa,雾化压力为0.4-0.5MPa,进风温度为100-110℃,出风温度为40-50℃,喷雾干燥结束得到改性分散剂;
所述纳米氮化硼的粒径为60-80nm;所述纳米石墨烯的粒径为120-150nm;
纳米氮化硼,纳米石墨烯,硫代硫酸钠,N,N-亚甲基双丙烯酰胺,二乙烯三胺,丙烯酸月桂酯,去离子水的质量比为20-25:30-35:2-3:4-5:3-4:1-2:50-55;
所述的凝胶注模反应烧结碳化硅陶瓷工艺,包括搅浆,陈腐,浇筑成型,干燥,坯体改性,烧结;
所述坯体改性,采用UV紫外灯管对烘干后的坯体进行臭氧处理,控制UV紫外灯管的发射波长为185nm,UV紫外灯管的照射时间为35-45min,臭氧处理结束得到改性后的坯体;
所述烧结,将改性后的坯体置于真空度为10-30Pa的真空状态下,然后进行升温,首先以7-7.5℃/min的升温速度升温至300-320℃;待升温至300-320℃,通入氮气作为保护气体,并控制气体压力为0.5-0.6MPa,同时将升温速度调整为5-5.5℃/min;待升温至1400-1420℃,保温20-25min,然后继续升温,将升温速度调整为3-3.5℃/min;待升温至1680-1700℃,保温60-65min,然后自然降温,得到碳化硅陶瓷。
2.根据权利要求1所述的凝胶注模反应烧结碳化硅陶瓷工艺,其特征在于,所述搅浆,将碳化硅微粉、氮化硼、石油焦、异丁烯马来酸酐共聚物、羧甲基纤维素钠、酚醛树脂、改性分散剂、乙醇胺、蔗糖脂肪酸酯、去离子水混合后,控制搅拌速度为800-1000rpm,搅拌3-4h后,得到浆料。
3.根据权利要求1所述的凝胶注模反应烧结碳化硅陶瓷工艺,其特征在于,所述陈腐,将浆料在相对湿度为45-50%,温度为25-30℃下静止存放24-26h,得到陈腐后的浆料。
4.根据权利要求1所述的凝胶注模反应烧结碳化硅陶瓷工艺,其特征在于,所述干燥,将陶瓷坯体放入真空烘箱内,控制真空度为0.07-0.08MPa,以5-5.5℃/min的升温速度升至80-85℃后烘干8-8.5h,得到烘干后的坯体。
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