CN113912399B - 一种高密度无压烧结碳化硅陶瓷的制备方法 - Google Patents
一种高密度无压烧结碳化硅陶瓷的制备方法 Download PDFInfo
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Abstract
本发明公开了一种高密度无压烧结碳化硅陶瓷的制备方法,属于陶瓷制备技术领域,包括粉料处理,制备混合粉,混合粉改性,压制,真空脱脂,烧结;所述粉料处理,将碳化硅粉末加入到处理剂中,将温度升高后进行搅拌,搅拌10‑20min后使用紫外灯进行紫外照射,紫外照射40‑50min后,停止搅拌和紫外照射,并将温度降低至室温,得到粉料液,然后对粉料液进行抽滤,将滤渣烘干,得到处理后的粉料;本发明的制备方法能够在提高碳化硅陶瓷的断裂韧性,降低碳化硅陶瓷的脆性的同时,提高碳化硅陶瓷的高温强度及抗弯强度、抗氧化性、耐腐蚀性、抗磨损等性能。
Description
技术领域
本发明涉及陶瓷制备技术领域,具体涉及一种高密度无压烧结碳化硅陶瓷的制备方法。
背景技术
碳化硅陶瓷属于陶瓷材料的一种,不仅具有优良的常温力学性能,如高的抗弯强度、优良的抗氧化性、良好的耐腐蚀性、高的抗磨损以及低的摩擦系数,而且高温力学性能是已知陶瓷材料中最佳的,由热压烧结、无压烧结、热等静压烧结制备的碳化硅陶瓷,其高温强度可一直维持到1600℃,是陶瓷材料中高温强度最好的材料。
但是碳化硅陶瓷断裂韧性较低,脆性较大,而且易氧化和烧结困难,影响了碳化硅的应用和发展。现有的提高碳化硅陶瓷的断裂韧性的方法有:将纤维均匀地分布于碳化硅陶瓷原料之中,以提高陶瓷的强度和韧性;向碳化硅陶瓷中加入其他陶瓷材料制成复合陶瓷;向碳化硅陶瓷表面添加涂层;制备纳米陶瓷材料。但是上述方法主要是通过掺杂,复合和涂层等方法对碳化硅陶瓷进行改性,改性后会对碳化硅陶瓷的高温强度产生影响,而且还会影响碳化硅陶瓷的抗弯强度、抗氧化性、耐腐蚀性、抗磨损等。因此,研发一种新的碳化硅陶瓷的制备方法,能够在提高断裂韧性,降低脆性的同时,提高碳化硅陶瓷的高温强度及抗弯强度、抗氧化性、耐腐蚀性、抗磨损等性能,是目前的研发重点。
专利CN112279648A公开了一种无压烧结高韧性碳化硅,包括以下重量份的原料:碳化硅96-98份、碳化硼0.8-1.2份、石墨烯1-3份、分散剂0.6-0.8份、粘结剂4-6份、酚醛树脂5-7份、润滑液0.8-1.2份、去离子水90-110份;该专利的不足:制备的无压烧结高韧性碳化硅的高温强度低。
专利CN112062574A公开了一种高性能纳米的碳化硅陶瓷及其制备方法和应用,该碳化硅陶瓷是将聚碳硅烷作为前驱体和烧结助剂Al2O3-CeO2球磨混合后,在保护气氛下,先升温至200-400℃保温,再升温至500-1200℃裂解,得到混合粉体;再将混合粉体进行球磨、造粒,装入石墨模具中,施加压力1-20MPa,在保护气氛下1200-1450℃进行烧结制得;该专利的不足:制备的碳化硅陶瓷耐磨损性能差。
发明内容
针对现有技术存在的不足,本发明提供了一种高密度无压烧结碳化硅陶瓷的制备方法,能够在提高碳化硅陶瓷的断裂韧性,降低碳化硅陶瓷的脆性的同时,提高碳化硅陶瓷的高温强度及抗弯强度、抗氧化性、耐腐蚀性、抗磨损等性能。
为解决以上技术问题,本发明采取的技术方案如下:
一种高密度无压烧结碳化硅陶瓷的制备方法,包括粉料处理,制备混合粉,混合粉改性,压制,真空脱脂,烧结。
所述粉料处理,将碳化硅粉末加入到处理剂中,将温度升高至50-55℃后进行搅拌,控制搅拌速度为300-350rpm,搅拌10-20min后使用紫外灯进行紫外照射,并将搅拌速度控制到400-450rpm,紫外照射40-50min后,停止搅拌和紫外照射,并将温度降低至室温,得到粉料液,然后对粉料液进行抽滤,将滤渣于50-55℃下烘干,得到处理后的粉料。
其中,碳化硅粉末与处理剂的重量比为1:5-8。
所述紫外照射过程中的紫外光波长为280-320nm。
所述碳化硅的纯度为98.5-99.5%,粒径为1-3μm。
所述处理剂的组成,按重量份计,包括:30-35份双氧水,8-10份次氯酸,2-4份过硫酸钠,3-5份氯化铝,2-3份羟丙基甲基纤维素,90-95份去离子水。
所述制备混合粉,将处理后的粉料,纳米二氧化钛,碳化硼粉末,氧化锌混合均匀后置于热处理炉中,将热处理炉内的气体抽空,然后向热处理炉内充入氮气和氧气的混合气体,控制热处理炉内混合气体的气体压力为60-80kPa,然后将热处理炉缓慢升温,控制升温速度为3-5℃/min,待升温至450-550℃,保温45-50min后自然冷却至室温,得到预混合粉,然后对预混合粉进行球磨,控制球磨时的球料比为15-20:1,球磨速度为550-600rpm,球磨时间为3-4h,球磨结束得到混合粉。
所述纳米二氧化钛的粒径为100-200nm。
所述碳化硼粉末的粒径为10-20μm。
其中,处理后的粉料,纳米二氧化钛,碳化硼粉末,氧化锌的质量比为35-40:2-3:5-7:2-4。
其中,混合气体中氮气和氧气的体积比为10-12:1。
所述混合粉改性,将纳米碳化硅,葡萄糖,纳米氧化铝混合均匀后得到包覆粉,然后采用高频爆炸喷涂方式,使包覆粉在9-10bar,3600-3800℃的爆炸能量下,以1000-1100m·s-1的速度被加热加速轰击到混合粉表面,得到改性后的混合粉。
其中,纳米碳化硅,葡萄糖,纳米氧化铝,混合粉的质量比为5-8:3-5:2-4:30-35。
所述压制,将改性后混合粉置于等静压机中,在180-200MPa的条件下进行冷等静压压制,得到胚体。
所述真空脱脂,将胚体置于真空脱脂炉中脱脂,控制真空脱脂炉的真空度为20-30kPa,将真空脱脂炉升温至700-750℃,控制升温速度为5-8℃/min,然后在700-750℃下保温1.5-2h后得到真空脱脂后的胚体。
所述烧结,将真空脱脂后的胚体置于无压烧结炉内,使用流动氮气作为保护气体,将无压烧结炉升温至2000-2100℃,然后自然冷却至室温,得到碳化硅陶瓷。
与现有技术相比,本发明的有益效果为:
(1)本发明制备的高密度无压烧结碳化硅陶瓷,通过在制备混合粉步骤中向热处理炉中通入氮气和氧气的混合气体,以及在混合粉改性步骤中使用纳米碳化硅,葡萄糖,纳米氧化铝对混合粉进行包覆,能够提高制备的碳化硅陶瓷的密度,硬度,强度和断裂韧性,本发明制备的碳化硅陶瓷的密度为3.18-3.25g/cm3,致密度为98.8-99.1%,维氏硬度为28-30GPa,弹性模量为452-465GPa,抗拉强度为324-341MPa,抗弯强度为442-458MPa,抗压强度为1960-2070MPa,断裂韧性为4.9-5.3MPa·m1/2;
(2)本发明制备的高密度无压烧结碳化硅陶瓷,通过在制备混合粉步骤中向热处理炉中通入氮气和氧气的混合气体,以及在混合粉改性步骤中使用纳米碳化硅,葡萄糖,纳米氧化铝对混合粉进行包覆,能够提高制备的碳化硅陶瓷的抗氧化性,按照JC/T 2530-2019标准对本发明制备的碳化硅陶瓷的抗氧化性进行测试,将试样放入炉子中,于1400℃中氧化60h后质量变化为0.24-0.32g/cm3;
(3)本发明制备的高密度无压烧结碳化硅陶瓷,通过在制备混合粉步骤中向热处理炉中通入氮气和氧气的混合气体,以及在混合粉改性步骤中使用纳米碳化硅,葡萄糖,纳米氧化铝对混合粉进行包覆,能够提高制备的碳化硅陶瓷的耐腐蚀性,本发明制备的碳化硅陶瓷在酸中的质量变化为0.02-0.05g/m2,在碱中的质量变化为0.01-0.04g/m2;
(4)本发明制备的高密度无压烧结碳化硅陶瓷,通过在粉料处理步骤中进行紫外照射,在制备混合粉步骤中向热处理炉中通入氮气和氧气的混合气体,以及在混合粉改性步骤中使用纳米碳化硅,葡萄糖,纳米氧化铝对混合粉进行包覆,能够提高制备的碳化硅陶瓷的耐磨损性,本发明制备的碳化硅陶瓷的耐磨度为145-152mm3;
(5)本发明制备的高密度无压烧结碳化硅陶瓷,通过在粉料处理步骤中进行紫外照射,在制备混合粉步骤中向热处理炉中通入氮气和氧气的混合气体,以及在混合粉改性步骤中使用纳米碳化硅,葡萄糖,纳米氧化铝对混合粉进行包覆,能够提高制备的碳化硅陶瓷的高温强度,制备的碳化硅陶瓷在1500℃下的弹性模量为438-454GPa,抗拉强度为315-329MPa,抗弯强度为435-441MPa,抗压强度为1900-1970MPa,断裂韧性为4.8-5.1 MPa·m1 /2。
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
一种高密度无压烧结碳化硅陶瓷的制备方法,具体为:
1.粉料处理:将碳化硅粉末加入到处理剂中,将温度升高至50℃后进行搅拌,控制搅拌速度为300rpm,搅拌10min后使用紫外灯进行紫外照射,并将搅拌速度控制到400rpm,紫外照射40min后,停止搅拌和紫外照射,并将温度降低至室温,得到粉料液,然后对粉料液进行抽滤,将滤渣于50℃下烘干,得到处理后的粉料。
其中,碳化硅粉末与处理剂的重量比为1:5。
所述紫外照射过程中的紫外光波长为280nm。
所述碳化硅的纯度为98.5%,粒径为1μm。
所述处理剂的组成,按重量份计,包括:30份双氧水,8份次氯酸,2份过硫酸钠,3份氯化铝,2份羟丙基甲基纤维素,90份去离子水。
2.制备混合粉:将处理后的粉料,纳米二氧化钛,碳化硼粉末,氧化锌混合均匀后置于热处理炉中,将热处理炉内的气体抽空,然后向热处理炉内充入氮气和氧气的混合气体,控制热处理炉内混合气体的气体压力为60kPa,然后将热处理炉缓慢升温,控制升温速度为3℃/min,待升温至450℃,保温45min后自然冷却至室温,得到预混合粉,然后对预混合粉进行球磨,控制球磨时的球料比为15:1,球磨速度为550rpm,球磨时间为3h,球磨结束得到混合粉。
所述纳米二氧化钛的粒径为100nm。
所述碳化硼粉末的粒径为10μm。
其中,处理后的粉料,纳米二氧化钛,碳化硼粉末,氧化锌的质量比为35:2:5:2。
其中,混合气体中氮气和氧气的体积比为10:1。
3.混合粉改性:将纳米碳化硅,葡萄糖,纳米氧化铝混合均匀后得到包覆粉,然后采用高频爆炸喷涂方式,使包覆粉在9bar,3600℃的爆炸能量下,以1000m·s-1的速度被加热加速轰击到混合粉表面,得到改性后的混合粉。
其中,纳米碳化硅,葡萄糖,纳米氧化铝,混合粉的质量比为5:3:2:30。
4.压制:将改性后混合粉置于等静压机中,在180MPa的条件下进行冷等静压压制,得到胚体。
5.真空脱脂:将胚体置于真空脱脂炉中脱脂,控制真空脱脂炉的真空度为20kPa,将真空脱脂炉升温至700℃,控制升温速度为5℃/min,然后在700℃下保温1.5h后得到真空脱脂后的胚体。
6.烧结:将真空脱脂后的胚体置于无压烧结炉内,使用流动氮气作为保护气体,将无压烧结炉升温至2000℃,然后自然冷却至室温,得到碳化硅陶瓷。
实施例2
一种高密度无压烧结碳化硅陶瓷的制备方法,具体为:
1.粉料处理:将碳化硅粉末加入到处理剂中,将温度升高至52℃后进行搅拌,控制搅拌速度为320rpm,搅拌15min后使用紫外灯进行紫外照射,并将搅拌速度控制到420rpm,紫外照射45min后,停止搅拌和紫外照射,并将温度降低至室温,得到粉料液,然后对粉料液进行抽滤,将滤渣于52℃下烘干,得到处理后的粉料。
其中,碳化硅粉末与处理剂的重量比为1:7。
所述紫外照射过程中的紫外光波长为300nm。
所述碳化硅的纯度为99%,粒径为2μm。
所述处理剂的组成,按重量份计,包括:32份双氧水,9份次氯酸,3份过硫酸钠,4份氯化铝,2份羟丙基甲基纤维素,92份去离子水。
2.制备混合粉:将处理后的粉料,纳米二氧化钛,碳化硼粉末,氧化锌混合均匀后置于热处理炉中,将热处理炉内的气体抽空,然后向热处理炉内充入氮气和氧气的混合气体,控制热处理炉内混合气体的气体压力为70kPa,然后将热处理炉缓慢升温,控制升温速度为4℃/min,待升温至500℃,保温47min后自然冷却至室温,得到预混合粉,然后对预混合粉进行球磨,控制球磨时的球料比为18:1,球磨速度为570rpm,球磨时间为3.5h,球磨结束得到混合粉。
所述纳米二氧化钛的粒径为150nm。
所述碳化硼粉末的粒径为15μm。
其中,处理后的粉料,纳米二氧化钛,碳化硼粉末,氧化锌的质量比为37:2:6:3。
其中,混合气体中氮气和氧气的体积比为11:1。
3.混合粉改性:将纳米碳化硅,葡萄糖,纳米氧化铝混合均匀后得到包覆粉,然后采用高频爆炸喷涂方式,使包覆粉在9bar,3700℃的爆炸能量下,以1050m·s-1的速度被加热加速轰击到混合粉表面,得到改性后的混合粉。
其中,纳米碳化硅,葡萄糖,纳米氧化铝,混合粉的质量比为6:4:3:32。
4. 压制:将改性后混合粉置于等静压机中,在190MPa的条件下进行冷等静压压制,得到胚体。
5.真空脱脂:将胚体置于真空脱脂炉中脱脂,控制真空脱脂炉的真空度为25kPa,将真空脱脂炉升温至720℃,控制升温速度为7℃/min,然后在720℃下保温1.7h后得到真空脱脂后的胚体。
6.烧结:将真空脱脂后的胚体置于无压烧结炉内,使用流动氮气作为保护气体,将无压烧结炉升温至2050℃,然后自然冷却至室温,得到碳化硅陶瓷。
实施例3
一种高密度无压烧结碳化硅陶瓷的制备方法,具体为:
1.粉料处理:将碳化硅粉末加入到处理剂中,将温度升高至55℃后进行搅拌,控制搅拌速度为350rpm,搅拌20min后使用紫外灯进行紫外照射,并将搅拌速度控制到450rpm,紫外照射50min后,停止搅拌和紫外照射,并将温度降低至室温,得到粉料液,然后对粉料液进行抽滤,将滤渣于55℃下烘干,得到处理后的粉料。
其中,碳化硅粉末与处理剂的重量比为1:8。
所述紫外照射过程中的紫外光波长为280-320nm。
所述碳化硅的纯度为99.5%,粒径为3μm。
所述处理剂的组成,按重量份计,包括:35份双氧水,10份次氯酸,4份过硫酸钠,5份氯化铝,3份羟丙基甲基纤维素,95份去离子水。
2.制备混合粉:将处理后的粉料,纳米二氧化钛,碳化硼粉末,氧化锌混合均匀后置于热处理炉中,将热处理炉内的气体抽空,然后向热处理炉内充入氮气和氧气的混合气体,控制热处理炉内混合气体的气体压力为80kPa,然后将热处理炉缓慢升温,控制升温速度为5℃/min,待升温至550℃,保温50min后自然冷却至室温,得到预混合粉,然后对预混合粉进行球磨,控制球磨时的球料比为20:1,球磨速度为600rpm,球磨时间为4h,球磨结束得到混合粉。
所述纳米二氧化钛的粒径为200nm。
所述碳化硼粉末的粒径为20μm。
其中,处理后的粉料,纳米二氧化钛,碳化硼粉末,氧化锌的质量比为40: 3:7:4。
其中,混合气体中氮气和氧气的体积比为12:1。
3.混合粉改性:将纳米碳化硅,葡萄糖,纳米氧化铝混合均匀后得到包覆粉,然后采用高频爆炸喷涂方式,使包覆粉在10bar,3800℃的爆炸能量下,以1100m·s-1的速度被加热加速轰击到混合粉表面,得到改性后的混合粉。
其中,纳米碳化硅,葡萄糖,纳米氧化铝,混合粉的质量比为8:5:4: 35。
4. 压制:将改性后混合粉置于等静压机中,在200MPa的条件下进行冷等静压压制,得到胚体。
5.真空脱脂:将胚体置于真空脱脂炉中脱脂,控制真空脱脂炉的真空度为30kPa,将真空脱脂炉升温至750℃,控制升温速度为8℃/min,然后在750℃下保温2h后得到真空脱脂后的胚体。
6.烧结:将真空脱脂后的胚体置于无压烧结炉内,使用流动氮气作为保护气体,将无压烧结炉升温至2100℃,然后自然冷却至室温,得到碳化硅陶瓷。
对比例1
采用实施例1所述的高密度无压烧结碳化硅陶瓷的制备方法,其不同之处在于:第1步粉料处理步骤中不进行紫外照射。
对比例2
采用实施例1所述的高密度无压烧结碳化硅陶瓷的制备方法,其不同之处在于:第2步制备混合粉步骤中热处理炉中只加入氮气,不加入氧气,控制热处理炉内氮气的气体压力为80kPa。
对比例3
采用实施例1所述的高密度无压烧结碳化硅陶瓷的制备方法,其不同之处在于:第3步混合粉改性步骤改为直接将纳米碳化硅,葡萄糖,纳米氧化铝,混合粉按照质量比为5:3:2:30混合均匀后得到改性后的混合粉。
对实施例1-3和对比例1-3制备的高密度无压烧结碳化硅陶瓷的致密度,维氏硬度,弹性模量,抗拉强度,抗弯强度,抗压强度,断裂韧性进行检测,检测结果如下所示:
按照JC/T 2530-2019标准对实施例1-3和对比例1-3制备的高密度无压烧结碳化硅陶瓷的抗氧化性进行测试,将试样放入炉子中,于1400℃中氧化60h,测质量变化,测试结果如下:
按照JC/T 2138-2012标准对实施例1-3和对比例1-3制备的高密度无压烧结碳化硅陶瓷的耐腐蚀性进行测试,测试结果如下:
按照GB/T 3810.6-2016标准对实施例1-3和对比例1-3制备的高密度无压烧结碳化硅陶瓷的耐磨损性能进行测试,测试结果如下:
在1500℃下对实施例1-3和对比例1-3制备的高密度无压烧结碳化硅陶瓷的弹性模量,抗拉强度,抗弯强度,抗压强度,断裂韧性进行检测,检测结果如下所示:
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 (1)
1.一种高密度无压烧结碳化硅陶瓷的制备方法,其特征在于,包括粉料处理,制备混合粉,混合粉改性,压制,真空脱脂,烧结;
所述粉料处理,将碳化硅粉末加入到处理剂中,将温度升高至50-55℃后进行搅拌,控制搅拌速度为300-350rpm,搅拌10-20min后使用紫外灯进行紫外照射,并将搅拌速度控制到400-450rpm,紫外照射40-50min后,停止搅拌和紫外照射,并将温度降低至室温,得到粉料液,然后对粉料液进行抽滤,将滤渣于50-55℃下烘干,得到处理后的粉料;
所述粉料处理步骤中碳化硅粉末与处理剂的重量比为1:5-8;
所述处理剂的组成,按重量份计,包括:30-35份双氧水,8-10份次氯酸,2-4份过硫酸钠,3-5份氯化铝,2-3份羟丙基甲基纤维素,90-95份去离子水;
所述制备混合粉,将处理后的粉料,纳米二氧化钛,碳化硼粉末,氧化锌混合均匀后置于热处理炉中,将热处理炉内的气体抽空,然后向热处理炉内充入氮气和氧气的混合气体,控制热处理炉内混合气体的气体压力为60-80kPa,然后将热处理炉缓慢升温,控制升温速度为3-5℃/min,待升温至450-550℃,保温45-50min后自然冷却至室温,得到预混合粉,然后对预混合粉进行球磨,控制球磨时的球料比为15-20:1,球磨速度为550-600rpm,球磨时间为3-4h,球磨结束得到混合粉;
所述制备混合粉步骤中处理后的粉料,纳米二氧化钛,碳化硼粉末,氧化锌的质量比为35-40:2-3:5-7:2-4;
所述混合气体中氮气和氧气的体积比为10-12:1;
所述混合粉改性,将纳米碳化硅,葡萄糖,纳米氧化铝混合均匀后得到包覆粉,然后采用高频爆炸喷涂方式,使包覆粉在9-10bar,3600-3800℃的爆炸能量下,以1000-1100m·s-1的速度被加热加速轰击到混合粉表面,得到改性后的混合粉;
所述混合粉改性中纳米碳化硅,葡萄糖,纳米氧化铝,混合粉的质量比为5-8:3-5:2-4:30-35;
所述真空脱脂,将胚体置于真空脱脂炉中脱脂,控制真空脱脂炉的真空度为20-30kPa,将真空脱脂炉升温至700-750℃,控制升温速度为5-8℃/min,然后在700-750℃下保温1.5-2h后得到真空脱脂后的胚体。
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