CN110054497A - 一种致密的纳米增韧碳化硅复相陶瓷的制备方法 - Google Patents
一种致密的纳米增韧碳化硅复相陶瓷的制备方法 Download PDFInfo
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Abstract
本发明公开了一种致密的纳米增韧碳化硅复相陶瓷的制备方法,所述方法包括如下步骤:步骤一、以α‑SiC粒子为原料,纳米β‑SiC粒子为增韧相,添加烧结助剂和粘结剂,配好原料后投入到氧化铝质球磨罐中,加入蒸馏水,投入研磨球进行研磨,获得组分均匀分散的浆料;步骤二、采用喷雾造粒工艺进行造粒;步骤三、将造粒粉干压成型,得到素坯;步骤四、将素坯放置于真空烧结炉中进行常压烧结,得到致密的纳米增韧碳化硅复相陶瓷。本发明解决了陶瓷的脆性问题,提高了强度和韧性,且操作简单,安全可靠,成本低廉,具有良好的推广应用前景。
Description
技术领域
本发明属于陶瓷材料制备技术领域,涉及一种制备碳化硅复相陶瓷的方法。
背景技术
SiC陶瓷具有很多优良的性能,例如高硬度、高强度、低热膨胀系数等特点,已经广泛的应用于石油化学工业、汽车制造、半导体材料等诸多领域。其中,SiC陶瓷除了具有密度小、热导率高的特点外,更具有硬度高、耐高温及化学性质稳定的特点。因此,SiC陶瓷的应用也越来越广泛,由SiC陶瓷制成的轴承、发动机部件和耐火材料等在汽车、航空航天、空间技术等多个行业得到了广泛的应用。
SiC陶瓷具有高硬度、高强度、低热膨胀系数等优点,广泛应用于严苛的环境下服役,展现出较高的稳定性和良好的机械性能。但由于陶瓷的脆性,即在外载荷的作用下,陶瓷材料会发生突然的断裂,表现为冲击阻力低、损伤容限低等。为解决SiC陶瓷这一缺陷,可通过将陶瓷材料制备成陶瓷基复合材料来提高性能。纳米技术的出现,在改善陶瓷材料性能的方面显示出极大的优势,加入纳米相可提高材料的韧性。
现阶段,SiC陶瓷制备的原料主要采用α-SiC粉体,与常见的α-SiC相比,β-SiC属于低温晶型,超过1800℃时可转化为α-SiC,在转化过程中体积发生变化,其组织更加致密,从而提高了SiC陶瓷的强度和韧性。
发明内容
为了解决现有技术中存在的制备SiC陶瓷强度和韧性较低的问题,本发明提供了一种成本低廉、操作简单的致密的纳米增韧碳化硅复相陶瓷的制备方法。该方法以α-SiC为主,加入纳米β-SiC作为增韧相,β-SiC粒子在1800℃以上的高温下会发生相变产生长轴状晶体,会产生裂纹偏转及桥连的作用,起到增韧的作用。本发明解决了陶瓷的脆性问题,提高了强度和韧性,且操作简单,安全可靠,成本低廉,具有良好的推广应用前景。
本发明的目的是通过以下技术方案实现的:
一种致密的纳米增韧碳化硅复相陶瓷的制备方法,以α-SiC粒子为原料,纳米β-SiC粒子为增韧相,加入一定的烧结助剂和粘结剂,进行高温烧结,最终形成纳米增韧碳化硅复相陶瓷。具体包括如下步骤:
步骤一、纳米β-SiC粒子的制备:将碳粉、硅粉和二氧化硅粉混合均匀,在高温下烧结,得到纳米β-SiC粒子,其中:碳粉、硅粉和二氧化硅粉的摩尔比为1:3~7:1;混合时间为30~90min;烧结温度为1200~1900℃,烧结时间为2~6h;
步骤二、混料:采用湿混工艺,以α-SiC粒子为原料,纳米β-SiC粒子为增韧相,添加烧结助剂和粘结剂,配好原料后投入到氧化铝质球磨罐中,加入蒸馏水,投入研磨球进行研磨,获得组分均匀分散的浆料,其中:α-SiC粒子与增韧相纳米β-SiC粒子的质量比为1:0.05~1;原料、研磨球与蒸馏水的质量比为3:6~9:1;烧结助剂为B4C,添加量为原料总质量的1~5%;粘结剂为酚醛树脂,添加量为原料总质量的10~15%;研磨的转速为300~390r/min;时间为8~12h;
步骤三、造粒:采用喷雾造粒工艺,首先用蠕动泵通入清水,待整个体系得到润湿后,通入混合均匀的浆料,在喷雾干燥机喷头的一定转速下进行造粒,收集造粒粉,其中:喷雾干燥机的喷头转速为20000~24000r/min;
步骤四、成型:将造粒粉干压成型,得到素坯,其中:成型压力为100~600MPa;
步骤五、烧结:将素坯放置于真空烧结炉中进行常压烧结,得到致密的纳米增韧碳化硅复相陶瓷,其中:烧结气氛为惰性气体,烧结温度为1900~2100℃,时间为0.5~2h。
上述方法在β-SiC粒子生成的过程中体系中会发生如下化学反应:
一、固-气反应:
C(s)+ Si(s) = SiC(s) (1);
SiO(g) + 2C(s) = SiC(s) + CO(g) (2);
二、气相反应:
SiO2(s)+ Si(s) = 2SiO(g) (3);
SiO2(s)+ C(s) = SiO(g) + CO(g) (4);
C(s)+ CO2(g) = 2CO(g) (5);
SiO(g)+3CO(g) = SiC(s) + 2CO2(g) (6)。
相比于现有技术,本发明具有如下优点:
1、本发明提供了一种简便、易于放大的制备致密的纳米碳化硅复相陶瓷的方法,该方法改善了陶瓷的脆性,起到了强化和增韧的效果,制备的陶瓷耐高温、力学性能优异。
2、本发明通过改变纳米β-SiC粒子的用量来调节碳化硅复相陶瓷的微观形貌和力学性能。
3、本发明使用纳米β-SiC粒子作为增韧相,纳米粒子周围的局部拉伸应力诱发穿晶断裂,并由于硬粒子对裂纹尖端的反射作用而产生韧化。
4、本发明使用的粘结剂是酚醛树脂,在高温下,酚醛树脂会发生碳化并产生65%的残炭,为烧结提供了少量碳源,有利于烧结致密化的进行。
5、本发明在高温烧结时,通过改变烧结温度和保温时间,可以调节碳化硅复相陶瓷的致密度和机械性能。
附图说明
图1为实施例1制备的纳米增韧碳化硅复相陶瓷的样品图;
图2为实施例1制备的纳米增韧碳化硅复相陶瓷的SEM照片;
图3为实施例1制备的纳米增韧碳化硅复相陶瓷的XRD图;
图4为实施例2制备的纳米增韧碳化硅复相陶瓷的SEM照片;
图5为实施例2制备的纳米增韧碳化硅复相陶瓷的XRD照片;
图6为实施例3制备的纳米增韧碳化硅复相陶瓷的SEM照片;
图7为实施例3制备的纳米增韧碳化硅复相陶瓷的XRD图;
图8为实施例1~5制备的纳米增韧碳化硅复相陶瓷的压缩强度。
具体实施方式
下面结合实施例对本发明的技术方案作进一步的说明,但并不局限于此,凡是对本发明技术方案进行修改或者等同替换,而不脱离本发明技术方案的精神和范围,均应涵盖在本发明的保护范围中。
实施例1:
本实施例提供了一种致密的纳米增韧碳化硅复相陶瓷的制备方法,所述方法是按以下步骤完成的:
一、纳米β-SiC粒子的制备:将碳粉、硅粉和二氧化硅粉以1:4:1的摩尔比在高速混合机中混合60min,在1600℃下烧结;
二、混料:采用湿混工艺,以α-SiC粒子为原料,纳米β-SiC粒子为增韧相,添加B4C和酚醛树脂,其中:α-SiC粒子与增韧相纳米β-SiC粒子的质量比为1:0.05,B4C的添加量为原料总质量的3%;酚醛树脂的添加量为原料总质量的10%,按设计的配方配好原料后,投入到氧化铝质球磨罐中,加入蒸馏水,投入研磨球,其中:原料、研磨球、蒸馏水的质量比为3:8:1,以380r/min的转速研磨9h,获得组分均匀分散的实验浆料;
三、造粒:采用喷雾造粒工艺,首先用蠕动泵通入清水,待整个体系得到润湿后,通入混合均匀的浆料,在喷雾干燥机喷头的19000r/min转速下,造粒完成,然后在喷雾干燥机的下方收集造粒粉;
四、成型:将造粒粉在500MPa的压力下干压成型,得到素坯;
五、烧结:将压制的素坯置于石墨坩埚中,以惰性气体作为保护气,在高温烧结炉中于2000℃下烧结1.5h,冷却至室温,得到致密的纳米增韧碳化硅复相陶瓷。
图1为本实施例制备的复相SiC陶瓷的样品图,由图中可以看到:表面无裂纹,无明显宏观缺陷,并出现了一定程度的体积收缩。
图2为本实施例制备的复相SiC陶瓷的SEM图,由图中可以看到:添加了β-SiC的样品断面,晶界模糊,呈凹凸新装,它的断裂模式为沿晶/穿晶混合断裂模式,在裂纹产生的过程中,晶界对其扩展产生了阻碍,从而提高了材料的强度。
图3为本实施例制备的复相SiC陶瓷的XRD图,由图中可以看到:烧结后的材料的主要晶相为6H-SiC相,添加的β-SiC已经全部转化为α-SiC。
实施例2:
本实施例与实施例1不同点是:α-SiC粒子与增韧相纳米β-SiC粒子的比例为1:0.1。
图4为本实施例制备的复相SiC陶瓷的SEM图,由图中可以看到:β-SiC含量提高以后,制得的材料样品致密度提高。
图5为本实施例制备的复相SiC陶瓷的XRD图,由图中可以看到:烧结后的材料的主要晶相为6H-SiC相,添加的β-SiC已经全部转化为α-SiC。
实施例3:
本实施例与实施例1不同点是:α-SiC粒子与增韧相纳米β-SiC粒子的比例为1:0.2。
图6为本实施例制备的复相SiC陶瓷的SEM图,由图中可以看到:β-SiC含量继续提高,制得的材料样品致密度提高。
图7为本实施例制备的复相SiC陶瓷的XRD图,由图中可以看到:烧结后的材料的主要晶相为6H-SiC相,添加的β-SiC已经全部转化为α-SiC。
实施例4:
本实施例与实施例1不同点是:α-SiC粒子与增韧相纳米β-SiC粒子的比例为1:0.3。
实施例5:
本实施例与实施例1不同点是:α-SiC粒子与增韧相纳米β-SiC粒子的比例为1:0.4。
图8为实施例1~5制备的复相SiC陶瓷的压缩强度,由图中可以看到:当:α-SiC粒子与增韧相纳米β-SiC粒子的比例为1:0.2时,复相SiC陶瓷的压缩强度最大,为411MPa。
Claims (10)
1.一种致密的纳米增韧碳化硅复相陶瓷的制备方法,其特征在于所述方法包括如下步骤:
步骤一、混料:以α-SiC粒子为原料,纳米β-SiC粒子为增韧相,添加烧结助剂和粘结剂,配好原料后投入到氧化铝质球磨罐中,加入蒸馏水,投入研磨球进行研磨,获得组分均匀分散的浆料,其中:α-SiC粒子与增韧相纳米β-SiC粒子的质量比为1:0.05~1;烧结助剂的添加量为原料总质量的1~5%;粘结剂为的添加量为原料总质量的10~15%;原料、研磨球与蒸馏水的质量比为3:6~9:1;
步骤二、造粒:采用喷雾造粒工艺进行造粒;
步骤三、成型:将造粒粉干压成型,得到素坯;
步骤四、烧结:将素坯放置于真空烧结炉中进行常压烧结,得到致密的纳米增韧碳化硅复相陶瓷。
2.根据权利要求1所述的致密的纳米增韧碳化硅复相陶瓷的制备方法,其特征在于所述纳米β-SiC粒子的制备方法如下:将碳粉、硅粉和二氧化硅粉混合均匀,在高温下烧结,得到纳米β-SiC粒子,其中:碳粉、硅粉和二氧化硅粉的摩尔比为1:3~7:1。
3.根据权利要求2所述的致密的纳米增韧碳化硅复相陶瓷的制备方法,其特征在于所述混合时间为30~90min;烧结温度为1200~1900℃,烧结时间为2~6h。
4.根据权利要求1所述的致密的纳米增韧碳化硅复相陶瓷的制备方法,其特征在于所述烧结助剂为B4C,粘结剂为酚醛树脂。
5.根据权利要求1所述的致密的纳米增韧碳化硅复相陶瓷的制备方法,其特征在于所述研磨的转速为300~390r/min,时间为8~12h。
6.根据权利要求1所述的致密的纳米增韧碳化硅复相陶瓷的制备方法,其特征在于所述步骤三的具体步骤如下:首先用蠕动泵通入清水,待整个体系得到润湿后,通入混合均匀的浆料,在喷雾干燥机喷头的一定转速下进行造粒,收集造粒粉。
7.根据权利要求6所述的致密的纳米增韧碳化硅复相陶瓷的制备方法,其特征在于所述喷雾干燥机的喷头转速为20000~24000r/min。
8.根据权利要求1所述的致密的纳米增韧碳化硅复相陶瓷的制备方法,其特征在于所述成型压力为100~600MPa。
9.根据权利要求1所述的致密的纳米增韧碳化硅复相陶瓷的制备方法,其特征在于所述烧结气氛为惰性气体。
10.根据权利要求1所述的致密的纳米增韧碳化硅复相陶瓷的制备方法,其特征在于所述烧结温度为1900~2100℃,时间为0.5~2h。
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