CN111747752A - 一种表面改性的反应烧结碳化硅陶瓷及制备工艺 - Google Patents
一种表面改性的反应烧结碳化硅陶瓷及制备工艺 Download PDFInfo
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Abstract
本发明涉及一种表面改性的反应烧结碳化硅陶瓷及制备工艺,反应烧结碳化硅陶瓷,由F90的碳化硅、F180的碳化硅、F1200的碳化硅、炭黑、粘结剂、分散剂以及去离子水组成;其制备工艺包括原料混合、醒料工艺、烧结工艺以及表面氮化工艺。本发明尽可能的减少了反应烧结碳化硅表面的游离硅,提高了反应烧结碳化硅陶瓷的性能和使用寿命。
Description
技术领域
本发明涉及一种表面改性的反应烧结碳化硅陶瓷及制备工艺,属于无机非金属材料领域。
背景技术
由于对新型能源的发展,也为陶瓷窑具行业提供了新的契机。碳化硅由于具有硬度高、高温抗氧化性好,可作为烧结锂电池的辊棒,但是由于碳化硅材料具有稳定的共价键,熔点高,难烧结,故采用反应烧结来降低其烧结温度。反应烧结虽然可以得到强度高、硬度高的陶瓷材料,但是由于游离硅的存在影响了反应烧结碳化硅在高温下的使用性能和寿命。许多研究表明,可以采取表面改性,来减少反应烧结碳化硅表面的游离硅含量,保证其在高温下的使用性能和延长其使用寿命。
王彤彤采用等离子辅助沉积技术在反应烧结碳化硅表面镀制了一层硅改性层,消除了缺陷,再精细抛光硅改性层,获得了质量良好的光学表面。田贵山等采用碳化硅晶须来增强碳化硅-碳基体,研究表明碳化硅晶须经高温反应烧结后仍保持表面的竹节结构、且晶须增强体与反应烧结碳化硅基体间形成适中的界面结合强度,随着晶须含量的增加,材料的抗弯强度从200MPa提高到310MPa,断裂韧性从3.3MPa·m1/2提高到4.3MPa·m1/2。中国专利文献CN110304933A公开了一种表面改性碳化硅晶须增韧反应烧结碳化硅的制备方法;该方法制备的PyC-SiCw表面的热解碳涂层在反应烧结过程中与液硅发生反应在PyC-SiCw表面原位生成一层SiC涂层,SiC涂层将SiCw与高温液硅相互隔离,壁面了高温下液硅对SiCw的侵蚀损伤问题,PyC-SiCw/RBSC陶瓷具有弯曲强度、断裂韧性大、维氏硬度高的特点,是一种力学性能良好的陶瓷基复合材料。专利文献CN108285355A公开了一种制备SiC纳米线增强反应烧结碳化硅陶瓷基复合材料的方法;采用SiC纳米线作为增强体通过反应烧结原理制备陶瓷基复合材料,有效的改善了纳米纤维与基体的结合截面,实现有效增加增韧。专利文献CN101887139A公布了一种以反应烧结碳化硅和无压烧结碳化硅反射镜镜坯为衬底的反射镜,属于材料表面改性领域的一种碳化硅反射镜;通过表面改性,其表面缺陷少,表面粗糙度RMS低。
发明内容
本发明针对上述问题,提供了一种表面改性的反应烧结碳化硅陶瓷及制备工艺,本发明尽可能的减少了反应烧结碳化硅表面的游离硅,提高了反应烧结碳化硅陶瓷的性能和使用寿命。本发明的技术方案如下:
一种表面改性的反应烧结碳化硅陶瓷,由以下按重量份数的原料组成:
F90的碳化硅20-50份,F180的碳化硅30-60份,F1200的碳化硅5-35份,炭黑5-20份,粘结剂1-5份,分散剂0.1-0.3份,去离子水10-30份。
优选的,所述的粘结剂为羧甲基纤维素;所述分散剂为聚乙二醇(PEG);所述炭黑的粒径为0.1-2微米。
进一步的,所述表面改性的反应烧结碳化硅陶瓷,由以下按重量份数的原料组成:
F90的碳化硅35-45份,F180的碳化硅40-50份,F1200的碳化硅10-20份,炭黑10-15份,粘结剂2-4份,分散剂0.15-0.2份,去离子水15-20份。
更进一步的,所述表面改性的反应烧结碳化硅陶瓷,由以下按重量份数的原料组成:
F90的碳化硅40份,F180的碳化硅45份,F1200的碳化硅5份,炭黑12份,粘结剂3份,分散剂0.18份,去离子水18份。
本发明还包括,上述表面改性的反应烧结碳化硅陶瓷的制备工艺,步骤如下:
(1)原料混合
称取去离子水,将分散剂和粘结剂充分混合均匀,再称取F90的碳化硅、F180的碳化硅、F1200的碳化硅以及炭黑,在常温下混合4-10h,使各组分均匀混合制备混合粉料;
(2)醒料工艺
将步骤(1)制得的混合粉料,在常温下醒料4-20h,将醒好的料放入挤出机中,挤出成型,得到碳化硅陶瓷坯体;
(3)烧结工艺
将步骤(2)制得的陶瓷坯体置于真空反应烧结炉中,在1500-1900℃条件下烧结3-8h,制得碳化硅陶瓷制品;
(4)表面氮化工艺
将步骤(3)制得的陶瓷坯体,放入高温炉中,抽真空后,再通入流动的氨气,氮化温度为450-600℃,渗氮时间10-40h,渗氮次数3-8次,获得表面改性的反应烧结碳化硅陶瓷。
优选的,所述步骤(1)中,混料时间为6-8h,使原料混合均匀;所述步骤(2)中,在常温下醒料8-15h;所述步骤(3)中,陶瓷素坯在1600-1800℃下烧结4-7h;所述步骤(4)中,渗氮温度为500-580℃,渗氮时间15-35h。
更优选的,所述步骤(1)中,混料时间为7h,使原料混合均匀;所述步骤(2)中,在常温下醒料10h;所述步骤(3)中,陶瓷素坯在1700℃下烧结5h;所述步骤(4)中,渗氮温度为550℃,渗氮时间20h。
本发明与现有技术相比具有以下优点:
本发明以反应烧结制备碳化硅陶瓷,以不同粒径的碳化硅、炭黑、粘结剂、分散剂及去离子水为原料,按照一定的比例混料、醒料、挤出成型及高温烧结,制备反应烧结碳化硅陶瓷。将制备的反应烧结碳化硅陶瓷,放入高温炉中,通入流动的氨气,在一定的氮化温度和氮化时间中,进行不同时间表面氮化处理,使得表面的游离硅可以尽可能的减少,提高了反应烧结碳化硅的性能和使用寿命。
附图说明
图1为氮化20h的表面改性的反应烧结碳化硅陶瓷材料断面图;
图2为氮化20h的表面改性的反应烧结碳化硅陶瓷材料断面由内部到表面的残余硅含量的能谱图;
图3为本发明制备的表面改性的反应烧结碳化硅陶瓷的XRD图;
图4为本发明制备的表面改性的反应烧结碳化硅陶瓷的SEM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。
实例1:
一种表面改性的反应烧结碳化硅陶瓷,由以下按重量份数的原料组成:
F90的碳化硅40份,F180的碳化硅45份,F1200的碳化硅5份,炭黑12份,粘结剂3份,分散剂0.18份,去离子水18份;
所述的粘结剂为羧甲基纤维素;所述分散剂为聚乙二醇(PEG);所述炭黑的粒径为0.1-2微米。
上述表面改性的反应烧结碳化硅陶瓷的制备工艺,步骤如下:
(1)原料混合
称取去离子水,将分散剂和粘结剂充分混合均匀,再称取F90的碳化硅、F180的碳化硅、F1200的碳化硅以及炭黑,在常温下混合7h,使各组分均匀混合制备混合粉料;
(2)醒料工艺
将步骤(1)制得的混合粉料,在常温下醒料10h,将醒好的料放入挤出机中,挤出成型,得到碳化硅陶瓷坯体;
(3)烧结工艺
将步骤(2)制得的陶瓷坯体置于真空反应烧结炉中,在1700℃条件下烧结5h,制得碳化硅陶瓷制品;
(4)表面氮化工艺
将步骤(3)制得的陶瓷坯体,放入高温炉中,抽真空后,再通入流动的氨气,氮化温度为550℃,渗氮时间20h,渗氮次数5次,获得表面改性的反应烧结碳化硅陶瓷。
实例2:
一种表面改性的反应烧结碳化硅陶瓷,由以下按重量份数的原料组成:
F90的碳化硅45份,F180的碳化硅57份,F1200的碳化硅30份,炭黑6份,粘结剂4份,分散剂0.25份,去离子水28份;
所述的粘结剂为羧甲基纤维素;所述分散剂为聚乙二醇(PEG);所述炭黑的粒径为0.1-2微米。
上述表面改性的反应烧结碳化硅陶瓷的制备工艺,步骤如下:
(1)原料混合
称取去离子水,将分散剂和粘结剂充分混合均匀,再称取F90的碳化硅、F180的碳化硅、F1200的碳化硅以及炭黑,在常温下混合9h,使各组分均匀混合制备混合粉料;
(2)醒料工艺
将步骤(1)制得的混合粉料,在常温下醒料15h,将醒好的料放入挤出机中,挤出成型,得到碳化硅陶瓷坯体;
(3)烧结工艺
将步骤(2)制得的陶瓷坯体置于真空反应烧结炉中,在1900℃条件下烧结4h,制得碳化硅陶瓷制品;
(4)表面氮化工艺
将步骤(3)制得的陶瓷坯体,放入高温炉中,抽真空后,再通入流动的氨气,氮化温度为600℃,渗氮时间35h,渗氮次数4次,获得表面改性的反应烧结碳化硅陶瓷。
实例3:
一种表面改性的反应烧结碳化硅陶瓷,由以下按重量份数的原料组成:
F90的碳化硅21份,F180的碳化硅32份,F1200的碳化硅35份,炭黑18份,粘结剂2份,分散剂0.13份,去离子水15份;
所述的粘结剂为羧甲基纤维素;所述分散剂为聚乙二醇(PEG);所述炭黑的粒径为0.1-2微米。
上述表面改性的反应烧结碳化硅陶瓷的制备工艺,步骤如下:
(1)原料混合
称取去离子水,将分散剂和粘结剂充分混合均匀,再称取F90的碳化硅、F180的碳化硅、F1200的碳化硅以及炭黑,在常温下混合5h,使各组分均匀混合制备混合粉料;
(2)醒料工艺
将步骤(1)制得的混合粉料,在常温下醒料8h,将醒好的料放入挤出机中,挤出成型,得到碳化硅陶瓷坯体;
(3)烧结工艺
将步骤(2)制得的陶瓷坯体置于真空反应烧结炉中,在1500℃条件下烧结8h,制得碳化硅陶瓷制品;
(4)表面氮化工艺
将步骤(3)制得的陶瓷坯体,放入高温炉中,抽真空后,再通入流动的氨气,氮化温度为480℃,渗氮时间15h,渗氮次数7次,获得表面改性的反应烧结碳化硅陶瓷。
试验例1:
本发明表面改性的反应烧结碳化硅陶瓷材料的力学性能随氮化时间的变化,如表1所示,本发明表面改性的反应烧结碳化硅陶瓷的性能有明显改善;氮化20h的表面改性的反应烧结碳化硅陶瓷材料断面图如图1所示;反应烧结碳化硅陶瓷材料断面由内部到表面的残余硅含量的能谱图如图2所示。
表1
试验例2:
将本发明获得的反应烧结碳化硅陶瓷进行性能检测,其XRD图如图3所示,SEM图如图4所示,由图3可知,反应烧结碳化硅的陶瓷表面具有氮化硅生成,结晶度良好。由图4可知,通过渗氮后的表面,具有一层均匀的氮化硅涂层,可以有效的抑制碳化硅的氧化,提高反应烧结碳化硅的表面性能。
Claims (9)
1.一种表面改性的反应烧结碳化硅陶瓷,其特征在于,所述反应烧结碳化硅陶瓷由以下按重量份数的原料组成:
F90的碳化硅20-50份,F180的碳化硅30-60份,F1200的碳化硅5-35份,炭黑5-20份,粘结剂1-5份,分散剂0.1-0.3份,去离子水10-30份。
2.根据权利要求1所述的反应烧结碳化硅陶瓷,其特征在于,所述的粘结剂为羧甲基纤维素。
3.根据权利要求1所述的反应烧结碳化硅陶瓷,其特征在于,所述分散剂为聚乙二醇。
4.根据权利要求1所述的反应烧结碳化硅陶瓷,其特征在于,所述炭黑的粒径为0.1-2微米。
5.根据权利要求1所述的反应烧结碳化硅陶瓷,其特征在于,所述表面改性的反应烧结碳化硅陶瓷,由以下按重量份数的原料组成:
F90的碳化硅35-45份,F180的碳化硅40-50份,F1200的碳化硅10-20份,炭黑10-15份,粘结剂2-4份,分散剂0.15-0.2份,去离子水15-20份。
6.根据权利要求5所述的反应烧结碳化硅陶瓷,其特征在于,所述表面改性的反应烧结碳化硅陶瓷,由以下按重量份数的原料组成:
F90的碳化硅40份,F180的碳化硅45份,F1200的碳化硅5份,炭黑12份,粘结剂3份,分散剂0.18份,去离子水18份。
7.如权利要求1-6任一项所述反应烧结碳化硅陶瓷的制备工艺,步骤如下:
(1)原料混合
称取去离子水,将分散剂和粘结剂充分混合均匀,再称取F90的碳化硅、F180的碳化硅、F1200的碳化硅以及炭黑,在常温下混合4-10h,使各组分均匀混合制备混合粉料;
(2)醒料工艺
将步骤(1)制得的混合粉料,在常温下醒料4-20h,将醒好的料放入挤出机中,挤出成型,得到碳化硅陶瓷坯体;
(3)烧结工艺
将步骤(2)制得的陶瓷坯体置于真空反应烧结炉中,在1500-1900℃条件下烧结3-8h,制得碳化硅陶瓷制品;
(4)表面氮化工艺
将步骤(3)制得的陶瓷坯体,放入高温炉中,抽真空后,再通入流动的氨气,氮化温度为450-600℃,渗氮时间10-40h,渗氮次数3-8次,获得表面改性的反应烧结碳化硅陶瓷。
8.根据权利要求7所述的制备工艺,其特征在于,所述步骤(1)中,混料时间为6-8h,使原料混合均匀;所述步骤(2)中,在常温下醒料8-15h;所述步骤(3)中,陶瓷素坯在1600-1800℃下烧结4-7h;所述步骤(4)中,渗氮温度为500-580℃,渗氮时间15-35h。
9.根据权利要求8所述的制备工艺,其特征在于,所述步骤(1)中,混料时间为7h,使原料混合均匀;所述步骤(2)中,在常温下醒料10h;所述步骤(3)中,陶瓷素坯在1700℃下烧结5h;所述步骤(4)中,渗氮温度为550℃,渗氮时间20h。
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CN116573940A (zh) * | 2023-04-28 | 2023-08-11 | 合肥陶陶新材料科技有限公司 | 一种高韧性碳化硅陶瓷材料及其制备方法 |
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