CN107500794A - 一种原位生成碳化硅纤维结合碳化硅耐磨材料及其制备方法 - Google Patents
一种原位生成碳化硅纤维结合碳化硅耐磨材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种原位生成碳化硅纤维结合碳化硅耐磨材料及其制备方法,属于耐磨陶瓷材料技术领域。该碳化硅耐磨材料由复合原料和结合剂制成,所述复合原料由以下重量百分比的原料组成:68%~80%碳化硅,13.7%~21.1%硅源,5.4%~7.7%碳源,0.45%~1.68%催化剂,0.45%~1.72%烧结助剂;所述结合剂的质量为所述复合原料总质量的2%~5%;所述碳化硅由碳化硅颗粒和碳化硅微粉组成,二者质量比为(90~98):(2~10)。本发明所用原料价格低、来源广,制备工艺简单;所得制品具有强度高、韧性大、耐磨损、烧结温度低等优点,克服了现有碳化硅陶瓷材料韧性差、难烧结等缺陷,适合推广应用。
Description
技术领域
本发明涉及一种原位生成碳化硅纤维结合碳化硅耐磨材料及其制备方法,属于耐磨陶瓷材料技术领域。
背景技术
材料和设备主要失效于磨损,我国每年由磨损造成的经济损失约为1000亿人民币,且正以15%的速度增长,这预示着耐磨材料具有巨大的市场空间和应用前景。但随着科技的发展,要求耐磨材料必须具有耐高温、抗腐蚀、耐冲击等优越性能,才能在较苛刻的工作环境中使用,而现有产品满足不了该使用要求。因此,人类迫切需要开发研制出具有优良性能,并具有广泛应用领域的新型耐磨材料,以满足磨损行业迅速发展的需要。
碳化硅耐磨材料具有强度高、硬度大、耐高温、抗腐蚀等一系列优良性能,且价格低廉,大量应用于石油化工、冶金机械、航空航天、微电子、汽车、钢铁等领域,在耐磨领域中展示着重要的应用前景。但其存在韧性差的缺陷,且因Si-C键以共价键为主(约占88%),导致其扩散系数较低,采用无压烧结难以制备出致密的碳化硅耐磨材料,这些均限制了其在工业中的推广应用。
目前,科研工作者多在碳化硅耐磨材料中添加低熔点的烧结助剂,在烧结过程中这些低熔点的烧结助剂形成液相,使烧结过程由扩散传质变为粘滞流动,降低烧结活化所需要的能量,进而实现碳化硅耐磨材料的低温烧结。此方法虽简便易行,但若烧结助剂添加量过多,其在碳化硅耐磨材料中会形成空间网络结构,高温下使用时低共熔相发生软化,将弱化碳化硅耐磨材料的高温力学性能,且过多外来烧结助剂的引入将减小碳化硅耐磨材料的优良特性。
在现有研究中,专利申请公布号为201110154829.3(申请日为2011.06.10)的发明专利公开了碳化硅纤维增强碳化硅复合材料的制备方法,包括以下步骤:(1)制备SiC纤维编织件;(2)以甲烷或丙烯为原料气,在编织件表面沉积碳涂层;(3)以液态SiC陶瓷先驱体为浸渍液,真空浸渍纤维编织体;(4)将编织体在流动氮气气氛下进行热模压交联;(5)将交联后的编织件放入裂解炉中,在流动氮气气氛下进行高温裂解;(6)重复真空浸渍-热模压交联-高温裂解周期,完成制备。此方法存在制备工艺复杂,周期长,且性能不稳定等缺陷,不易在精密结构部件中应用。因此,寻找高致密度、高性能碳化硅耐磨材料的有效制备方法,已成为亟待解决的关键性课题。
发明内容
本发明的目的是提供一种原位生成碳化硅纤维结合碳化硅耐磨材料,解决现有碳化硅耐磨材料制品韧性差、难以烧结致密化、强度低等缺陷,所得制品具有强度高、韧性大、耐磨损、烧结温度低等特点,综合性能优良。
本发明的第二个目的是提供一种原位生成碳化硅纤维结合碳化硅耐磨材料的制备方法,该方法成本低、工艺简便易行,利于规模化生产。
为实现上述目的,本发明所采用的技术方案为:
一种原位生成碳化硅纤维结合碳化硅耐磨材料,由复合原料和结合剂在还原气氛下烧结制成,所述复合原料由以下重量百分比的原料组成:68%~80%碳化硅,13.7%~21.1%硅源,5.4%~7.7%碳源,0.45%~1.68%催化剂,0.45%~1.72%烧结助剂;所述碳化硅由碳化硅颗粒和碳化硅微粉组成,二者质量比为(90~98):(2~10);所述结合剂的质量为所述复合原料总质量的2%~5%。
所述碳化硅颗粒由大、中、小三组份颗粒组成,粒径分别为180~325µm、120~212µm、45~80µm,其质量比为17:7:1,纯度≥99%;所述碳化硅微粉的粒径≤10µm,纯度≥99%。
所述的硅源为二氧化硅微粉、石英粉、硅溶胶中的一种或几种;所述二氧化硅微粉和石英粉中的SiO2含量≥99.9%,粒径≤5μm;所述硅溶胶中的SiO2含量为35%,粒径≤100nm。
所述的碳源为石墨粉、活性炭、炭黑中的一种或几种;所述碳源中的C含量≥99.9%,粒径≤5µm。
所述的催化剂为Si-Fe合金粉、Ni粉、Fe粉、H3BO3、NaCl、NaF中的一种或几种;所述催化剂的纯度≥99.9%,粒径≤5µm。
所述的烧结助剂为Y2O3、CeO2、La2O3、钙长石中的一种或几种;所述烧结助剂的纯度≥99.9%,粒径≤5µm。
所述的结合剂为聚乙烯醇溶液或糊精液;所述聚乙烯醇溶液的浓度为2.5%~3%;所述糊精液浓度为30%~40%。
一种上述原位生成碳化硅纤维结合碳化硅耐磨材料的制备方法,包括以下步骤:
1)取配方量的碳化硅、硅源、碳源、烧结助剂、催化剂、结合剂,混合均匀,制成坯料;
2)将步骤1)所得坯料成型制成坯体;
3)将步骤2)所得坯体进行干燥并在还原气氛下烧成,自然冷却,即得原位生成碳化硅纤维结合碳化硅耐磨材料。
步骤1)中,结合剂为2.5%~3%浓度的聚乙烯醇溶液或30%~40%浓度的糊精液;添加量为所述复合原料总质量的2%~5%。
步骤2)中所述成型为机压成型,成型压力为200~300MPa,保压的时间为10~20s。
步骤3)中所述干燥的温度为100~150℃,干燥的时间为8~12h。
步骤3)中所述的还原气氛为在刚玉坩埚中利用埋碳法所制造的还原条件。
步骤3)中,所述的烧成的温度为1450~1600℃,保温的时间为3~8h。
本发明的有益效果:
本发明制造的耐磨材料中,原位生成的碳化硅纤维等径率高、纯度大,在碳化硅颗粒间形成致密均匀的空间网络结构,以纤维拔出、裂纹桥联和偏转等增韧机制大幅提升了碳化硅耐磨材料的强度、韧性和耐磨性等,且制备工艺简单、成本较低,在国民经济中的能源、航空航天、冶金机械、汽车制造、石油化工及军事等方面均有广阔的应用前景。
具体实施方式
为了更好的理解本发明,下面结合具体实施例进一步阐明本发明的内容,但本发明的内容不仅仅局限于下面的实施例。
为避免重复,将本具体实施例中原料作如下统一描述,实施例中不再赘述:所述碳化硅纯度≥99%;所述硅源中,二氧化硅微粉和石英粉中的SiO2含量≥99.9%,粒径≤5μm,硅溶胶中的SiO2含量为35%,粒径≤100nm;所述碳源中,石墨粉、活性炭和炭黑中的C含量≥99.9%,粒径≤5µm;所述催化剂和烧结助剂的粒径≤45µm,纯度≥99.9%。
实施例1
一种原位生成碳化硅纤维结合碳化硅耐磨材料,由复合原料和结合剂在还原气氛下烧结制成,所述复合原料由以下重量百分比的原料组成:80%的碳化硅(粒径为180µm、120µm、45µm和10µm,对应含量分别为49.0%、20.1%、2.9%和8.0%),13.7%的二氧化硅微粉,5.4%的活性炭,0.45%的H3BO3,0.45%的Y2O3,结合剂为40%浓度的糊精液,糊精液的质量为所述复合原料总质量的2%。
本实施例的原位生成碳化硅纤维结合碳化硅耐磨材料的制备方法,包括下列步骤:
1)按上述方案,取配方量的碳化硅、二氧化硅微粉、活性炭、H3BO3和Y2O3置于球磨罐中,于行星磨上干混120min,再加入糊精液,混合10min制成坯料;
2)将步骤1)所得坯料成型制成坯体;所述成型为机压成型,成型的压力为300MPa,保压的时间为10s;
3)将步骤2)所得坯体进行干燥并在还原气氛下烧成,自然冷却,即得原位生成碳化硅纤维结合碳化硅耐磨材料。
步骤3)中所述的干燥温度为150℃,时间为8h;所述的烧成温度为1500℃,升温速率为2.5℃/min,保温时间为6h。所得耐磨材料的各性能参数列于表1中。
实施例2
一种原位生成碳化硅纤维结合碳化硅耐磨材料,由复合原料和结合剂在还原气氛下烧结制成,所述复合原料由以下重量百分比的原料组成:73%的碳化硅(粒径为325µm、212µm、80µm和5µm,对应含量分别为44.7%、18.4%、2.6%和7.3%),8.5%的石英粉,8.6%的二氧化硅微粉,6.8%的炭黑,0.45%的Si-Fe合金粉,0.9%的NaF,0.45%的Y2O3,1.3%的钙长石,结合剂为2.5%浓度的聚乙烯醇溶液,聚乙烯醇溶液的质量为所述复合原料总质量的5%。
本实施例的原位生成碳化硅纤维结合碳化硅耐磨材料的制备方法,包括下列步骤:
1)按上述方案,取配方量的碳化硅、石英粉、二氧化硅微粉、炭黑、Si-Fe合金粉、NaF、Y2O3和钙长石置于球磨罐中,于行星磨上干混120min,再加入聚乙烯醇溶液,混合10min制成坯料;
2)将步骤1)所得坯料成型制成坯体;所述成型为机压成型,成型的压力为250MPa,保压的时间为15s;
3)将步骤2)所得坯体进行干燥并在还原气氛下烧成,自然冷却,即得原位生成碳化硅纤维结合碳化硅耐磨材料。
步骤3)中所述的干燥温度为120℃,时间为12h;所述的烧成温度为1600℃,升温速率为2.5℃/min,保温时间为3h。所得耐磨材料的各性能参数列于表1中。
实施例3
一种原位生成碳化硅纤维结合碳化硅耐磨材料,由复合原料和结合剂在还原气氛下烧结制成,所述复合原料由以下重量百分比的原料组成:68%的碳化硅(粒径为212µm、150µm、45µm和2µm,对应含量分别为45.3%、18.6%、2.7%和1.4%),17.6%的石英粉,3.5%的硅溶胶,6%的炭黑,1.6%的石墨粉,1.68%的Ni粉,0.42%的Y2O3,1.2%的CeO2,结合剂为3%浓度的聚乙烯醇溶液,聚乙烯醇溶液的质量为所述复合原料总质量的3%。
本实施例的原位生成碳化硅纤维结合碳化硅耐磨材料的制备方法,包括下列步骤:
1)按上述方案,取配方量的碳化硅、石英粉、炭黑、石墨粉、Ni粉、Y2O3和CeO2置于球磨罐中,于行星磨上干混90min后,添加硅溶胶混合30min,再加入聚乙烯醇溶液混合10min制成坯料;
2)将步骤1)所得坯料成型制成坯体;所述成型为机压成型,成型的压力为200MPa,保压的时间为20s;
3)将步骤2)所得坯体进行干燥并在还原气氛下烧成,自然冷却,即得原位生成碳化硅纤维结合碳化硅耐磨材料。
步骤3)中所述的干燥温度为100℃,时间为12h;所述的烧成温度为1450℃,升温速率为2.5℃/min,保温时间为8h。所得耐磨材料的各性能参数列于表1中。
实施例4
一种原位生成碳化硅纤维结合碳化硅耐磨材料,由复合原料和结合剂在还原气氛下烧结制成,所述复合原料由以下重量百分比的原料组成:70%的碳化硅(粒径为180µm、120µm、45µm和5µm,对应含量分别为45.2%、18.6%、2.7%和3.5%),15.9%的二氧化硅微粉,3.4%的石英粉,4.7%的活性炭,3.0%的炭黑,0.85%的Fe粉,0.43%的NaCl,1.29%的钙长石,0.43%的La2O3,结合剂为30%浓度的糊精液,糊精液的质量为所述复合原料总质量的3.5%。
本实施例的原位生成碳化硅纤维结合碳化硅耐磨材料的制备方法,包括下列步骤:
1)按上述方案,取配方量的碳化硅、二氧化硅微粉、石英粉、活性炭、炭黑、Fe粉、NaCl、钙长石和La2O3置于球磨罐中,于行星磨上干混120min,再加入糊精液,混合10min制成坯料;
2)将步骤1)所得坯料成型制成坯体;所述成型为机压成型,成型压力为300MPa,保压的时间为10s;
3)将步骤2)所得坯体进行干燥并在还原气氛下烧成,自然冷却,即得原位生成碳化硅纤维结合碳化硅耐磨材料。
步骤3)中所述的干燥温度为120℃,时间为8h;所述的烧成温度为1550℃,升温速率为2.5℃/min,保温时间为6h。所得耐磨材料的各性能参数列于表1中。
表1 实施例1-4所得耐磨材料的性能参数
性能 | 实施例1 | 实施例2 | 实施例3 | 实施例4 |
密度(g/cm3) | 2.71 | 2.92 | 2.78 | 2.98 |
显气孔率(%) | 9.73 | 6.59 | 8.93 | 5.25 |
弯曲强度(MPa) | 226 | 305 | 248 | 312 |
断裂韧性(MPa·m1/2) | 3.1 | 4.8 | 3.7 | 4.9 |
磨损量(g/min) | 0.011 | 0.003 | 0.009 | 0.002 |
硬度(HV) | 2618 | 3106 | 2810 | 3154 |
上述说明并非是对本发明的限制,本发明也并不限于上述举例,本技术领域的普通技术人员,在本发明的实质范围内,作出的变化、添加或替换,都应属于本发明的保护范围。
Claims (10)
1.一种原位生成碳化硅纤维结合碳化硅耐磨材料,其特征在于,由复合原料和结合剂在还原气氛下烧结制成,所述复合原料由以下重量百分比的原料组成:68%~80%碳化硅,13.7%~21.1%硅源,5.4%~7.7%碳源,0.45%~1.68%催化剂,0.45%~1.72%烧结助剂;所述碳化硅由碳化硅颗粒和碳化硅微粉组成,二者质量比为(90~98):(2~10);所述结合剂的质量为所述复合原料总质量的2%~5%。
2.根据权利要求1所述的一种原位生成碳化硅纤维结合碳化硅耐磨材料,其特征在于,所述碳化硅颗粒由大、中、小三组份颗粒组成,粒径分别为180~325µm、120~212µm、45~80µm;所述碳化硅微粉的粒径≤10µm。
3.根据权利要求1所述的一种原位生成碳化硅纤维结合碳化硅耐磨材料,其特征在于,所述的硅源为二氧化硅微粉、石英粉、硅溶胶中的一种或几种。
4.根据权利要求1所述的一种原位生成碳化硅纤维结合碳化硅耐磨材料,其特征在于,所述的碳源为石墨粉、活性炭、炭黑中的一种或几种。
5.根据权利要求1所述的一种原位生成碳化硅纤维结合碳化硅耐磨材料,其特征在于,所述的催化剂为Si-Fe合金粉、Ni粉、Fe粉、H3BO3、NaCl、NaF中的一种或几种。
6.根据权利要求1所述的一种原位生成碳化硅纤维结合碳化硅耐磨材料,其特征在于,所述的烧结助剂为Y2O3、CeO2、La2O3、钙长石中的一种或几种。
7.根据权利要求1所述的一种原位生成碳化硅纤维结合碳化硅耐磨材料,其特征在于,所述结合剂为聚乙烯醇溶液或糊精液;所述聚乙烯醇溶液的浓度为2.5%~3%;所述糊精液的浓度为30%~40%。
8.权利要求1所述的一种原位生成碳化硅纤维结合碳化硅耐磨材料的制备方法,其特征在于包括下列步骤:
取配方量的碳化硅、硅源、碳源、烧结助剂、催化剂、结合剂,混合均匀,制成坯料;
将步骤1)所得坯料成型制成坯体;
将步骤2)所得坯体进行干燥并在还原气氛下烧成,自然冷却,即得原位生成碳化硅纤维结合碳化硅耐磨材料。
9.根据权利要求8所述的一种原位生成碳化硅纤维结合碳化硅耐磨材料的制备方法,其特征在于,步骤2)中所述成型为机压成型,成型压力为200~300MPa,保压的时间为10~20s。
10.根据权利要求8所述的一种原位生成碳化硅纤维结合碳化硅耐磨材料的制备方法,其特征在于,步骤3)中所述干燥的温度为100~150℃,干燥的时间为8~12h;所述的还原气氛为在刚玉坩埚中利用埋碳法所制造的还原条件;所述的烧成的温度为1450~1600℃,保温的时间为3~8h。
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