CN115093227A - 一种以镀膜金刚石为原料制备聚晶金刚石的方法 - Google Patents
一种以镀膜金刚石为原料制备聚晶金刚石的方法 Download PDFInfo
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Abstract
本发明公开了一种以镀膜金刚石为原料制备聚晶金刚石的方法,属于超硬材料磨料磨具领域。主要过程分为金刚石表面净化、金刚石表面镀覆、预压及高温高压烧结三个部分。其中镀覆材料选用铁、钴、镍等常见触媒中的一种或几种组合,通过调控镀覆时间改变镀层厚度能有效调控金刚石生长情况。本发明操作简单,由此方法合成的聚晶金刚石与传统方法相比在硬度、致密度、磨耗比方面都有较大的提升,且在一定程度上能降低聚晶金刚石合成的条件,适合工业化生产。
Description
技术领域
本发明专利涉及超硬材料磨料磨具领域,是一种以镀膜金刚石为原料制备聚晶金刚石的方法。
背景技术
聚晶金刚石(PCD)是由金刚石微粉与金属触媒在高温高压下烧结而成的,其具有金刚石的高硬度和高耐磨性,由于其良好的性能,所以被广泛应用于石油钻头、刀具等多个行业。1964年GE公司第一次以“某些金属添加剂能使金刚石与金刚石之间直接结合”申请专利,1971年GE公司发明了历史上第一个实用型聚晶金刚石,此后被大量推广。
聚晶金刚石合成主要有爆炸合成法、低压气相沉积法、直接转化法、高温高压溶剂法四种方法。爆炸合成法是指在耐高压容器中,爆炸产生的高温和动能使金属片高速撞击石墨片,从而使石墨转化为微粉状态的聚晶金刚石;低压气相沉积法是指在低于1标准大气压下,含碳元素的气态原材料经过一系列化学反应,碳原子以金刚石相沉积在基体表面,形成一层聚晶金刚石膜;直接转化法是指高纯度石墨微粉在高温高压下直接转化为聚晶金刚石,此方法条件极其苛刻,无法达到工业化生产的需求;高温高压溶剂法是指经过铁、钴、镍、等金属触媒的催化,金刚石微粉在高温高压条件下转变为聚晶金刚石,此方法操作简单,合成周期短,适合工业化生产。
目前高温高压溶剂法制备聚晶金刚石工艺已经较为成熟,聚晶金刚石的合成与烧结温度、压力以及金属触媒种类有关。一般烧结温度在1200℃以上,压力在5GPa以上。在烧结过程中,随着温度升高,金属触媒熔融进入金刚石颗粒缝隙间,金刚石表面石墨化并溶解于液态触媒中,当液态金属触媒中的石墨达到饱和状态后,此时一旦达到金刚石的稳定区,金刚石便从触媒中析出,在析出过程中金刚石颗粒间以液态存在的触媒发生迁移,在迁移过程中金刚石颗粒相互结合,金刚石颗粒之间直接成键。但上述方法在高温高压下无法保证金刚石颗粒与触媒均匀接触,导致合成聚晶金刚石出现局部成键局部不成键的现象,使聚晶金刚石各项性能无法达到最优。
发明内容
本发明的目的在于:提供一种以镀膜金刚石为原料制备聚晶金刚石的方法,通过在金刚石颗粒表面镀覆金属触媒,能有效的改善金刚石与触媒之间的均匀接触,调控金刚石生长情况,使聚晶金刚石在硬度、致密度以及磨耗比方面都能有较大提升,具有较高的实用价值和应用前景。
技术方案
为实现本发明之目的,采用以下技术方案予以实现:
a、金刚石表面净化,其具体过程为:将金刚石与强酸混合均匀,进行加热净化处理,后将洗净的金刚石烘干备用;
b、金刚石表面镀覆处理,其具体过程为:选用磁控溅射技术在金刚石表面镀覆铁、钴、镍镀层,镀层为铁、钴、镍中的一种或几种组合,将表面净化处理后的金刚石放入磁控溅射设备中,设备真空度调至4×10-3~6×10-3Pa,选用纯度99.99%以上的铁靶、钴靶与镍靶,在额定功率下进行镀覆,溅射时间为10~30min,在溅射过程中腔体保持室温,且对金刚石进行超声振动,确保粉体均匀镀覆;
c、预压及高温高压烧结,其具体过程为:先将镀覆后的金刚石进行预压成型得到纳米金刚石胚体,预压成型压力为300~500MPa,将金刚石胚体放入模具中在高温高压下进行烧结得到致密的聚晶金刚石块,高温高压烧结温度为1200℃~1800℃,烧结压力为5~10GPa,保温保压时间为50~150min。
优选的,所述步骤a中强酸为适量浓度的稀硝酸,首先使用稀硝酸清洗金刚石表面污渍,然后用蒸馏水洗净硝酸,接着用丙酮溶液在超声波清洗仪清洗金刚石表面的有机溶剂10~30min,再用乙醇溶液对残留在金刚石表面的丙酮进行清洗,最后用蒸馏水洗净,在烘箱中烘干备用。
优选的,所述步骤b中镀覆技术选用磁控溅射技术,镀覆腔室真空度到4×10-3~6×10-3Pa,溅射时间为10~30min,镀层为铁、钴、镍中的一种或几种组合。
优选的,所述步骤c中预压成型压力为300~500MPa,高温高压烧结温度为1200℃~1800℃,烧结压力为5~10GPa,保温保压时间为50~150min。
本发明的有益效果是:
1.通过磁控溅射技术对金刚石表面镀覆金属触媒,更大程度的保证了金刚石与金属触媒的接触面积,与常见聚晶金刚石高温高压下合成方法相比,避免了烧结过程中金刚石与触媒接触不均匀现象发生,能有效的改善金刚石之间的结合生长,提高合成聚晶金刚石各项性能;
2.镀覆材料选择聚晶金刚石合成中常见的触媒铁、钴、镍中的一种或几种组合,通过调控镀覆时间能有效地调控金刚石的生长情况。
具体实施方式
该发明以下结合具体实施例进行进一步描述:
实施例1:
a、金刚石表面净化处理,其具体过程为:首先使用适量浓度稀硝酸清洗金刚石表面污渍,然后用蒸馏水洗净硝酸,接着用丙酮溶液在超声波清洗仪清洗金刚石表面的有机溶剂10min,再用乙醇溶液对残留在金刚石表面的丙酮进行清洗,最后用蒸馏水洗净,在烘箱中烘干备用;
b、金刚石表面镀覆处理,其具体过程为:选用磁控溅射技术在金刚石表面镀覆铁镀层,将表面净化处理后的金刚石放入磁控溅射设备中,设备真空度调至4×10-3Pa,选用纯度99.99%以上的铁靶,在额定功率下进行镀覆,溅射时间为10min,在溅射过程中腔体保持室温,且对金刚石进行超声振动,确保粉体均匀镀覆;
c、预压及高温高压烧结,其具体过程为:先将镀覆后的金刚石进行预压成型得到金刚石胚体,预压成型压力为300MPa,将纳米金刚石胚体放入模具中在高温高压下进行烧结得到致密的聚晶金刚石块。高温高压烧结温度为1200℃,烧结压力为5GPa,保温保压时间为50min。
实施例2:
a、金刚石表面净化处理,其具体过程为:首先使用适量浓度稀硝酸清洗金刚石表面污渍,然后用蒸馏水洗净硝酸,接着用丙酮溶液在超声波清洗仪清洗金刚石表面的有机溶剂20min,再用乙醇溶液对残留在金刚石表面的丙酮进行清洗,最后用蒸馏水洗净,在烘箱中烘干备用;
b、金刚石表面镀覆处理,其具体过程为:选用磁控溅射技术在金刚石表面镀覆钴镀层,将表面净化处理后的金刚石放入磁控溅射设备中,设备真空度调至5×10-3Pa,选用纯度99.99%以上的钴靶,在额定功率下进行镀覆,溅射时间为20min,在溅射过程中腔体保持室温,且对金刚石进行超声振动,确保粉体均匀镀覆;
c、预压及高温高压烧结,其具体过程为:先将镀覆后的金刚石进行预压成型得到金刚石胚体,预压成型压力为400MPa,将纳米金刚石胚体放入模具中在高温高压下进行烧结得到致密的聚晶金刚石块。高温高压烧结温度为1500℃,烧结压力为7GPa,保温保压时间为100min。
实施例3:
a、金刚石表面净化处理,其具体过程为:首先使用适量浓度稀硝酸清洗金刚石表面污渍,然后用蒸馏水洗净硝酸,接着用丙酮溶液在超声波清洗仪清洗金刚石表面的有机溶剂30min,再用乙醇溶液对残留在金刚石表面的丙酮进行清洗,最后用蒸馏水洗净,在烘箱中烘干备用;
b、金刚石表面镀膜处理,其具体过程为:选用磁控溅射技术在金刚石表面镀覆镍镀层,将表面净化处理后的金刚石放入磁控溅射设备中,设备真空度调至6×10-3Pa,选用纯度99.99%以上的镍靶,在额定功率下进行镀覆,溅射时间为30min,在溅射过程中腔体保持室温,且对金刚石进行超声振动,确保粉体均匀镀覆;
c、预压及高温高压烧结,其具体过程为:先将镀覆后的金刚石进行预压成型得到金刚石胚体,预压成型压力为500MPa,将金刚石胚体放入模具中在高温高压下进行烧结得到致密的聚晶金刚石块。高温高压烧结温度为1800℃,烧结压力为10GPa,保温保压时间为150min。
Claims (3)
1.一种以镀膜金刚石为原料制备聚晶金刚石的方法,其特征在于由以下步骤实现:
a、金刚石表面净化,其具体过程为:首先使用适量浓度稀硝酸清洗金刚石表面污渍,然后用蒸馏水洗净硝酸,接着用丙酮溶液在超声波清洗仪清洗金刚石表面的有机溶剂10~30min,再用乙醇溶液对残留在金刚石表面的丙酮进行清洗,最后用蒸馏水洗净,在烘箱中烘干备用;
b、金刚石表面镀覆处理,其具体过程为:选用磁控溅射技术在金刚石表面镀覆铁、钴、镍镀层,镀层为铁、钴、镍中的一种或几者组合,将表面净化处理后的金刚石放入磁控溅射设备中,设备真空度调至4×10-3~6×10-3Pa,选用纯度99.99%以上的铁靶、钴靶与镍靶,在额定功率下进行镀覆,溅射时间为10~30min,在溅射过程中腔体保持室温,且对金刚石进行超声振动,确保粉体均匀镀覆;
c、预压及高温高压烧结,其具体过程为:先将镀覆后的金刚石进行预压成型得到金刚石胚体,预压成型压力为300~500MPa,将金刚石胚体放入模具中在高温高压下进行烧结得到致密的聚晶金刚石块,高温高压烧结温度为1200℃~1800℃,烧结压力为5~10GPa,保温保压时间为50~150min。
2.根据权利要求1所述的制备方法,其特征在于:步骤b中选择的镀覆技术为磁控溅射技术,设备真空度调至4×10-3~6×10-3Pa,选用纯度99.99%以上的铁靶、钴靶与镍靶,在额定功率下进行镀覆,溅射时间为10~30min。
3.根据权利要求1所述的制备方法,其特征在于:步骤c中预压成型压力为300~500MPa,高温高压烧结温度为1200℃~1800℃,烧结压力为5~8GPa,保温保压时间为50~150min。
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