CN108274009B - 一种Cr靶材的修复方法 - Google Patents
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Abstract
本发明公开了一种Cr靶材的修复方法,其是将待修复的Cr靶材放入石墨模具中,然后加入修复所需的Cr粉,使Cr粉位于Cr靶材的待修复表面上,预压后,再放入放电等离子烧结系统中进行烧结连接,使Cr粉填充在Cr靶材待修复表面的不平整缺陷区域,即完成Cr靶材的修复。本发明采用SPS技术,通过选择合适的烧结参数,可将Cr靶材表面的缺陷修补完整,且修补后组织细小、致密度高、拉伸性能与原靶材一致,有效解决了现有Cr靶材表面产生缺陷后无法修补再利用的问题,且工艺简单、周期短、生产效率高,可大幅度降低Cr靶材的使用成本。
Description
技术领域
本发明属于粉末冶金领域,具体涉及一种铬靶材的修复方法。
背景技术
Cr溅射靶材广泛应用于电子及信息产业,如集成电路、信息存储、液晶显示屏、激光存储器、电子控制器件等;亦可应用于玻璃镀膜领域;还可以应用于耐磨材料、高温耐蚀、高档装饰用品等行业。其原理是在被溅射的靶极(阴极)与阳极之间加一个正交磁场和电场,在高真空室中充入所需要的惰性气体(通常为Ar气),永久磁铁在靶材料表面形成250~350高斯的磁场,同高压电场组成正交电磁场。在电场的作用下,Ar气电离成正离子和电子,靶上加有一定的负高压,从靶极发出的电子受磁场的作用与工作气体的电离几率增大,在阴极附近形成高密度的等离子体,Ar离子在洛仑兹力的作用下加速飞向靶面,以很高的速度轰击靶面,使靶上被溅射出来的原子遵循动量转换原理以较高的动能脱离靶面飞向基片淀积成膜。长时间工作条件下,Cr靶材表面会出现缺陷,影响材料的性能和使用寿命。但目前尚无对Cr靶材进行修复的有效方法,导致在Cr靶材表面产生缺陷后无法修补再利用,不但会造成严重的资源浪费,而且还会引起重金属污染。
发明内容
针对现有技术所存在的不足之处,本发明提供了一种Cr靶材的修复方法,旨在通过放电等离子烧结(SPS)的方法实现Cr靶材的修复。
本发明解决技术问题,采用如下技术方案:
本发明提供了一种Cr靶材的修复方法,其特点在于:将待修复的Cr靶材放入石墨模具中,然后加入修复所需的Cr粉,使Cr粉位于Cr靶材的待修复表面上,预压后,再放入放电等离子烧结系统中进行烧结连接,使Cr粉填充在Cr靶材待修复表面的不平整缺陷区域,即完成Cr靶材的修复。具体包括以下步骤:
步骤1、对待修复的Cr靶材的待修复表面进行清理,以去除杂质和氧化层,然后利用阿基米德排水法计算出填补Cr靶材待修复表面的不平整缺陷区域所需Cr粉的体积;
称取相应体积的氧含量低于500ppm、粒径在80~400目之间的Cr粉备用;
步骤2、将清理后的Cr靶材放入石墨模具中,再加入Cr粉,并使Cr粉位于Cr靶材的待修复表面上;采用手动液压机对装好Cr靶材和Cr粉的石墨模具进行预压,压力在8~12MPa;
步骤3、在预压后石墨模具外围裹上与石墨模具等高的4~6mm厚的碳毡,再将其置于放电等离子烧结系统的炉腔中,抽真空至5Pa以下,对Cr粉和Cr靶材进行烧结连接,烧结工艺为:
轴向机械压力:10~50MPa,
升温速率:10~80℃/min,
烧结温度:1200~1350℃,
保温时间:5~20min;
随炉冷却后,即完成Cr靶材的修复,获得致密度高、力学性能优异的修复后Cr靶材。
进一步地,所修复的Cr靶材直径大于20mm、长径比为0.05~1.0。
进一步地,所述升温速率在室温至1000℃区间为30~80℃/min,1000℃以上为10~30℃/min。
进一步地,所述轴向机械压力采用梯度加压的方式:当温度<1200时,轴向压力为10MPa;当温度≥1200℃时,轴向压力为40~50MPa。
本发明的有益效果体现在:
1、本发明采用SPS技术,通过选择合适的烧结参数,可将Cr靶材表面的缺陷修补完整,且修补后组织细小、致密度高,和原靶材几乎一致,有效解决了现有Cr靶材表面产生缺陷后无法修补再利用的问题,且工艺简单、周期短、生产效率高,可大幅度降低Cr靶材的使用成本。
2、本发明可根据待修复Cr靶材的尺寸,选择合适尺寸的石墨模具和压头,从而可实现各种Cr靶材修复。
3、本发明优化了Cr靶材的修复工艺,对不同直径和长径比的Cr靶材圆柱锭采用不同的工艺条件,可使其性能进一步改善。
4、本发明修复得到的Cr靶材材料具有良好的硬度,且拉伸性能和原靶材拉伸性能一致,应用前景广阔。
附图说明
图1为本发明实施例3中修复后Cr靶材连接处的微观组织照片。
具体实施方式
下面结合实施例对本发明作详细说明,下述实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。
下述实施例中,选用氧含量低于500ppm、粒径在80~400目之间的金属Cr粉。
下述实施例所用放电等离子烧结炉为日本Sinter Land Inc公司生产的LABOX系列放电等离子烧结系统,其电流类型为直流脉冲电流,脉冲序列为40:7。
实施例1
本实施例对Φ30mm×30mm的Cr靶材圆柱锭进行修复,具体步骤如下:
步骤1、选用车工对待修复的Cr靶材的待修复表面进行清理,以去除杂质和氧化层,然后利用阿基米德排水法计算出填补Cr靶材待修复表面的不平整缺陷区域所需Cr粉的体积;
称取相应体积的Cr粉备用;
步骤2、将清理后的Cr靶材放入石墨模具中,再加入Cr粉,并使Cr粉位于Cr靶材的待修复表面上;采用手动液压机对装好Cr靶材和Cr粉的石墨模具进行预压,压力为~10MPa;
步骤3、在预压后石墨模具外围裹上与石墨模具等高的~5mm厚的碳毡,再将其置于放电等离子烧结系统的炉腔中,抽真空至5Pa以下,对Cr粉和Cr靶材进行烧结连接,烧结工艺为:
轴向机械压力:采用梯度加压的方式(室温至1200℃,压力为10MPa;1200~1250℃,压力为40MPa)
升温速率:室温至1000℃,升温速率为50℃/min;1000~1250℃,升温速率为30℃/min;
烧结温度:1250℃,
保温时间:10min;
随炉冷却后,即完成Cr靶材的修复,获得高致密度的Φ30mm×30mm修复后Cr靶材圆柱锭,其氧含量为270ppm、致密度为97.01%、拉伸强度为40.53MPa。
实施例2
本实施例对Φ30mm×30mm的Cr靶材圆柱锭进行修复,具体步骤如下:
步骤1、选用车工对待修复的Cr靶材的待修复表面进行清理,以去除杂质和氧化层,然后利用阿基米德排水法计算出填补Cr靶材待修复表面的不平整缺陷区域所需Cr粉的体积;
称取相应体积的Cr粉备用;
步骤2、将清理后的Cr靶材放入石墨模具中,再加入Cr粉,并使Cr粉位于Cr靶材的待修复表面上;采用手动液压机对装好Cr靶材和Cr粉的石墨模具进行预压,压力为~10MPa;
步骤3、在预压后石墨模具外围裹上与石墨模具等高的~5mm厚的碳毡,再将其置于放电等离子烧结系统的炉腔中,抽真空至5Pa以下,对Cr粉和Cr靶材进行烧结连接,烧结工艺为:
轴向机械压力:采用梯度加压的方式(室温至1200℃,压力为10MPa;1200-1300℃,压力为50MPa);
升温速率:室温至1000℃,升温速率为50℃/min;1000~1300℃,升温速率为30℃/min;
烧结温度:1300℃;
保温时间:15min;
随炉冷却后,即完成Cr靶材的修复,获得高致密度的Φ30mm×30mm修复后Cr靶材圆柱锭,其氧含量为300ppm、致密度为97.90%、拉伸强度为86.50MPa。
实施例3
本实施例对Φ30mm×30mm的Cr靶材圆柱锭进行修复,具体步骤如下:
步骤1、选用车工对待修复的Cr靶材的待修复表面进行清理,以去除杂质和氧化层,然后利用阿基米德排水法计算出填补Cr靶材待修复表面的不平整缺陷区域所需Cr粉的体积;
称取相应体积的Cr粉备用;
步骤2、将清理后的Cr靶材放入石墨模具中,再加入Cr粉,并使Cr粉位于Cr靶材的待修复表面上;采用手动液压机对装好Cr靶材和Cr粉的石墨模具进行预压,压力为~10MPa;
步骤3、在预压后石墨模具外围裹上与石墨模具等高的~5mm厚的碳毡,再将其置于放电等离子烧结系统的炉腔中,抽真空至5Pa以下,对Cr粉和Cr靶材进行烧结连接,烧结工艺为:
轴向机械压力:采用梯度加压的方式(室温至1200℃,压力为10MPa;1200~1350℃,压力为50MPa);
升温速率:室温至1000℃,升温速率为50℃/min;1000~1350℃,升温速率为30℃/min;
烧结温度:1350℃;
保温时间:20min;
随炉冷却后,即完成Cr靶材的修复,获得高致密度的Φ30mm×30mm修复后Cr靶材圆柱锭,其氧含量为300ppm、致密度为98.80%、拉伸强度为90.83MPa。
图1为本实施例修复后Cr靶材连接处的微观组织照片,可以看出靶材修补后组织细小、致密度高。
实施例4
本实施例对Φ50mm×30mm的Cr靶材圆柱锭进行修复,具体步骤如下:
步骤1、选用车工对待修复的Cr靶材的待修复表面进行清理,以去除杂质和氧化层,然后利用阿基米德排水法计算出填补Cr靶材待修复表面的不平整缺陷区域所需Cr粉的体积;
称取相应体积的Cr粉备用;
步骤2、将清理后的Cr靶材放入石墨模具中,再加入Cr粉,并使Cr粉位于Cr靶材的待修复表面上;采用手动液压机对装好Cr靶材和Cr粉的石墨模具进行预压,压力为~10MPa;
步骤3、在预压后石墨模具外围裹上与石墨模具等高的~5mm厚的碳毡,再将其置于放电等离子烧结系统的炉腔中,抽真空至5Pa以下,对Cr粉和Cr靶材进行烧结连接,烧结工艺为:
轴向机械压力:采用梯度加压的方式(室温至1200℃,压力为10MPa;1200-1300℃,压力为40MPa);
升温速率:室温至1000℃,升温速率为50℃/min;1000~1300℃,升温速率为30℃/min;
烧结温度:1300℃;
保温时间:10min;
随炉冷却后,即完成Cr靶材的修复,获得高致密度的Φ50mm×30mm修复后Cr靶材圆柱锭,其氧含量为360ppm、致密度为97.95%、拉伸强度为85.35MPa。
实施例5
本实施例对Φ60mm×45mm的Cr靶材圆柱锭进行修复,具体步骤如下:
步骤1、选用车工对待修复的Cr靶材的待修复表面进行清理,以去除杂质和氧化层,然后利用阿基米德排水法计算出填补Cr靶材待修复表面的不平整缺陷区域所需Cr粉的体积;
称取相应体积的Cr粉备用;
步骤2、将清理后的Cr靶材放入石墨模具中,再加入Cr粉,并使Cr粉位于Cr靶材的待修复表面上;采用手动液压机对装好Cr靶材和Cr粉的石墨模具进行预压,压力为~10MPa;
步骤3、在预压后石墨模具外围裹上与石墨模具等高的~5mm厚的碳毡,再将其置于放电等离子烧结系统的炉腔中,抽真空至5Pa以下,对Cr粉和Cr靶材进行烧结连接,烧结工艺为:
轴向机械压力:采用梯度加压的方式(室温至1200℃,压力为10MPa;1200-1300℃,压力为50MPa);
升温速率:室温至1000℃,升温速率为50℃/min;1000~1300℃,升温速率为30℃/min;
烧结温度:1200℃;
保温时间:15min;
随炉冷却后,即完成Cr靶材的修复,获得高致密度的Φ60mm×45mm修复后Cr靶材圆柱锭,其氧含量为400ppm、致密度为96.75%、拉伸强度为45.37MPa。
以上仅为本发明的示例性实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (3)
1.一种Cr靶材的修复方法,其特征在于:将待修复的Cr靶材放入石墨模具中,然后加入修复所需的Cr粉,使Cr粉位于Cr靶材的待修复表面上,预压后,再放入放电等离子烧结系统中进行烧结连接,使Cr粉填充在Cr靶材待修复表面的不平整缺陷区域,即完成Cr靶材的修复;具体包括以下步骤:
步骤1、对待修复的Cr靶材的待修复表面进行清理,以去除杂质和氧化层,然后利用阿基米德排水法计算出填补Cr靶材待修复表面的不平整缺陷区域所需Cr粉的体积;
称取相应体积的氧含量低于500ppm、粒径在80~400目之间的Cr粉备用;
步骤2、将清理后的Cr靶材放入石墨模具中,再加入Cr粉,并使Cr粉位于Cr靶材的待修复表面上;采用手动液压机对装好Cr靶材和Cr粉的石墨模具进行预压,压力在8~12MPa;
步骤3、在预压后石墨模具外围裹上与石墨模具等高的4~6mm厚的碳毡,再将其置于放电等离子烧结系统的炉腔中,抽真空至5Pa以下,对Cr粉和Cr靶材进行烧结连接,烧结工艺为:
轴向机械压力采用梯度加压的方式:当温度<1200℃时,轴向压力为10MPa;当温度≥1200℃时,轴向压力为40~50MPa;
升温速率:10~80℃/min;
烧结温度:1200~1350℃;
保温时间:5~20min;
随炉冷却后,即完成Cr靶材的修复,获得修复后Cr靶材。
2.根据权利要求1所述的Cr靶材的修复方法,其特征在于:所修复的Cr靶材直径大于20mm、长径比为0.05~1.0。
3.根据权利要求1所述的Cr靶材的修复方法,其特征在于:所述升温速率在室温至1000℃区间为30~80℃/min,1000℃以上为10~30℃/min。
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