CN116356319A - 一种高致密耐腐蚀高洁净的复合镀层的制备方法 - Google Patents
一种高致密耐腐蚀高洁净的复合镀层的制备方法 Download PDFInfo
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Abstract
本发明涉及一种高致密耐腐蚀高洁净的复合镀层的制备方法,使用多套设备进行制备包括电源整流器,径向大气等离子体喷涂设备、轴向大气等离子体喷涂设备。制备方法为:(1)使用喷砂方法对待镀层表面进行预处理;(2)使用电源整流器,对待镀层表面进行阳极化处理;(3)对阳极化后的表面进行清洗清洁;(4)使用大气等离子体喷涂设备,进行涂层喷涂;(5)使用超洁净水对喷涂后表面进行清洗清洁;(6)使用大气等离子体喷涂设备,对喷涂后表面进行致密层喷涂;(7)将喷涂后产品进行百级以上无尘室进行清洗。该方法获得的氧化钇涂层具有高致密性,高耐腐蚀性、高洁净度和抗电压性。在耐等离子体刻蚀的环境中具有优异的表现。
Description
技术领域
本发明涉及一种多制程制备氧化物陶瓷层复合层领域,特别是具有高耐腐蚀性,高致密涂层,高洁净度要求的涂层领域制备方法。
背景技术
随着半导体设备的不断发展,对刻蚀腔内的铝制零部件的耐腐蚀性要求越来越高。传统的铝制零部件采用阳极氧化的方式,在铝制零部件表面形成一层阳极膜来耐腐蚀,但其耐腐蚀性已不能满足先进半导体设备的要求,铝制零部件的寿命降低,其更换频率越来越高,目前,很多企业采用在铝基体上进行氧化物等离子喷涂的方式来增强其耐腐蚀耐磨性能,但这种喷涂涂层具有较多的孔隙,使得涂层内部在使用过程中会不断被破坏从而影响寿命。使用低微纳米材料做喷涂涂层,可以有效解决孔隙率问题,但成本的增加及随着镀层越厚,结合力问题的不足,都暴露了其弊端。随着集成电路纳米制程越来越精细,对涂层的致密度和洁净度要求会越来越高。
发明内容
本发明一种高致密耐腐蚀高洁净的复合镀层的制备方法,使用多项制程进行复合镀层的制备,具有良好的耐腐蚀性、耐电压性和洁净度,可用于集成电路刻蚀过程的高严苛环境中。
本发明的目的是通过如下技术方案实现的:
一种高致密耐腐蚀高洁净的复合镀层的制备方法,该镀层制备方法包括以下步骤:
(1)使用喷砂方法对待镀层表面进行预处理;
(2)使用电源整流器,对待镀层表面进行阳极化处理;
(3)对阳极化后的表面进行清洗清洁;
(4)使用大气等离子体喷涂设备,进行涂层喷涂;
(5)使用超洁净水对喷涂后表面进行清洗清洁;
(6)使用大气等离子体喷涂设备,对喷涂后表面进行致密层喷涂;
(7)将喷涂后产品进行百级以上无尘室进行清洗。
步骤(1)所述喷砂方法,使用手动或自动编程方式进行喷砂。
步骤(1)所述喷砂方法,使用砂材包括棕刚玉、石榴石、白刚玉、玻璃珠、碳化硅材质。
步骤(2)所述的阳极化处理,使用的电源整流器包含以下的一种,直流电压电源、交流电压电源、脉冲电压电源。
步骤(2)所述的阳极化处理,所使用的槽液包含以下的一种或两种混合,硫酸、盐酸、硝酸、硼酸、草酸、氢氟酸。
步骤(2)所述的阳极化处理,阳极膜厚范围在40-100um。
步骤(3)所述的清洗清洁,使用水质>200K Ohm-cm.
步骤(3)所述的清洗清洁,清洗方式包含以下方式的一种或多种:脱脂清洗、硫酸化学清洗、盐酸化学清洗、硝酸化学清洗、去离子水超声波清洗、去离子水高压清洗、去离子水擦拭、醇类化学药剂擦拭、丙酮化学药剂擦拭。
步骤(4)所述的涂层喷涂,所使用原料包括以下的一种或多种:氧化铝、氧化钇、碳化钨、氟化钇、钇铝石榴石。
步骤(4)所述的涂层喷涂,选用的设备包含以下的一种或多种:径向大气等离子喷涂设备、轴向大气等离子喷涂设备、电弧喷涂设备。
步骤(5)所述的涂层后清洁清洗,使用水质>200K Ohm-cm.
步骤(5)所述的涂层后清洁清洗,清洗环境高于Class 1000无尘室环境。
步骤(5)所述的涂层后清洁清洗,清洗方式包含以下方式的一种或多种:脱脂清洗、硫酸化学清洗、盐酸化学清洗、硝酸化学清洗、去离子水超声波清洗、去离子水高压清洗、去离子水擦拭、醇类化学药剂擦拭、丙酮化学药剂擦拭。
步骤(6)所述的致密层喷涂,选用的设备包含以下的一种或多种:径向大气等离子喷涂设备、轴向大气等离子喷涂设备、电弧喷涂设备、气溶胶沉积设备、超音速火焰喷涂设备。
步骤(6)所述的致密层喷涂,选用材料粒径范围为0.1um-10um。
步骤(7)所述的无尘室清洗,使用水质>200K Ohm-cm。
步骤(7)所述的无尘室清洗,清洗方式包含以下方式的一种或多种:脱脂清洗、硫酸化学清洗、盐酸化学清洗、硝酸化学清洗、去离子水超声波清洗、去离子水高压清洗、去离子水擦拭、醇类化学药剂擦拭、丙酮化学药剂擦拭。
本发明的有益效果是:
1、本发明选用的高致密耐腐蚀高洁净的复合镀层,各部分镀层均可发挥自身的优势,即化学稳定性,高耐腐蚀性,高抗电性及高洁净度,从而可使用在更严苛的集成电路制造等离子体刻蚀环境中
2、本发明选用的高致密耐腐蚀高洁净的复合镀层,可通过其他镀层复合,来避免自身的弊端。如致密镀层的成本、低沉积效率及高厚度下的结合力问题。
具体实施方式
下面结合实施例对本发明进一步详细说明。
一种高致密耐腐蚀高洁净的复合镀层的制备方法,该镀层制备方法包括以下步骤:
(1)使用喷砂方法对待镀层表面进行预处理;
(2)使用电源整流器,对待镀层表面进行阳极化处理;
(3)对阳极化后的表面进行清洗清洁;
(4)使用大气等离子体喷涂设备,进行涂层喷涂;
(5)使用超洁净水对喷涂后表面进行清洗清洁;
(6)使用大气等离子体喷涂设备,对喷涂后表面进行致密层喷涂;
(7)将喷涂后产品进行百级以上无尘室进行清洗。
其制备设备使用径向大气等离子体喷涂设备或轴向大气等离子体喷涂设备。
步骤(1)所述喷砂方法,使用手动或自动编程方式进行喷砂。
步骤(1)所述喷砂方法,使用砂材包括棕刚玉、石榴石、白刚玉、玻璃珠、碳化硅材质。
步骤(2)所述的阳极化处理,使用的电源整流器包含以下的一种,直流电压电源、交流电压电源、脉冲电压电源。
步骤(2)所述的阳极化处理,所使用的槽液包含以下的一种或两种混合,硫酸、盐酸、硝酸、硼酸、草酸、氢氟酸。
步骤(2)所述的阳极化处理,阳极膜厚范围在40-100um。
步骤(3)所述的清洗清洁,使用水质>200K Ohm-cm.
步骤(3)所述的清洗清洁,清洗方式包含以下方式的一种或多种:脱脂清洗、硫酸化学清洗、盐酸化学清洗、硝酸化学清洗、去离子水超声波清洗、去离子水高压清洗、去离子水擦拭、醇类化学药剂擦拭、丙酮化学药剂擦拭。
步骤(4)所述的涂层喷涂,所使用原料包括以下的一种或多种:氧化铝、氧化钇、碳化钨、氟化钇、钇铝石榴石。
步骤(4)所述的涂层喷涂,选用的设备包含以下的一种或多种:径向大气等离子喷涂设备、轴向大气等离子喷涂设备、电弧喷涂设备。
步骤(5)所述的涂层后清洁清洗,使用水质>200K Ohm-cm.
步骤(5)所述的涂层后清洁清洗,清洗环境高于Class 1000无尘室环境。
步骤(5)所述的涂层后清洁清洗,清洗方式包含以下方式的一种或多种:脱脂清洗、硫酸化学清洗、盐酸化学清洗、硝酸化学清洗、去离子水超声波清洗、去离子水高压清洗、去离子水擦拭、醇类化学药剂擦拭、丙酮化学药剂擦拭。
步骤(6)所述的致密层喷涂,选用的设备包含以下的一种或多种:径向大气等离子喷涂设备、轴向大气等离子喷涂设备、电弧喷涂设备、气溶胶沉积设备、超音速火焰喷涂设备。
步骤(6)所述的致密层喷涂,选用材料粒径范围为0.1um-10um。
步骤(7)所述的无尘室清洗,使用水质>200K Ohm-cm。
步骤(7)所述的无尘室清洗,清洗方式包含以下方式的一种或多种:脱脂清洗、硫酸化学清洗、盐酸化学清洗、硝酸化学清洗、去离子水超声波清洗、去离子水高压清洗、去离子水擦拭、醇类化学药剂擦拭、丙酮化学药剂擦拭。
实施例
首先,使用自动编程喷砂方式,使用棕刚玉砂材,对待镀层区域进行喷砂。喷砂后使用脉冲电压电源,对表面进行阳极化处理,阳极膜厚45um,阳极化处理后对表面进行脱脂清洗、硝酸化学清洗及超声波清洗,水质>300K Ohm-cm,后用丙酮化学试剂擦拭。清洗后使用轴向大气等离子喷涂设备,进行氧化钇喷涂,喷涂后在Class1000无尘室环境中,使用硝酸化学清洗、高压清洗洁净表面。清洁后使用径向大气等离子喷涂设备,原料粒径0.2um,进行致密涂层氟化钇喷涂。喷涂后在Class100无尘室环境中,使用水质>300K Ohm-cm进行超声波清洗及高压清洗,最后用乙醇化学试剂擦拭。得到完成镀层。所得到的镀层总厚度为230um,孔隙率1.2%,耐击穿电压8300V,耐腐蚀性盐酸测试14小时。
以上所述仅为本发明的优选实施例而已,并不用于限制本发明,对于本领域技术人员来说,本发明可有各种更改和变化。本发明可用于半导体行业的各种需要具有耐腐蚀功能涂层的零部件,但也不仅仅限制于半导体领域。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种高致密耐腐蚀高洁净的复合镀层的制备方法,其特征在于,该镀层制备方法包括以下步骤:
(1)使用喷砂方法对待镀层表面进行预处理;
(2)使用电源整流器,对待镀层表面进行阳极化处理;
(3)对阳极化后的表面进行清洗清洁;
(4)使用大气等离子体喷涂设备,进行涂层喷涂;
(5)使用超洁净水对喷涂后表面进行清洗清洁;
(6)使用大气等离子体喷涂设备,对喷涂后表面进行致密层喷涂;
(7)将喷涂后产品进行百级以上无尘室进行清洗。
2.按照权利要求1所述的一种高致密耐腐蚀高洁净的复合镀层的制备方法,其特征在于:所述步骤(1)喷砂方法,使用手动或自动编程方式进行喷砂;使用砂材包括棕刚玉、石榴石、白刚玉、玻璃珠、碳化硅材质。
3.按照权利要求1所述的一种高致密耐腐蚀高洁净的复合镀层的制备方法,其特征在于:
所述步骤(2)阳极化处理,使用的电源整流器包含以下的一种,直流电压电源、交流电压电源、脉冲电压电源。
4.按照权利要求1所述的一种高致密耐腐蚀高洁净的复合镀层的制备方法,其特征在于:所述步骤(2)阳极化处理,所使用的槽液包含以下的一种或两种混合,硫酸、盐酸、硝酸、硼酸、草酸、氢氟酸。
5.按照权利要求1所述的一种高致密耐腐蚀高洁净的复合镀层的制备方法,其特征在于:所述步骤(2)阳极化处理,阳极膜厚范围在40-100um。
6.按照权利要求1所述的一种高致密耐腐蚀高洁净的复合镀层的制备方法,其特征在于:所述步骤(3)清洗清洁,使用水质>200KOhm-cm;
清洗方式包含以下方式的一种或多种:脱脂清洗、硫酸化学清洗、盐酸化学清洗、硝酸化学清洗、去离子水超声波清洗、去离子水高压清洗、去离子水擦拭、醇类化学药剂擦拭、丙酮化学药剂擦拭。
7.按照权利要求1所述的一种高致密耐腐蚀高洁净的复合镀层的制备方法,其特征在于:步骤(4)所述的涂层喷涂,所使用原料包括以下的一种或多种:氧化铝、氧化钇、碳化钨、氟化钇、钇铝石榴石;涂层喷涂选用的设备包含以下的一种或多种:径向大气等离子喷涂设备、轴向大气等离子喷涂设备、电弧喷涂设备。
8.按照权利要求1所述的一种高致密耐腐蚀高洁净的复合镀层的制备方法,其特征在于:所述步骤(5)涂层后清洁清洗,使用水质>200KOhm-cm;清洗环境高于Class1000无尘室环境;清洗方式包含以下方式的一种或多种:脱脂清洗、硫酸化学清洗、盐酸化学清洗、硝酸化学清洗、去离子水超声波清洗、去离子水高压清洗、去离子水擦拭、醇类化学药剂擦拭、丙酮化学药剂擦拭。
9.按照权利要求1所述的一种高致密耐腐蚀高洁净的复合镀层的制备方法,其特征在于:所述步骤(6)致密层喷涂,选用的设备包含以下的一种或多种:径向大气等离子喷涂设备、轴向大气等离子喷涂设备、电弧喷涂设备、气溶胶沉积设备、超音速火焰喷涂设备;致密层喷涂选用材料粒径范围为0.1um-10um。
10.按照权利要求1所述的一种高致密耐腐蚀高洁净的复合镀层的制备方法,其特征在于:所述步骤(7)无尘室清洗,使用水质>200KOhm-cm;无尘室清洗清洗方式包含以下方式的一种或多种:脱脂清洗、硫酸化学清洗、盐酸化学清洗、硝酸化学清洗、去离子水超声波清洗、去离子水高压清洗、去离子水擦拭、醇类化学药剂擦拭、丙酮化学药剂擦拭。
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