CN104294206B - 一种半导体装备用抗高温蠕变接地基片的制备方法 - Google Patents
一种半导体装备用抗高温蠕变接地基片的制备方法 Download PDFInfo
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Abstract
本发明涉及一种在金属或合金基片上制备纯铝涂层的方法，特别是涉及一种半导体装备用抗高温蠕变接地基片的制备方法。该制备方法包括如下步骤：(1)接地基片基体的前处理；(2)将基体放置于专用夹具上；(3)冷喷涂纯铝；(4)喷涂后热处理；(5)涂层表面后续处理。本发明的制备方法能够在各种金属或合金基片上形成纯铝涂层，使产品既在基体上保持基片的性能，如抗高温蠕变性能，同时在表面又有纯铝涂层的各种性能。
Description
技术领域
本发明涉及一种在金属或合金基片上制备纯铝涂层的方法，特别是涉及一种半导体装备用抗高温蠕变接地基片的制备方法。
背景技术
半导体装备中的接地基片处于高温等离子辐射和氟化物气体共同作用环境，不仅要求其具有良好的导电性能，而且对其抗高温蠕变性也提出了越来越高的要求。纯铝材料是半导体装备、尤其是大规模集成电路装备中理想的导电材料，这主要是因为铝除了具有良好的导电性外，在集成电路刻蚀、光刻以及镀膜等工艺过程中对元器件的污染最小。但是铝的熔点较低，只能在较低温度下(300℃以下)使用，随着工艺优化设计的要求，接地基片所处腔室的温度不断提高，已超过350℃，且还在提高，甚至超过400℃，此时纯铝已无法满足使用要求。不锈钢、镍基合金等具备优异的高温性能，但是导电性较差，而且在强等离子辐射条件下释放铁、镍等有害金属离子，污染半导体工艺环境，导致刻蚀、光刻以及镀膜过程中元器件报废。
目前，采用冷喷涂或热喷涂在不锈钢或镍基合金表面涂覆纯铝制备半导体装备接地基片的方法尚未见报道。
发明内容
本发明的目的是提供一种半导体装备用抗高温蠕变接地基片的制备方法，以不锈钢、镍合金或耐热钢等高温力学性能较好的材料做为半导体装备用抗高温蠕变接地基片的基体，在其表面制备厚度均匀、结合力良好的无氧化纯铝涂层，一方面利用纯铝的导电性能及其与大规模集成电路工艺的相容性，另一方面利用基体的力学性能解决接地基片抗高温蠕变性不够的问题。
本发明的技术方案如下：
一种半导体装备用抗高温蠕变接地基片的制备方法，包括如下步骤：
(1)接地基片基体的前处理：将所述接地基片的基体表面先进行纹理处理，纹理处理工艺参数为：320#砂纸抛光，去除基体表面积碳层；再用无水乙醇进行清洗；
(2)冷喷涂系统包括喷涂设备、喷涂室和专用夹具，所述专用夹具设置在所述喷涂室内，将所述基体放置于专用夹具上；
(3)喷涂：采用冷喷涂工艺制备纯铝涂层，利用所述冷喷涂系统，使压缩气体携带铝粉以超音速喷涂于所述基体表面，形成纯铝涂层，制得接地基片；喷涂工艺参数如下：喷涂距离5～50mm、气体压力0.5～4.5MPa、气体温度150～500℃、气体流量5～50g/s、铝粉纯度90％以上，铝粉粉末粒度200～600目；
(4)喷涂后热处理工艺：将所述接地基片置于热处理炉中随炉升温至100～500℃，在该温度下保温1～5小时；
(5)涂层表面后续处理：用菜瓜布和酒精对接地基片进行湿抛光，使接地基片表面无色差。
所述的半导体装备用抗高温蠕变接地基片的制备方法，优选方案为，其中专用夹具包括底座、侧壁和上板，所述侧壁上设置抽气口，所述抽气口可以接通真空泵；所述上板设置多个吸气孔，所述基体放置于所述吸气孔的上面，真空泵开动时将所述基体吸附在所述专用夹具上。
所述的半导体装备用抗高温蠕变接地基片的制备方法，优选方案为，所述基体由不锈钢、镍基合金或耐热钢制成；所述基体厚度为0.1～0.6mm。
所述的半导体装备用抗高温蠕变接地基片的制备方法，优选方案为，所述喷涂设备包括进气管、加热器、送粉器和超音速喷嘴，进气管的一端与高压气源连接，进气管的另一端分别经送粉器和加热器与超音速喷嘴相连接，所述基体表面与超音速喷嘴出口相对。
所述的半导体装备用抗高温蠕变接地基片的制备方法，优选方案为，超音速喷嘴包括进气口、收缩段、喉部、扩张段和出口，超音速喷嘴安装于喷涂室入口处，压缩气体分两路，一路进入送粉器，作为载带气将铝粉粉末引入超音速喷嘴；另一路连接加热器使气体膨胀，提高气流速度及加热铝粉粉末，之后两路气体进入超音速喷嘴，在其中形成气-固双相流，双相流中高动能铝粉颗粒撞击所述基体表面后产生塑性变形并沉积于所述基体表面形成铝导电层。
所述的半导体装备用抗高温蠕变接地基片的制备方法，优选方案为，所述压缩气体为空气、氮气或者氦气。
本发明的有益效果如下：
1.本发明是冷喷涂方法在半导体装备用抗高温蠕变接地基片上的应用，所制备的涂层厚度均匀、与基体结合良好、孔隙率低，从而提高接地基片的导电性能。
2.本发明采用冷气动力喷涂方法，纯铝粉末主要依靠塑性变形沉积形成涂层，喷涂温度远低于纯铝熔点，因此涂层中的氧含量低，从而提高接地基片的导电性能。
3.本发明还具有沉积效率高、能耗小、无热辐射、粉末可循环利用，操作简单、安全、成本低和无环境污染等特点。
4、半导体装备中接地基片非常薄，处于柔软状态，因此称之为软基片。在软基片上喷涂导电涂层，要达到厚度均匀、结合力良好很难实现。本发明采用专用夹具，通过抽真空将软基片吸附于专用夹具上来定位，这样喷涂铝涂层，能够实现喷涂的涂层厚度均匀、结合力良好。
总之，本发明采用的工艺可以实现低温状态下的金属铝涂层沉积，这种工艺过程对金属粉末结构几乎无热影响，仅通过颗粒获得的超音速实现金属涂层的沉积。因此，该方法能够在镍基合金等材料上形成涂层，而不影响基体材料的性能，为制备高性能无氧涂层提供一种重要的工艺方法，本发明采用冷喷涂方法在镍基合金表面成功地制备出性能良好的导电涂层。
附图说明
图1为冷喷涂系统结构示意图；
图2为涂层SEM截面形貌图；
图3为涂层SEM表面形貌图；
图4为超音速喷嘴结构示意图；
图5为专用夹具结构示意图。
具体实施方式
如图1～5所示，一种半导体装备用抗高温蠕变接地基片的制备方法，包括如下步骤：
(1)接地基片的基体6前处理：以620×64×0.2mm的镍基合金做为基体6，将所述基体6表面先进行纹理处理，纹理处理工艺参数为：320#砂纸抛光，去除基体6表面积碳层；再用无水乙醇对基体6进行清洗；
(2)冷喷涂系统包括喷涂设备、喷涂室4和专用夹具5，所述专用夹具5设置在所述喷涂室4内，将所述基体6放置于冷喷涂系统的专用夹具5上；喷涂设备包括进气管、加热器2、送粉器1和超音速喷嘴3，进气管的一端与高压气源连接，进气管的另一端分别经送粉器1和加热器2与超音速喷嘴3相连接，超音速喷嘴3安装于喷涂室4入口处，所述基体6表面与超音速喷嘴3出口相对；超音速喷嘴3采用中国专利申请(申请号为：01128130.8)中的形状结构及设计原理，超音速喷嘴3由收缩段31、喉部32、扩张段33三部分组成，所述收缩段31为亚音速段，为维托辛基曲线形光滑连续收缩结构，与喉部32过渡连接，所述扩张段33为超音速段轴对称位流式结构，与喉部32过渡连接，它包括初始膨胀段331和消波段332，初始膨胀段331为光滑连续过渡结构，其间为泉流区，消波段332为平行于轴线的轴对称结构，其间为均匀区，所述收缩段31通过过渡管件分别与送粉器1、加热器2相连接；专用夹具包括底座7、侧壁8和上板9，所述侧壁8上设置抽气口11，所述抽气口11接通真空泵；所述上板9设置多个吸气孔10，所述基体6放置于所述吸气孔10的上面，开动真空泵将所述基体6吸附在所述专用夹具5上；
(3)喷涂：采用所述喷涂设备，利用压缩氮气携带铝粉以超音速喷涂于所述基体6表面，压缩氮气分两路，一路进入送粉器1，作为载带气将铝粉引入超音速喷嘴3；另一路连接加热器2使气体膨胀，提高气流速度及加热喷涂粉末，之后两路气流进入超音速喷嘴3，在其中形成气-固双相流，双相流中高动能金属颗粒撞击放置于专用夹具5上的基体6表面后产生塑性变形并沉积于基体6表面形成铝导电层，制得接地基片；喷涂工艺参数如下：喷涂距离35mm、气体压力3MPa、气体温度300℃、气体流量30g/s、铝粉纯度99％，铝粉粉末粒度300目；
(4)喷涂后热处理工艺：将所述接地基片置于热处理炉中随炉升温至100～500℃，在该温度下保温1～5小时；
(5)涂层表面后续处理：用菜瓜布和酒精对接地基片进行湿抛光，使接地基片表面无色差。
如图2所示，接地基片涂层的SEM截面形貌，可以看出涂层厚度均匀，大致约为120μm，涂层致密，无明显的孔洞，并且涂层与基片结合良好。
如图3所示，接地基片涂层的SEM表面形貌，涂层表面均匀致密，大量铝颗粒分布于涂层表面，涂层整体质量较好。
以上是本发明的优选实施例，在不脱离本发明构思的前提下，采用热喷涂技术或其它喷涂技术制备的半导体工艺装备用抗高温蠕变接地基片，也应视为本发明的保护范围。
Claims (6)
1.一种半导体装备用抗高温蠕变接地基片的制备方法，其特征在于，所述制备方法包括如下步骤：
（1）接地基片基体的前处理：将所述接地基片的基体表面先进行纹理处理，纹理处理工艺参数为：320#砂纸抛光，去除基体表面积碳层；再用无水乙醇进行清洗；
（2）冷喷涂系统包括喷涂设备、喷涂室和专用夹具，所述专用夹具设置在所述喷涂室内；所述专用夹具包括底座、侧壁和上板，所述侧壁上设置抽气口，所述抽气口用于接通真空泵；所述上板设置多个吸气孔，所述基体放置于所述吸气孔的上面，真空泵开动时将所述基体吸附在所述专用夹具上；
（3）喷涂：采用冷喷涂工艺制备纯铝涂层，利用所述冷喷涂系统，使压缩气体携带铝粉以超音速喷涂于所述基体表面，形成纯铝涂层，制得接地基片；喷涂工艺参数如下：喷涂距离5~50mm、气体压力0.5~4.5MPa、气体温度150~500℃、气体流量5~50g/s、铝粉纯度90%以上，铝粉粉末粒度200~600目；
（4）喷涂后热处理工艺：将所述接地基片置于热处理炉中随炉升温至100~500℃，在该温度下保温1~5小时；
（5）涂层表面后续处理：用菜瓜布和酒精对接地基片进行湿抛光，使接地基片表面无色差。
2.根据权利要求1所述的半导体装备用抗高温蠕变接地基片的制备方法，其特征在于，所述基体由不锈钢、镍基合金或耐热钢制成。
3.根据权利要求2所述的半导体装备用抗高温蠕变接地基片的制备方法，其特征在于，所述基体厚度为0.1~0.6mm。
4.根据权利要求1所述的半导体装备用抗高温蠕变接地基片的制备方法，其特征在于，所述喷涂设备包括进气管、加热器、送粉器和超音速喷嘴，进气管的一端与高压气源连接，进气管的另一端分别经送粉器和加热器与超音速喷嘴相连接，所述基体表面与超音速喷嘴出口相对。
5.根据权利要求4所述的半导体装备用抗高温蠕变接地基片的制备方法，其特征在于，超音速喷嘴包括进气口、收缩段、喉部、扩张段和出口，超音速喷嘴安装于喷涂室入口处，压缩气体分两路，一路进入送粉器，作为载带气将铝粉粉末引入超音速喷嘴；另一路连接加热器使气体膨胀，提高气流速度及加热铝粉粉末，之后两路气体进入超音速喷嘴，在其中形成气-固双相流，双相流中高动能铝粉颗粒撞击所述基体表面后产生塑性变形并沉积于所述基体表面形成铝导电层。
6.根据权利要求5所述的半导体装备用抗高温蠕变接地基片的制备方法，其特征在于，所述压缩气体为空气、氮气或者氦气。
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| US9839932B2 (en) * | 2013-02-14 | 2017-12-12 | Shimadzu Corporation | Surface chemical treatment apparatus for drawing predetermined pattern by carrying out a chemical treatment |
| CN104928625B (zh) * | 2015-05-22 | 2017-06-16 | 沈阳富创精密设备有限公司 | 一种pvd制备半导体装备用抗高温蠕变接地基片的方法 |
| CN108085674B (zh) * | 2016-11-23 | 2020-01-03 | 中国科学院金属研究所 | 一种发动机汽缸用铝合金材料的制备方法 |
| US11167864B2 (en) * | 2018-04-27 | 2021-11-09 | The Boeing Company | Applying cold spray erosion protection to an airfoil |
| CN109825827A (zh) * | 2019-02-22 | 2019-05-31 | 沈阳富创精密设备有限公司 | 一种ic装备等离子体刻蚀腔防护涂层的制备方法 |
| CN113555287B (zh) * | 2021-07-22 | 2022-05-24 | 吉林建筑大学 | 一种水分触发降解的p型瞬态薄膜晶体管制备方法 |
| CN114799201A (zh) * | 2022-05-05 | 2022-07-29 | 广东省科学院新材料研究所 | 收缩-扩展喷嘴及其制备方法、增材制造设备和方法 |
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| US6277235B1 (en) * | 1998-08-11 | 2001-08-21 | Novellus Systems, Inc. | In situ plasma clean gas injection |
| WO2003014234A1 (en) * | 2001-08-03 | 2003-02-20 | Florida State University Research Foundation, Inc. | Composite polyelectrolyte films for corrosion control |
| US20040101620A1 (en) * | 2002-11-22 | 2004-05-27 | Elmoursi Alaa A. | Method for aluminum metalization of ceramics for power electronics applications |
| US7534301B2 (en) * | 2004-09-21 | 2009-05-19 | Applied Materials, Inc. | RF grounding of cathode in process chamber |
| US20060121187A1 (en) * | 2004-12-03 | 2006-06-08 | Haynes Jeffrey D | Vacuum cold spray process |
| DE102006023483A1 (de) * | 2006-05-18 | 2007-11-22 | Linde Ag | Vorrichtung zum Kaltgasspritzen |
| CN101767080B (zh) * | 2008-12-26 | 2012-10-24 | 中国科学院金属研究所 | 一种金属与塑料粉末混合制备涂层的方法及装置 |
| CN102021586A (zh) * | 2009-09-15 | 2011-04-20 | 鞍钢股份有限公司 | 一种单面镀层钢板生产方法及其单面镀层钢板 |
| CN102059218B (zh) * | 2010-12-14 | 2013-01-30 | 北京科技大学 | 一种聚合物基复合材料表面金属化涂层的制备方法及装置 |
| CN102154639B (zh) * | 2011-03-10 | 2012-11-28 | 上海交通大学 | 基于铝粒子的冷喷涂沉积制备涂层的方法 |
| US10441962B2 (en) * | 2012-10-29 | 2019-10-15 | South Dakota Board Of Regents | Cold spray device and system |
| US9337002B2 (en) * | 2013-03-12 | 2016-05-10 | Lam Research Corporation | Corrosion resistant aluminum coating on plasma chamber components |
| KR102126275B1 (ko) * | 2013-05-03 | 2020-06-25 | 삼성디스플레이 주식회사 | 기판정렬장치 및 이를 이용한 기판절단장치 |
| US9663870B2 (en) * | 2013-11-13 | 2017-05-30 | Applied Materials, Inc. | High purity metallic top coat for semiconductor manufacturing components |
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