CN101380636B - 用于阳极化腔室部件的湿法清洁工艺 - Google Patents
用于阳极化腔室部件的湿法清洁工艺 Download PDFInfo
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Abstract
本文公开了一种用于恢复阳极化铝质部件的清洁工艺，该工艺对于已经暴露至蚀刻反应器中的含氟等离子体下的部件特别有用。将部件浸泡于氟化物酸(例如，氟化铵)的搅拌溶液中，氟化物酸可将氟化铝转换成可溶解的氟化物(86)。以水清洗部件(88)。将部件浸置于搅动的热去离子水中，可使经清洁的阳极处理物的孔被重新密封(90)。
Description
技术领域
本发明一般涉及等离子体处理装置。具体地说，本发明涉及用于等离子体蚀刻反应器中的腔室部件的清洁。
背景技术
等离子体反应器用于许多制造半导体集成电路的步骤中，包括等离子体辅助化学气相沉积(PECVD)、磁控溅镀(magnetron sputtering)或更一般的物理气相沉积(PVD)、蚀刻与清洁以及其他用于调整或处理晶圆上即将形成的电路的一层或多层的一般等离子体处理。近代等离子体处理装置趋向非常昂贵，因为其需要在相当窄的处理窗口内执行，并需要能够以极短的停工期来进行维修与保养。因此，人们需要加宽处理窗口并缩短停工期且不会明显地提高成本。
等离子体反应器操作中的一个问题是材料倾向除了沉积在即将处理的晶圆上之外还沉积在腔室部件上。沉积可不仅发生于沉积室(例如，用于PECVD与PVD)中，并也可发生于等离子体蚀刻与清洁反应器中，其中蚀刻处理自晶圆移除材料但沉积蚀刻残余物于腔室壁与其他腔室部件上。等离子体蚀刻反应器的一个实例为可得自Applied Materials，Inc.(Santa Clara，California)的DPS蚀刻反应器10，其概要示于图1的横截面图中。其包括界定处理室16与泵浦室18的腔室主体12与腔室盖14，泵浦室18内含有阴极20，阴极20上有静电吸盘22或其他晶圆固定装置以支撑即将蚀刻的晶圆24。边缘环25在处理过程中围绕晶圆24。
经晶圆端口26将晶圆24插入处理室16，晶圆端口26被狭缝阀门28(slit valve door，还示于图2的正交视图中)选择性地关闭，好让真空泵浦30抽吸泵浦室18与处理室16至通常在中等毫托(milliTorr)范围内的压强。计量自气体供应器33进入气体管线32并经过盖14底部的气体喷嘴34注入处理室的处理气体。加热器36选择性加热盖14并因此加热晶圆24。盖14背部上的RF线圈38诱导耦合RF功率进入处理室16以激发处理气体成为等离子体来蚀刻晶圆24。可通过电容性耦合电路对阴极20进行RF偏压以帮助蚀刻处理，特别是帮助形成高深宽比(aspect-ratio)的孔洞。筛子40(还示于图3的正交视图中)分隔处理室16与泵浦室18同时允许气体流动于其间。电性接地以将等离子体限制于处理室16。
蚀刻处理倾向产生蚀刻残余物，其沉积于处理室16与泵浦室18的侧壁四周，因此需要周期性的清洁。另外，人们希望腔室主体12由便宜的金属(如，铝)所制成，而由较抗蚀刻且昂贵的材料来内衬(line)处理室16与泵浦室18。因此，下衬里(liner)42(还示于图4的正交视图中)内衬泵浦室18而上衬里44(还示于图5的正交视图中)内衬处理室16的侧面并界定泵浦室18顶部的部分。同样地，阴极衬里46(还示于图6的正交视图中)内衬阴极46的横向侧面。
长期应用之后，可能会产生氟化物残余物的表面涂层，可从反应器10移除衬里42、44、46以及狭缝阀门28与筛子40，并由新的部件取代。可有利地清洁使用过的部件并再次使用。
腔室的衬里与其他可移除部件一般由铝构成。具体地说，金属蚀刻反应器中，铝本身某种程度受到与晶圆的金属部件所暴露的相同蚀刻化学作用。即便在硅与电介质蚀刻室中，蚀刻硅或介电层的化学作用也倾向蚀刻铝质腔室部件。因此，传统上在许多等离子体蚀刻反应器中对铝质腔室主体与腔室部件进行阳极化以产生阳极化铝的表面层(通常成分为Al2O3)，其通常实质上不与金属蚀刻等离子体反应。通常系利用热H2SO4电解液执行第III型硬式阳极化处理(hard anodization)以产生厚、硬、黑的表面层。如图7的横截面图所示，阳极化处理工艺氧化作为基材的下方铝质部件60。可以理解铝可包含高达约10wt％非故意的杂质或故意的合金成分(例如，硅)。阳极化处理首先产生阳极化铝的相当一致且密集的薄界面层62。然而，进一步的阳极化处理产生阳极化铝较厚的圆柱区域64，其中圆柱66围绕孔68形成。电解液可填满孔68以有效地成长厚的阳极化层。孔68可让圆柱66自铝源材料向上成长相当远。
阳极化铝的固体部分62、64提供下方铝质部件60相当结实的保护层。然而，孔68提供蚀刻等离子体通道以便相当接近铝质部件60。因此，标准工艺是以密封层70(示于图8的横截面图中)密封孔68，密封层70可避免蚀刻等离子体进入孔68。传统密封层70系由水软铝石(boehmite)所构成，其为γ-AlO(OH)，氢氧化铝。可通过将阳极化表面浸于热的去离子水(DI)中而形成水软铝石密封层70。
基于氟的等离子体蚀刻对于阳极化铝腔室部件有特定的问题。蚀刻金属的典型处理气体包括氟碳化合物CxFy，虽然可加入其他气体与其他基于氟的蚀刻气体(包括NF3、SF6与其他氟化物)。介电蚀刻处理同样地应用氟碳化合物气体的等离子体。氟在铝质部件(甚至阳极化部件)存在下可能会产生氟化铝(AlFx)与氧氟化铝(AlOF)，其不易挥发并沉积于阳极化部件上且开始增厚。虽然微粒是潜在的问题，但更急迫的问题是增厚的氟化铝或氧氟化铝膜倾向于改变腔室的化学作用并造成蚀刻处理偏移。不像大部分的其他氟化物或卤化物，氟化铝是不易挥发且不溶于水与许多溶剂的硬质材料。并尚未无发现可在原位等离子体干法清洁过程中移除氟化铝的等离子体清洁工艺。进一步的问题是氟化铝易于被玻璃二氧化硅(SiO2)薄层所覆盖，玻璃二氧化硅是由石英腔室部件或者蚀刻硅或氧化硅层的反应副产物所形成。
传统清洁工艺已经应用剧烈的研磨擦洗(scrubbing)来移除AlF与二氧化硅层。然而，剧烈的擦洗易于伤害阳极涂层。有时应用稀释的草酸(C2H2O4)作为湿法清洁溶液。然而，草酸无法有效地移除来自晶圆处理的副产物与残余物。再者，酸性溶液易于降解阳极化层与密封层。
可简单地以新的且新近阳极化的部件替换腔室部件。然而，部件趋向昂贵而铝质真空室本身也需要偶尔的清洁。
发明内容
提供了从阳极化的铝质表面或其他金属氧化物表面移除氟化物残余物的清洁方法。将表面暴露于可溶解氟化物的溶剂(例如，氟化物酸)中，氟化物酸例如氟化铵。优选地，溶剂将氟化物残余物溶解于水中。此方法对于清洁曾暴露于等离子体蚀刻反应器中的氟等离子体的阳极化铝质部件来说，特别有用。
在施加湿法溶剂之前，可先进行表面的湿法研磨擦洗(优选地利用非金属研磨料)。研磨擦洗可移除倾向形成的硬二氧化硅表面层。
清洁之后，可通过将部件浸于热水浴槽中而重新密封阳极处理物，热水浴槽可以以水软铝石(boehmite)密封阳极处理物的孔。
附图说明
图1是应用本发明的等离子体蚀刻反应器的概要横截面图。
图2是图1的反应器的狭缝阀门的正交视图。
图3是图1的反应器的筛子的正交视图。
图4与图5是图1的反应器的下衬里与上衬里的正交视图。
图6是图1的反应器的阴极衬里的正交视图。
图7是阳极化铝质表面的横截面图。
图8是经密封的阳极化铝质表面的横截面图。
图9是描述实施本发明的方法的一实施例的流程图。
附图标号说明
10 等离子体蚀刻反应器
12 腔室主体
14 腔室盖
16 处理室
18 泵浦室
20 阴极
22 静电吸盘
24 晶圆
26 晶圆端口
28 狭缝阀门
30 真空泵浦
32 气体管线
33 气体供应器
34 气体喷嘴
36 加热器
38 RF线圈
40 筛子
42 下衬里
44 上衬里
46 阴极衬里
60 铝质部件
62 密集氧化铝界面层
64 氧化铝圆柱区域
66 圆柱
68 孔
70 密封层
具体实施方式
本发明提供轻柔但却有效的阳极化腔室部件湿法清洁方法，以移除氟化铝与氧氟化铝沉积物。再者，本发明可包括重新密封经清洁的阳极化部件。
为了清洁，需要自腔室卸下部件。专门的部件需要特殊的前处理。例如，某些腔室衬里可能包括冷却通道。需要排空、注满、清洗并接着可能堵筛这些通道以将其与随后的湿法清洁分隔。可用在去离子(DI)水中实施前清洗步骤来清洁外来的微粒。
清洁各个部件的工艺概述于图9的流程图中。步骤80中，通过轻柔湿法擦洗手工清洁移除沉积物。当蚀刻室包含石英部件时，擦洗可有效地移除倾向于形成的玻璃二氧化硅涂层。用于悬浮二氧化硅微粒的湿法介质可为DI水。研磨料可为来自3M Corporation(St.Paul，Minnesota)的灰色Scotch-BriteTM研磨垫或海棉。灰色Scotch-Brite研磨料为包含超细碳化硅微粒的超细编织硬塑胶研磨料。步骤82中，清洗(例如，在DI水中)经擦洗的部件并吹干(例如，以氮或干净的干燥空气)。
步骤84中，遮蔽部件以保护不需清洁的区域，例如未阳极化表面或未经历外来沉积物的表面。
步骤86中，对部件进行溶解氟化物的湿法处理。优选的溶剂是ACTNE-14，其为可得自Ashland Speciality Chemical Company(Dublin，Ohio)的缓冲氟化物酸。商业上可取得的NE-14可不经稀释便加以使用但也可选地稀释它。一般认为NE-14的主要活性成分是水溶液中的氟化铵(NH4F)。氟化铵也可描述成氟化盐类或含铵的碱类。以醋酸铵达成缓冲。残余物AlCl3、AlF3与Al(OH)3不溶于水中，但氟化铵将其转化成非常易溶于水的NH4AlF4。不像HF，氟化铵没有强到足以还原Al2O3或以其他方式降解铝质阳极处理物，且会改造氟化物成为不期望的AlFx。同样地，NE-14无法有效地蚀刻或攻击陶瓷氧化物(诸如，氧化铝(Al2O3)与氧化钇(Y2O3))或其他离子键结合的金属氧化物(例如，氧化锆)。
为了转化氟化铝，在室温或高于室温下将部件浸于NE-14的持续搅拌槽中较长的时间(例如，大于10分钟)。实例包括在20℃下的1小时浸泡。溶剂浸泡的效果是从阳极化表面移除所有的氟并将其溶解于溶剂中。
步骤88中，接着自阳极化部件移除含氟溶剂。例如，以DI水喷洒清洗部件并接着浸入DI水清洗的超声波槽中。接着以经过滤的氮气或干净的干燥空气完全吹干。优选地重复步骤86、88，且优选地重复1次。
已经移除氟化物之后，步骤90中，可选地执行阳极化处理后调整以重新密封孔。该调整可与在铝质部件最初的阳极化处理后执行的调整相同，尽管在示出的序列中没有阳极化处理步骤。调整或重新密封步骤的实例为优选在95°与115℃之间的温度下在热DI水中持续搅动热密封数个小时。一个方案包括四小时浸置于搅动的沸腾(100℃)DI水中。然而，可应用其他重新密封条件，而较高的温度可减少处理时间但有可能使脆弱的阳极处理物断裂。
步骤92中，可进行两项测量以检验处理的有效性。一种类型的试验利用离子色谱仪来测量部件表面上的氟阴离子浓度。预期具有最高污染的部件(经清洁的衬里)测量出0.92至3.2×1014cm-2的氟阴离子(F-)浓度。其他腔室部件(诸如，门与阴极)测量出程度稍微较低的0.9至1.3×1014cm-2。为了进行比较，在清洁之前执行相似的试验并显示某些衬里表面上氟阴离子浓度为45至110×1014cm-2。也就是说，清洁减少氟阴离子浓度约50倍或更多倍。为了进一步比较，新的阳极化部件测量出0.62×1014cm-2的氟阴离子浓度。也就是说，经清洁的部件的氟污染没有超出未用于氟式等离子体处理的部件的大约两倍。
第二型试验测量重新密封阳极处理物的孔的有效性。在湿法工艺中测量密封值，湿法工艺将阳极化表面暴露于电解液中并在电解液与铝质基材间测量电导纳(阻抗的倒数)。若孔被不良地密封，电解液渗入孔中并提高导纳(admittance)，因此高导纳或密封值代表密封不良的阳极处理物。清洁与重新密封后测量的密封值不超过约8000。相反地，清洁与重新密封之前，阴极上的密封值约24,000而内衬上的密封值不超过约18,000。也就是说，清洁与重新密封不仅没有降解反而明显地提高使用后的密封。若部件无法通过这两个试验任一的最低阀值，将重复清洁处理或者摒弃部件并用新的部件替换。
处理进展过程中，在各个清洁循环中执行试验。一但处理进入长期生产，将减少一个或多个试验的频率至例如仅为时间的20％，以确保令人满意地执行清洁处理。
在部件重新进入生产之前，其在步骤94中进行温暖的超声波清洗，例如在38至46℃范围中固定于DI水中30分钟。较宽的温度范围包括任何高于35℃的温度。该步骤有效地自阳极化部件上移除任何盐类(例如，氟化物化合物)。接着吹干该部件。
最后，步骤96中，对清洁过的部件进行干烤，例如在优选介于90°与115℃间的高温下(例如，100℃)固定于烤箱中至少约3小时，虽然烘烤温度有可能低至80℃。在烘烤过程中用经过滤的氮气或干净的干燥空气清洁烤箱。烘烤移除任何湿法残余物，例如在不完全密封的孔中的残余物。较高的烤箱温度可允许较短的烘烤时间。
可以将本发明方法应用更较大、更复杂的部件，例如为节省成本以阳极化铝制造的腔室主体。
虽然本发明不须重新阳极化便可自阳极化铝质部件移除氟化物残余物，其也可应用至其他材料的清洁表面，例如由耐火金属氧化物(诸如，氧化铝、氧化钇、氧化锆与其他离子键结合的金属氧化物)所构成的陶瓷。特别在陶瓷实例中，在清洁之后通常不需要重新密封表面。另一方面，本发明恢复的部件无法直接用于被视为共价键结合的氧化物的干净石英(SiO2)。已知NE-14会攻击石英与含碳聚合式光刻胶两者。
因此，本发明提供刷新暴露至等离子体的腔室部件的经济方法，该等离子体倾向在部件上形成不溶的残余物，例如利用含氟蚀刻气体的等离子体蚀刻所得的结果。
Claims (13)
1.一种用于清洁阳极化铝质构件的方法，其至少包括下列步骤：
用非金属研磨料湿法擦洗该铝质构件的阳极化表面；及
接着暴露该阳极化表面于一包括氟化铵作为主要活性成分的液体溶剂，该液体溶剂能溶解氟化物但在该铝质构件上留下至少部分的暴露于所述液体溶剂的阳极化表面。
2.如权利要求1所述的方法，其中所述溶剂包括氟化铵水溶液。
3.如权利要求1或2所述的方法，其中所述阳极化表面在湿法擦洗步骤之前是被密封的，并且所述方法还包括在所述暴露步骤之后的密封该阳极化表面的多个孔的步骤。
4.如权利要求3所述的方法，其中所述构件在所述暴露步骤与所述暴露步骤之后的密封步骤之间未被重新阳极化。
5.如权利要求3所述的方法，其中所述密封步骤包括将所述阳极化表面浸泡于高于95℃的温度的水中。
6.如权利要求5所述的方法，其中所述浸泡步骤持续数个小时。
7.如权利要求3所述的方法，还包括随后在高于35℃的温度下于水中超声波清洗所述阳极化表面的步骤。
8.如权利要求7所述的方法，还包括随后在至少80℃的温度下于干燥环境中烘烤所述构件的步骤。
9.一种清洁铝质构件的经阳极化和密封的表面的方法，其至少包括下列步骤：
利用包括氟化铵的的液体溶剂自该经阳极化和密封的表面移除氟化物；及
在该移除步骤后未进一步阳极化该铝质构件，就密封该经阳极化和密封的表面的多个孔。
10.如权利要求9所述的方法，其中所述密封步骤包括将所述经阳极化和密封的表面浸泡于至少95℃的温度的水中。
11.如权利要求10所述的方法，其中所述浸泡步骤持续数个小时。
12.如权利要求9所述的方法，其中所述密封步骤在所述经阳极化和密封的表面上产生一包括水软铝石的层。
13.如权利要求9至12任何一项所述的方法，还包括用非金属研磨料湿法擦洗所述经阳极化和密封的表面的先前步骤。
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| CN107706089B (zh) * | 2017-09-19 | 2020-08-11 | 上海华虹宏力半导体制造有限公司 | 铝线干法刻蚀后湿法清洗方法 |
| JP7218201B2 (ja) * | 2019-02-13 | 2023-02-06 | アルバックテクノ株式会社 | アルミニウム製部品の酸化皮膜の再生方法 |
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| CN114395784A (zh) * | 2021-11-19 | 2022-04-26 | 昆明理工大学 | 一种双通大面积三氧化二铝、二氧化钛或二氧化锆纳米管阵列膜及其制备方法 |
| CN115799172B (zh) * | 2023-02-08 | 2023-04-28 | 粤芯半导体技术股份有限公司 | 金属互连线及其制造方法 |
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- 2008-08-21 JP JP2008212533A patent/JP5324160B2/ja not_active Expired - Fee Related
- 2008-08-26 KR KR1020080083318A patent/KR101037530B1/ko not_active IP Right Cessation
- 2008-08-27 CN CN2008102105375A patent/CN101380636B/zh not_active Expired - Fee Related
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Also Published As
| Publication number | Publication date |
|---|---|
| CN101380636A (zh) | 2009-03-11 |
| US20090056745A1 (en) | 2009-03-05 |
| TW200912044A (en) | 2009-03-16 |
| JP2009052142A (ja) | 2009-03-12 |
| KR101037530B1 (ko) | 2011-05-26 |
| EP2031088A3 (en) | 2011-05-18 |
| US8231736B2 (en) | 2012-07-31 |
| EP2031088A2 (en) | 2009-03-04 |
| JP5324160B2 (ja) | 2013-10-23 |
| KR20090023167A (ko) | 2009-03-04 |
| TWI397612B (zh) | 2013-06-01 |
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