CN108779568B - 在半导体处理设备上以电化学方式形成氧化钇的方法 - Google Patents
在半导体处理设备上以电化学方式形成氧化钇的方法 Download PDFInfo
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- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 title abstract description 6
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Abstract
此公开内容一般地涉及以电化学方式形成三氧化二钇或氧化钇的方法。所述方法可包括视情况地制备电化学浴、将钇电沉积至基板上、从基板的表面上去除溶剂,及后处理其上具有经电沉积的钇的基板。
Description
背景
技术领域
此公开内容的实施方式一般地涉及在机械部件(mechanical component)上形成保护层,且尤其是,涉及在半导体处理设备上以电化学方式形成诸如氧化钇(yttriumoxide)之类的涂层。
背景技术
半导体处理设备表面上通常包括某些涂层,以提供免遭腐蚀性处理环境影响的一定程度的保护,或者增进对设备的表面保护。用于涂覆保护层的几种常规方法包括物理气相沉积(PVD)、化学气相沉积(CVD)、等离子体喷涂、气溶胶沉积和类似方法。然而,这些常规方法不能令人满意地涂覆半导体设备,特别是在具有小孔或气室(plenum)的区域中,例如喷淋头。
图3A及3B分别图示使用诸如热喷涂或电子束沉积的常规方法涂覆的喷淋头320及面板325的局部截面图。如图3A所示,喷淋头320由铝制成并包括形成于其中的多个气室321(图中绘示两个)。气室321可视情况地包括位在其一个端部处的倾斜边缘322。使用常规的涂覆技术,由于常规涂覆技术的限制,倾斜边缘322没有涂覆保护涂层323。举例而言,由于常规技术的定向沉积本质所致,常规技术不能适当涂覆靠近气室的基板。因此常规技术会使倾斜边缘322暴露,从而在等离子体存在的情况下经由未涂覆的表面与等离子体的反应而造成污染。暴露于等离子体的未受保护表面容易降解,从而将不期望的颗粒物质引入处理区域,因此而降低了装置质量。
图3B图示面板325,面板325包括气室326,气室326上沉积有保护涂层327。类似于上文所述的喷淋头320,常规技术不能适当涂覆面板325,特别是气室326。尽管面板325的上表面,其通常接近保护涂层327沉积期间的沉积源,可能受到涂覆,但气室326的内表面仍未被涂覆。未涂覆的表面有利于在处理腔室内因与处理等离子体的不期望相互作用而导致的污染。
因此,需要改进用于保护涂层的沉积方法。
发明内容
在一个实施方式中,一种在基板上沉积材料的方法包含:将铝基板安置于电镀浴中,所述电镀浴包含非水性溶剂及沉积前驱物;将涂层沉积于铝基板上,所述涂层包含钇;从铝基板去除过量的镀覆溶液;和后处理其上具有所述涂层的铝基板。
在另一个实施方式中,一种在基板上沉积材料的方法包含:将铝基板安置于电镀浴中,所述铝基板具有一或多个气室(plenum)形成于该铝基板中,所述电镀浴包含非水性溶剂及沉积前驱物,所述沉积前驱物包含YCl3或Y(NO3)3;将涂层沉积在铝基板上,所述涂层包含钇;从铝基板去除过量的镀覆溶液,其中去除的步骤包含清洗铝基板并以压缩干空气干燥铝基板;和后处理其上具有所述涂层的铝基板。
在另一个实施方式中,一种在基板上沉积材料的方法包含:将铝基板安置于电镀浴中,所述铝基板具有一或多个气室(plenum)形成于该铝基板中,所述电镀浴包含非水性溶剂及沉积前驱物;将涂层沉积于铝基板上,所述涂层包含钇;从铝基板去除过量的镀覆溶液;和后处理其上具有所述涂层的铝基板。
附图说明
以上简要概述的本公开内容的上述详述特征可以被详细理解的方式,以及本公开内容的更特定描述可以通过参照实施方式来获得,一些实施方式绘示于附图中。然而,应注意,附图仅绘示示例性实施方式,因而不应视为对本公开内容的范围的限制,因为本公开内容可允许其他等同有效的实施方式。
图1图解根据本公开内容的一个实施方式的用于在基板上电沉积钇的方法的流程图。
图2图示根据本公开内容的一个实施方式的电化学浴。
图3A及3B分别图示使用常规方法涂覆的喷淋头及面板的局部截面图。
图4A及4B分别图示使用本文所述的方法涂覆的喷淋头及面板的局部截面图。
为了有助于理解,已尽可能地使用相同的附图标号来标示附图中共通的相同元件。考虑到,一个实施方式的元件和特征在没有进一步描述下可以有益地并入到其他实施方式中。
具体实施方式
此公开内容一般地涉及以电化学方式形成三氧化二钇的方法。所述方法可包括视情况地制备电化学浴、将钇电沉积至基板上、从基板的表面上去除溶剂,及后处理其上具有经电沉积的钇的基板。
图1图解根据本公开内容的一个实施方式的用于在基板上电沉积钇的方法100的流程图。图2图示根据本公开内容的一个实施方式的电化学浴。将结合解释图1及2,以有助于对本公开内容的各方面的说明。
方法100开始于操作101。在操作101中,制备电化学浴210。电化学浴210包括容器211,容器211具有设置于其中的溶液212。溶液212可包括一或多种溶剂、电解质或其它沉积前驱物,及镀覆添加剂。该溶液可具导电性以有助于电化学沉积。阳极213和充当阴极的基板214被安置在溶液212中,且可被分隔件215隔开,分隔件例如是多孔板件。多孔板件可以是其中具有多个开口的聚丙烯(polypropylene)或聚四氟乙烯。所述开口可具有约0.025英寸的直径,并且具有每平方厘米5个或更少的开口的密度。阳极213和基板214耦接至电源216,例如DC电源,以有助于将材料镀覆至基板214上。可在恒定电流或电压或脉冲式电流或电压下供应功率。在一个实例中,基板214为半导体处理设备。半导体处理设备的实例可包括由铝或铝合金制成的部件,例如喷淋头或气体分配器,或可具有多个气体通道形成于其中的其它设备。铝合金的实例包括Al6061和Al6063,还有其它合金。可以预期没有气体通道形成于其中的那些基板亦可以经受镀覆。在一个实例中,阳极213亦可由铝制成,例如由Al6061铝合金制成。
溶液212可包括一或多种水性溶剂,诸如水;或者非水性溶剂,诸如无水乙腈(dryacetonitrile)、乙醇、甲苯或异丙醇。可将诸如YCl3、Y(NO3)3、醋酸钇的一或多种镀覆前驱物、或诸如Y-(CxHy)x的有机金属前驱物溶解于溶液212中。所述一或多种镀覆前驱物可被溶解在溶液中达约0.001体积摩尔浓度(M)至约2M,例如约0.1M至约1M,例如约0.5M至约1M的浓度。一或多种添加剂,诸如,硝酸钾(KNO3)、氟化钠、醋酸钠及四丁胺六氟磷(tetrabutylammonium hexaflurophosphate),可被加入溶液212中以改善镀覆材料的特性。举例而言,可选择添加剂来改善沉积涂层的平整度、调整沉积涂层的成分,或减少镀覆涂层的粗糙度或裂纹。亦可选择添加剂来改善溶液212的导电性,从而增加镀覆材料的沉积速率并提高沉积均匀性。一或多种添加剂可以0.001体积摩尔浓度(M)至约1M,如约0.1M至约0.5M,例如约0.1M至约0.3M的浓度存在于溶液212中。可在制备溶液212后将基板214安置于溶液212中。
在操作102中,可将诸如钇的材料电沉积于基板214上。可由电源216负偏压阳极213,同时由电源216正偏压基板214。阳极213及基板214的偏压有助于将诸如钇的期望材料从溶液212镀覆至基板214上。可以用在约1伏特至约300伏特的范围内的电压,例如在约1伏特至约50伏特、或约1伏特至约10伏特的范围内的电压,来偏压阳极213和基板214。可以用在约-0.1毫安培至约-2安培的范围内的电流,例如在约-0.1毫安培至约-50毫安培、或约-0.1毫安培至约-10毫安培的范围内的电流,来偏压阳极213和基板214。于操作102期间,可将溶液212维持在约0摄氏度至约100摄氏度的范围内的温度下。在一个实例中,可将溶液维持在约10摄氏度至约50摄氏度的温度下,例如是约25摄氏度。可施加操作102的偏电压达约3小时或更少的时间段,例如约5分钟至约60分钟,例如约10分钟至约30分钟。
额外地或可替代地,可考虑使用脉冲沉积技术,其中电位或电流在两个不同值之间迅速改变。此快速交替可产生由零电流分开的一连串具有相等振幅、持续时间和极性的脉冲。各脉冲由ON时间(TON)和OFF时间(TOFF)构成。在TOFF期间,离子迁移到浴中的耗尽区域(depleted area)。在TON期间,更均匀分布的离子能够被沉积至基板214上。在一个实例中,TON可为约0.001秒至60秒,且TOFF时间可为约0.001秒至60秒。
可考虑改变操作101及102的特性,以达成期望的镀覆材料厚度或成分。举例而言,为了增加镀覆材料的沉积速率或厚度,可考虑增加镀覆前驱物的浓度、偏电压的持续时间,或偏电压的大小。在一个实例中,可将诸如钇等镀覆材料沉积至约3纳米至约8微米的厚度,例如约10纳米至约500纳米,例如约200至约400纳米。在另一个实施方式中,可将镀覆材料沉积至约1微米至约50微米的厚度。在另一个实例中,可考虑在惰性环境中进行操作102,例如在氩或双原子氮的环境中。在另一个实施方式中,可考虑在操作102期间搅拌溶液212。
接着,在操作103中,可从溶液212移出基板214,并从基板214的表面去除过量的溶液212。可去除过量的溶液212,例如经由蒸发或干燥来去除。干燥器、热源(heat source)、光源或风扇中的一或多个装置可以有助于从基板214去除过量的溶液212。额外地或可替代地,在操作103期间,可用乙醇或异丙醇清洁基板214,并接着用压缩干空气清洁基板214。
在一个镀覆实例中,钇在基板214上的电化学沉积进行如下:
阴极:
Y3++2H++3e-=Y+H2
阳极:
4OH-→2O-+2H2O+4e-
在操作104中,在过量的溶液212蒸发之后,可对基板214进行后处理工艺。在一个实例中,操作104的后处理工艺为退火工艺。在这样的实例中,可在约400摄氏度或更高的温度下退火基板214。可选择退火温度以有助于在后处理工艺期间,从基板214的表面移除羟基部分(hydroxyl moieties)。在另一个实施方式中,后处理工艺可为氧化工艺。在这样的实例中,可使基板214暴露于含氧环境,以有助于基板214上镀覆材料的氧化。举例而言,可使基板暴露于氧、臭氧或经离子化的氧或含氧气体。可通过使用等离子体或热处理来促进镀覆材料的氧化。操作104的退火工艺亦可增加镀覆材料对下方基板214的附着度。可考虑到,不同的氧化技术以及不同的氧化源可能影响膜的质量,包括密度、粗糙度及氧含量。
在另一个实例中,后处理工艺可为第二浴。在第二浴中,可使用约10伏特至约200伏特的中性电解质来阳极氧化基板214,以在镀覆涂层的外表面上形成氧化物层。在另一个实施方式中,后处理工艺可包括使基板暴露于硝酸以氧化已沉积涂层的上表面。硝酸浴可以包括约20%至约69%的硝酸,且可处在约0摄氏度至约25摄氏度的温度下。考虑到,与在室温或更高的温度下发生的类似硝酸阳极化工艺相比,低于室温的温度增加阳极化层的密度。在一个实例中,镀覆涂层的经氧化部分可具有约200纳米或更小的厚度,例如约100纳米或更小,例如约5纳米或更小。在一个实例中,可使约5百分比的镀覆铝层被阳极化。
在一个实例中,根据方法100将涂层沉积在铝基板上。在此实例中,将铝基板安置于电镀浴中,该电镀浴使用乙醇作为溶剂并具有沉积前驱物溶解于其中达0.1M的浓度。将所述浴维持在10摄氏度的温度下,并施加10伏特的偏压持续30分钟。接着使膜暴露于氧化工艺。所述氧化膜具有在约14原子百分比至约47原子百分比的范围内的钇的成分;在约2原子百分比至约3原子百分比的范围内的铝的成分;及在约50原子百分比至约83原子百分比的范围内的氧的浓度。
在另一个实例中,可将铝基板安置在电镀浴中,该电镀浴使用乙醇作为溶剂并具有沉积前驱物溶解于其中达0.1M的浓度。将所述浴维持在10摄氏度的温度下,并施加50伏特的偏压持续30分钟。接着使膜暴露于氧化工艺。所述氧化膜具有在约12原子百分比至约43原子百分比的范围内的钇的成分;在约9原子百分比至约10原子百分比的范围内的铝的成分;及在约35原子百分比至约55原子百分比的范围内的氧的浓度。
图4A及4B分别图示使用本文所述的方法涂布的喷淋头420及面板425的局部截面图。本文所述的电镀方法产生对机械部件的改良镀覆,特别是那些包括孔(orifice)、孔洞(hole)、气室和类似部件。参见图4A,喷淋头420包括与常规方式(如图3A所示)相比已改善的气室421的斜面422的涂层覆盖度(coverage)。类似地,与常规方式(如图3B所示)相比,面板425包括由涂层427改良的覆盖度,例如在靠近孔口和在孔口中。使用本文所述的方法,电镀可导致在浸没于镀覆浴中的所有表面上的完整且均匀地沉积相应涂层423、427。喷淋头420的浸没部分由线430标示。然而,应了解到,可将整个喷淋头420浸没在镀覆浴中。在这样的实施方式中,可遮蔽不希望被沉积的区域,以防止镀覆。
尽管本文所描述的实施方式涉及钇的沉积,亦可考虑镀覆其它材料。举例而言,可预期镀覆稀土金属盐、铯、镧,及其氧化物。可考虑镀覆一或多种材料的交替层,诸如钇及铯的交替层。
本公开内容的优点包括材料在部件上更完整的沉积,还有无裂纹、均匀而致密的氧化物涂层。与常规的沉积技术相反,本文公开的电镀方法导致在孔口、气室或基板的其它小特征附近改良的镀覆。更为完全的覆盖导致对部件的保护增加,特别是在半导体材料的处理中常用的等离子体环境中。
此外,在此形成的阳极氧化层比传统的阳极氧化层更致密(例如,更少孔洞),因此提供较佳的耐腐蚀性,特别是对等离子体。在某些实例中,此公开内容的阳极化层在气泡试验(bubble test)中经受5%的HCl的浴。该阳极化层显示出对HCl气泡试验的抗性达约20至47小时。相比之下,传统的阳极化层显示出对HCl气泡试验的抗性达约5小时。
尽管前述针对本公开内容的实施方式,但是在不背离本公开内容的基本范畴的情况下可设计本公开内容的其它和进一步的实施方式,且本公开内容的范围由随附的权利要求书来确定。
Claims (20)
1.一种在基板上沉积材料的方法,包含以下步骤:
将铝基板安置于电镀浴中,所述电镀浴包含非水性溶剂及沉积前驱物;
将涂层沉积于所述铝基板上,所述涂层包含钇;
从所述铝基板去除过量的镀覆溶液;和
后处理其上具有所述涂层的所述铝基板以阳极氧化所述涂层,其中所述后处理包含在0℃至25℃的温度下将所述铝基板暴露于具有20%至69%硝酸的硝酸浴。
2.如权利要求1所述的方法,其中所述铝基板包含Al6061或Al6063合金。
3.如权利要求1所述的方法,其中所述沉积前驱物包含YCl3、Y(NO3)3、醋酸钇或Y(CxHy)z。
4.如权利要求3所述的方法,其中所述沉积前驱物具有在0.001M至2M的范围内的浓度。
5.如权利要求3所述的方法,其中所述沉积前驱物具有在0.1M至1M的范围内的浓度。
6.如权利要求3所述的方法,其中所述沉积前驱物具有在0.5M至1M的范围内的浓度。
7.如权利要求1所述的方法,其中所述电镀浴包含添加剂,所述添加剂包含硝酸钾、氟化钠或醋酸钠中的至少一种。
8.如权利要求1所述的方法,其中所述涂层具有3纳米至8微米的厚度。
9.如权利要求8所述的方法,其中所述涂层具有200纳米至400纳米的厚度。
10.如权利要求1所述的方法,其中所述后处理进一步包含:将所述涂层暴露于氧化剂,以氧化所述涂层。
11.如权利要求1所述的方法,其中,在所述后处理之后,所述涂层包含在14原子百分比至47原子百分比范围内的钇的成分、在2原子百分比至3原子百分比范围内的铝的成分及在50原子百分比至83原子百分比范围内的氧的浓度。
12.如权利要求1所述的方法,其中,在所述后处理之后,所述涂层包含在12原子百分比至43原子百分比范围内的钇的成分、在9原子百分比至10原子百分比范围内的铝的成分及在35原子百分比至55原子百分比范围内的氧的浓度。
13.如权利要求1所述的方法,其中所述后处理进一步包含:热处理所述涂层。
14.如权利要求1所述的方法,其中沉积所述涂层包含:施加1伏特至300伏特的范围内的偏电压。
15.一种在基板上沉积材料的方法,包含以下步骤:
将铝基板安置于电镀浴中,所述铝基板具有一或多个气室形成于所述铝基板中,所述电镀浴包含非水性溶剂及沉积前驱物,所述沉积前驱物包含YCl3、Y(NO3)3、醋酸钇或Y(CxHy)z;
将涂层沉积于所述铝基板上,所述涂层包含钇;
从所述铝基板去除过量的镀覆溶液,其中所述去除包含:清洗所述铝基板并使用压缩干空气干燥所述铝基板;和
通过如下步骤后处理其上具有所述涂层的所述铝基板以阳极氧化所述涂层:在0℃至25℃的温度下将所述铝基板暴露于具有20%至69%硝酸的硝酸浴。
16.如权利要求15所述的方法,其中,在所述后处理之后,所述涂层包含在14原子百分比至47原子百分比范围内的钇的成分、在2原子百分比至3原子百分比范围内的铝的成分及在50原子百分比至83原子百分比范围内的氧的浓度,并且其中所述后处理包含:氧化所述涂层。
17.如权利要求15所述的方法,其中所述铝基板包含Al6061或Al6063合金。
18.如权利要求15所述的方法,其中沉积所述涂层包含:施加1伏特至300伏特的范围内的偏电压。
19.一种在基板上沉积材料的方法,包含以下步骤:
将铝基板安置于电镀浴中,所述铝基板具有一或多个气室形成于所述铝基板中,所述电镀浴包含非水性溶剂及沉积前驱物;
将涂层沉积于所述铝基板上,所述涂层包含钇;
通过施加多个脉冲而在所述涂层的沉积期间将脉冲式的偏电压施加至所述基板,所述多个脉冲中的每一脉冲由0.001秒至60秒的on时间和0.001秒至60秒的off时间组成;
从所述铝基板去除过量的镀覆溶液;和
后处理其上具有所述涂层的所述铝基板,以氧化所述涂层,其中在所述后处理之后,所述涂层具有改善的耐腐蚀性和以下一项:
(1)在14原子百分比至47原子百分比的范围内的钇的成分、在2原子百分比至3原子百分比范围内的铝的成分和在50原子百分比至83原子百分比的范围内的氧的浓度;或
(2)在12原子百分比至43原子百分比的范围内的钇的成分、在9原子百分比至10原子百分比范围内的铝的成分和在35原子百分比至55原子百分比的范围内的氧的浓度。
20.如权利要求19所述的方法,其中所述沉积前驱物包含YCl3、Y(NO3)3、醋酸钇或Y(CxHy)z。
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TWI669420B (zh) | 2019-08-21 |
WO2017155711A1 (en) | 2017-09-14 |
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US10253406B2 (en) | 2019-04-09 |
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