CN101048531A - 基材上的保护涂层及其制备方法 - Google Patents

基材上的保护涂层及其制备方法 Download PDF

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CN101048531A
CN101048531A CNA2005800297746A CN200580029774A CN101048531A CN 101048531 A CN101048531 A CN 101048531A CN A2005800297746 A CNA2005800297746 A CN A2005800297746A CN 200580029774 A CN200580029774 A CN 200580029774A CN 101048531 A CN101048531 A CN 101048531A
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protective layer
supercoat
stress
goods
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江畑俊树
守川友治
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Abstract

本发明公开了一种压应力小于280MPa的保护涂层，该涂层可用在使用于诸如含卤素气体或卤素等离子体气氛等腐蚀环境中的装置，例如用在半导体加工装配件中的晶片支撑装置，譬如静电卡盘，加热器等等。在一实施方式中的保护涂层无裂缝且具有小于250MPa的压应力。将其通过离子电镀法沉积在装置的至少一个表面上，其中Ar流速保持在低于5sccm，为得到无裂缝的保护层，一个实施方式的Ar流速保持在0sccm。

Description

基材上的保护涂层及其制备方法
相关申请的交叉引用
本申请要求于2004年7月7日提交、序列号为60/586059的美国临时申请的权益。
背景技术
在半导体工业中，通常将装置暴露于高温下的腐蚀环境，诸如氨、氢和卤素中。这种装置的实例包括基材、衬里、蒸发器、坩埚、加热元件、静电卡盘(electrostatic chucks)、晶片载体、衬托器(susceptor)等等。就计算机集成电路(例如电脑芯片)的生产而言，通常将称作静电卡盘(ESC)的装置用于支撑例如晶片等基材，在该工艺中，可以选择性地对材料层进行沉积和从晶片上除去。
在晶片涂覆过程中，一些涂覆于晶片或芯片的材料也沉积在沉积室内的装置上。这就需要周期性地清洗该装置，通常这是使用高能气体等离子体进行处理的。腐蚀性的清洁剂通常使用例如三氟化氮(NF3)的带卤素的气体来产生氟等离子体，其虽然清洁了该室，但是同时会侵蚀该装置的部件，引起腐蚀。这一腐蚀限制了部件和装置的使用寿命。因此，通过使用耐用的保护涂层来延长部件和装置的使用寿命是合乎需要的。
日本公开专利申请号JP62-123094A2公开了使用由热化学气相沉积法(CVD)形成于高纯碳基材料基材上的AlN涂层的衬托器。日本公开专利申请号H06-061335公开了一种具有保护涂层的静电卡盘，该涂层包括AlN、Al2O3、AlON，并通过包括溅射法、离子电镀法和CVD法的方法进行沉积，以保护置于下面的PBN层。PBN相对卤素气体和卤素等离子体没有抗腐蚀性能。现有技术的保护涂层中，在涂层上已显示出开裂，从而通常导致超过每分钟5000埃(/min)的刻蚀速度。在现有技术的保护涂层中也会经历剥落。
对于多层结构来说，膜内应力的测量使用了现有技术中的公知技术，例如在″Mechanical Properties of Thin Films，″W.D.Nix，MetallurgicalTransactions A，20A，2217(1989)；″The Mechanical Properties of ThinCondensed Films″R.W.Hoffman，Physics of Thin Films，Vol 3，Academic Press，New York，1966和P.H Townsend等人，J.Appl.Phys.62，4438(1987)中所阐述的。对于AlN涂膜来说，残余(机械)应力是由于AlN和基材之间的CTE(热膨胀系数)失配而产生的应力和所沉积的AlN的内部应力的总和。膜的总机械应力或残余应力可通过下述公式(1)加以概括：
应力(残余)s＝应力sT(热)+应力si(内部)    (1)
该等式中，si是内部应力，其是薄膜生长条件和方法的根本结果，并在很大程度上是膜结构和杂质存在的反映。术语sT系指由于膜与基材之间的CTE失配而产生的热应力。热应力sT依赖于各种因素，包括基材的CTE，保护膜的CTE，加工温度(Tdep)和参考温度(Tref)，该参考温度可以是室温或者是在所考虑的操作条件下装置的温度。
对于pBN基材上的AlN涂层来说，因为与包括例如氮化铝、氧氮化铝和其类似物等保护层的材料相比，PBN是一种具有低热膨胀系数的材料，所以在高温下制备并再在室温下冷却的保护层内会形成有强的拉伸应力。由于这一原因，在现有技术的工艺中形成的保护层内预期会开裂和剥落。
因此，仍然需要使用于腐蚀环境中的装置的保护涂层，其能牢固地附着到置于下面的基材上，该装置例如是晶片支撑装置，诸如ESC，衬托器，加热器等等。也需要用于包括PBN、石墨或其组合的基材的保护涂层，以便在卤素气体/卤素等离子体环境中具有优异的抗腐蚀性能。
发明概述
本发明涉及一种基材上的保护涂层及其制备方法。在一实施方式中，本发明涉及一种用于涂覆装置的至少一个表面的保护涂层，该装置使用于含卤素的气体和/或等离子体的环境中，该保护涂层具有小于280MPa的压应力，其中，所述表面包括热解氮化硼、石墨、热解石墨和它们的组合之一。
本发明进一步涉及一种用于涂覆装置的至少一个表面的保护涂层，该装置使用于含卤素的气体和/或等离子体的环境中，其中，当设置在基材上时，该保护涂层处在大于或等于约50kg/cm2的压应力下，并且，其中通过Ar流速小于6sccm的反应性离子电镀法将涂层沉积在该装置的表面上。在本发明的一个实施方式中，将Ar流速保持在0sccm。
最后，本发明涉及包括前述保护涂层的制品，以及由前述制备保护涂层的方法生产的制品。
附图简述
图1例示了使用本发明的保护涂层的制品，即静电卡盘的一实施方式的剖面图。
图2显示了三张AlN涂层的照片，图(a)是显示由热CVD法形成的AlN保护层(a)的扫描电子显微(SEM)像。图(b)是显示由离子电镀法形成的AlN层(b)的SEM像，其中Ar流速保持在大约15sccm。图(c)是显示由离子电镀法形成的AlN层(c)的SEM像，Ar流速保持在0sccm。
图3是例示离子电镀法中AlN保护涂层的压应力与Ar流速之间的关系图。
图4包含两幅图，显示了在拉应力(a)和压应力下保护层的性能。
图5是比较由本发明实施方式之一的离子电镀法制备的AlN层与相对照的由其它方法形成的包括pBN和烧结AlN表面的保护层的柱状图。
优选实施方式详述
如本文使用的术语“第一”、“第二”等等并不表示任何的顺序和重要性，而只是用来将一个元件与另一个相区别，且术语“the”、“a”和“an”并不是表示数量的限定，而只是表示存在至少一个所涉及的名目。而且，本文公开的所有范围都包括端值在内，并且可独立地进行组合。
如本文中所使用的，可将近似的术语用来修饰任何定量的表述，该表述可以进行变化而不会导致与其相关的基本功能的改变。因此，有时候用一个术语或多个术语，例如“大约”和“基本上”所修饰的数值并不限制于确定的精确数值上。至少在一些情况下，该近似的术语可能对应了测量数值的设备的精确度。
如本文所用的，“基材”(“substrate”)或“多个基材”(“substrates”)可与“表面”(“surface”)或“多个表面”(“surfaces”)相互替换。
如本文所用的，“保护涂层”可与“涂层”或“涂膜”或“保护层”或“保护涂膜”相互替换。
如本文所用的，“无裂缝”或“基本上无裂缝”意指用10K的放大倍数借助光学显微镜或SEM观察不到裂缝。裂缝(cracks)也包括空洞(holes)、穿孔(perforations)、微孔(pores)或裂纹(lines)。
粘合(adhesion)意指两种不同的材料相粘接，而内聚(cohesive)意指抗分开的一块物质。如本文所用的，具有优异的粘合性或者具有无剥落的层或不会剥落的涂层的意思是指该涂层的粘合强度超过了置于下方的层或多个层的内聚强度。通过使Tdep接近Tref，或者为一给定的固定δCTE(Delta CTE)而调整内部应力来降低在温度Tref的应力，其中：
应力ST(热)与((CTE基材-CTE膜)*(Tdep-Tref))成正比。
如现有技术中所公知的，膜内应力或机械应力是在例如AlN的涂膜面内作用在该膜横截面的每单位面积上的力。该机械应力性质上可以是压缩的或者是拉伸的。压应力可阻止裂缝的形成，从而增加制品的使用寿命。
在一实施方式中，本申请涉及了一种包括保护涂层的制品，该制品可有利地用于高温下包含氨、氢和卤素的苛刻的半导体制造环境中。在集成电路、半导体、硅片、化合物半导体晶片、液晶显示设备和其玻璃衬底等的制备过程中，这些经涂覆的制品可有利地用作静电卡盘、加热元件和晶片载体。
涂层特征  保护涂层包括AlN、AlON或其组合的至少之一。在一实施方式中，该保护涂层是AlN、AlON或其组合的单层。在另一实施方式中，它是经连续涂覆的多层，或者是相同材料，例如AlN、AlON等的多个涂层，或者是AlN、AlON等的多个不同的层。
在一实施方式中，其上沉积该保护涂层的基材包括：氮化硼(BN)、热解氮化硼(PBN)、或掺碳热解氮化硼(C-PBN)、石墨、热解石墨(pG)或其组合。
当设置在基材上时，该保护涂层也有利地处在压应力的状态，从而便于保留尺寸稳定性和机械强度，以及裂缝数量的减少。与由诸如热化学气相沉积法等方法制备的其它保护涂层相比，该保护涂层也具有显著减少的裂缝数量。在一实施方式，该保护涂层具有与基材极好的粘合性并且没有裂缝。减少的裂缝数量以及涂层的形态使装置的周期性清洗过程中基材的任何刻蚀减到最小。
当施用于基材上时，本发明的保护涂层显著地增加了制品的寿命周期。寿命周期是指制品在作为保护涂层刻蚀掉的结果而不得不被替换之前所能经受清洗环境的时间数量。合适的清洗环境实例包括卤素基等离子体、产生自远程等离子源的卤素基基团、经热分解的卤素基物质、卤素基气体、氧等离子体、氧基等离子体等等。卤素基等离子体的一个实例是三氟化氮(NF3)等离子体。诸如实例四氟化碳(CF4)的氟代烃可单独地加以使用或者与氧结合使用。该制品也可以经受反应性的离子刻蚀环境，并且在这种环境中也应该能提供抗刻蚀性。
在一实施方式中，与具有无保护的PBN作为基材的制品相比，该保护涂层将制品的寿命周期增加了大于或等于约5个小时的时间段。在一实施方式中，与具有无保护的PBN的相似制品相比，该保护涂层将制品的寿命周期增加了大于或等于约10个小时的时间段。在另一实施方式中，与具有无保护的PBN的相似制品相比，该保护涂层将制品的寿命周期增加了大于或等于约50个小时的时间段。在又另一实施方式中，与具有无保护的PBN的相似制品相比，该保护涂层将制品的寿命周期增加了大于或等于约100个小时的时间段。
保护涂层的厚度可依赖于应用和清洗环境加以变化。虽然厚度约1-5μm的保护涂层通常允许在晶片和静电卡盘之间有良好的热接触，但是并不能与具有较大厚度的涂层持续的一样长。然而，厚度大于5μm的涂层比厚度小于5μm的涂层要具有较长的寿命周期。在一实施方式中，该涂层的厚度大于或等于约2微米(μm)。在另一实施方式中，该保护涂层的厚度大于或等于约10μm。在第三实施方式中，该保护涂层的厚度大于或等于约50μm。在又一实施方式中，该保护涂层的厚度大于或等于约75μm。
正如现有技术中所公知的，保护涂膜或涂层中的压应力会阻止裂缝的形成，因而增加了制品的使用寿命。当沉积在包括PBN、PG或C-PBN的基材上时，本发明的保护涂层通常就处在压应力下。
在一实施方式中，该保护膜的压应力小于300Mpa。在第二实施方式中，该膜的压应力小于280Mpa。在第三实施方式中，该膜的压应力小于250Mpa。
该压应力允许保护涂层经受热循环而没有裂缝。该保护涂层具有极少的裂缝，该特点提供了显著的抗刻蚀性能。在一实施方式中，起始保护涂层可能具有裂缝，所述裂缝所占的体积要小于涂层总体积的10％。在另一实施方式中，起始保护涂层可能具有裂缝，所述裂缝所占的体积要小于涂层总体积的5％。在又一实施方式中，当其最初制备成时，该保护涂层可以是完全没有裂缝的。
该保护涂层的特点是，在包括卤素的环境中或者当暴露于等离子体刻蚀、反应性离子刻蚀、等离子净化和气体净化时，其具有耐蚀性，或者具有低的刻蚀速度。该保护涂层的刻蚀速度要比经烧结的相同化学组成的涂层低得多。该保护涂层的刻蚀速度也低于PBN基材的刻蚀速度。这一低的刻蚀速度为PBN提供了保护，因而延长了制品的寿命。在一实施方式中，该刻蚀速度小于100埃/分钟(/min)。在第二实施方式中，在该刻蚀速度小于50埃/分钟(/min)。在第三实施方式中，在包含卤素的清洗环境中或者当暴露在反应性离子刻蚀环境时，该速度小于或等于约40埃/分钟(/min)。
沉积保护涂层的方法-IP  使用离子电镀(IP)对保护涂层进行沉积。在离子电镀中，使用射频(RF)放电将铝电离。电离和等离子体主要是通过由氮气形成的氮离子加以维持。由等离子体放电产生电离，该电离不仅仅能通过射频(RF)线圈加以维持，而且也能通过使用电容耦合等离子体或电感耦合等离子体加以维持。通常将沉积发生的室保持在真空条件下。将氮气导入该室中，并通过射频(RF)放电电离。通常将基材放置在阴极上或其附近，以导引电离气体。将基材连同铝金属一起放置在氩气/氮气等离子体中，其加热蒸发，并当其扩散通过放电区域时变得部分电离(获得带电原子)，以形成保护涂层。
在离子电镀过程中，将室内的温度保持在小于或等于约400℃。离子电镀过程中的沉积速度要大于或等于约0.1μm/h。在一实施方式中，沉积速度大于或等于约0.15μm/h。在另一实施方式中，沉积速度大于或等于约0.2μm/h。在又一实施方式中，沉积速度大于或等于约0.25μm/h。
在离子电镀方法中，可以将惰性气体/非反应性气体，例如氩气，导入到真空反应器中。申请人已经发现，对于无裂缝/最少或者无剥落(在涂层和PBN/PG基材之间的强粘合强度)的抗腐蚀性保护层来说，通过控制反应器中的氩气流量，可以对保护涂层的抗腐蚀性能加以控制。
在离子电镀法的一实施方式中，当氩气流量减少到10sccm时，沿整个保护层有一些明显的剥落。当氩气流量减少到5sccm时，在保护涂层的某个部分内可观察到剥落。在其中的氩气流量保持在低于6sccm的实施方式中，该保护涂层显示出小于280Mpa的压应力，并且很少或没有剥落。在另一实施方式中，为获得粘合到基材上(无剥落)且具有小于250Mpa压应力的无裂缝保护涂层，将氩气流速保持在0sccm。
本发明的应用  该保护涂层可有利用于半导体的加工部件，例如基材、衬里、蒸发器、坩埚、加热元件、晶片载体、静电卡盘、衬托器等。当这些部件暴露于温度大于或等于约200℃下的氨，氢和例如氟、氯、三氟化氮等卤素中时，该保护涂层增加了前述半导体加工部件的寿命。
图1例示了使用本发明保护涂层的制品的剖面图。该制品可以是加热元件、静电卡盘或晶片载体，在晶片上沉积表面层的过程中可将它们用于定位和/或加热硅晶片。在一实施方式中，制品8是静电卡盘。该制品包括大约10mm的石墨芯1。该芯也可以由PBN、热压BN或复合材料制成。设置于石墨芯上的是约300μm的热解氮化硼层(BN)2。在一实施方式中，该pBN层2可通过热化学气相沉积法(热CVD)、热压法、烧结法或等离子增强化学气相法(PECVD)加以沉积。
沉积在BN层2上的是热解石墨(PG)层，该PG层通过化学气相沉积法(CVD)或现有技术中的其它已知方法沉积到BN层2上。将该PG层加工成理想结构，形成在制品上表面的卡盘电极3和在下表面的加热电极(4)。经加工的PG层3和4，连同第一pBN层2和石墨基材1一起形成制品的基体5。将热解氮化硼(PBN)涂层6设置在制品基体上，以使其基本上覆盖制品的基体。该pBN涂层6是在相对于1摩尔三氯化硼，具有3摩尔氨和2.4摩尔甲烷气体的减压压力下，于1850℃的热CVD炉内加以制备的。在基体5的整个表面上，形成厚度约100μm的掺碳PBN绝缘层6，其电阻率为2.8×1012Ω-cm。
该PBN涂层6抗氧化，且提供电绝缘、化学和机械保护，并使晶片碳污染的机会最小。它在a-b方向上也具有很高的热导率，从而使加热器顶部上的任何热量的不均匀性最小。然后在该PBN涂层6上设置AlN保护涂层7。
在一实施方式中，为了给静电卡盘提供保护，以用于甚至腐蚀性的环境，例如卤素气体和/或卤素等离子气氛中，将AlN涂层7在反应性离子电镀过程中施用于静电卡盘8之上，其中氩流速分别保持在0sccm(无氩气)、5sccm、10sccm和15sccm。在离子电镀过程中，氮和铝在约400℃下进行反应，形成相对卤素气体和卤素等离子体具有抗腐蚀性能的本发明AlN保护层7。
作为对照静电卡盘的比较实施例，使用热CVD法在950℃下形成AlN保护层，而代替使用通过离子电镀法的AlN保护涂层。图2(a)-2(c)是SEM(扫描电子显微镜)照片，对本发明的AlN保护层与现有技术经热CVD制备的AlN涂层进行了比较。
图2(a)显示了由热CVD法形成的AlN中的裂缝，证实了在腐蚀性环境中，使用该涂层是不现实的。图2(c)是显示由离子电镀法形成的AlN涂层的SEM像，其中，氩流速减小为0，因而形成无裂缝的AlN层且没有变形。图2(b)显示了当氩流速减少到15sccm时的SEM像，尽管有一些剥落的出现，但是AlN层仍然没有裂缝。
图3是例示离子电镀过程中AlN保护层的压应力与氩流速之间的关系图。在一实施方式中，当氩流量减小为0sccm时，其中形成的AlN保护层7的厚度为0.5μm，杨氏模量值为130GPa，由偏位法测量的泊松比为0.28，经测量的压应力为248Mpa。当氩流速保持在5sccm时，经测量的压应力为267Mpa。当氩流速设置在10sccm时，压应力为344Mpa。最后，当氩气流速为15sccm时，压应力为360Mpa。
应该注意的是，由CVD法形成的AlN保护层，其SEM示于图2(a)中，因为所有的样品都显示了裂缝的存在，所以不能测量出压应力。
图4包括两幅图，显示了在拉应力(a)和压应力下保护层的性能。如前述，在现有技术由热CVD法形成且发生裂缝的AlN涂层中，与包括诸如氮化铝、氧氮化铝或类似物等的保护层的材料相比，pBN的热膨胀系数要小。因为热膨胀系数的差异，所以有强烈的拉应力，这一残余拉应力超过保护层自身的拉伸强度，使保护层断裂，因而引起裂缝。这种情况示于图4(a)中。如图4(b)中所示，在由离子电镀法形成的AlN保护层中，会形成压应力，从而减少或消除了裂纹的发生。
图5是由离子电镀法所形成的本发明AlN涂层与其他的保护表面的抗腐蚀性能比较图，将该抗腐蚀性能作为在NF3等离子气氛下的刻蚀速度加以例示，速度越低，抗腐蚀性能越高。在图中，对由氩流量为0sccm的离子电镀法形成的AlN保护层中所测的刻蚀速度，与烧结AlN、热CVD法的PBN和硅晶片中所测的刻蚀速率进行了比较。本发明的离子电镀AlN的刻蚀速度为4.8/min，作为对比，烧结AlN中的速率为33/min，硅晶片中为455/min，pBN中为大于10000/min。

Claims (10)

1.一种保护层，用来涂敷用于含卤素气体和/或等离子体环境的制品的至少一个表面，其中所述的至少一个表面包括热解氮化硼、石墨、热解石墨和其组合中的一种，其特征在于，所述保护层具有小于280Mpa的压应力。
2.如权利要求1所述的保护层，其特征在于，所述保护层具有小于250Mpa的压应力。
3.如权利要求1-2任一项所述的保护层，其特征在于，所述保护层包括氮化铝、氧氮化铝和其组合之一。
4.如权利要求1-3任一项所述的保护层，其特征在于，将所述保护层通过离子电镀法沉积到所述制品的至少一个表面上。
5.如权利要求1-4任一项所述的保护层，其特征在于，离子电镀法包含作为非反应性气体的氩气且其中的氩气流量保持在低于10sccm的速度。
6.如权利要求1-5任一项所述的保护层，其特征在于，所述表面包括热解氮化硼。
7.如权利要求1-6任一项所述的保护层，其具有3-200μm之间的厚度。
8.如权利要求1-7任一项所述的保护层，其特征在于，所述涂层基本上无裂缝。
9.如权利要求1-8任一项所述的保护层，当暴露于含卤素气体和/或等离子体环境时，其耐刻蚀速度小于50/min。
10.一种包括如权利要求1-9任一项所述的保护涂层的制品。
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