CN114250117A - 使用包含氧化剂的清洁剂的cmp后缺陷的有效减少 - Google Patents
使用包含氧化剂的清洁剂的cmp后缺陷的有效减少 Download PDFInfo
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- CN114250117A CN114250117A CN202111030957.7A CN202111030957A CN114250117A CN 114250117 A CN114250117 A CN 114250117A CN 202111030957 A CN202111030957 A CN 202111030957A CN 114250117 A CN114250117 A CN 114250117A
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Abstract
本发明涉及使用包含氧化剂的清洁剂的CMP后缺陷的有效减少。本技术总体上涉及用于清洁CMP后半导体表面的液体组合物,和其上具有二氧化铈(CeO2)颗粒的半导体表面的清洁方法。
Description
技术领域
本技术总体上涉及用于清洁CMP后半导体表面的液体组合物,和其上具有二氧化铈(CeO2)颗粒的半导体表面的清洁方法。
背景技术
半导体器件节点的制造需要浅沟槽隔离(STI)工艺。STI化学机械抛光(CMP)工艺需要高SiO2去除率、高SiO2:Si3N4选择性、和低表面缺陷的组合。通常,CMP中采用的CeO2颗粒得到高SiO2去除率和高SiO2:Si3N4选择性的最佳组合。然而,CeO2 CMP倾向于产生具有高缺陷数的主要由残留CeO2颗粒组成的晶圆(wafer)。CeO2抛光晶圆的CMP后清洁由此存在一个主要技术问题。需要用于CeO2的有效、且低成本的CMP后清洁化学品,以能够实现STI技术。
用于CeO2 CMP后的基于商品的清洁方法通常利用苛刻的化学条件,例如SCI(5份H2O、1份NH4OH、1份H2O2)、稀氢氟酸(DHF)、或SPM(1份H2SO4、4份H2O2)。这些方法在减少CMP后CeO2缺陷方面是有效的,但是并非没有明显的缺点:SCI在晶圆表面上留下大量废渣,DHF会导致不可接受的高材料损失,并且SPM负担与较长的处理时间和附加的基础设施支出相关的成本无效。
正是在该背景下,需要开发本文所述的实施方案。
发明内容
本文提供用于清洁CMP后半导体表面和其上具有CeO2颗粒的半导体表面的组合物和方法。
某些实施方案包括用于清洁CMP后半导体表面的液体组合物,该液体组合物包括:氧化剂组合物,其中氧化剂组合物的标准还原电位(E°)>2.0V;和碱性胺化合物和表面活性剂中的至少之一。在一些实施方案中,液体组合物进一步包括酸。在一些实施方案中,酸选自膦酸和双膦酸。在一些实施方案中,酸选自1-羟基乙叉-1,1-二膦酸(1-hydroxyethylidene-1,1-diphosphonic acid)、NTMP(次氮基三(亚甲基膦酸)(Nitrilotris(Methylene Phosphonic Acid)))、PBTC(膦酸丁烷三羧酸)、EDTMP(乙二胺四(亚甲基膦酸))、焦磷酸、氨基亚乙基膦酸(aminoethylene phosphonic acid)、亚甲膦酸(medronic acid)、和(2-羧基乙叉)双膦酸((2-carboxyethylidene)bisphosphonicacid)。在一些实施方案中,组合物包括表面活性剂和碱。在一些实施方案中,表面活性剂为羧酸表面活性剂。在一些实施方案中,表面活性剂选自辛醇聚醚-9羧酸(capryleth-9carboxylic acid)或本领域已知的适合用作表面活性剂的其它聚氧乙烯烷基醚羧酸。在一些实施方案中,碱性胺化合物为烷基化胺。在一些实施方案中,碱性胺化合物选自3-氨基-4-辛醇,2-(二乙氨基)乙硫醇,卡普他明,二乙基乙醇胺,甲基半胱胺,2-(叔丁氨基)乙硫醇,2,2′-二甲氧基-1,1-二甲基-二甲胺,3-丁氧基丙胺,N-乙酰基半胱胺,高半胱胺(homocysteamine),N,N-二甲基羟胺,2-(异丙基氨基)乙醇,2-(甲硫基乙基)胺,1-氨基丙烷-2-硫醇,亮氨酸,半胱胺,选自由N,O-二甲基羟胺、氨基甲基丙醇、氨基甲基丙二醇、氨基乙基丙二醇、2-氨基-2-(羟基甲基)丙烷-1,2-二醇、2-二甲基氨基-2-甲基-1-丙醇、二甲基2-氨基-2-甲基-1,3-丙二醇、二甲基2-氨基-2-乙基-1,3-丙二醇、三(羟基甲基)(二甲基氨基)甲烷、和2-氨基-1-丁醇组成的组中的至少一种。在一些实施方案中,氧化剂组合物的标准还原电位(E°)>2.5V。在一些实施方案中,氧化剂组合物包括至少两种不同的氧化性化合物。在一些实施方案中,该至少两种不同的氧化性化合物包括过硫酸盐和过氧化氢。在一些实施方案中,过硫酸盐选自过硫酸铵、过硫酸钠、过硫酸钾、过硫酸钙、和过硫酸镁。在一些实施方案中,组合物的pH为2至6。在一些实施方案中,氧化剂组合物小于用于清洁CMP后半导体表面的液体组合物的5重量%。在一些实施方案中,用于清洁CMP后半导体表面的液体组合物的水含量占至少95重量%。
其它实施方案包括半导体表面的清洁方法,该半导体表面上具有CeO2颗粒,该方法包括施加前述实施方案中任一项所述的液体组合物。其它实施方案包括半导体表面的清洁方法,该半导体表面上具有CeO2颗粒,该方法包括施加包括氧化剂组合物的液体组合物,其中氧化剂组合物的标准还原电位(E°)>2.0V。在一些实施方案中,对具有CeO2颗粒的半导体表面预先进行化学机械抛光。在一些实施方案中,半导体表面包括TEOS。
附图说明
图1示出本公开的某些实施方案的清洁后TEOS SP1缺陷数与氧化剂添加剂的标准还原电位的关系。
具体实施方式
本文提供用于清洁CMP后半导体表面和其上具有CeO2颗粒的半导体表面的组合物和相关的方法和系统。如本文中所用,术语“化学机械抛光”或“平面化”是指用表面化学反应和机械研磨(mechanical abrasion)的组合将表面平面化(planarizing)(抛光)的工艺。在一些实施方案中,通过将能够与表面材料反应的组合物(可交换地称为‘抛光浆料’、‘抛光组合物’、‘浆料组合物’或简称为‘浆料’)施加至表面来引发化学反应,由此将表面材料变为可以通过同步机械研磨更容易除去的产品。在一些实施方案中,机械研磨通过使抛光垫与表面接触,并且使抛光垫相对于表面移动来进行。
组合物
用于清洁CMP后半导体表面的液体组合物可以包括以下组分、基本上由以下组分组成、或由以下组分组成。
组合物可以包括氧化剂组合物,以及碱性胺化合物和表面活性剂中的至少之一。在一些实施方案中,组合物还包括酸。在一些实施方案中,组合物还包括水,例如去离子水。
氧化剂
组合物可以包括氧化剂组合物。在一些实施方案中,氧化剂组合物的标准还原电位(E°)>2.0V(例如>2.1V、>2.2V、>2.3V、>2.4V、>2.5V、>2.6V、>2.7V、>2.8V、>2.9V、或>3.0V)。在一些实施方案中,氧化剂组合物的标准还原电位(E°)小于4V、或小于3.5V、或小于3V。在一些实施方案中,氧化剂组合物包括至少两种不同的氧化性化合物。例如,在一些实施方案中,至少两种不同的氧化性化合物包括过硫酸盐和过氧化物。对过硫酸盐没有特别限制,并且包括,例如,过硫酸铵、过硫酸钠、过硫酸钾、过硫酸钙、和过硫酸镁。在一些实施方案中,过氧化物为过氧化氢。
氧化剂组合物可以占组合物的约0.05至约4重量%。在一些实施方案中,过硫酸盐氧化剂可以占组合物的约0.05至约0.2重量%(例如,0.05、0.06、0.07、0.08、0.09、0.1、0.11、0.12、0.13、0.14、0.15、0.16、0.17、0.18、0.19或0.2重量%)。在一些实施方案中,过氧化物氧化剂可以占组合物的约0至约4重量%。在一些实施方案中,过氧化物氧化剂仅在使用时添加。本领域技术人员应当理解,这些浓度是在使用时的浓度,并且如果在使用前配制成浓缩组合物,则组合物可以包括更高重量百分比的氧化剂。
碱性胺化合物
组合物可以包括一种或多种碱性胺化合物。在一些实施方案中,碱性胺化合物为烷基化胺。对碱性胺化合物没有特别限制,并且包括,例如,3-氨基-4-辛醇,2-(二乙氨基)乙硫醇,卡普他明,二乙基乙醇胺,甲基半胱胺,2-(叔丁氨基)乙硫醇,2,2′-二甲氧基-1,1-二甲基-二甲胺,3-丁氧基丙胺,N-乙酰基半胱胺,高半胱胺,N,N-二甲基羟胺,2-(异丙基氨基)乙醇,2-(甲硫基乙基)胺,1-氨基丙烷-2-硫醇,亮氨酸,半胱胺,选自由N,O-二甲基羟胺、氨基甲基丙醇、氨基甲基丙二醇、氨基乙基丙二醇、2-氨基-2-(羟基甲基)丙烷-1,2-二醇、2-二甲基氨基-2-甲基-1-丙醇、二甲基2-氨基-2-甲基-1,3-丙二醇、二甲基2-氨基-2-乙基-1,3-丙二醇、三(羟基甲基)(二甲基氨基)甲烷、和2-氨基-1-丁醇组成的组中的至少一种。
碱性胺化合物可以占组合物的约0.05至约0.2重量%(例如,0.05、0.06、0.07、0.08、0.09、0.1、0.11、0.12、0.13、0.14、0.15、0.16、0.17、0.18、0.19或0.2重量%)。本领域技术人员应当理解,这些浓度是在使用时的浓度,并且如果在使用前配制成浓缩组合物,则组合物可以包括更高重量百分比的碱性胺化合物。
表面活性剂
组合物可以包括一种或多种表面活性剂。在一些实施方案中,表面活性剂为羧酸表面活性剂。对表面活性剂没有特别限制,并且包括,例如,辛醇聚醚-9羧酸或本领域已知的适合用作表面活性剂的其它聚氧乙烯烷基醚羧酸。
表面活性剂可以占组合物的约0至约0.02重量%(例如,0.001、0.002、0.003、0.004、0.005、0.006、0.007、0.008、0.009、0.01、0.011、0.012、0.013、0.014、0.015、0.016、0.017、0.018、0.019或0.02重量%)。本领域技术人员应当理解,这些浓度是在使用时的浓度,并且如果在使用前配制成浓缩组合物,则组合物可以包括更高重量百分比的表面活性剂。
酸
组合物可以包括一种或多种酸。在一些实施方案中,酸为膦酸或双膦酸。例如,在一些实施方案中,酸选自1-羟基乙叉-1,1-二膦酸、NTMP(次氮基三(亚甲基膦酸))、PBTC(膦酸丁烷三羧酸)、EDTMP(乙二胺四(亚甲基膦酸))、焦磷酸、氨基亚乙基膦酸、亚甲膦酸、和(2-羧基乙叉)双膦酸。
酸可以占组合物的约0至约0.2重量%(例如,0.01、0.02、0.03、0.04、0.05、0.06、0.07、0.08、0.09、0.1、0.11、0.12、0.13、0.14、0.15、0.16、0.17、0.18、0.19或0.2重量%)。本领域技术人员应当理解,这些浓度是在使用时的浓度,并且如果在使用前配制成浓缩组合物,则组合物可以包括更高重量百分比的酸。
附加组分/方面
在一些实施方案中,组合物还包括水,例如去离子水。水可以以大于90重量%,例如,91、92、93、94、95、96、97、98或99重量%的量存在。
组合物的pH的值通常为约2至约6(例如,约2、3、4、或5)。可以在组合物中包括适当的pH调节剂和/或缓冲剂以调节pH。
方法
在本公开的另一个方面中,本文提供具有二氧化铈颗粒的表面的清洁方法,其包括使表面与本公开的组合物接触。在一些实施方案中,该表面是包括TEOS的半导体表面。在一些实施方案中,对具有二氧化铈颗粒的表面预先进行化学机械抛光(CMP)。在一些实施方案中,清洁方法在与包括台板的抛光区域分开的单元中进行。在一些实施方案中,该单元为刷盒。在一些实施方案中,清洁方法在没有预先台上CMP冲洗的情况下进行。在一些实施方案中,清洁方法通过使表面与不包括研磨剂的本公开的组合物接触来进行。在一些实施方案中,清洁方法进一步包括随后用例如水洗涤的步骤。
在本公开的另一个方面中,本文提供具有二氧化铈颗粒的表面的冲洗方法,其包括使表面与本公开的组合物接触。在一些实施方案中,表面为包括TEOS的半导体表面。在一些实施方案中,对具有二氧化铈颗粒的表面预先进行化学机械抛光(CMP)。在一些实施方案中,表面的冲洗方法在抛光之后在台板上进行,或者在随后的台板上进行。在一些实施方案中,该台板是与用于CMP的台板不同的台板。在一些实施方案中,冲洗方法通过使表面与不包括研磨剂的本公开的组合物、或包括少于用于CMP的抛光组合物的量的研磨剂的本公开的组合物接触来进行。在一些实施方案中,冲洗方法在没有随后的清洁步骤的情况下进行。
在本公开的另一个方面中,本文提供具有二氧化铈颗粒的表面的冲洗和清洁方法,其包括进行如本文公开的冲洗方法,随后进行如本文公开的清洁方法。在一些实施方案中,与不进行冲洗处理的具有二氧化铈颗粒的表面相比,冲洗和清洁的组合方法能够减少清洁具有二氧化铈颗粒的表面所需的时间。
实施例
实施例1
为了试验二氧化铈去除性能,用表1中列出的以下材料配制清洁组合物。所有清洁剂在PoU中在pH为3.3+/-0.3下配制,由于配方中未添加附加的pH调节剂,因此允许pH有一些变化。以等摩尔量使用氧化剂(H2O2除外);在H2O2的情况下,由于在PoU中添加H2O2,以3重量%使用氧化剂。缺陷数在一个刷盒中的200mm TEOS BTW上生成。抛光条件:Ebara、200mm、IC1010、1.4psi、100/95rpm、200ml/分钟、以1000ml/分钟冲洗30秒(BB清洁)。
表1.本研究中使用的清洁剂、清洁剂组成、以及从各清洁剂获得的SP1缺陷数。
将以上组合物用于在表2中列出的以下参数下调节后抛光。
表2.用于二氧化铈CMP的P1抛光条件。
图1示出清洁后TEOS SP1缺陷数与从SP1测量的氧化剂添加剂的标准还原电位的关系。还原电位报告为标准还原电位,取为E°。Ce4+的标准还原电位示出为垂直虚线。未添加氧化剂的参考清洁剂A的缺陷数示出为水平灰色虚线(清洁剂D)。
图1中绘制的结果突出了氧化剂添加剂E°和清洁后SP1缺陷数之间清晰地负相关。清洁剂配方D偏离该趋势。配方D利用KMnO4作为氧化剂,这在酸性条件下会沉淀MnO2(s),如表2中所示。即使KMnO4的标准还原电位高于1.61V,沉淀的固体也会导致高SP1缺陷数。
“E”、“F”和“G”的比较清晰地示出通过组合NH4S2O8和H2O2(“G”与“E”和“F”相比)协同减少TEOS缺陷数。该协同效应可以通过由过硫酸盐的H2O2活化产生的硫酸根来解释。该方法由于不使用酸而与食人鱼蚀刻(piranha etching)(H2SO4+H2O2+Δ)显著不同,该方法可以在温和的酸性条件(pH>3)下应用,并且可以在接近室温下产生硫酸根。
等同情况
本技术不限于本申请中描述的特定实施方案,其旨在作为本技术的各个方面的单一说明。在不脱离本技术的精神和范围的情况下,可以对其进行许多修改和变化,这对本领域技术人员来说是明显的。除了本文列举的那些之外,在本技术的范围内的功能等效的方法和设备从前述描述中对于本领域技术人员来说将是明显的。此类修改和变化旨在落入本技术的范围内。应当理解,本技术不限于特定的方法、试剂、化合物组合物、或生物系统,其当然可以变化。还应理解,本文中使用的术语仅用于描述特定实施方案的目的,并不旨在进行限制。
另外,在根据马库什组描述本公开的特征或方面的情况下,本领域技术人员将认识到本公开由此也根据马库什组的任意个体成员或成员子组进行描述。
如本领域技术人员将理解的,对于任意和所有目的,特别是在提供书面描述方面,本文公开的所有范围还包括任意和所有可能的子范围及其子范围的组合。任意列出的范围均可以容易地识别为充分描述并能够将相同的范围分解为至少相等的一半、三分之一、四分之一、五分之一、十分之一等。作为非限制性实例,本文讨论的各范围均可以容易地分为下三分之一、中三分之一和上三分之一等。如本领域技术人员还将理解的,例如“高达”、“至少”、“大于”、和“小于”等所有语言包括所列举的数并且是指可以随后分为如上所述的子范围的范围。最后,如本领域技术人员将理解的,范围包括各单独的成员。
所有数字标号,例如pH、温度、时间、浓度、量和分子量,包括范围,均是近似值,其视情况而变化(+)或(-)10%、1%或0.1%。应当理解,虽然并未总是明确说明,但所有数字标号前面均可以是术语“约”。如本文中所使用的,术语“约”将被本领域普通技术人员理解并且将根据其使用的上下文在一定程度上变化。如果在使用该术语的上下文中术语的使用对于本领域的普通技术人员来说是不清楚的,则“约”将意味着高达特定术语的正负10%。还应理解,尽管并未总是明确说明,但本文所述的试剂仅是示例性的并且其等价物在本领域中是已知的。
在本文中提及或引用的所有专利、专利申请、临时申请和出版物均通过引用整体并入,包括所有表格,至它们与本说明书的明确教导不矛盾的程度。
在所附权利要求中阐明其它实施方案。
Claims (20)
1.一种用于清洁CMP后半导体表面的液体组合物,其包括:
氧化剂组合物,其中所述氧化剂组合物的标准还原电位(E°)>2.0V;和
碱性胺化合物和表面活性剂中的至少之一。
2.根据权利要求1所述的液体组合物,其进一步包括酸。
3.根据权利要求2所述的液体组合物,其中所述酸选自膦酸和双膦酸。
4.根据权利要求3所述的液体组合物,其中所述酸选自1-羟基乙叉-1,1-二膦酸、NTMP(次氮基三(亚甲基膦酸))、PBTC(膦酸丁烷三羧酸)、EDTMP(乙二胺四(亚甲基膦酸))、焦磷酸、氨基亚乙基膦酸、亚甲膦酸、和(2-羧基乙叉)双膦酸。
5.根据权利要求1至4中任一项所述的液体组合物,其包括表面活性剂和碱。
6.根据权利要求1至5中任一项所述的液体组合物,其中所述表面活性剂为羧酸表面活性剂。
7.根据权利要求1至6中任一项所述的液体组合物,其中所述表面活性剂选自辛醇聚醚-9羧酸或本领域已知的适合用作表面活性剂的其它聚氧乙烯烷基醚羧酸。
8.根据权利要求1至7中任一项所述的液体组合物,其中所述碱性胺化合物为烷基化胺。
9.根据权利要求1至8中任一项所述的液体组合物,其中所述碱性胺化合物选自3-氨基-4-辛醇,2-(二乙氨基)乙硫醇,卡普他明,二乙基乙醇胺,甲基半胱胺,2-(叔丁氨基)乙硫醇,2,2′-二甲氧基-1,1-二甲基-二甲胺,3-丁氧基丙胺,N-乙酰基半胱胺,高半胱胺,N,N-二甲基羟胺,2-(异丙基氨基)乙醇,2-(甲硫基乙基)胺,1-氨基丙烷-2-硫醇,亮氨酸,半胱胺,选自由N,O-二甲基羟胺、氨基甲基丙醇、氨基甲基丙二醇、氨基乙基丙二醇、2-氨基-2-(羟基甲基)丙烷-1,2-二醇、2-二甲基氨基-2-甲基-1-丙醇、二甲基2-氨基-2-甲基-1,3-丙二醇、二甲基2-氨基-2-乙基-1,3-丙二醇、三(羟基甲基)(二甲基氨基)甲烷、和2-氨基-1-丁醇组成的组中的至少一种。
10.根据权利要求1至9中任一项所述的液体组合物,其中所述氧化剂组合物的标准还原电位(E°)>2.5V。
11.根据权利要求1至10中任一项所述的液体组合物,其中所述氧化剂组合物包括至少两种不同的氧化性化合物。
12.根据权利要求11所述的液体组合物,其中所述至少两种不同的氧化性化合物包括过硫酸盐和过氧化氢。
13.根据权利要求12所述的液体组合物,其中所述过硫酸盐选自过硫酸铵、过硫酸钠、过硫酸钾、过硫酸钙、和过硫酸镁。
14.根据权利要求1至13中任一项所述的液体组合物,其中所述组合物的pH为2至6。
15.根据权利要求1至14中任一项所述的液体组合物,其中所述氧化剂组合物小于所述用于清洁CMP后半导体表面的液体组合物的5重量%。
16.根据权利要求1至15中任一项所述的液体组合物,其中用于清洁CMP后半导体表面的液体组合物的水含量占至少95重量%。
17.一种半导体表面的清洁方法,所述半导体表面上具有CeO2颗粒,所述方法包括施加根据权利要求1至16中任一项所述的液体组合物。
18.一种半导体表面的清洁方法,所述半导体表面上具有CeO2颗粒,所述方法包括施加包括氧化剂组合物的液体组合物,其中所述氧化剂组合物的标准还原电位(E°)>2.0V。
19.根据权利要求17或18所述的方法,其中对具有CeO2颗粒的所述半导体表面预先进行化学机械抛光。
20.根据权利要求17至19中任一项所述的方法,其中所述半导体表面包括TEOS。
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