CN103857780A - 用于清洁后化学机械抛光的基板的组合物 - Google Patents
用于清洁后化学机械抛光的基板的组合物 Download PDFInfo
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Abstract
一种用于清洁后化学机械抛光的半导体晶片的半导体加工组合物和方法，其包含磷碱和任选的至少一种表面活性剂。
Description
相关专利申请的交叉引用
本专利申请要求2011年8月22日提交的美国专利申请13/214,920的优先权，该专利申请全文以引用方式并入本文。
背景技术
目前公开并要求保护的一种或多种发明构思涉及用于从物体表面除去不希望的颗粒和残留物的组合物和方法，并且，更具体地涉及用于清洁后化学机械抛光（CMP）的半导体晶片或相关的其它基板的半导体加工组合物和方法。所述组合物包含氢氧化
碱，诸如氢氧化四丁基
并且已在基本上减少缺陷数方面示出令人惊奇的结果。
化学机械抛光（CMP）已成为使半导体晶片和其它相关基板，诸如绝缘膜和金属材料的平面化的主要方法。CMP展示已经从仔细选择的物理和化学组分中观察到明显的协同效应以确保晶片的均匀抛光。将负载力施加到放置在可旋转垫上的晶片的背面，然后将垫（以及晶片）反转，同时使包含磨料（物理组分）的浆液和反应性化学物质通过反转垫下方。
CMP的主要目的是在整个半导体晶片表面或其它基板上获得均匀全面的平面化。相对于半导体晶片，所述晶片可由很多小晶片和图案成，所述小晶片和图案通常采用铜和氧化物诸如二氧化硅的互连线（也称为“互联体”）的形式。当在整个晶片上实现均匀的形貌特征从而造成其成为完全平坦的或平面的时（即，互联体抛光至铜和二氧化硅线两者处理相同的平面），全面平面化出现。
将磨料和化学物质的浆液选择成与在平面化过程中从晶片中除去的材料同时反应和/或使之减少。用于金属CMP（即，铜CMP）的浆液通常为磨料颗粒（包括但不限于氧化铝、二氧化硅、二氧化锰、氧化铈、氧化锆等）与氧化剂（诸如但不限于硝酸铁（III）、含水的过氧化氢等）的组合。将胺和含氮化合物用于CMP方法并不希奇，然而，当或者如果它们被捕获在半导体晶片的互联体内时，则观察到这些化合物更容易造成制造缺陷（即，造成抗蚀剂中毒）。氮（即，氮原子）和含氮化合物杂质可污染生产线并劣化或破坏晶片本身所期望的电性能。
因此，在晶片可被进一步加工之前，在CMP加工期间附着到基板上的杂质和颗粒需要有效并迅速地除去。除去过程被称为后CMP清洁。目前，后CMP清洁制剂使用含氮碱以调节清洁溶液的pH，这继而可导致在制造过程中引入不期望的胺和其它含氮化合物，从而造成晶片的抗蚀剂中毒。因此，存在对于不含氮组合物（和方法）的需要，所述组合物（和方法）从半导体晶片基板中有效清除后CMP残留物和颗粒，并且不在晶片表面上引入含氮化合物。
发明内容
本发明要求保护并公开的一个或多个发明构思涉及用于清洁后化学机械抛光的半导体晶片或相关的其它基板的半导体加工组合物和方法。所述组合物包含至少一种含磷碱以及任选地至少一种表面活性剂。
包括在本发明产生的要求保护并公开的一个或多个发明构思内的是改善的不含氮半导体加工组合物，其包含至少一种含磷碱并可任选地包含一种或多种其它组分，所述组分选自膦酸和/或表面活性剂，例如非离子表面活性剂、阳离子表面活性剂、阴离子表面活性剂。
本发明的加工组合物尤其良好地适用于后CMP清洁（即，后化学机械抛光）以从待清洁物体的表面，例如从半导体晶片的表面除去CMP残留物。因此，在本发明要求保护和公开的一个或多个发明构思内的是用于从物体的表面除去CMP残留物的后CMP清洁方法，所述方法包括以下步骤：（a）形成不含氮加工组合物，所述组合物包含至少一种含磷碱；以及（b）使物体的表面与加工组合物接触，从而从物体的表面除去CMP残留物的主要部分，即材料。
附图说明
图1、2和3为对应于以下实例中的实验制剂A至O的总缺陷数的图。
具体实施方式
本发明要求保护并公开的一个或多个发明构思涉及并定义了改善的半导体加工组合物和方法，其用于清洁后化学机械抛光的半导体晶片或相关的其它基板。所述组合物包含（i）至少一种含磷碱，以及任选地（ii）至少一种表面活性剂。优选地，所述组合物是不含氮的并且表现出负ζ电位。
用于本文的术语“不含氮”是指组合物不包含含氮酸、含氮碱、或可在制剂中引入氮原子的任何其它组分或化合物。
本文所用的术语“ζ电位”是指包含加工组合物的胶体体系的电动电位。本文所设想的胶态体系类型还包含用于CMP浆液的典型的磨料颗粒。ζ电位是加工组合物（即，分散介质）和附着到磨料颗粒或晶片表面的流体的静态层之间的电势差。ζ电位表示带相同电荷的颗粒之间或者浸在清洁组合物中的颗粒与晶片表面之间的排斥程度。据信，并且观察支持如下理论：加工组合物的颗粒/残留物可除去性能可通过ζ电位来预计。例如，已发现具有负ζ电位的胶态二氧化硅的加工组合物表现出可从基板除去的示例性颗粒/残留物。就最佳结果而言，加工组合物的负ζ电位优选在约-80至约-30毫伏（mV）的范围内，尽管该范围可向上或向下变化，只要该变化不减损达到最佳颗粒/残留物除去效果即可。如上所述，ζ电位表示相邻的带相同电荷的颗粒之间或者分散体中的颗粒与晶体表面之间的排斥程度。此外，如果ζ电位高于-10毫伏（mV），则磨料颗粒容易彼此聚集和/或附着到基板表面，这使得其更难以除去。如果ζ电位低于-10毫伏（mV），优选地-30毫伏（mV），则磨料颗粒在分散相中通常是稳定的。
本发明的半导体加工组合物或制剂包含至少一种含磷碱，诸如，以举例的方式并且不受限制，氢氧化
碱。如上所述，组合物可包含一种或多种附加的组分，所述组分选自膦酸，所述膦酸已被示为是与金属离子的优异的螯合剂（从而有助于从基板中除去金属离子）。与膦酸共混的氢氧化
碱不在制剂中引入氮原子，从而维持非常期望的不含氮环境和制剂。虽然许多不同的膦酸可适于完成本发明所公开并要求保护的一个或多个发明构思的目的，但是用于加工组合物的优选的膦酸为‘1-羟基亚乙基-1,1-二膦酸（HEDP）。氢氧化
碱（以及同样地，膦酸）用于调节加工组合物/制剂的pH。虽然可使用许多含磷碱来实现该目的，但是就符合令人满意的性能而言，优选的含磷碱为氢氧化
并且甚至更优选为氢氧化四丁基
表面活性剂增强了加工组合物的润湿性能（即，一种或多种表面活性剂的存在降低了加工组合物的表面张力，这继而使得加工组合物更容易在物体或基板表面之上扩散。）此外，非离子表面活性剂通常以较高的浓度用作洗涤剂胶束。从而，与非离子表面活性剂相关联的润湿性能和洗涤剂胶束形成提高了加工组合物从物体/基板，例如，从半导体晶片表面除去残留物/颗粒的能力。适用于本文所述的加工组合物的非离子表面活性剂包括但不限于：聚乙二醇，烷基多葡糖苷（即，由Dow Chemical Company制造的Triton BG-10和Triton CG-110表面活性剂），辛基苯酚乙氧基化物（即，由Dow Chemical Company制造的Triton X-114），硅烷聚亚烷基氧化物（共聚物）（即，由Momentive Performance Materials制造的Y-17112-SGS样品），壬基苯酚乙氧基化物（即，由Dow Chemical Company制造的Tergitol NP-12），
HS-312（由Momentive Performance Materials制造），以及三苯乙烯基酚乙氧基化物（即，由Stepan Company制造的MAKON TSP-20），聚氧乙烯烷基醚，聚氧乙烯烷基苯基醚，烷基烯丙基甲醛缩合聚氧乙烯醚，聚氧乙烯聚氧丙烯嵌段聚合物，聚氧乙烯聚氧丙烯烷基醚，甘油酯的聚氧乙烯醚，脱水山梨醇酯的聚氧乙烯醚，以及山梨醇酯的聚氧乙烯醚，聚乙二醇脂肪酸酯，甘油酯，聚甘油酯，脱水山梨糖醇酯，丙二醇酯，蔗糖酯，脂族酸链烷醇酰胺，聚氧乙烯脂肪酸酰胺，聚氧乙烯烷基酰胺，壬基酚乙氧基化物诸如
X-114、X-102、X-100、X-45、X-15、BG-10、CG-119，醇乙氧基化物诸如56(C16H33(OCH2CH2)10OH)、
58(C16H33(OCH2CH2)20OH)、
35(C12H25(OCH2CH2)23OH)，醇（伯醇和仲醇）乙氧基化物，胺乙氧基化物，葡萄糖苷，葡糖酰胺，聚乙二醇，聚(乙二醇-共聚-丙二醇)，鲸蜡醇，硬脂醇，十八十六醇（主要由鲸蜡醇和硬脂醇组成），油醇，八甘醇单十二烷基醚，五甘醇单十二烷基醚，聚丙二醇烷基醚，癸基葡糖苷，月桂基葡糖苷，辛基葡糖苷，聚氧乙二醇辛基酚醚，壬苯醇醚-9，甘油烷基酯，月桂酸甘油酯，聚氧乙二醇脱水山梨糖醇烷基酯：聚山梨醇酯；脱水山梨醇烷基酯，司盘（span），椰油酰胺MEA，椰油酰胺DEA，十二烷基二甲基氧化胺，聚乙二醇的嵌段共聚物，聚丙二醇，以及硅烷聚亚烷基氧化物（共聚物）诸如
HS-312、Y-17112-SGS（由Momentive PerformanceMaterials制造）、或它们的组合与混合物。
适用于本文所述的后CMP加工组合物的阴离子表面活性剂包括但不限于：烷基苯磺酸及其盐，诸如十二烷基苯磺酸和十二烷基苯磺酸铵；烷基萘磺酸及其盐，诸如丙基萘磺酸和三异丙基萘磺酸；烷基苯基醚二磺酸，诸如十二烷基苯基醚二磺酸、烷基二苯基醚磺酸及其盐；烷基二苯基醚二磺酸及其盐，诸如十二烷基二苯基醚二磺酸和十二烷基二苯基醚磺酸铵；苯酚磺酸-甲醛缩合物及其盐；芳基苯酚磺酸-甲醛缩合物及其盐；羧酸盐，诸如癸烷羧酸、N-酰基氨基酸盐、聚氧乙烯或聚氧丙烯烷基醚羧酸盐；酰化肽；磺酸盐；硫酸酯盐，诸如硫酸化油、烷基硫酸盐、烷基醚硫酸盐、聚氧乙烯或聚氧丙烯烷基烯丙基醚硫酸盐、烷基酰胺硫酸盐、磷酸酯盐；烷基磷酸盐；以及聚氧乙烯或聚氧丙烯烷基烯丙基醚磷酸盐；十二烷基硫酸铵；月桂基硫酸钠（SDS，十二烷基硫酸钠）；月桂基聚氧乙烯醚硫酸钠，也称为月桂基醚硫酸钠（SLES）；肉豆蔻醇聚醚硫酸钠；二辛基磺基琥珀酸钠；辛磺酸盐；全氟辛磺酸盐；全氟丁磺酸盐；烷基苯磺酸盐；烷基芳基醚磷酸盐；烷基醚磷酸盐；烷基羧酸盐；脂肪酸盐（皂）；硬脂酸钠；月桂酰肌氨酸钠；全氟壬酸盐；全氟辛酸盐；以及它们的混合物。
适用于本文所述的后CMP加工组合物的阳离子表面活性剂包括但不限于：癸双辛胺啶二盐酸盐、烷基三甲基铵盐、鲸蜡基三甲基溴化铵（CTAB）、十六烷基三甲基溴化铵、鲸蜡基三甲基氯化铵（CTAC）、氯化十六烷吡啶（CPC）、多乙氧基化牛脂胺（POEA）、烷基苄基二甲基氯化铵（BAC）、苄索氯铵（BZT）、5-溴代-5-硝基-1,3-二氧杂环己烷、二甲基双十八烷基氯化铵、双十八烷基二甲基溴化铵（DODAB）、脂族胺盐；脂族季铵盐；苯扎氯铵盐；氯化苄乙氧铵；吡啶
盐、和咪唑啉盐、两性表面活性剂羧基甜菜碱型、磺基甜菜碱型、氨基羧酸盐、咪唑啉甜菜碱、卵磷脂、烷基胺氧化物、以及它们的混合物。
如上所述，本发明的半导体加工组合物尤其良好地适用于后CMP清洁（即，后化学机械抛光）以从半导体晶片的表面除去CMP残留物。因此，包括在本发明要求保护和公开的一个或多个发明构思内的是用于从物体的表面除去CMP残留物的后CMP清洁方法，所述方法包括以下步骤：（a）形成不含氮的加工组合物，其包含：（i）至少一种含磷碱，以及任选地（ii）至少一种非离子表面活性剂，其中所述组合物最优化地，但不是必须地表现出负ζ电位，以及（b）使物体的表面与所述加工组合物接触以从物体的表面除去所述CMP残留物的至少一部分。
实例
用于抛光测试的组分材料和用于下列实验制剂A至O的化学物质得自下文所示的来源。
抛光垫：Rohm and Haas EU4000
浆液：DuPont Air Products and Nanomaterials
4366
200mm硅晶片上的毯式铜膜：SVTC Technologies L.L.C。
1-羟基亚乙基-1,1-二膦酸（HEDP）的60%水溶液：Thermophos Japan。
氢氧化四甲基铵（TMAH）的25%水溶液：SACHEM，Inc。
氢氧化四丁基
（TBPH）的40%水溶液：Tokyo Chemical Industry CO.，LTD。
Triton BG10、Triton X114和Triton X100：The Dow Chemical Company
PEG（C13EO10）、聚氧乙烯（10）十三烷基醚：Sigma-Aldrich Co。
抛光和后CMP清洁的实验结果
抛光实验用标准抛光配方在Applied Mirra200mm CMP工具上进行，这种配方是本领域技术人员已知的。在每次抛光实验之前，使用金刚石砂垫调理剂调理抛光垫。抛光后，后CMP清洁实验在Lam Ontrak清洁工具上用标准清洁配方与PVA清洁刷进行。实验制剂如表1、2、3中所示。
然后在KLA-Tencor Surfscan SP1上扫描晶片。将SP1配方设定在0.15μm的阈值内，以表征经后CMP清洁的晶片的缺陷。缺陷数也示出在图1、2和3中。
表1
| 制剂 | A | B | C | D | E | F |
| HEDP | 0.0063 | 0.0038 | 0.0063 | 0.0063 | 0.0063 | 0.0063 |
| TMAH | 0.0048 | 0.0029 | 0.0048 | |||
| TBPH | 0.0143 | 0.0143 | 0.0143 | |||
| Triton BG10 | 0.007 | 0.007 | ||||
| Triton X114 | 0.015 | 0.025 | ||||
| PEG(C13EO10) | ||||||
| Triton X100 | ||||||
| pH | 3.1 | 3.1 | 3.1 | 3.1 | 3.1 | 3.1 |
| Cu(0.2μm) | 238 | 171 | 162 | 166 | 117 | 104 |
| TEOS(0.13μm) | 105 | 64 | 56 | 71 | 71 | 42 |
包含氢氧化四丁基
（TBPH）的制剂不包含任何含氮化合物，并且结合图1，它们表现出比常规TMAH制剂更低的缺陷数。
表2
| 制剂 | G | H | I |
| HEDP | 0.0062 | 0.0062 | 0.0062 |
| TMAH | |||
| TBPH | 0.0143 | 0.0143 | 0.0143 |
| Triton BG10 | |||
| Triton X114 | 0.0025 | ||
| PEG(C13EO10) | 0.0025 | ||
| Triton X100 | 0.0025 | ||
| pH | 3.1 | 3.1 | 3.1 |
| Cu(0.2μm) | 190 | 149 | 145 |
| TEOS(0.13μm) | 45 | 29 | 24 |
制剂G、H和I指示TBPH用多种不同的表面活性剂，例如TritonX114、PEG和Triton X100功能化。
表3
| 制剂 | J | K | L | M | N | O |
| HEDP | 0.0062 | 0.0063 | 0.0062 | 0.0062 | 0.0062 | 0.0062 |
| TMAH | ||||||
| TBPH | 0.0143 | 0.0232 | 0.0274 | 0.0232 | 0.0274 | 0.0274 |
| Triton BG10 | 0.007 | 0.007 | 0.007 | |||
| Triton X114 | ||||||
| PEG (C13EO10) | ||||||
| Triton X100 | 2.5 | |||||
| pH | 3.1 | 7 | 10 | 7 | 10 | 10 |
| Cu (0.2μm) | 193 | 193 | 224 | 95 | 85 | 147 |
| TEOS (0.13μm) | 36 | 40 | 29 | 21 | 36 | 24 |
制剂J至O指示TBPH在宽pH值范围内功能化。
尽管出于清楚和理解的目的，已借助举例说明和实例对前述一个或多个发明构思进行了详细说明，但是本领域技术人员将理解并显而易见可在不脱离其实质和范围的情况下，实施某些改变和修改，如本说明书中所述。
Claims (10)
1.后CMP清洁组合物，其不含氮原子并且包含至少一种含磷碱。
2.根据权利要求1所述的后CMP清洁组合物，其还包含至少一种表面活性剂。
3.根据权利要求1或权利要求2所述的组合物，其表现出在-80毫伏至约-10毫伏范围内的负ζ电位。
4.根据权利要求1或权利要求2所述的组合物，其中所述至少一种含磷碱为
化合物，所述
化合物选自氢氧化和氢氧化烷基
5.根据权利要求6所述的组合物，其中所述氢氧化
为氢氧化四丁基
6.根据权利要求2所述的组合物，其中所述表面活性剂为非离子表面活性剂。
7.用于清洁后化学机械抛光的半导体晶片以从所述晶片表面除去CMP残留物的方法，所述方法包括以下步骤：
(a)形成加工组合物，所述加工组合物包含：
至少一种含磷碱；以及任选地
至少一种表面活性剂，以及
(b)使所述晶片的表面与所述加工组合物接触，从而从物体的表面除去
所述CMP残留物的至少一部分。
8.根据权利要求7所述的方法，其中所述组合物表现出在约-80毫伏至约-10毫伏范围内的负ζ电位。
9.根据权利要求7或权利要求8所述的方法，其中所述至少一种含磷碱为氢氧化
10.根据权利要求9所述的方法，其中所述氢氧化
为氢氧化四丁基
并且所述表面活性剂为非离子表面活性剂。
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| US13/214,920 US20130053291A1 (en) | 2011-08-22 | 2011-08-22 | Composition for cleaning substrates post-chemical mechanical polishing |
| US13/214,920 | 2011-08-22 | ||
| PCT/US2012/051672 WO2013028662A2 (en) | 2011-08-22 | 2012-08-21 | Composition for cleaning substrates post-chemical mechanical polishing |
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| CN107075411A (zh) * | 2014-09-18 | 2017-08-18 | 应用材料公司 | 使用经设计的黏性流体的高效率后cmp清洗的方法与设备 |
| WO2016069576A1 (en) * | 2014-10-31 | 2016-05-06 | Entegris, Inc. | Non-amine post-cmp compositions and method of use |
| JP6728011B2 (ja) * | 2016-09-27 | 2020-07-22 | 株式会社ダイセル | Ｃｍｐ用研磨材組成物、及び該ｃｍｐ用研磨材組成物を使用した半導体デバイスの製造方法 |
| KR20210090294A (ko) * | 2017-01-18 | 2021-07-19 | 엔테그리스, 아이엔씨. | 표면으로부터 세리아 입자를 제거하기 위한 조성물 및 방법 |
| JP7299102B2 (ja) * | 2018-09-25 | 2023-06-27 | 株式会社フジミインコーポレーテッド | 中間原料、ならびにこれを用いた研磨用組成物および表面処理組成物 |
| US11060051B2 (en) | 2018-10-12 | 2021-07-13 | Fujimi Incorporated | Composition for rinsing or cleaning a surface with ceria particles adhered |
| US10640681B1 (en) * | 2018-10-20 | 2020-05-05 | Rohm And Haas Electronic Materials Cmp Holdings, Inc. | Chemical mechanical polishing composition and method for tungsten |
| WO2022070969A1 (ja) * | 2020-09-30 | 2022-04-07 | 株式会社フジミインコーポレーテッド | 酸化ガリウム基板用洗浄剤 |
| CN114989898B (zh) * | 2022-04-02 | 2023-10-20 | 三达奥克化学股份有限公司 | 一种研磨抛光残留物清洗液及其制备方法与应用 |
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- 2012-08-21 SG SG11201400137WA patent/SG11201400137WA/en unknown
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| TWI472610B (zh) | 2015-02-11 |
| WO2013028662A3 (en) | 2013-06-27 |
| TW201319246A (zh) | 2013-05-16 |
| WO2013028662A2 (en) | 2013-02-28 |
| EP2748296A2 (en) | 2014-07-02 |
| KR20140066725A (ko) | 2014-06-02 |
| EP2748296A4 (en) | 2015-05-27 |
| JP2014526153A (ja) | 2014-10-02 |
| US20130053291A1 (en) | 2013-02-28 |
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| SG11201400137WA (en) | 2014-03-28 |
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