CN1053933C - 改良的抛光组合物和抛光方法 - Google Patents

改良的抛光组合物和抛光方法 Download PDF

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CN1053933C
CN1053933C CN94192249A CN94192249A CN1053933C CN 1053933 C CN1053933 C CN 1053933C CN 94192249 A CN94192249 A CN 94192249A CN 94192249 A CN94192249 A CN 94192249A CN 1053933 C CN1053933 C CN 1053933C
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G·布兰卡罗尼
L·M·库克
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Abstract

一种改良的组合物，用于抛光硅，二氧化硅，含硅或二氧化硅的物品，包括金属和二氧化硅的复合体，该组合物包括水介质，磨料颗粒，一种氧化剂和一种抑制去除二氧化硅速率的阴离子。产生该阴离子的一类化合物含有至少两个酸基团，且其中第一种可离解酸的pKa不明显大于抛光组合物的pH。还提供了用该组合物对工件表面进行抛光或平面化的方法，以及用该方法制得的产品。

Description

改良的抛光组合物和抛光方法
本发明涉及玻璃，半导体，电介质/金属复合体和集成电路的抛光。本发明特别涉及复合材料的表面制备方面的改良，该材料要求在二氧化硅和其他成分之间的抛光速率有改良的差别。
常规抛光组合物或抛光膏液一般由含有磨料颗粒的溶液构成。部件或基片浸浴或淋浴在该膏液中，与此同时一种弹性衬垫压在基片上并旋转，使得膏液颗粒在负荷下压在基片上。衬垫的横向运动使膏液颗粒的运动跨越基片表面，造成基片表面磨损去除一定体积。
许多情况下表面去除的速率完全由施加压力的程度，衬垫旋转速度和膏液颗粒的化学活性来决定。因此，对基片有高度化学活性的膏液颗粒(例如CeO2对SiO2)，和比较惰性的颗粒(例如La2O3对SiO2)相比，表现出明显高的抛光速率。抛光颗粒化学活性的这种增加已是众多专利的基础，例如US4959113。
增加抛光速率的一种替代方式是向膏液添加一些组分，这些组分本身对基片有腐蚀的作用。与磨料颗粒一起使用时，可以获得明显较高的抛光速率。这种工艺，通常叫做化学机械抛光(CMP)，对半导体和半导体器件特别是集成电路的抛光是一种优选技术。用于增强硅片表面抛光的这种CMP工艺实例已被Payne的专利公开，见US4169337。Beyer等人(US4944836)和Chow等人(US4702792)告知，在诸如集成电路结构中内联通路的电介质/金属复合体结构的抛光方面，CMP在改良速率选择性的效用。他们特别告知引入加速溶解金属成分的添加剂。这些和其他相关技术的目的是优选去除电路的金属部分，使得所得表面变成共平面。该工艺通常叫做平面化。
尽可能多地改良金属平面化的选择性是高度需要的。Carr等人(US4954142)告知，向对感兴趣的金属组分具有选择性的膏液中添加螯合剂，可进一步改良电介质/金属复合体结构的CMP平面化。这就造成进一步增加金属相的腐蚀速率，增加金属对电介质相而言去除的选择性，使得平面化工艺更加有效。
已论证许多的阴离子以这样一种方式与Si4+螯合或配合，以加速二氧化硅或硅酸盐材料的腐蚀。如Bacon和Raggon所述，(J.Amer.Cerm.Soc.vol.42，pp.199-205，1959)，许多弱酸在中性溶液(pH～7)中可加速二氧化硅和硅酸盐玻璃的腐蚀。这种作用归因于酸的游离阴离子(共轭碱)配合Si4+阳离子的能力，其配合方式更类似于Rosenheim等人所述的邻苯二酚-硅酸盐配合物(A.Rosenhejm，B.Raibmann，G.Schendel；Z.anorg.u. augem.chem.，vol.196，pp.160-76，1931)，如下所示，
Figure C9419224900051
Bacon和Raggon所述腐蚀性阴离子都有相似结构，该结构本身又密切相似于邻苯二酚(1，，2-二羟基苯)，通常都是一元或二羧酸，该酸在二级或三级碳位置亦即位于相对羧酸基团的α位置上有羟基。同非活性化合物相较活性化合物的实例表达如下：HOOC-CHOH-CHOH-COOH：酒石酸(活性)pKa1＝3.02相较于HOOC-CH2-CH2-COOH：琥珀酸(非活性)pKa1＝4.2。pKa是形成游离阴离子缔合常数Ka的对数，如以下反应式限定：
Figure C9419224900061
K ' a = [ RCOO - ] [ H 3 O + ] [ RCOOH ] [ H 2 O ] , orKa = K ' a [ H 2 O ] = [ RCOO - ] [ H 3 O + ] [ RCOOH ] . 因此，较低的pKa表示一种强酸。在相等的pH时发现溶液有较高的共轭碱浓度。现有技术文章也叙述了邻苯二酚在静态溶液中的腐蚀作用。如Ernsberger所示(J.Amer.Cerm.Soc.，vol.42，pp.373-5，1959)，向乙二胺四乙酸(EDTA)溶液中添加邻苯二酚，pH范围为10-14时可增强钠钙硅酸盐玻璃的腐蚀。其速率至少为只有EDTA的溶液的两倍，因此这种增强是显著的。发现在pH＝12.5时有最大的作用。又一次，该作用归因于游离Si4+与邻苯二酚的配合。
以上可清楚得知，以此目的出版的文章显示出，添加剂在静态裸露条件下对二氧化硅或硅酸盐有腐蚀性。认为腐蚀模式是与游离Si4+阳离子形成配合物或螯合物。因此，在US4954142告知的类似方式中，抛光溶液存在这种添加剂时，可以预料抛光期间较高的二氧化硅去除速率。结果，这些类型的添加剂从来不用在金属平面化方面，因为预计到金属/二氧化硅的选择性严重受损。
上述现有技术CMP工艺显现出有吸引力的同时，它们也有明显的缺点。特别是结合进入现有技术CMP膏液的浸蚀剂是各向同性的，亦即它们浸蚀裸露相的所有部分，而不管其位置。因此，浸蚀剂结合进入CMP膏液在凹进部位受到浸蚀时，常常造成明显增大表面粗糙度和纹理度。集成电路抛光中，这种作用叫做表面凹陷，并且当基片表面的大部分由更耐久成分构成时，表面凹陷常常发生在工艺末期。这是特别不希望发生的，因为抛光的目的是制备没有纹理的均匀平坦的表面。
以上讨论清楚得知，如果复合体结构的二氧化硅相抛光速率以可控方式降低，则明显改良了选择性。这就允许使用对其他(金属)相浸蚀较小的溶液，因而导致具有降低表面凹陷的金属/二氧化硅复合体的有效CMP加工。
因此，本发明的目的是提供一种抛光硅，二氧化硅，含硅或二氧化硅物品的溶液，其中通过添加特定添加剂或配合剂来调节或控制硅或二氧化硅相的抛光速率。
本发明另个目的是提供一种用于复合体物品的抛光膏液和方法，使得抛光工艺期间对该物品具有改良的选择性，特别是对诸如集成电路结构中出现的那些金属/电介质复合体。
本领域技术人员参照下面详述和实施例将显然明了本发明的这些和其他目的。
实现本发明目的的方式是提供一种组合物，用于抛光硅，二氧化硅，含硅或二氧化硅物品，包括金属和二氧化硅复合体，该组合物包括水介质，磨料颗粒，一种氧化剂和一种抑制去除二氧化硅速率的阴离子。产生该阴离子的化合物含有至少两个酸基团，且其中第一种可离解酸的pKa不明显大于抛光组合物的pH。
在本发明中我们发现一类化合物有出乎意料的抑制物体的抛光速率能力，该物体表面包括二氧化硅和硅酸盐。这些化合物结合进入抛光膏液可对所述表面抛光速率给予控制，因此当所述表面是复合体物品(例如电介质/金属复合体)的成分时，可产生前所未有程度的选择性。甚至更出乎意料的是，现有技术告知这些相同的化合物在静态条件下起加速腐蚀二氧化硅和硅酸盐的作用。
如上所讨论的，所述抑制速率的化合物是在溶液中离解产生特殊一类游离阴离子的那些化合物，可以认为所述阴离子经与表面羟基基团相互反应，配合或键合到硅，二氧化硅或硅酸盐表面(Si-OH)。
我们出乎意料地发现，反过来也是真的；这类阴离子引入抛光组合物实际上在抛光工艺期间抑制了二氧化硅的去除。这种抑制作用在下面实施例中可清楚说明。
具体说来，我们观察到，抑制速率化合物的所述阴离子必须同时有两个特征，以便抑制SiO2的抛光速率。首先，它们在结构中必须存在至少两个酸基团，该结构可影响对二氧化硅或硅酸盐表面的配合，其次，第一种可离解酸的pKa必须不明显大于抛光组合物的pH，以便产生二氧化硅的有效抑制。本文限定的“明显”是0.5单位(pKa或pH)。
酸物质是指官能团具有可离解质子的那些酸。它们非限制性地包括羧酸根，羟基，磺酸的和磷酸的基团。羧酸根和羟基基团因为在许许多多的有效物质中存在而是优选的。
第一种可离解酸的pKa强烈地受结构影响。我们发现很多结构是有效的，只要满足前述两个必要条件。特别有效的结构是具有两个或多个羧酸基团，其在α位置带有羟基，诸如直链一元和二元羧酸及其盐，例如包括马来酸及其盐，酒石酸及其盐，葡糖酸及其盐。还有效的是三元和多元羧酸及其盐，相对于羧酸基团α位置带有二级或三级羟基基团，例如柠檬酸及其盐。有效的化合物也有含苯环的，例如邻二羟基和多羟基苯甲酸及其盐，苯二甲酸及其盐，邻苯二酚，1，2，3，-苯三酚，酸及其盐和鞣酸及其盐。这些化合物之所以有效的原因在于在这种结构中观察到扩展的电子离域作用。这种离域作用导致了溶液中共轭碱的高度稳定性，如以下低pKa值证实：酸：     pKa1＝4.4
马来酸：    pKa1＝3.4
酒石酸：    pKa1＝3.02
柠檬酸：    pKa1＝3.1
苯二甲酸：  pKa1＝2.95。
本发明所述限制pKa是由于需要游离阴离子或共轭碱以合理的浓度存在，以便产生速率抑制作用。在pH＜＜pKa时存在很少的游离阴离子。在pKa＝pH时，酸有50％离解。在pH＞＞pKa时所有酸基本上以阴离子存在。因此，必须选择离解常数使之对应抛光中通常遇到的pH范围值。理想地，抛光组合物的pH值应当等于或大于抑制二氧化硅速率所用添加剂的pKa1等效值。如果添加剂的pKa1明显大于组合物pH，溶液中不能产生足够的游离阴离子，因此不产生抑制作用。所以，诸如酒石酸，柠檬酸和苯二甲酸(pKa≤3.1)的添加剂覆盖的pH范围相应于抛光硅酸盐遇到的正常pH范围(pH～4-11)，应当是有效的并且是优选的。与此相反，添加邻苯二酚(pKa1～10)就仅仅可用于非常高pH的溶液，诸如在抛光硅片中所发现的，并且要更严格使用。
抑制去除二氧化硅速率的化合物有效量通常是0.1摩尔或更大，直至使用温度下抛光组合物中化合物的溶解度。
本发明抛光组合物中的磨料颗粒可是任何精抛光常用的那些，诸如SiO2，ZrO2，CeO2，Al2O3和金刚石。抛光组合物中磨料颗粒的用量通常是，以抛光组合物重量计，大约1％-15％固体。下面实施例中使用的磨料颗粒是亚微级氧化铝颗粒(Al2O3)。
本发明抛光组合物中的氧化剂是任何可溶在水介质中的氧化剂，条件是氧化剂的氧化势要大于被抛光复合体内金属的氧化势。通常的氧化剂是氯酸盐，高氯酸盐，亚氯酸盐，硝酸盐，过硫酸盐和过氧化物。在下面实施例中，使用过氧化氢作氧化剂，发现对加速去除钨是有效的。本发明抛光组合物对之有效的复合体中的金属通常是钨，铜和铝，然而任何金属都落入本发明范围。氧化剂用量可高达抛光组合物重量的50％，但最常用的范围是10％-40％。
本发明制备几个组合物的实施例叙述如下，以便说明和澄清必要特点，绝非以任何方式进行限制。
                     实施例1
如下制备两个抛光组合物。两个组合物仅有的区别是第2个组合物含有0.3摩尔苯二甲酸氢钾作为添加剂引入以便抑制二氧化硅的抛光速率。两个组合物用来抛光的样品都是硅基片上CVD-沉积的钨金属膜，以及硅基片上热生长二氧化硅，在Strasbaugh6DS抛光机上使用同样抛光条件。抛光条件是：压力：       7psi轴速：       40rpm压板速：     50rpm衬垫类型；   Rodel IC1000，直径38″膏液流量：   150ml/min温度：       230℃。组合物1
1000克亚微级氧化铝膏剂(33％固体)
1000克水
2000ml 50％过氧化氢
pH＝5.6
钨金属的抛光速率＝436埃/min
二氧化硅抛光速率＝140埃/min
选择性(W/SiO2)＝3.1∶1。组合物2
1000克亚微级氧化铝膏剂(33％固体)
1000克水
2000ml 50％过氧化氢
221.6克苯二甲酸氢钾
pH＝2.9
钨金属的抛光速率＝1038埃/min
二氧化硅抛光速率＝168埃/min
选择性(W/SiO2)＝15.3∶1。
加入苯二甲酸盐导致膏液pH降低至大约苯二甲酸的pKa1。较低的pH使钨的抛光速率增加。苯二甲酸盐的加入导致二氧化硅抛光速率降低大约1/2。这就造成相对二氧化硅的钨去除选择性增大五倍，这是非常好的结果。本实施例中，向组合物引入过氧化氢可加速去除钨。组合物2在低pH时高度有效是出乎意料的。这与US4956313和US4992135的所指出的相反，那两篇专利告知，使用pH大于6的溶液得到钨对二氧化硅去除选择性最佳效果。因此，本实施例的组合物2在用于抛光金属/电介质复合体时代表了本发明优选实施方案。
                    实施例2
为了更清楚显示二氧化硅的速率抑制不是由于加入过氧化氢，重复实施例1的试验而不添加过氧化氢，其中加入以相对于苯二甲酸盐等摩尔浓度的非活性盐(硝酸铵)。基片和抛光条件和实施例1所用的相同。如下所示，钨的速率相同，与此同时，当苯二甲酸盐加入组合物时，二氧化硅的速率降低大约1/2。本实施例中，含有苯二甲酸盐的组合物pH明显在pKa1以上。组合物3
1000克亚微级氧化铝膏剂(33％固体)
3000克水
177克硝酸铵(0.6N)
pH＝7.6
钨金属的抛光速率＝71埃/min
二氧化硅抛光速率＝227埃/min组合物4
1000克亚微级氧化铝膏剂(33％固体)
3000克水
221.6克苯二甲酸氢钾(0.6N)
pH＝3.6
钨金属的抛光速率＝71埃/min
二氧化硅抛光速率＝119埃/min。
                      实施例3
还为了进一步说明本发明阴离子对二氧化硅抛光速率的作用，向上述许多新制备的组合物1一部分中变换浓度添加苯二甲酸氢钾。基片和抛光条件同实施例1和2的再次相同。试验结果概括如下：
                      表1
试验                  1       2       3       4
添加苯二甲酸氢钾
                      0.00    0.05    0.10    0.20
的摩尔数
pH                    6.0     3.6     3.5     3.3
钨抛光速率
                      444     978     1164    1164
埃/分
二氧化硅抛光速率
                      167     137     93      76
埃/分
                      2.7     7.1     12.5    15.3
选择性(W/SiO2)
不添加苯二甲酸盐组合物的钨抛光速率和二氧化硅抛光速率两者以及选择性与实施例1的数据良好吻合。二氧化硅抛光速率直接随着苯二甲酸盐浓度的增大而降低，与此同时，在苯二甲酸盐添加剂为0.05摩尔以上时钨抛光速率保持相对恒定。这些数据也与实施例1含有苯二甲酸盐的组合物2的数据相吻合。这些数据清楚表明，本发明组合物的作用是抑制二氧化硅抛光速率并且带有相对于金属相抛光选择性的相应改良。本实施例中，为有效起见，～0.1摩尔的临界浓度是需要的。化合物在这个临界浓度以上添加也是本发明优选实施方案。当然，使用它们的最大浓度只能等于使用温度下它们在组合物中的溶解度。对于苯二甲酸氢钾，溶解度的限制在室温是大约0.5摩尔。
                   实施例4
制备上述实施例1的一部分组合物2，并用来抛光钨板和二氧化硅板两个样品以及集成电路样品。集成电路由器件构成，该器件包括层间通路(接线柱)和用大约2000埃钨金属覆盖的二氧化硅介质层。板状基片的组合物相同于集成电路所含有的。所有样品在Strasbaugh Model 6DS平面机上抛光，所用条件设定如下：压力：      7psi载体速：    25rpm压板速：    25rpm衬垫类型；  IC-1000膏液流量：  100ml/min。
钨板基片表明去除速率为900埃/分，同时二氧化硅板速率是70埃/分，得到的选择性是12.9∶1。这与实施例1使用不同机器条件观察到的选择性相近。继续抛光集成电路样品，直至所有可见金属覆层的痕迹消失。抛光后50X下肉眼观察金属(表面)面貌，显示出清晰的线条和凸起。没有见到表面凹陷的痕迹。见到的氧化物层非常光滑，没有划痕、麻坑或雾朦的痕迹。200X下检验显示了锐利的线条和光滑的金属表面。没有观察到氧化物层的损坏。用Tencor P1薄片形貌测定仪进行表面形貌测量表明，基片的总偏斜读数(TIR)在500μm扫描长度时在1200-4000埃之间，取决于位置和面貌特征，表示电路已被成功地平面化。TIR是在扫描长度内最大和最小表面面貌特征之间的差值，通常是测量基片平面度时可接受的量度。

Claims (8)

1.一种抛光金属和二氧化硅复合体的组合物，包括水介质，磨料颗粒，一种其氧化势高于所述复合体中金属氧化势的氧化剂和一种或多种化合物，其中该化合物的每种含有至少两种酸物质，每种酸物质含有一个可离解的质子以及形成的阴离子，所述阴离子抑制二氧化硅的去除速率，并以足以抑制二氧化硅去除速率的浓度存在，其中所述酸物质选自马来酸及其盐、酒石酸及其盐、葡糖酸及其盐、柠檬酸及其盐、苯二甲酸及其盐、邻苯二酚、1，2，3-苯三酚、棓酸及其盐，鞣酸及其盐。
2.根据权利要求1的组合物，其中所述抑制去除二氧化硅速率的化合物含有苯环。
3.根据权利要求1的组合物，其中所述抑制去除二氧化硅速率的化合物是直链一元和二元羧酸及其盐，且在相对于羧酸基团α位置上有二级羟基基团。
4.根据权利要求1的组合物，其中所述抑制去除二氧化硅速率的化合物是三元或多元羧酸及其盐，且在相对于羧酸基团α位置带有二级或三级羟基基团。
5.根据权利要求2的组合物，基本上由水介质，磨料颗粒，过氧化氢和苯二甲酸氢钾组成，其中苯二甲酸盐的溶液浓度为0.1摩尔到使用温度下抛光组合物中上述化合物的溶解度。
6.根据权利要求5的组合物，基本由，以重量份计，3.2份水，0.33份磨料颗粒，1.5份过氧化氢和0.22份苯二甲酸氢钾组成。
7.权利要求1-6中任一项的抛光组合物在抛光成分之一是硅，二氧化硅或硅酸盐的复合体的方法中的用途。
8.权利要求1-6中任一项的抛光组合物在抛光表面由金属和二氧化硅构成的集成电路的方法中的用途。
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US5391258A (en) 1995-02-21
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ATE200916T1 (de) 2001-05-15
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DE69427165T3 (de) 2004-09-09

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