CN100355819C - 化学机械抛光组合物及有关的方法 - Google Patents
化学机械抛光组合物及有关的方法 Download PDFInfo
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- CN100355819C CN100355819C CNB2005100823705A CN200510082370A CN100355819C CN 100355819 C CN100355819 C CN 100355819C CN B2005100823705 A CNB2005100823705 A CN B2005100823705A CN 200510082370 A CN200510082370 A CN 200510082370A CN 100355819 C CN100355819 C CN 100355819C
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- vinylformic
- multipolymer
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Abstract
本发明提供一种可用于抛光半导体晶片上非铁金属互连的含水组合物，它含有氧化剂、非铁金属的抑制剂、非铁金属的络合剂、改性纤维素、0.01～5重量%丙烯酸和甲基丙烯酸共聚物、以及余量的水，其中丙烯酸与甲基丙烯酸的共聚物的单体比(丙烯酸/甲基丙烯酸)为1∶30～30∶1，上述共聚物的分子量为1K～1000K。
Description
技术领域
本发明涉及半导体晶片材料的化学机械平面化(CMP)，更具体地涉及在电介质和防渗透材料的存在下用于抛光半导体晶片上金属互连(interconnect)的化学机械平面化组合物和方法。
背景技术
半导体晶片一般是电介质层中含有排列成电路互连图案的许多沟槽的硅晶片。这些图案排列通常具有镶嵌结构或双镶嵌结构。防渗透层覆盖有图案的电介质层，且金属层覆盖防渗透层。金属层的厚度至少足以用金属填充成图案的沟槽，形成电路互连。
化学机械平面化法通常包括多个抛光步骤。例如，第一步以初始高速除去多余的互连金属，如铜。第一步骤除去后，第二步抛光可以除去留在防渗透层上金属互连外面的金属。以后的抛光从下面的半导体晶片电介质层上除去防渗透层，以便在电介质层和金属互连上形成平面抛光的表面。
半导体基片上沟槽中的金属提供了形成金属电路的金属线。需要克服的问题之一是抛光操作会从各个沟槽中除去金属，使这些金属凹陷。凹陷是不合需要的，因为它使金属电路的临界尺寸发生变化。为了减少凹陷，需在较低的抛光压力下进行抛光。然而，仅减少抛光压力会延长抛光时间。然而，在整个延长时间内仍产生凹陷。因此，目前需要的是一种能减少沟槽中金属凹陷同时不会延长抛光操作时间的方法。在短时间第二步抛光后产生没有互连金属残留物的表面的抛光组合物也是需要的。
美国专利6632259描述了工程共聚物(engineered copolymer)在用于化学机械平面化的含水抛光组合物中的应用。这些工程共聚物包括由摩尔比约为1∶20～20∶1的丙烯酸单体和甲基丙烯酸单体混合物形成的共聚物。据报道，这些工程共聚物用于不含改性纤维素的抛光组合物中。
发明内容
第一方面，本发明提供一种可用于半导体晶片化学机械平面化的含水组合物，它含有含金属的氧化剂、非铁金属的抑制剂、非铁金属的络合剂、改性纤维素、0.01～5重量％丙烯酸和甲基丙烯酸共聚物、以及余量的水，其中丙烯酸与甲基丙烯酸的共聚物的单体比(丙烯酸/甲基丙烯酸)为1∶30～30∶1，上述共聚物的分子量为1K～1000K。该抛光组合物可任选地含有高达3重量％研磨剂。
第二方面，本发明提供一种含金属的半导体晶片的化学机械平面化方法，它包括a)使晶片与抛光组合物接触和b)用抛光垫抛光该晶片，所述的抛光组合物含有氧化剂、非铁金属的抑制剂、非铁金属的络合剂、改性纤维素、0.01～5重量％丙烯酸和甲基丙烯酸共聚物、以及余量的水，其中丙烯酸与甲基丙烯酸的共聚物的单体比(丙烯酸/甲基丙烯酸)为1∶30～30∶1，上述共聚物的分子量为1K～1000K。该抛光组合物可任选地含有高达3重量％研磨剂。
附图说明
图1是清除时间的图示说明。
具体实施方式
当对半导体晶片进行化学机械平面化时，本发明的组合物和方法提供了良好的金属除去速率和足够的清除，又不会使金属互连过分凹陷。本发明的组合物使用丙烯酸和甲基丙烯酸的水溶性共聚物以及用羧酸官能团改性的水溶性纤维素。虽然本发明特别适用于铜互连，但本发明的含水抛光组合物也提供对铝、金、镍、铂族金属、银、钨和它们合金之类其它非铁金属互连的增强抛光。
本发明的共聚物由摩尔比为1∶30～30∶1，较好为1∶9～9∶1，最好为约2∶3的丙烯酸单体和甲基丙烯酸单体合成。本发明共聚物的分子量为1K～1000K，优选为20K～200K。对于本说明书而言，分子量是指重均分子量。
本发明的抛光组合物含有用羧酸官能团改性的水溶性纤维素。该组合物较好含有0.01～5.0重量％水溶性纤维素，最好含有约0.3重量％水溶性纤维素。示例性的改性纤维素是阴离子胶，如琼脂胶、阿拉伯胶、茄替胶、刺梧桐树胶、瓜耳胶、果胶、刺槐豆胶、黄蓍胶、罗望子树胶、角叉菜胶和黄原胶、改性淀粉、藻酸、甘露糖醛酸、古洛糖醛酸、以及它们的改性物和混合物。优选的水溶性纤维素是取代度为0.1～3.0和分子量为1K～1000K的羧甲基纤维素(CMC)。更优选的羧甲基纤维素的取代度为0.7～1.2，分子量为40～250K。羧甲基纤维素的取代度是被取代的纤维素分子中每个葡糖酐单元上的羟基数。它可以认为是羧甲基纤维素中羧酸基“密度”的一个量度。
该溶液优选含有高达25重量％氧化剂。更优选的是，氧化剂为5～10重量％。氧化剂特别有助于该溶液在低pH值范围内除去铜。该氧化剂可以是许多氧化剂中的至少一种，如过氧化氢(H2O2)、一过硫酸盐、碘酸盐、过邻苯二甲酸镁、过乙酸和其它过酸，过硫酸盐、溴酸盐、过碘酸盐、硝酸盐、铁盐、铈盐、Mn(III)盐、Mn(IV)盐和Mn(VI)盐、银盐、铜盐、铬盐、钴盐、卤素、次氯酸盐和它们的混合物。另外，使用氧化剂化合物的混合物通常是有利的。当该抛光浆料含有过氧化氢之类不稳定的氧化剂时，通常最好在使用时把氧化剂混合到该组合物中。
另外，为了通过静电蚀刻或其它除去机理控制铜互连的除去速率，该溶液含有抑制剂。调节抑制剂的浓度可以保护金属免受静电蚀刻，从而调节互连金属的除去速率。该溶液较好含有0.05～5.0重量％抑制剂，最好含有0.2～1.0重量％抑制剂。该抑制剂可以是抑制剂的混合物。唑类抑制剂对铜和银的互连特别有效。常见的唑类抑制剂包括苯并三唑(BTA)、巯基苯并噻唑(MBT)、甲苯基三唑(TTA)和咪唑。对于铜和银来说，苯并三唑是一种特别有效的抑制剂。
除了抑制剂以外，该组合物较好含有非铁金属的络合剂。络合剂有助于提高铜之类金属膜的除去速率。该组合物较好含有0.01～15重量％非铁金属的络合剂，最好含有0.1～1重量％非铁金属的络合剂。络合剂的例子包括乙酸、柠檬酸、乙酰乙酸乙酯、羟基乙酸、乳酸、苹果酸、草酸、水杨酸、二乙基二硫代氨基甲酸钠、琥珀酸、酒石酸、巯基乙酸、甘氨酸、丙氨酸、天冬氨酸、乙二胺、三甲基三胺、丙二酸、戊二酸(gluteric acid)、3-羟基丁酸、丙酸、邻苯二甲酸、间苯二甲酸、3-羟基水杨酸、3，5-二羟基水杨酸、五倍子酸、葡糖酸、焦儿茶酚、焦棓酚、单宁酸，包括它们的盐和混合物。该络合剂较好选自乙酸、柠檬酸、乙酰乙酸乙酯、葡糖酸、乳酸、苹果酸、草酸和它们的混合物。该络合剂最好是苹果酸。
在含有余量水的溶液中，这些化合物在宽的pH值范围内具有效果。该溶液有用的pH值范围为至少2至5。另外，该溶液较好依靠余量的去离子水来限定附加的杂质。本发明抛光液的pH值较好为2.5～4.2，更好为2.6～3.8。用于调节本发明组合物的pH值的酸例如是硝酸、硫酸、盐酸、磷酸等。用于调节本发明组合物的pH值的碱例如是氢氧化铵和氢氧化钾。
另外，该抛光组合物可任选地含有高达3重量％研磨剂，以促进金属层的除去。在该范围内，研磨剂的含量宜小于或等于1重量％。本发明的抛光组合物最好不含研磨剂。
为了防止过度的金属凹陷、电介质磨蚀和改善平面化，研磨剂的平均粒度宜小于或等于500纳米(nm)。对本说明书而言，粒度是研磨剂的平均粒度。更优选的是使用平均粒度小于或等于100纳米的胶态研磨剂。另外，用平均粒度小于或等于70纳米的胶态二氧化硅也可以减少电介质磨蚀和金属凹陷。另外，优选的胶态研磨剂可包含添加剂，如分散剂、表面活性剂、缓冲剂、杀生物剂，以提高胶态研磨剂的稳定性。一种这样的胶态研磨剂是购自Chariant S.A.，ofPuteaux，France的胶态二氧化硅。也可以使用其它研磨剂，包括热解法二氧化硅、沉淀二氧化硅、团聚的二氧化硅等。
该抛光组合物可以包含用于“机械”除去金属互连层的研磨剂。研磨剂的例子包括无机氧化物，无机氢氧化物、无机羟基氧化物、金属硼化物、金属碳化物、金属氮化物、聚合物颗粒和含有至少一种上述物质的混合物。合适的无机氧化物例如包括二氧化硅(SiO2)、氧化铝(Al2O3)、氧化锆(ZrO2)、氧化铈(CeO2)、氧化锰(MnO2)、氧化钛(TiO2)或含有至少一种上述氧化物的混合物。合适的无机羟基氧化物例如包括羟基氧化铝(“勃姆石”)。如有需要，也可以使用这些无机氧化物的改性形式，如涂有有机聚合物的无机氧化物颗粒和无机涂覆颗粒。合适的金属碳化物、硼化物和氮化物例如包括碳化硅、氮化硅、碳氮化硅(SiCN)、碳化硼、碳化钨、碳化锆、硼化铝、碳化钽、碳化钛或含有至少一种上述金属碳化物、硼化物和氮化物的混合物。如有需要，金刚石也可以用作研磨剂。替代的研磨剂也包括聚合物颗粒、涂覆的聚合物颗粒和用表面活性剂稳定的颗粒。如果使用，优选的研磨剂是二氧化硅。
本发明的组合物可应用于含有导电金属、防渗透膜即衬底膜和下层电介质层的任何半导体晶片。上述的导电金属例如是铜、铝、钨、铂、钯、金或铱。上述的防渗透膜例如是钽、氮化钽、钛或氮化钛。对于本说明书而言，术语“电介质”是指介电常数为k的半导电材料，包括低k值和超低k值的电介质材料。上述组合物和方法特别有利于防止多种晶片组份的腐蚀，如多孔或无孔的低k值电介质、有机和无机低k值电介质、有机硅酸盐玻璃(OSG)、氟硅酸盐玻璃(FSG)、掺杂碳的氧化物(CDO)、原硅酸四乙酯(TEOS)和由TEOS形成的二氧化硅。本发明的组合物也可用于ECMP(电化学机械抛光)。
实施例
为了制备高分子量(～200000MW)丙烯酸(AA)/甲基丙烯酸(MAA)(摩尔比为2∶3)共聚物，使用75克100％丙烯酸、135克100％甲基丙烯酸、0.5克+1.9克过硫酸钠(Na2S2O8，MW＝238)、270克+42克+380克去离子水、20克50％NaOH。将25克混合单体加入到一个2000毫升四颈反应器中，然后加入270克去离子水和0.5克过硫酸钠。将该混合物加热到92℃，然后将其余的混合单体和1.9克过硫酸钠在42克水中的溶液一起加入到反应器中，分别历时40和50分钟。将反应混合物在92℃再保持1小时，然后让其冷却到室温。检测粗产物的气相色谱(GC)和凝胶渗透色谱(GPC)，并用50％NaOH溶液中和10％酸。该过程得到Mw/Mn＝198000/30000，AA＝532ppm，MAA＝38ppm，pH＝3.7，粗产物的固体％为45.6％。用20克50％NaOH和380克水将粗产物稀释到24.45％，800克粗产物进一步稀释到10％溶液。
为了制备低分子量(～27000)丙烯酸(AA)/甲基丙烯酸(MAA)(摩尔比为2∶3)共聚物，使用179克AA(100％丙烯酸)、321克MAA(100％甲基丙烯酸)、23.4克过硫酸钠(Na2S2O8)、815克+110克去离子水、49.7克50％NaOH溶液。将25克混合单体加入到一个2000毫升四颈反应器中，然后加入815克去离子水和2.4克过硫酸钠。将该混合物加热到95℃，然后将其余的混合单体和21克过硫酸钠在110克水中的溶液一起加入到反应器中，分别历时140和160分钟。将反应混合物在92℃再保持1小时，然后让其冷却到室温。用49.7克50％NaOH中和10％酸。该过程得到Mw/Mn＝30860/6656，AA＝0ppm，MAA＝47ppm，pH＝1.2。用49.7克50％NaOH将粗产物中和到pH＝3.6，最终的固体％＝37.8％。
在本实施例中，所有的组合物含有0.50重量％BTA、0.22重量％苹果酸、0.32重量％羧甲基纤维素(CMC)和9.00重量％过氧化氢，pH＝2.8。
本实验在中等向下压力下测量铜的抛光速率，并测定从半导体晶片上残余铜的清除率。具体地说，本试验测定在丙烯酸和甲基丙烯酸共聚物的存在下使用改性纤维素化合物对抛光速率、清除时间(clear time)和残余铜清除率的影响。清除时间定义为EPD2-EPD1，其中EPD1是透过铜层检测到防渗透层第一信号时的初始终点检测时间，EPD2是检测器仅看见防渗透层的检测时间。图1图示了清除时间的定义。用一台Applied Material，Inc.Mirra 200毫米抛光机使试样平面化。该抛光机装有ISRM检测系统，使用ICl010TM聚氨酯抛光垫(Rohmand Haas Electronic Material CMP Inc.)，向下力条件约为2psi(13.8kPa)，抛光液流速为150毫米/分钟，板(platen)速为80RPM，底盘(carrier)速度为40RPM。抛光液的pH值用硝酸调节。所有的溶液含有去离子水。
表1
| 浆料 | AA∶MAA | 分子量 | 浓度，重量％ | RRA/分钟 | 残余物清除 | 平均凹陷(A)90％/100微米 | 清除时间EPD2-EPD1 |
| 1 | 3∶2 | 0.1 | 2755 | 否 | 637/463 | 18 | |
| 2 | 1∶1 | 0.1 | 2119 | 否 | 335/341 | 25 | |
| 3 | 2∶3 | 22K | 0.05 | 1496 | 否 | 358/426 | 23 |
| 4 | 2∶3 | 27K | 0.1 | 2426 | 是 | 418/397 | 27 |
| 5 | 2∶3 | 22K | 0.5 | 1419 | 否 | 428/411 | 25 |
| 6 | 2∶3 | 200K | 0.1 | 3172 | 是 | 642/754 | 19 |
| 7 | 1∶4 | 0.1 | 1821 | 否 | 363/457 | 25 | |
| 8 | 1∶9 | 0.1 | 1822 | 否 | 243/441 | 26 | |
| 9 | 0∶1 | 0.1 | 1640 | 否 | 305/445 | 21 |
如表1所示，加入0.1重量％摩尔比为2∶3的丙烯酸/甲基丙烯酸共聚物提供了最佳的铜除去速率和残余铜的清除以及低的凹陷。凹陷结果是中心和90％边缘位置间的步进高度ASH结果的平均值，且在200毫米Sematech 854 maskTEOS晶片上为100微米。虽然在大多数试样上都发现一些残留的铜，但清除时间都少于30秒钟。
Claims (8)
1.一种用于半导体晶片化学机械平面化的含水组合物，它含有0～25重量％含金属的氧化剂、0～3重量％研磨剂、0.05～5.0重量％非铁金属的抑制剂、0.01～15重量％非铁金属的络合剂、0.01～5重量％具有羧酸官能团的改性纤维素、0.01～5重量％丙烯酸和甲基丙烯酸共聚物、以及余量的水，其中所述的络合剂选自乙酸、柠檬酸、乙酰乙酸乙酯、羟基乙酸、乳酸、苹果酸、草酸、水杨酸、二乙基二硫代氨基甲酸钠、琥珀酸、酒石酸、巯基乙酸、甘氨酸、丙氨酸、天冬氨酸、乙二胺、三甲基三胺、丙二酸、戊二酸、3-羟基丁酸、丙酸、邻苯二甲酸、间苯二甲酸、3-羟基水杨酸、3，5-二羟基水杨酸、五倍子酸、葡糖酸、焦儿茶酚、焦桔酚、单宁酸，包括它们的盐和混合物，丙烯酸与甲基丙烯酸的共聚物中的丙烯酸/甲基丙烯酸单体比为1∶30～30∶1，上述共聚物的重均分子量为1K～1000K。
2.如权利要求1所述的组合物，其特征在于所述的丙烯酸和甲基丙烯酸共聚物中的丙烯酸/甲基丙烯酸单体比为1∶9～9∶1。
3.如权利要求2所述的组合物，其特征在于所述的丙烯酸和甲基丙烯酸共聚物中的丙烯酸/甲基丙烯酸单体比约为2∶3。
4.如权利要求1所述的组合物，其特征在于所述共聚物的重均分子量为20K～200K。
5.如权利要求1所述的组合物，其特征在于所述的改性纤维素是用羧酸官能团改性的水溶性纤维素，选自羧甲基纤维素、琼脂胶、阿拉伯胶、茄替胶、刺梧桐树胶、瓜耳胶、果胶、刺槐豆胶、黄蓍胶、罗望子树胶、角叉菜胶和黄原胶、改性淀粉、藻酸、甘露糖醛酸、古洛糖醛酸、以及它们的改性物和混合物。
6.如权利要求5所述的组合物，其特征在于所述的改性纤维素是羧甲基纤维素。
7.如权利要求1所述的组合物，其特征在于所述的组合物不含研磨剂。
8.一种半导体晶片上非铁金属的抛光方法，它包括使含有非铁金属的晶片与抛光组合物接触，然后用抛光垫抛光该晶片，所述的抛光组合物含有0～25重量％氧化剂、0～3重量％研磨剂、0.05～5.0重量％非铁金属的抑制剂、0.01～15重量％非铁金属的络合剂、0.01～5重量％具有羧酸官能团的改性纤维素、0.01～5重量％丙烯酸和甲基丙烯酸的共聚物，以及余量的水，其中所述的络合剂选自乙酸、柠檬酸、乙酰乙酸乙酯、羟基乙酸、乳酸、苹果酸、草酸、水杨酸、二乙基二硫代氨基甲酸钠、琥珀酸、酒石酸、巯基乙酸、甘氨酸、丙氨酸、天冬氨酸、乙二胺、三甲基三胺、丙二酸、戊二酸、3-羟基丁酸、丙酸、邻苯二甲酸、间苯二甲酸、3一羟基水杨酸、3，5-二羟基水杨酸、五倍子酸、葡糖酸、焦儿茶酚、焦桔酚、单宁酸，包括它们的盐和混合物，丙烯酸与甲基丙烯酸的共聚物中的丙烯酸/甲基丙烯酸单体比为1∶9～9∶1，所述共聚物的重均分子量为1K～1000K。
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