CN103154168B - 研磨用组合物及研磨方法 - Google Patents
研磨用组合物及研磨方法 Download PDFInfo
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- CN103154168B CN103154168B CN201180038885.9A CN201180038885A CN103154168B CN 103154168 B CN103154168 B CN 103154168B CN 201180038885 A CN201180038885 A CN 201180038885A CN 103154168 B CN103154168 B CN 103154168B
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
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- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30625—With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
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- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
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Abstract
本发明的研磨用组合物含有水溶性聚合物、研磨促进剂及氧化剂。水溶性聚合物为具有150mgKOH/1g·固体以上的胺值的聚酰胺多胺聚合物。
Description
技术领域
本发明涉及在用于例如形成半导体器件的布线的研磨中使用的研磨用组合物。
背景技术
在形成半导体器件的布线时,首先,在具有沟槽的绝缘体层上依次形成阻隔层及导体层。然后,通过化学机械研磨至少去除位于沟槽外的导体层的部分(导体层的外侧部分)及位于沟槽外的阻隔层的部分(阻隔层的外侧部分)。用于该至少去除导体层的外侧部分及阻隔层的外侧部分的研磨通常分为第1研磨工序和第2研磨工序来进行。第1研磨工序中,为了露出阻隔层的上表面,去除导体层的外侧部分的一部分。在接下来的第2研磨工序中,为了露出绝缘体层并得到平坦的表面,至少去除导体层的外侧部分的剩余部分及阻隔层的外侧部分。
在这样的用于形成半导体器件的布线的研磨中使用的研磨用组合物通常包含酸等研磨促进剂及氧化剂、以及根据需要使用的研磨磨粒。另外,为了改善研磨后的研磨对象物的平坦性,也提出了使用进一步添加有水溶性聚合物的研磨用组成。例如专利文献1中公开了使用含有聚氧乙烯月桂基醚硫酸铵等阴离子表面活性剂、苯并三唑等保护膜形成剂、及聚氧乙烯烷基醚等非离子表面活性剂的研磨用组合物。专利文献2中公开了使用含有表卤代醇改性聚酰胺的研磨用组合物。另外,专利文献3中还公开了使用包含具有利用羧酸修饰过的氨基的化学修饰明胶的研磨用组合物。
但是,通过化学机械研磨形成半导体器件的布线时,尤其是导体层由铜或铜合金形成时,有时在形成的布线侧面产生不希望产生的不合适的凹陷。认为该布线侧面的凹陷主要是因位于与绝缘体层的边界附近的导体层的部分表面在研磨中腐蚀而导致的。即使使用上述现有的研磨用组合物也难以防止该布线侧面的凹陷的产生。
现有技术文献
专利文献
专利文献1:日本特开2008-41781号公报
专利文献2:日本特开2002-110595号公报
专利文献3:日本特开2008-244316号公报
发明内容
发明要解决的问题
因此,本发明的目的在于,提供可以在用于形成半导体器件的布线的研磨中更适宜地使用的研磨用组合物及使用其的研磨方法。
用于解决问题的方案
为了达成上述目的,本发明的一个实施方式提供一种含有水溶性聚合物、研磨促进剂及氧化剂的研磨用组合物。水溶性聚合物为具有150mgKOH/1g·固体以上的胺值的聚酰胺多胺聚合物。
水溶性聚合物优选包含下述通式(1)表示的化合物作为共聚单体。通式(1)中,R1及R3分别独立地表示氢原子、或者碳数1~4的无取代或取代的直链烷基,R2表示碳数1~4的无取代或取代的直链烷基。
(1)
通式(1)表示的化合物例如为戊二酸或琥珀酸。
水溶性聚合物优选含有在氮原子间连续的碳原子的数目为4以下的聚亚烷基多胺作为共聚单体。
研磨用组合物优选还含有具有三唑骨架的化合物。
本发明的其它实施方式提供一种研磨方法,其包括:使用上述实施方式中的研磨用组合物对具有铜或铜合金的研磨对象物的表面进行研磨。
发明的效果
根据本发明,可以提供能够在用于形成半导体器件的布线的研磨中更适宜地使用的研磨用组合物及使用其的研磨方法。
具体实施方式
以下对本发明的一个实施方式进行说明。
本实施方式的研磨用组合物通过将特定的水溶性聚合物、研磨促进剂及氧化剂与优选使用的金属防腐剂及磨粒一起在水中混合来制备。因此,研磨用组合物含有特定的水溶性聚合物、研磨促进剂及氧化剂,优选还含有金属防腐剂及磨粒。
通常,在形成半导体器件的布线时,首先在具有沟槽的绝缘体层上依次形成阻隔层及导体层。其后,通过化学机械研磨至少去除位于沟槽外的导体层的部分(导体层的外侧部分)及位于沟槽外的阻隔层的部分(阻隔层的外侧部分)。用于该至少去除导体层的外侧部分及阻隔层的外侧部分的研磨通常分为第1研磨工序和第2研磨工序来进行。第1研磨工序中,为了露出阻隔层的上表面,去除导体层的外侧部分的一部分。在接下来的第2研磨工序中,为了在露出绝缘体层的同时得到平坦的表面,至少去除导体层的外侧部分的剩余部分及阻隔层的外侧部分。本实施方式的研磨用组合物主要被用在这样的用于形成半导体器件的布线的研磨、特别是第2研磨工序的研磨中。即,研磨用组合物主要用于对具有导体层的研磨对象物的表面进行研磨并形成半导体器件的布线的用途。通过化学机械研磨形成半导体器件的布线的情况下,尤其是导体层由铜或铜合金形成时,有时在形成的布线的侧面产生不希望产生的不合适的凹陷,本实施方式的研磨用组合物能够抑制该布线侧面的凹陷的产生。因此,该研磨用组合物在导体层由铜或铜合金形成时特别有用。
(水溶性聚合物)
研磨用组合物中所含的水溶性聚合物发挥如下的作用:通过在研磨对象物的导体层表面形成保护膜,抑制在通过使用研磨用组合物的研磨而形成的布线侧面产生凹陷。作为发挥这样的作用的水溶性聚合物,使用聚酰胺多胺聚合物(polyamidepolyamine polymer)。
认为聚酰胺多胺聚合物以自身的氮原子作为吸附位置吸附在研磨对象物的导体层表面,形成保护膜,但在聚酰胺多胺聚合物的分子内存在氮原子密度高的地方。因此,聚酰胺多胺聚合物与被阳离子化的聚乙烯醇、被阳离子化的丙烯酸系树脂等其它水溶性聚合物相比,能在包含位于和绝缘体层的边界附近的导体层的部分在内的研磨对象物的导体层表面更可靠地形成保护膜。认为由此,位于和绝缘体层的边界附近的导体层的部分的表面不易在研磨中被腐蚀,其结果,能够抑制布线侧面的凹陷的发生。
水溶性聚合物的分子内的氮原子密度可以以胺值为指标来推断。本实施方式中,使用具有150mgKOH/1g·固体以上的胺值的聚酰胺多胺聚合物。使用胺值低于150mg KOH/1g·固体的聚酰胺多胺聚合物时,难以充分抑制在通过使用研磨用组合物的研磨而形成的布线的侧面产生凹陷。为了更强地抑制布线侧面的凹陷的产生,优选聚酰胺多胺聚合物的胺值为200mgKOH/1g·固体以上,更优选为250mg KOH/1g·固体以上,进一步优选为350mgKOH/1g·固体以上,最优选为450mgKOH/1g·固体以上。
另外,从磨粒的分散稳定性方面考虑,聚酰胺多胺聚合物的胺值优选为3000mgKOH/1g·固体以下,更优选为2000mgKOH/1g·固体以下,最优选为1000mgKOH/1g·固体以下。
水溶性聚合物的胺值是指,与中和单位重量的水溶性聚合物中所含的伯、仲及叔胺所必需的盐酸当量的氢氧化钾(KOH)的mg数。
水溶性聚合物的胺值例如可以如下测定。首先,在固体成分量1.0g的水溶性聚合物中加入水使其为100g。然后,向其中加入0.1当量的氢氧化钠水溶液,制作将pH调节为11.0的试样。然后,用0.5当量的盐酸滴定该试样,测定直至pH变为10所滴加的盐酸的量及直至pH变为5所滴加的盐酸的量。其后,可以由下式求出胺值。
胺值=((V5-V10)×F×0.5×56.1)/S
其中,V10:直至pH变为10所滴加的0.5当量盐酸的量(cc)
V5:直至pH变为5所滴加的0.5当量盐酸的量(cc)
F:滴定中使用的0.5当量盐酸的滴定度
S:水溶性聚合物的固体成分量(g)
0.5:滴定中使用的盐酸的当量浓度
56.1:氢氧化钾的分子量
聚酰胺多胺聚合物的制造方法公开在例如特许第3666442号公报及特许第4178500号公报中。具体而言,可以使用使多元酸和/或其低级烷基酯与聚亚烷基多胺反应而得到的聚酰胺多胺聚合物。
作为聚酰胺多胺聚合物的制造中能用作共聚单体的多元酸的例子,可列举出以下的通式(1)表示的化合物。
(1)
通式(1)中,R1及R3分别独立地表示氢原子、或者碳数1~4的无取代或取代的直链烷基,R2表示碳数1~4的无取代或取代的直链烷基。R1及R3为取代的直链烷基时,侧链的取代基可以为甲基、乙基、羟基、氨基、羧基、苯基、乙酰基、羟甲基及羟乙基的任一种。
作为通式(1)表示的多元酸的具体例,可列举出:草酸、丙二酸、琥珀酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸等脂肪族饱和二元酸类,马来酸、富马酸、衣康酸、烯基琥珀酸等脂肪族不饱和多元酸类,二醇酸、乳酸、羟基丙酸、α-羟基丁酸、β-羟基丁酸、α-羟基异丁酸、2-羟基丙酸、α-羟基异己酸、β,β,β-三氯乳酸、甘油酸、苹果酸、α-甲基苹果酸、酒石酸、柠檬酸、羟丙二酸、四羟基琥珀酸、β-羟基戊二酸、羟基丙二酸、葡糖酸等羟基多元酸类,二聚酸、聚合蓖麻油脂肪酸等聚合脂肪酸类,偏苯三酸等三元酸类。可以组合这些多元酸中的多种使用。
其中特别优选的多元酸为脂肪族饱和二元酸,特别优选为草酸、丙二酸、琥珀酸、戊二酸及己二酸,最优选为琥珀酸。
作为多元酸的低级烷基酯的例子,可列举出通式(1)表示的多元酸的甲酯、乙酯、丙酯及丁酯。
作为在聚酰胺多胺聚合物的制造中能用作共聚单体的聚亚烷基多胺的例子,可列举出具有2个以上能形成酰胺键的氨基的化合物。作为这样的化合物的具体例,可列举出:二乙烯三胺、三乙烯四胺、四乙烯五胺、亚氨基二丙胺、二甲氨基乙胺、二甲氨基丙胺、二乙氨基乙胺、二乙氨基丙胺、二丁氨基丙胺、乙氨基乙胺、1,2-二氨基丙烷、1,3-二氨基丙烷、1,4-二氨基丁烷、甲氨基丙胺、二乙烯三胺、三乙烯四胺、四乙烯五胺、五乙烯六胺、二丙烯三胺、三丙烯四胺、2-羟基氨基丙胺、甲基双-(3-氨丙基)胺、二甲氨基乙氧基丙胺、1,2-双-(3-氨基丙氧基)-乙烷、1,3-双-(3-氨基丙氧基)-2,2-二甲基丙烷、α,ω-双-(3-氨基丙氧基)-聚乙二醇醚、亚氨基二丙胺、甲基亚氨基二丙胺、月桂基氨基丙胺、二乙醇氨基丙胺、N-氨乙基哌啶、N-氨乙基哌可啉、N-氨乙基吗啉、N-氨丙基哌啶(piperindine)、N-氨丙基-2-哌可啉、N-氨丙基-4-哌可啉、N-氨丙基-4-吗啉及N-氨丙基吗啉。
在聚亚烷基多胺的分子内的氮原子间连续的碳原子的数目优选为4以下,更优选为3以下。由于乙烯二胺、二乙烯三胺、三乙烯四胺、四乙烯五胺、五乙烯六胺及甲基二(3-氨丙基)胺中在氮原子间连续的碳原子的数目均2,因此可以优选使用。
聚亚烷基多胺与多元酸和/或其低级烷基酯的反应摩尔比优选为0.1/1~10/1,更优选为0.2/1~8/1,进一步优选为0.5/1~5/1。聚亚烷基多胺的比率越高,得到的聚酰胺多胺聚合物越容易在研磨对象物的导体层表面形成保护膜,能够进一步抑制在通过使用研磨用组合物的研磨而形成的布线的侧面产生凹陷。另外,多元酸和/或其低级烷基酯的比率越高,越能够期待磨粒的稳定性的提高。
聚酰胺多胺聚合物可以用尿素、表卤代醇等进行改性。
研磨用组合物中的水溶性聚合物的重均分子量根据研磨用组合物中所含的研磨促进剂的量、氧化剂的量等适当设定,通常优选为100以上,更优选为200以上,进一步优选为300以上。随着水溶性聚合物的重均分子量变大,能够进一步抑制在通过使用研磨用组合物的研磨而形成的布线的侧面产生凹陷。
研磨用组合物中的水溶性聚合物的重均分子量还优选为20,000以下,更优选为10,000以下,进一步优选为5,000以下。随着水溶性聚合物的重均分子量变小,能够抑制研磨用组合物的材料成本,并且还能够抑制在使用研磨用组合物进行研磨后的研磨对象物的表面产生碟形坑(dishing)。
需要说明的是,水溶性聚合物的重均分子量的测定可以利用GPC-MALS法这样的一般的方法来进行。为相对低分子量的水溶性聚合物时,也可以利用NMR法来测定重均分子量。
研磨用组合物中的水溶性聚合物的含量也根据研磨用组合物中所含的研磨促进剂的量、氧化剂的量等来适当设定,通常优选为0.001g/L以上,更优选为0.01g/L以上,进一步优选为0.05g/L以上。随着水溶性聚合物的含量变多,能够进一步抑制在通过使用研磨用组合物的研磨而形成的布线的侧面产生凹陷。
研磨用组合物中的水溶性聚合物的含量还优选为1g/L以下,更优选为0.5g/L以下,进一步优选为0.3g/L以下,最优选为0.1g/L以下。随着水溶性聚合物的含量变少,能够抑制研磨用组合物的材料成本,并且还能够抑制在使用研磨用组合物进行研磨后的研磨对象物的表面产生碟形坑。
(研磨促进剂)
研磨用组合物中所含的研磨促进剂具有对研磨对象物的表面进行化学性蚀刻的作用,使利用研磨用组合物的研磨对象物的研磨速度提高。
可使用的研磨促进剂为例如无机酸、有机酸、氨基酸及螯合剂。
作为无机酸的具体例,可列举出硫酸、硝酸、硼酸、碳酸、次亚磷酸、亚磷酸及磷酸。
作为有机酸的具体例,可列举出:甲酸、乙酸、丙酸、丁酸、戊酸、2-甲基丁酸、正己酸、3,3-二甲基丁酸、2-乙基丁酸、4-甲基戊酸、正庚酸、2-甲基己酸、正辛酸、2-乙基己酸、苯甲酸、二醇酸、水杨酸、甘油酸、草酸、丙二酸、琥珀酸、戊二酸、己二酸、庚二酸、马来酸、邻苯二甲酸、苹果酸、酒石酸、柠檬酸及乳酸。也可以使用甲磺酸、乙磺酸及羟乙基磺酸等有机硫酸。
也可以代替无机酸或有机酸、或者与无机酸或有机酸组合使用无机酸或有机酸的铵盐、碱金属盐等盐。为弱酸和强碱、强酸和弱碱、或弱酸和弱碱的组合时,可以期待pH的缓冲作用。
作为氨基酸的具体例,可列举出:甘氨酸、α-丙氨酸、β-丙氨酸、N-甲基甘氨酸、N,N-二甲基甘氨酸、2-氨基丁酸、戊氨酸、缬氨酸、亮氨酸、正亮氨酸、异亮氨酸、苯基丙氨酸、脯氨酸、肌氨酸、鸟氨酸、赖氨酸、牛磺酸、丝氨酸、苏氨酸、高丝氨酸、酪氨酸、N,N-二(羟乙基)甘氨酸(bicine)、三(羟甲基)甲基甘氨酸(tricine)、3,5-二碘-酪氨酸、β-(3,4-二羟苯基)-丙氨酸、甲状腺氨酸、4-羟基-脯氨酸、半胱氨酸、蛋氨酸、乙硫氨酸、羊毛硫氨酸、胱硫酸、胱氨酸、磺基丙氨酸、天冬氨酸、谷氨酸、S-(羧甲基)-半胱氨酸、4-氨基丁酸、天冬酰胺、谷氨酰胺、重氮丝氨酸、精氨酸、刀豆氨酸、瓜氨酸、δ-羟基-赖氨酸、肌氨酸、组氨酸、1-甲基-组氨酸、3-甲基-组氨酸及色氨酸。其中,优选甘氨酸、N-甲基甘氨酸、N,N-二甲基甘氨酸、α-丙氨酸、β-丙氨酸、N,N-二(羟乙基)甘氨酸及三(羟甲基)甲基甘氨酸,特别优选为甘氨酸。
作为螯合剂的具体例,可列举出:次氮基三乙酸、二乙烯三胺五醋酸、乙烯二胺四醋酸、N,N,N-三亚甲基亚磷酸、乙烯二胺-N,N,N’,N’-四亚甲基磺酸、反式环己烷二胺四醋酸、1,2-二氨基丙烷四醋酸、二醇醚二胺四醋酸、乙烯二胺邻羟苯基醋酸、乙烯二胺二琥珀酸(SS体)、N-(2-羧化乙基)-L-天冬氨酸、β-丙氨酸二醋酸、2-膦酸丁烷-1,2,4-三羧酸、1-羟基乙叉基-1,1-二亚磷酸、N,N’-双(2-羟基苄基)乙烯二胺-N,N’-二醋酸、及1,2-二羟基苯-4,6-二磺酸。
研磨用组合物中的研磨促进剂的含量优选为0.01g/L以上,更优选为0.1g/L以上,进一步优选为1g/L以上。随着研磨促进剂的含量变多,利用研磨用组合物的研磨对象物的研磨速度提高。
研磨用组合物中的研磨促进剂的含量还优选为50g/L以下,更优选为30g/L以下,进一步优选为15g/L以下。随着研磨促进剂的含量变少,能够进一步抑制由研磨促进剂引起的研磨对象物表面的过度蚀刻。
(氧化剂)
研磨用组合物中所含的氧化剂具有将研磨对象物的表面氧化的作用,使利用研磨用组合物的研磨对象物的研磨速度提高。
可以使用的氧化剂为例如过氧化物。作为过氧化物的具体例,可列举出:过氧化氢、过醋酸、过碳酸盐、过氧化尿素及高氯酸、以及过硫酸钠、过硫酸钾、过硫酸铵等过硫酸盐。其中尤其优选过硫酸盐及过氧化氢,特别优选为过氧化氢。
研磨用组合物中的氧化剂的含量优选为0.1g/L以上,更优选为1g/L以上、进一步优选为3g/L以上。随着氧化剂的含量变多,利用研磨用组合物的研磨对象物的研磨速度提高。
研磨用组合物中的氧化剂的含量还优选为200g/L以下,更优选为100g/L以下,进一步优选为40g/L以下。随着氧化剂的含量变少,能够抑制研磨用组合物的材料成本,并且还能够减轻研磨使用后的研磨用组合物的处理、即废液处理的负荷。另外,也能够减少由氧化剂引起研磨对象物表面过度氧化的担心。
(金属防腐剂)
在研磨用组合物中加入金属防腐剂时,能够进一步抑制通过使用研磨用组合物的研磨而形成的布线的侧面产生凹陷。另外,还能够进一步抑制在使用研磨用组合物进行研磨后的研磨对象物的表面产生碟形坑。
可以使用的金属防腐剂没有特别限定,优选为杂环式化合物或表面活性剂。杂环式化合物中的杂环的个数没有特别限定。另外,杂环式化合物可以是单环化合物,也可以是具有稠环的多环化合物。
作为能用作保护膜形成剂的杂环化合物的具体例,包括吡咯、吡唑、咪唑、三唑、四唑、吡啶、吡嗪、哒嗪、4-氮茚(Pyrindine)、中氮茚、吲哚、异吲哚、吲唑、嘌呤、喹嗪、喹啉、异喹啉、萘啶、酞嗪、喹喔啉、喹唑啉、噌啉、布替利嗪、噻唑、异噻唑、噁唑、异噁唑、呋咱等含氮杂环化合物。
吡唑的例子包括:1H-吡唑、4-硝基-3-吡唑羧酸、3,5-吡唑羧酸、3-氨基-5-苯基吡唑、5-氨基-3-苯基吡唑、3,4,5-三溴吡唑、3-氨基吡唑、3,5-二甲基吡唑、3,5-二甲基-1-羟甲基吡唑、3-甲基吡唑、1-甲基吡唑、3-氨基-5-甲基吡唑、4-氨基-吡唑并[3,4-d]嘧啶、别嘌醇、4-氯-1H-吡唑并[3,4-D]嘧啶、3,4-二羟基-6-甲基吡唑并(3,4-B)-吡啶、及6-甲基-1H-吡唑并[3,4-b]吡啶-3-胺。
咪唑的例子包括:咪唑、1-甲基咪唑、2-甲基咪唑、4-甲基咪唑、1,2-二甲基吡唑、2-乙基-4-甲基咪唑、2-异丙基咪唑、苯并咪唑、5,6-二甲基苯并咪唑、2-氨基苯并咪唑、2-氯苯并咪唑、2-甲基苯并咪唑、2-(1-羟乙基)苯并咪唑、2-羟基苯并咪唑、2-苯基苯并咪唑、2,5-二甲基苯并咪唑、5-甲基苯并咪唑、5-硝基苯并咪唑、及1H-嘌呤。
三唑的例子包括:1,2,3-三唑、1,2,4-三唑、1-甲基-1,2,4-三唑、1H-1,2,4-三唑-3-羧酸甲酯、1,2,4-三唑-3-羧酸、1,2,4-三唑-3-羧酸甲酯、1H-1,2,4-三唑-3-硫醇、3,5-二氨基-1H-1,2,4-三唑、3-氨基-1,2,4-三唑-5-硫醇、3-氨基-1H-1,2,4-三唑、3-氨基-5-苄基-4H-1,2,4-三唑、3-氨基-5-甲基-4H-1,2,4-三唑、3-硝基-1,2,4-三唑、3-溴-5-硝基-1,2,4-三唑、4-(1,2,4-三唑-1-基)苯酚、4-氨基-1,2,4-三唑、4-氨基-3,5-二丙基-4H-1,2,4-三唑、4-氨基-3,5-二甲基-4H-1,2,4-三唑、4-氨基-3,5-二庚基(ジペプチル)-4H-1,2,4-三唑、5-甲基-1,2,4-三唑-3,4-二胺、1H-苯并三唑、1-羟基苯并三唑、1-氨基苯并三唑、1-羧基苯并三唑、5-氯-1H-苯并三唑、5-硝基-1H-苯并三唑、5-羧基-1H-苯并三唑、5-甲基-1H-苯并三唑、5,6-二甲基-1H-苯并三唑、1-(1’,2’-二羧乙基)苯并三唑、1-[N,N-双(羟乙基)氨基甲基]苯并三唑、1-[N,N-双(羟乙基)氨甲基]-5-甲基苯并三唑、及1-[N,N-双(羟乙基)氨甲基]-4-甲基苯并三唑。
四唑的例子包括1H-四唑、5-甲基四唑、5-氨基四唑、及5-苯基四唑。
吲唑的例子包括:1H-吲唑、5-氨基-1H-吲唑、5-硝基-1H-吲唑、5-羟基-1H-吲唑、6-氨基-1H-吲唑、6-硝基-1H-吲唑、6-羟基-1H-吲唑、及3-羧基-5-甲基-1H-吲唑。
吲哚的例子包括:1H-吲哚、1-甲基-1H-吲哚、2-甲基-1H-吲哚、3-甲基-1H-吲哚、4-甲基-1H-吲哚、5-甲基-1H-吲哚、6-甲基-1H-吲哚、7-甲基-1H-吲哚、4-氨基-1H-吲哚、5-氨基-1H-吲哚、6-氨基-1H-吲哚、7-氨基-1H-吲哚、4-羟基-1H-吲哚、5-羟基-1H-吲哚、6-羟基-1H-吲哚、7-羟基-1H-吲哚、4-甲氧基-1H-吲哚、5-甲氧基-1H-吲哚、6-甲氧基-1H-吲哚、7-甲氧基-1H-吲哚、4-氯-1H-吲哚、5-氯-1H-吲哚、6-氯-1H-吲哚、7-氯-1H-吲哚、4-羧基-1H-吲哚、5-羧基-1H-吲哚、6-羧基-1H-吲哚、7-羧基-1H-吲哚、4-硝基-1H-吲哚、5-硝基-1H-吲哚、6-硝基-1H-吲哚、7-硝基-1H-吲哚、4-腈基-1H-吲哚、5-腈基-1H-吲哚、6-腈基-1H-吲哚、7-腈基-1H-吲哚、2,5-二甲基-1H-吲哚、1,2-二甲基-1H-吲哚、1,3-二甲基-1H-吲哚、2,3-二甲基-1H-吲哚、5-氨基-2,3-二甲基-1H-吲哚、7-乙基-1H-吲哚、5-(氨甲基)吲哚、2-甲基-5-氨基-1H-吲哚、3-羟甲基-1H-吲哚、6-异丙基-1H-吲哚、及5-氯-2-甲基-1H-吲哚。
其中特别优选的杂环化合物为具有三唑骨架的化合物,尤其优选1H-苯并三唑、5-甲基-1H-苯并三唑、5,6-二甲基-1H-苯并三唑、1-[N,N-双(羟乙基)氨甲基]-5-甲基苯并三唑、1-[N,N-双(羟乙基)氨甲基]-4-甲基苯并三唑、1,2,3-三唑、及1,2,4-三唑。这些杂环化合物对研磨对象物表面的化学或物理吸附力高,因此,在研磨对象物表面形成更牢固的保护膜。这在提高使用研磨用组合物进行研磨后的研磨对象物的表面的平坦性方面是有利的。
用作保护膜形成剂的表面活性剂可以为阴离子性表面活性剂、阳离子性表面活性剂、两性表面活性剂、及非离子性表面活性剂中的任一种。
阴离子性表面活性剂的例子包括:聚氧乙烯烷基醚醋酸、聚氧乙烯烷基硫酸酯、烷基硫酸酯、聚氧乙烯烷基硫酸、烷基硫酸、烷基苯磺酸、烷基磷酸酯、聚氧乙烯烷基磷酸酯、聚氧乙烯磺基琥珀酸、烷基磺基琥珀酸、烷基萘磺酸、烷基二苯基醚二磺酸、及它们的盐。
阳离子性表面活性剂的例子包括:烷基三甲基铵盐、烷基二甲基铵盐、烷基苄基二甲基铵盐、及烷基胺盐。
两性表面活性剂的例子包括:烷基甜菜碱及烷基胺氧化物。
非离子性表面活性剂的例子包括:聚氧乙烯烷基醚、聚氧亚烷基烷基醚、山梨糖醇酐脂肪酸酯、甘油脂肪酸酯、聚氧乙烯脂肪酸酯、聚氧乙烯烷基胺、及烷基烷醇酰胺。
其中特别优选的表面活性剂为聚氧乙烯烷基醚醋酸、聚氧乙烯烷基醚硫酸盐、烷基醚硫酸盐、烷基苯磺酸盐、及聚氧乙烯烷基醚。这些表面活性剂对研磨对象物表面的化学或物理吸附力高,因此,在研磨对象物表面形成更牢固的保护膜。这在提高使用研磨用组合物进行研磨后的研磨对象物的表面的平坦性方面是有利的。
研磨用组合物中的金属防腐剂的含量优选为0.001g/L以上,更优选为0.005g/L以上,进一步优选为0.01g/L以上。随着金属防腐剂的含量变多,使用研磨用组合物进行研磨后的研磨对象物的表面的平坦性进一步提高。
研磨用组合物中的金属防腐剂的含量还优选为10g/L以下,更优选为5g/L以下,进一步优选为1g/L以下。随着金属防腐剂的含量变少,利用研磨用组合物的研磨对象物的研磨速度进一步提高。
(磨粒)
研磨用组合物中任意包含的磨粒具有对研磨对象物进行机械研磨的作用,使利用研磨用组合物的研磨对象物的研磨速度提高。
所使用的磨粒可以为无机颗粒、有机颗粒、及有机无机复合颗粒的任一种。作为无机颗粒的具体例,可列举出例如:由二氧化硅、氧化铝、氧化铈、氧化钛等金属氧化物形成的颗粒、以及氮化硅颗粒、碳化硅颗粒及氮化硼颗粒。其中,优选二氧化硅,特别优选胶态二氧化硅。作为有机颗粒的具体例,可列举出例如聚甲基丙烯酸甲酯(PMMA)颗粒。
所使用的磨粒的平均一次粒径优选为5nm以上,更优选为7nm以上,进一步优选为10nm以上。随着磨粒的平均一次粒径变大,利用研磨用组合物的研磨对象物的研磨速度提高。
使用的磨粒的平均一次粒径还优选为100nm以下,更优选为60nm以下,进一步优选为40nm以下。随着磨粒的平均一次粒径变小,能够抑制使用研磨用组合物进行研磨后的研磨对象物的表面产生碟形坑。需要说明的是,磨粒的平均一次粒径的值基于例如用BET法测定的磨粒的比表面积来计算。
研磨用组合物中的磨粒的含量优选为0.005质量%以上,更优选为0.01质量%以上,进一步优选为0.05质量%以上。随着磨粒的含量变多,利用研磨用组合物的研磨对象物的研磨速度提高。
研磨用组合物中的磨粒的含量还优选为5质量%以下,更优选为1质量%以下,进一步优选为0.5质量%以下。随着磨粒的含量变少,能够抑制研磨用组合物的材料成本,并且还能够抑制使用研磨用组合物进行研磨后的研磨对象物的表面产生碟形坑。
(研磨用组合物的pH)
研磨用组合物的pH优选为3以上,更优选为5以上。随着研磨用组合物的pH变大,能够减少发生由研磨用组合物引起的研磨对象物表面的过度蚀刻的担心。
研磨用组合物的pH还优选为9以下,更优选为8以下。随着研磨用组合物的pH变小,能够进一步抑制通过使用研磨用组合物的研磨而形成的布线的侧面产生凹陷。
根据本实施方式,能获得以下的优点。
本实施方式的研磨用组合物含有具有150mg KOH/1g·固体以上的胺值的聚酰胺多胺聚合物。因此,通过该聚酰胺多胺聚合物的作用,能够抑制通过使用研磨用组合物的研磨而形成的布线的侧面产生凹陷。因此,本实施方式的研磨用组合物能够在用于形成半导体器件的布线的研磨中适宜使用。
前述实施方式可以如下进行变更。
·前述实施方式的研磨用组合物可以含有两种以上的研磨促进剂。
·前述实施方式的研磨用组合物可以含有两种以上的水溶性聚合物。这时,对于一部分水溶性聚合物,并不是必须为具有150mgKOH/1g·固体以上的胺值的聚酰胺多胺聚合物。作为这样的水溶性聚合物的具体例,可列举出:海藻酸、果胶酸、羧甲基纤维素、可得然胶(curdlan)、普鲁兰多糖等多糖类,多羧酸及其盐,聚乙烯醇、聚乙烯基吡咯烷酮、聚丙烯醛等乙烯基系聚合物,聚甘油、及聚甘油酯。在研磨用组合物中添加聚酰胺多胺聚合物以外的水溶性聚合物时,在该水溶性聚合物吸附在磨粒的表面或研磨对象物的表面从而能够控制利用研磨用组合物的研磨对象物的研磨速度、并且能够使研磨中产生的不溶性的成分在研磨用组合物中稳定化的方面有利。
·前述实施方式的研磨用组合物可以含有两种以上的氧化剂。
·前述实施方式的研磨用组合物可以含有两种以上的磨粒。
·前述实施方式的研磨用组合物可以含有两种以上的金属防腐剂。这时,例如,可以使用两种以上的杂环式化合物,也可以使用两种以上的表面活性剂。或者,也可以组合杂环式化合物和表面活性剂使用。组合杂环式化合物和表面活性剂使用时、即研磨用组合物含有杂环式化合物及表面活性剂时,容易兼顾利用研磨用组合物的研磨对象物的研磨速度的提高和使用研磨用组合物进行研磨后的研磨对象物的表面的平坦性的提高。
·前述实施方式的研磨用组合物可以根据需要进一步含有防腐剂及防霉剂这样的公知的添加剂。作为防腐剂及防霉剂的具体例,可列举出:2-甲基-4-异噻唑啉-3-酮、5-氯-2-甲基-4-异噻唑啉-3-酮等异噻唑啉系防腐剂、对羟基苯甲酸酯类、苯氧基乙醇等。
·前述实施方式的研磨用组合物可以为单组分型,也可以为以双组分型为代表的多组分型。
·前述实施方式的研磨用组合物也可以通过将研磨用组合物的原液用水等稀释液稀释至例如10倍以上来制备。
·前述实施方式的研磨用组合物也可以在用于形成半导体器件的布线的研磨以外的用途中使用。
以下,对本发明的实施例及比较例进行说明。
将水溶性聚合物、研磨促进剂、氧化剂、金属防腐剂及磨粒在水中混合,制备实施例1~28及比较例1~12的研磨用组合物。将研磨促进剂、氧化剂、金属防腐剂及磨粒在水中混合,制备比较例13的研磨用组合物。将各例的研磨用组合物中的水溶性聚合物的详细情况示于表1。需要说明的是,虽然表1中没有示出,但实施例1~28及比较例1~13的研磨用组合物均含有10g/L的作为研磨促进剂的甘氨酸、15g/L的作为氧化剂的过氧化氢、0.1质量%的作为磨粒的平均一次粒径为30nm的胶态二氧化硅。进而,实施例1~28及比较例1~13的研磨用组合物均含有0.08g/L的作为金属防腐剂的1-[N,N-双(羟乙基)氨甲基]-5-甲基苯并三唑和1-[N,N-双(羟乙基)氨甲基]-5-甲基苯并三唑的混合物、0.1g/L的月桂基醚硫酸铵、0.5g/L的聚氧乙烯烷基醚,其中的几个还进一步含有追加的金属防腐剂。一部分研磨用组合物中所含的追加的金属防腐剂的详细情况也示于表1。
[表1]
<布线侧面的凹陷>
使用各例的研磨用组合物,在表2所述的第1研磨条件下对铜图案晶圆(ATDF754掩模、研磨前的铜膜厚700nm、沟槽深度300nm)的表面进行研磨,直至铜膜厚变为250nm。其后,使用相同的研磨用组合物在表3所述的第2研磨条件下对研磨后的铜图案晶圆的表面进行研磨,直至阻隔膜露出。使用复查扫描电子显微镜(Review SEM)(Hitachi High-TechnologiesCorporation制造的RS-4000)观察如上进行了2阶段的研磨后的铜图案晶圆的表面,确认在0.18μm宽的布线和0.18μm宽的绝缘膜交替排列的区域及100μm宽的布线和100μm宽的绝缘膜交替排列的区域有无布线侧面凹陷。然后,在任意区域均没有确认到布线侧面的凹陷的情况评价为○○○(最优)、在仅任意一个区域确认到宽不足5nm的布线侧面的凹陷的情况评价为○○(优)、在两个区域均确认确认到宽不足5nm的布线侧面的凹陷的情况评价为○(良)、在至少任一个区域确认到宽为5nm以上且不足50nm的布线侧面的凹陷的情况评价为×(稍不良)、在至少任一个区域确认到50nm以上宽的凹陷的情况评价为××(不良)。将该评价结果示于表4的“布线侧面的凹陷”一栏。
<表面粗糙>
使用各例的研磨用组合物,在表2所述的第1研磨条件下对铜图案晶圆(ATDF754掩模、研磨前的铜膜厚700nm、沟槽深度300nm)的表面进行研磨,直至铜膜厚变为250nm。其后,使用相同的研磨用组合物,在表3所述的第2研磨条件下对研磨后的铜图案晶圆的表面进行研磨,直至阻隔膜露出。使用SIINanoTechnology Inc.制造的扫描型探针显微镜“S-image”测定如上进行了2阶段的研磨后的铜图案晶圆的、100μm宽的孤立布线部的中央附近的表面粗糙度Ra。该表面粗糙度Ra的测定使用Si探针以DFM模式进行,在1μm见方的区域内以纵横各256点、0.5Hz的扫描速度进行。测得的Ra的值不足1.0nm的情况评价为○○○(优)、为1.0nm以上的情况评价为○○(良)、为1.5nm以上且不足2.0nm的情况评价为○(合格)、为2.0nm以上的情况评价为×(不良)。将该评价结果示于表4的“表面粗糙”一栏。
<研磨速度>
将使用各例的研磨用组合物在表2所述的第1研磨条件及表3所述的第2研磨条件下对覆铜晶圆的表面进行60秒研磨时的第1条件及第2条件各自的研磨速度示于表4的“研磨速度”一栏。研磨速度的值由使用株式会社日立国际电气制造的薄层电阻测定器“VR-120SD/8”测定的研磨前后的覆铜晶圆的厚度之差除以研磨时间而求出。毋庸置疑,优选研磨速度的值较大,但在第1研磨条件下为400nm/分钟以上、在第2研磨条件下为200nm/分钟以上时,是实用的水平。
<碟形坑>
使用各例的研磨用组合物,在表2所述的第1研磨条件下对铜图案晶圆(ATDF754掩模、研磨前的铜膜厚700nm、沟槽深度300nm)的表面进行研磨,直至铜剩余膜变为250nm。其后,使用相同的研磨用组合物,在表3所述的第2研磨条件下对研磨后的铜图案晶圆表面进行研磨,直至阻隔膜露出。在如上进行了2阶段的研磨后的铜图案晶圆的9μm宽的布线和1μm宽的绝缘膜交替排列的第1区域及5μm宽的布线和1μm宽的绝缘膜交替排列的第2区域,使用Hitachi Construction Machinery Co.,Ltd.制造的ワイドエリアAFM“WA-1300”测定碟形坑量(碟形坑深度)。将该测定结果示于表5及表6的“碟形坑”一栏。测定的碟形坑量的值在第1研磨条件1的情况下为200nm以下、在第2研磨条件的情况下为120nm以下时,是实用的水平。
[表2]
[表3]
[表4]
Claims (6)
1.一种研磨用组合物,其为含有水溶性聚合物、研磨促进剂、磨粒、金属防腐剂及氧化剂的研磨用组合物,所述水溶性聚合物为具有150mgKOH/1g·固体以上的胺值的聚酰胺多胺聚合物。
2.根据权利要求1所述的研磨用组合物,其中,所述水溶性聚合物含有下述通式(1)表示的化合物作为共聚单体,通式(1)中,R1及R3分别独立地表示氢原子、或者碳数1~4的无取代或取代的直链烷基,R2表示碳数1~4的无取代或取代的直链烷基,
3.根据权利要求2所述的研磨用组合物,其中,通式(1)表示的所述化合物为戊二酸或琥珀酸。
4.根据权利要求1~3中任一项所述的研磨用组合物,其中,所述水溶性聚合物包含在氮原子间连续的碳原子的数目为4以下的聚亚烷基多胺作为共聚单体。
5.根据权利要求1~3中任一项所述的研磨用组合物,其中,所述金属防腐剂为具有三唑骨架的化合物。
6.一种研磨方法,其使用权利要求1~5中任一项所述的研磨用组合物对具有铜或铜合金的研磨对象物的表面进行研磨。
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JP5544244B2 (ja) | 2014-07-09 |
KR20130094817A (ko) | 2013-08-26 |
CN103154168A (zh) | 2013-06-12 |
EP2605270A1 (en) | 2013-06-19 |
JP2012038960A (ja) | 2012-02-23 |
WO2012020672A1 (ja) | 2012-02-16 |
TWI506128B (zh) | 2015-11-01 |
KR101811905B1 (ko) | 2017-12-22 |
US20130203254A1 (en) | 2013-08-08 |
US9117761B2 (en) | 2015-08-25 |
TW201211220A (en) | 2012-03-16 |
EP2605270A4 (en) | 2017-12-06 |
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