CN103155112B - 研磨液及使用该研磨液的基板的研磨方法 - Google Patents
研磨液及使用该研磨液的基板的研磨方法 Download PDFInfo
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- CN103155112B CN103155112B CN201180048658.4A CN201180048658A CN103155112B CN 103155112 B CN103155112 B CN 103155112B CN 201180048658 A CN201180048658 A CN 201180048658A CN 103155112 B CN103155112 B CN 103155112B
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- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
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- H01L21/3105—After-treatment
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Abstract
一种研磨液,其包含氧化铈粒子、有机酸A、具有羧酸基或羧酸盐基的高分子化合物B以及水,其中,有机酸A具有从‑COOM基、‑Ph‑OM基、‑SO3M基以及‑PO3M2基所组成的组中选择的至少一种基团,有机酸A的pKa小于9,有机酸A的含量相对于研磨液总质量为0.001~1质量%,高分子化合物B的含量相对于研磨液总质量为0.01~0.50质量%,所述研磨液的pH为4.0以上7.0以下。
Description
技术领域
本发明涉及研磨液及使用该研磨液的基板的研磨方法。更详细而言,本发明涉及在作为半导体元件制造技术的、基板表面的平坦化工序,特别是层间绝缘膜、BPSG膜(掺杂了硼、磷的二氧化硅膜)的平坦化工序,浅沟槽隔离(STI)的形成工序等中使用的研磨液及使用该研磨液的基板的研磨方法。
背景技术
在目前的ULSI半导体元件制造工序中,对用于使半导体元件高密度、微细化的加工技术进行了研究开发。作为该加工技术之一的CMP(Chemicalmechanical polishing:化学机械研磨)技术,逐渐成为在半导体元件制造工序中进行层间绝缘膜的平坦化、STI形成、插塞以及嵌入式金属线路形成等时所必须的技术。
以前,在半导体元件制造工序中,氧化硅膜等无机绝缘膜通过等离子体-CVD(化学气相生长)、低压-CVD(化学气相生长)等方法而形成。作为用于使该无机绝缘膜平坦化的化学机械研磨液,通常研究的是使用气相二氧化硅系研磨液。气相二氧化硅系研磨液可通过调整配合了粒子的浆料的pH而制造,该粒子是利用热分解四氯化硅等方法使颗粒生长而得到的。然而这样的气相二氧化硅系研磨液存在研磨速度低这样的技术问题。
另外,在设计标准0.25μm以后的代中,在集成电路内的元件隔离中可使用STI。在STI中,为了清除在基板上成膜的多余氧化硅膜而使用CMP技术。在这种情况下,为了使研磨在任意深度停止,可在氧化硅膜下形成研磨速度低的停止膜。停止膜可使用氮化硅膜等。为了高效率地清除多余的氧化硅膜,同时充分地抑制其之后的研磨进行,希望氧化硅膜与停止膜的研磨速度比较大。然而,对于以前的胶体二氧化硅系研磨液而言,氧化硅膜与停止膜的研磨速度比较小,为3左右,作为STI用不具有耐用的特性。
另一方面,作为针对光掩模、透镜等玻璃表面的研磨液,使用含有氧化铈粒子的氧化铈研磨液。氧化铈粒子与二氧化硅粒子、氧化铝粒子相比硬度更低,在研磨时不易在研磨表面产生损伤,因此对抛光镜面研磨有用。另外,氧化铈研磨液与气相二氧化硅系、胶体二氧化硅系等二氧化硅研磨液相比,具有研磨速度快的优点。
作为氧化铈研磨液,在下述专利文献1中记载了使用高纯度氧化铈研磨颗粒的半导体用CMP研磨液。另外,在下述专利文献2中记载了为了控制氧化铈研磨液的研磨速度、提高总体平坦性而加入添加剂的技术。
现有技术文献
专利文献
专利文献1:日本特开平10-106994号公报
专利文献2:日本特许3278532号公报
发明内容
发明要解决的问题
然而,伴随着线路、STI的设计标准的微细化进展,对于上述的氧化铈研磨液要求进一步提高平坦性(例如减少绝缘膜的碟陷(dishing)量)。另外,半导体器件的生产也要求进一步提高精度,例如,要求沟槽密度不同部分的绝缘膜的残膜厚差小、停止膜的过剩研磨量少。进一步,同时研磨工艺的尤度大,在精度高的半导体器件生产中也重要。
本发明是鉴于上述实情而作出的发明,目的在于提供一种研磨液以及使用该研磨液的基板的研磨方法,该研磨液在研磨形成于基板表面上的被研磨膜的CMP技术中,可以提高被研磨膜的研磨速度,并能够进一步提高研磨后的平坦性。
解决问题的方法
本发明提供一种研磨液,其是包含氧化铈粒子、有机酸A、具有羧酸基或羧酸盐基的高分子化合物B以及水的CMP用研磨液,其中,有机酸A具有从-COOM基、-Ph-OM基、-SO3M基以及-PO3M2基(式中,M是从H、NH4、Na以及K中选择的任一种,Ph表示可以具有也可以不具有取代基的苯基)所组成的组中选择的至少一种基团,有机酸A的pKa小于9,有机酸A的含量相对于研磨液总质量为0.001~1质量%,高分子化合物B的含量相对于研磨液总质量为0.01~0.50质量%,该研磨液的pH为4.0以上7.0以下。
本发明的研磨液,在研磨形成于基板表面上的被研磨膜(例如层间绝缘膜、BPSG膜、STI膜)的CMP技术中,可以提高被研磨膜的研磨速度且能提高研磨后的平坦性。
本发明的研磨液,可以作为由包含氧化铈粒子和水的第1液体与包含有机酸A、高分子化合物B和水的第2液体构成的二液式研磨液保存。由此,在使用研磨液之前可以更好地维持氧化铈粒子的分散稳定性,因此可以得到更有效的研磨速度以及平坦性。
另外,本发明的研磨液优选使上述第1液体进一步含有分散剂。由此,可以更好地维持氧化铈粒子的分散稳定性。
另外,本发明提供一种基板的研磨方法,使用本发明的研磨液研磨在基板表面上形成的被研磨膜。根据使用本发明研磨液的这样的研磨方法,可以提高被研磨膜的研磨速度,并能够进一步提高研磨后的平坦性。
发明效果
根据本发明,可以提供一种研磨液以及使用该研磨液的基板的研磨方法,该研磨液在研磨形成于基板表面上的被研磨膜(例如STI膜)的CMP技术中,可以提高被研磨膜的研磨速度,并能够进一步提高研磨后的表面平坦性。
附图说明
图1是表示研磨特性的评价基板的示意剖面图。
具体实施方式
以下对本发明的实施方式进行详细地说明。
[研磨液]
本实施方式的研磨液是包含氧化铈粒子、分散剂、有机酸A、高分子化合物B以及水的CMP用研磨液。以下,对本实施方式的研磨液所含的各成分进行详细地说明。
(氧化铈粒子)
作为氧化铈粒子,没有特别地限制,可以使用公知的物质。通常氧化铈是通过将碳酸盐、硝酸盐、硫酸盐、草酸盐等铈化合物氧化而得到的。作为制作氧化铈粒子的方法,可列举烧成、利用过氧化氢等的氧化法等。
在研磨通过TEOS-CVD法等形成的氧化硅膜时使用氧化铈粒子的情况下,氧化铈粒子的微晶直径(微晶的直径)越大且结晶形变越少,即结晶性越良好,则越能够进行高速研磨,但具有在被研磨膜上容易产生研磨损伤的倾向。从这样的观点考虑,氧化铈粒子优选由2个以上的微晶构成且具有晶界的粒子,更优选微晶直径为1~300nm范围内的粒子。
上述微晶直径可以通过扫描型电子显微镜(SEM)的观察来测定。具体而言,从由扫描型电子显微镜(SEM)观察得到的图像,对粒子的长径与短径进行测定,将长径与短径的积的平方根记为粒径。
氧化铈粒子中的碱金属以及卤素类的含有率,从可适合在半导体元件制造的研磨中使用的观点考虑,优选为10ppm以下。
氧化铈粒子的平均粒径优选为10~500nm,更优选为20~400nm,进一步优选为50~300nm。如果氧化铈粒子的平均粒径为10nm以上,则具有可得到良好的研磨速度的倾向,如果为500nm以下,则具有在被研磨膜上不易产生损伤的倾向。
这里,所谓氧化铈粒子的平均粒径,是指通过激光衍射式粒度分布仪(例如,Malvern公司制造商品名:Master Sizer Microplus,折射率:1.93,光源:He-Ne激光,吸收0)所测定的D50值(体积分布的中位径、累积中央值)。关于平均粒径的测定,使用将研磨液稀释成适宜浓度(例如对于He-Ne激光的测定时透过率(H)为60~70%的浓度)后的样品。另外,将氧化铈研磨液分成如后所述使氧化铈粒子分散在水中所得的氧化铈浆料与使添加剂溶解于水中所得的添加液进行保存的情况下,可以将氧化铈浆料稀释成适宜的浓度来测定。
氧化铈粒子的含量,从具有可得到良好的研磨速度的倾向的观点考虑,以研磨液总质量基准计优选为0.1质量%以上,更优选为0.5质量%以上。另外,氧化铈粒子的含量,从具有抑制粒子的凝聚并在被研磨膜上不易产生损伤的倾向的观点考虑,优选为20质量%以下,更优选为5质量%以下,进一步优选为1.5质量%以下。
(有机酸A)
本实施方式的研磨液含有有机酸和/或其盐作为有机酸A。由此,可以提高研磨速度,且提高研磨结束后的被研磨膜(例如氧化硅膜)的平坦性。更详细而言,研磨具有凹凸的被研磨面时,除了可以缩短研磨时间,还可以抑制由于一部分被过剩研磨而产生像碟子那样下陷的现象,即碟陷(Dishing)。通过并用有机酸和/或其盐与氧化铈粒子,可更高效率地得到该效果。
有机酸和/或其盐具有从-COOM基、-Ph-OM基(酚性-OM基)、-SO3M基以及-PO3M2基(式中,M是从H、NH4、Na以及K所组成的组中选择的任一种,Ph表示可以具有也可以不具有取代基的苯基)所组成的组中选择的至少一种基团,优选为水溶性的有机化合物。
作为有机酸A,例如可列举甲酸、乙酸、丙酸、丁酸、戊酸、环己烷羧酸、苯乙酸、苯甲酸、邻甲苯甲酸、间甲苯甲酸、对甲苯甲酸、邻甲氧基苯甲酸、间甲氧基苯甲酸、对甲氧基苯甲酸、丙烯酸、甲基丙烯酸、丁烯酸、戊烯酸、己烯酸、庚烯酸、辛烯酸、壬烯酸、癸烯酸、十一烯酸、十二烯酸、十三烯酸、十四烯酸、十五烯酸、十六烯酸、十七烯酸、异丁酸、异戊酸、肉桂酸、喹哪啶酸、烟酸、1-萘甲酸、2-萘甲酸、吡啶甲酸、乙烯基乙酸、苯乙酸、苯氧乙酸、2-呋喃甲酸、巯基乙酸、乙酰丙酸、草酸、丙二酸、丁二酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、1,9-壬烷二甲酸、1,10-癸烷二甲酸、1,11-十一烷二甲酸、1,12-十二烷二甲酸、1,13-十三烷二甲酸、1,14-十四烷二甲酸、1,15-十五烷二甲酸、1,16-十六烷二甲酸、马来酸、富马酸、衣康酸、柠康酸、中康酸、喹啉酸、奎宁酸、萘二甲酸、邻苯二甲酸、间苯二甲酸、对苯二甲酸、乙醇酸、乳酸、3-羟基丙酸、2-羟基丁酸、3-羟基丁酸、4-羟基丁酸、3-羟基戊酸、5-羟基戊酸、奎尼酸、犬尿喹啉酸、水杨酸、酒石酸、乌头酸、抗坏血酸、乙酰水杨酸、乙酰苹果酸、乙炔二甲酸、乙酰氧丁二酸、乙酰乙酸、3-氧代戊二酸、阿托酸、阿卓乳酸、蒽醌羧酸、蒽羧酸、异己酸、异樟脑三酸、异丁烯酸、2-乙基-2-羟基丁酸、乙基丙二酸、乙氧基乙酸、草酰乙酸、氧代二乙酸、2-氧代丁酸、樟脑三酸(camphoronic acid)、柠檬酸、乙醛酸、缩水甘油酸、甘油酸、葡萄糖二酸、葡萄糖酸、克酮酸、环丁烷羧酸、环己烷二甲酸、二苯基乙酸、二-O-苯甲酰酒石酸、二甲基丁二酸、二甲氧基邻苯二甲酸、羟基丙二酸、单宁酸、噻吩羧酸、惕各酸、脱草酸、四羟基丁二酸、四甲基丁二酸、季酮酸、脱氢乙酸、芸香酸、托品酸、香草酸、仲康酸、羟基间苯二甲酸、羟基肉桂酸、羟基萘甲酸、邻羟基苯乙酸、间羟基苯乙酸、对羟基苯乙酸、3-羟基-3-苯基丙酸、特戊酸、吡啶二羧酸、吡啶三羧酸、丙酮酸、α-苯基肉桂酸、苯基缩水甘油酸、苯基丁二酸、苯基乙酸、苯基乳酸、丙炔酸、山梨酸、2,4-己二烯二酸、2-亚苄基丙酸、3-亚苄基丙酸、亚苄基丙二酸、二苯基乙醇酸、苯三甲酸、1,2-苯二乙酸、苯酰氧基乙酸、苯酰氧基丙酸、苯甲酰甲酸、苯甲酰乙酸、O-苯甲酰乳酸、3-苯甲酰丙酸、没食子酸、中草酸、5-甲基间苯二甲酸、2-甲基丁烯酸、α-甲基肉桂酸、甲基丁二酸、甲基丙二酸、2-甲基丁酸、邻甲氧基肉桂酸、对甲氧基肉桂酸、巯基丁二酸、巯基乙酸、O-乳酰基乳酸、苹果酸、白酮酸、白氨酸、玫棕酸、玫红酸、α-酮戊二酸、L-抗坏血酸、艾杜糖醛酸、半乳糖醛酸、葡萄糖醛酸、焦谷氨酸、乙二胺四乙酸、氰化三乙酸、天冬氨酸、谷氨酸、N′-羟乙基-N,N,N′-三乙酸以及次氮基三乙酸等羧酸;
甲磺酸、乙磺酸、丙磺酸、丁磺酸、戊磺酸、己磺酸、庚磺酸、辛磺酸、壬磺酸、癸磺酸、十一烷磺酸、十二烷磺酸、十三烷磺酸、十四烷磺酸、十五烷磺酸、十六烷磺酸、十七烷磺酸、十八烷磺酸、苯磺酸、萘磺酸、甲苯磺酸、羟基乙磺酸、羟基苯酚磺酸以及蒽磺酸等磺酸;
癸基膦酸和苯基膦酸等膦酸;等。进一步,关于上述的羧酸、磺酸以及膦酸,也可以是它们主链的质子被1个或2个以上的F、Cl、Br、I、OH、CN以及NO2等原子或原子团取代而形成的衍生物。它们可以单独使用1种或组合2种以上使用。
有机酸A(有机酸和或其盐)的含量以研磨液总质量基准计为0.001~1质量%。如果有机酸和/或其盐的含量为0.001质量%以上,则具有可以提高研磨结束后的被研磨膜(例如氧化硅膜)的平坦性的倾向,从这个观点考虑,有机酸和/或其盐的含量优选0.005质量%以上,更优选0.01质量%以上。另一方面,如果含量为1质量%以下,则具有被研磨膜的研磨速度充分提高的倾向,另外还具有抑制氧化铈粒子凝聚的倾向,从这个观点考虑,有机酸和/或其盐的含量优选为0.1质量%以下,更优选为0.05质量%以下。
有机酸A在室温(25℃)下的酸解离常数pKa(pKa具有2个以上时,为最低的第一阶段的pKa1)小于9,但作为pKa,优选小于8,更优选小于7,进一步优选小于6,最优选小于5。如果有机酸A的pKa小于9,则研磨液中至少其一部分以上成为有机酸离子而放出氢离子,可以将pH保持在所希望的pH区域内。
(高分子化合物B)
本实施方式的研磨液含有高分子化合物B,该高分子化合物B具有羧酸基或羧酸盐基。这里,羧酸基是-COOH所表示的官能团,羧酸盐基是-COOX所表示的官能团(X是来自盐基的阳离子,例如可列举铵离子、钠离子以及钾离子)。特别地,优选包含具有羧酸基或羧酸盐基的水溶性有机高分子和/或其盐作为高分子化合物B。由此,可以提高研磨结束后的被研磨膜(例如,氧化硅膜)的平坦性。更详细而言,研磨具有凹凸的被研磨面时,可以抑制由于一部分被过剩研磨而产生像碟子那样下陷的现象、即所谓的碟陷。通过并用具有羧酸基或羧酸盐基的水溶性有机高分子和/或其盐、有机酸和/或其盐以及氧化铈粒子,可更高效率地得到该效果。
作为高分子化合物B(具有羧酸基或羧酸盐基的水溶性有机高分子)的具体例子,可列举:
聚天冬氨酸、聚谷氨酸、聚赖氨酸、聚苹果酸、聚酰胺酸、聚酰胺酸铵盐、聚酰胺酸钠盐以及聚乙醛酸等聚羧酸和其盐;
丙烯酸、甲基丙烯酸、马来酸等具有羧酸基的单体的均聚物以及该聚合物的羧酸基部分为铵盐等的均聚物等。
另外,可列举具有羧酸盐基的单体与羧酸的烷基酯等衍生物的共聚物。作为其具体例子,可列举聚(甲基)丙烯酸、或聚(甲基)丙烯酸的羧酸基的一部分被取代成羧酸铵盐基的聚合物(以下称为聚(甲基)丙烯酸铵)等。这里聚(甲基)丙烯酸表示聚丙烯酸与聚甲基丙烯酸的至少一方。
作为高分子化合物B,上述中优选丙烯酸、甲基丙烯酸、马来酸等具有羧酸基的单体的均聚物以及该聚合物的羧酸基部分为铵盐等的均聚物,更优选(甲基)丙烯酸的均聚物(聚(甲基)丙烯酸)及其铵盐,进一步优选聚丙烯酸及其铵盐。
高分子化合物B的含量,从具有可以提高研磨结束后的被研磨膜(例如氧化硅膜)的平坦性的倾向的观点考虑,以研磨液总质量基准计为0.01质量%以上,从同样的观点考虑,优选0.02质量%以上,更优选0.05质量%以上。另外,如果含量为0.50质量%以下,则具有被研磨膜的研磨速度充分提高的倾向,另外从具有抑制氧化铈粒子凝聚的倾向的观点考虑,高分子化合物B的含量以研磨液总质量基准计为0.50质量%以下,优选为0.40质量%以下,更优选为0.30质量%以下,进一步优选为0.20质量%以下。
高分子化合物B的重均分子量没有特别地限制,但从具有可充分地得到被研磨膜的研磨速度的倾向、以及具有容易抑制氧化铈粒子凝聚的观点考虑,优选100000以下,更优选10000以下。另外从具有容易得到平坦性提高效果的观点考虑,高分子化合物B的重均分子量优选为1000以上。另外,重均分子量是通过GPC(Gel Permeation Chromatography:凝胶渗透色谱)进行测定,并换算成标准聚氧乙烯所得的值。
(水)
作为水,没有特别地限制,但优选去离子水、离子交换水以及超纯水等。水的含量可以为上述各含有成分的含量的余量,只要在研磨液中含有就没有特别地限制。另外,研磨液根据需要,可以进一步含有除水以外的溶剂,例如乙醇、丙酮等极性溶剂等。
(分散剂)
本实施方式的研磨液中可以含有用于分散氧化铈粒子的分散剂。作为分散剂,可列举水溶性阴离子性分散剂、水溶性非离子性分散剂、水溶性阳离子性分散剂以及水溶性两性分散剂等,其中优选水溶性阴离子性分散剂。它们可以单独使用一种或组合两种以上使用。另外,也可以使用作为高分子化合物B所例示的上述化合物(例如聚丙烯酸铵)作为分散剂。
作为水溶性阴离子性分散剂,优选含有丙烯酸作为共聚成分的高分子及其盐,更优选该高分子的盐。作为含有丙烯酸作为共聚成分的高分子及其盐,例如可列举聚丙烯酸及其铵盐、丙烯酸与甲基丙烯酸的共聚物及其铵盐、以及丙烯酰胺与丙烯酸的共聚物及其铵盐。
作为其它水溶性阴离子性分散剂,例如可列举十二烷基硫酸三乙醇胺、十二烷基硫酸铵、聚氧乙烯烷基醚硫酸三乙醇胺以及特殊聚羧酸型高分子分散剂。
另外,作为水溶性非离子性分散剂,例如可列举聚乙二醇单月桂酸酯、聚乙二醇单硬脂酸酯、聚乙二醇二硬脂酸酯、聚乙二醇单油酸酯、聚氧乙烯烷基胺、聚氧乙烯氢化蓖麻油、甲基丙烯酸2-羟基乙酯以及烷基烷醇酰胺。
作为水溶性阳离子性分散剂,例如可列举聚乙烯基吡咯烷酮、椰子胺乙酸酯和十八烷胺乙酸酯。
作为水溶性两性分散剂,例如可列举十二烷基甜菜碱、十八烷基甜菜碱、十二烷基二甲基胺氧化物和2-烷基-N-羧甲基-N-羟乙基咪唑鎓甜菜碱。
分散剂的含量,从提高氧化铈粒子的分散性,抑制沉降,进一步减少被研磨膜的研磨损伤的观点考虑,以研磨液总质量基准计优选为0.001~10质量%的范围。
分散剂的重均分子量没有特别地限制,但优选为100~150000,更优选为1000~20000。如果分散剂的分子量为100以上,则在研磨氧化硅膜或氮化硅膜等被研磨膜时,具有容易得到良好的研磨速度的倾向。如果分散剂的分子量为150000以下,则具有研磨液的保存稳定性不易降低的倾向。另外,重均分子量是通过GPC来测定,并换算成标准聚氧乙烯所得的值。
[其它添加剂]
本实施方式的研磨液,可以使用水溶性高分子作为与有机酸和/或其盐、以及具有羧酸基或羧酸盐基的水溶性有机高分子和/或其盐不同的添加剂。作为这样的水溶性高分子,例如可列举褐藻酸、果胶酸、羧甲基纤维素、琼脂、凝胶多糖(curdlan)以及普鲁兰多糖(pullulan)等多糖类;聚乙烯醇、聚乙烯吡咯烷酮以及聚丙烯醛等乙烯基系聚合物等。
这些水溶性高分子的重均分子量优选为500以上。另外,重均分子量是通过GPC来测定,并换算成标准聚氧乙烯所得的值。另外这些水溶性高分子的含量以研磨液总质量基准计优选为0.01~5质量%。
[研磨液的调制、保存方法]
本实施方式的研磨液,例如可通过配合氧化铈粒子、水以及分散剂并使氧化铈粒子分散后,进一步添加有机酸A和高分子化合物B而得到。另外,本实施方式的研磨液可以作为含有氧化铈粒子、分散剂、有机酸A、高分子化合物B、水以及任意的水溶性高分子的一液式研磨液保存,也可以作为由氧化铈浆料(第1液体)与添加液(第2液体)构成的二液式研磨液保存,该氧化铈浆料包含氧化铈粒子、分散剂以及水,该添加液包含有机酸A、高分子化合物B、水及任意的水溶性高分子。
另外,在二液式研磨液的情况下,除了有机酸A和高分子化合物B以外的添加剂可以包含在氧化铈浆料与添加液任一者中,但是从不影响氧化铈粒子的分散稳定性方面来看,优选包含在添加液中。
作为将氧化铈浆料与添加液分开的二液式研磨液保存时,通过任意地改变该二液的配合,可以调整平坦化特性与研磨速度。使用二液式研磨液进行研磨时,可以使用如下方法:通过各自的配管分别输送氧化铈浆料与添加液,在供给配管出口之前使这些配管合并而混合两种液体并供给至研磨垫上的方法;在研磨之前就混合氧化铈浆料与添加液的方法。
本实施方式的研磨液和浆料,从能抑制储藏、搬运、保管等的成本的观点考虑,可以作为使用时用水等液状介质稀释成例如2倍以上来使用的、研磨液用储藏液或浆料用储藏液进行保管。上述各储藏液可以在研磨之前用液状介质来稀释,也可以将储藏液与液状介质供给至研磨垫上,在研磨垫上进行稀释。
作为上述储藏液的稀释倍率,由于倍率越高则储藏、搬运、保管等的成本抑制效果就越高,因此优选2倍以上、更优选3倍以上。另外,作为上限没有特别地限制,但是由于倍率越高则储藏液所含的成分量就越多(浓度越高),保管中的稳定性有降低的倾向,因此通常优选10倍以下,更优选7倍以下,进一步优选5倍以下。另外,也可以将构成成分分成三种液体以上,关于该情况,也同样。
将本实施方式的研磨液调整到所希望的pH而供于研磨。作为pH调整剂没有特别地限制,例如可列举硝酸、硫酸、盐酸、磷酸、硼酸以及乙酸等酸,以及氢氧化钠、氨水、氢氧化钾以及氢氧化钙等碱。在半导体研磨中使用研磨液的情况下,可优选使用氨水、酸成分。作为pH调整剂,可以使用预先用氨进行了部分中和的水溶性高分子的铵盐。
另外,在室温(25℃)下研磨液的pH为4.0以上7.0以下。通过使pH为4.0以上,具有研磨液的保存稳定性提高的倾向,具有被研磨膜的损伤发生数减少的倾向,从同样的观点考虑,上述pH优选为4.5以上,更优选为4.8以上。另外,通过使pH为7.0以下,可以充分地发挥平坦性的提高效果,从同样的观点考虑,上述pH优选为6.5以下,更优选为6.0以下,进一步优选为5.5以下。研磨液的pH可以通过pH计(例如横河电机株式会社制造的ModelPH81(商品名))测定。例如使用标准缓冲液(邻苯二甲酸盐pH缓冲液pH:4.21(25℃)、中性磷酸盐pH缓冲液pH6.86(25℃))进行2点校正后,将电极放入研磨液中,测定在25℃下经过2分钟以上稳定后的值,从而可以测定研磨液的pH。
接着,对本实施方式的研磨液对于研磨在基板表面上形成的被研磨膜的应用(Use)进行说明。
[研磨方法]
本实施方式的基板研磨方法是使用上述研磨液来研磨在基板表面形成的被研磨膜。更详细而言,例如,在研磨平台的研磨垫上挤压在基板表面形成的被研磨膜的状态下,一边将上述研磨液供给至被研磨膜与研磨垫之间,一边使基板与研磨平台相对移动,从而研磨被研磨膜。
作为基板,可列举形成了电路元件和线路图形阶段的半导体基板、在形成了电路元件阶段的半导体基板等半导体基板上形成了无机绝缘膜的基板等半导体元件制造的基板等。
作为上述被研磨膜,例如可列举氧化硅膜、氮化硅膜、氧化硅膜的复合膜等无机绝缘膜等。通过使用本实施方式的研磨液来研磨在这样的基板上形成的无机绝缘膜,可以消除无机绝缘膜表面的凹凸,使基板整面成为平滑的面。另外,本实施方式的研磨液也可在浅沟槽隔离中使用。
以下列举形成了无机绝缘膜的半导体基板的情况,进一步详细地说明基板的研磨方法。
作为研磨装置,可使用一般的研磨装置,其具备保持具有被研磨膜的半导体基板等基板的支架、以及安装有可以变更转数的电动机等并能够贴附研磨垫(研磨布)的研磨平台。作为研磨装置,例如可使用株式会社荏原制作所制造的研磨装置:型号EPO-111,AMAT制造的MIRRA、Reflexion等。
作为研磨垫,可以使用一般的无纺布、发泡聚氨酯和多孔质氟树脂等,没有特别地限制。此外,优选对研磨垫实施了用于积存研磨液那样的沟槽加工。
对研磨条件没有限制,但为了使半导体基板不飞出,平台的旋转速度优选为200转/分以下的低旋转,为了在研磨之后不产生损伤,施加于半导体基板的压力(加工负荷)优选为100kPa以下。研磨期间,通过泵等将研磨液连续地供给至研磨垫。该供给量没有限制,但优选使研磨垫的表面总是被研磨液所覆盖。
研磨结束后的半导体基板,优选在流水中充分洗涤后,用旋转干燥器等将附着在半导体基板上的水滴甩落后使其干燥。
通过如上使用研磨液研磨作为被研磨膜的无机绝缘膜,可以消除表面的凹凸,在半导体基板整面上得到平滑的面。形成被平坦化的浅沟槽后,在无机绝缘膜上形成铝路线,在该线路间以及线路上再次形成无机绝缘膜后,使用研磨液研磨该无机绝缘膜而得到平滑的面。通过以规定的次数重复进行该工序,能够制造具有所希望层数的半导体基板。
作为使用本实施方式的研磨液来研磨的无机绝缘膜,例如可列举氧化硅膜和氮化硅膜。氧化硅膜也可以掺杂有磷和硼等元素。作为无机绝缘膜的制作方法,可列举低压CVD法、等离子体CVD法。
通过低压CVD法的氧化硅膜形成,用单硅烷:SiH4作为Si源、用氧:O2作为氧源。通过使该SiH4-O2系氧化反应在400℃以下的低温进行而得到氧化硅膜。根据情况,通过CVD得到的氧化硅膜可在1000℃或其以下的温度下进行热处理。为了通过高温回流而实现表面平坦化,在氧化硅膜中掺杂磷:P时,优选使用SiH4-O2-PH3系反应气体。
等离子体CVD法具有能够使在通常的热平衡下需要高温的化学反应在低温下发生的优点。在等离子体发生法中,可以举出电容耦合型和电感耦合型两种。作为反应气体,可以举出用SiH4作为Si源、用N2O作为氧源的SiH4-N2O系气体,和用四乙氧基硅烷(TEOS)作为Si源的TEOS-O系气体(TEOS-等离子体CVD法)。优选基板温度为250~400℃、反应压力为67~400Pa。
通过低压CVD法的氮化硅膜形成,用二氯硅烷:SiH2Cl2作为Si源、用氨:NH3作为氮源。通过使该SiH2Cl2-NH3系氧化反应在900℃的高温下发生而得到氮化硅膜。通过等离子体CVD法的氮化硅膜形成,作为反应气体,可列举出用SiH4作为Si源、用NH3作为氮源的SiH4-NH3系气体。基板温度优选为300~400℃。
本实施方式的研磨液以及基板的研磨方法不仅可适用于在半导体基板上形成的无机绝缘膜,也可适用于各种半导体装置的制造工艺等。本实施方式的研磨液以及基板的研磨方法也可以适用于研磨例如在具有规定线路的线路板上形成的氧化硅膜、玻璃以及氮化硅等无机绝缘膜,主要含有多晶硅、Al、Cu、Ti、TiN、W、Ta以及TaN等的膜,光掩模·透镜·棱镜等光学玻璃,ITO等无机导电膜、由玻璃和结晶质材料所构成的光集成电路·光转换元件·光波导、光纤的端面、闪烁器等光学用单晶、固体激光器单晶、蓝色激光LED用蓝宝石基板、SiC、GaP以及GaAs等半导体单晶、磁盘用玻璃基板、以及磁头等。
实施例
以下,通过实施例对本发明进行说明,但本发明不受这些实施例的限制。
(氧化铈粒子的制作)
将40kg市售的碳酸铈水合物放入氧化铝制容器中,在830℃、空气中烧成2小时,从而得到20kg的黄白色粉末。通过X射线衍射法对该粉末进行相鉴定时,确认到是氧化铈。用气流粉碎机对得到的20kg氧化铈粉末进行干式粉碎,得到粉末状(粒子状)的氧化铈。通过扫描型电子显微镜(SEM)对得到的粉末状氧化铈进行观察时,含有微晶大小的粒子与由2个以上的微晶构成且具有晶界的粒子。从得到的SEM图像中任意地选出50个微晶,对于每个微晶,由长径与短径的积的平方根求出粒径时,微晶直径均包含在1~300nm的范围内。
(实施例1-1)
将200.0g上述所制作的氧化铈粒子和795.0g去离子水混合,添加5g作为分散剂的聚丙烯酸铵水溶液(重均分子量:8000、40质量%),一边搅拌一边进行超声波分散,从而得到氧化铈分散液。超声波分散在超声波频率为400kHz、分散时间为20分钟下进行。
之后,在1升容器(高度:170mm)中加入1kg的氧化铈分散液后静置,进行沉降分级。分级时间15小时后,用泵将距水面的深度13cm以上的上清液抽出来。接着,将得到的上清液的氧化铈分散液用去离子水稀释以使氧化铈粒子的含量为5质量%,得到氧化铈浆料。
为了测定氧化铈浆料中的氧化铈粒子的平均粒径(D50),将上述浆料稀释,使得对于He-Ne激光的测定时透过率(H)为60~70%,制成测定样品。用激光衍射式粒度分布仪Master Sizer Microplus(Malvern公司制造商品名),设定折射率:1.93、吸收:0,测定该测定样品,D50值为150nm。
将0.1g作为有机酸A的对甲苯磺酸-水合物(pKa(25℃)=-2.8)与800g去离子水混合,添加2.5g作为高分子化合物B的聚丙烯酸水溶液(重均分子量:4000、40质量%)后,添加氨水(25质量%)将pH调整为4.5(25℃)。进一步添加去离子水,使总量为850g,制成有机酸添加液。
此时,添加134g上述的氧化铈浆料,并添加氨水(25质量%),将pH调整为5.0(25℃),进一步添加去离子水使总量为1000g,从而制作了氧化铈研磨液(氧化铈粒子含量:0.67质量%)。
另外,与上述同样地调制测定样品,通过激光衍射式粒度分布仪对研磨液中的粒子的平均粒径进行测定,结果是D50值为150nm。
(绝缘膜的研磨)
作为研磨试验晶片,使用SEMATECH公司制造的商品名“图形晶片764”(直径:300mm)。使用图1对该研磨试验晶片与使用其的研磨特性的评价方法进行说明。
图1(a)是放大了研磨试验晶片的一部分的示意剖面图。在晶片1的表面上形成有多个沟槽,在晶片1的凸部表面上形成有厚度为150nm()的氮化硅膜2。沟槽的深度(从凸部的表面到凹部的底面的高低差)为500nm()。以下,将凸部称为活性部,将凹部称为沟槽部。另外,虽然在图1中没有明示,但在晶片1中,形成了沟槽部/活性部的剖面宽度为100μm/100μm、20μm/80μm以及80μm/20μm的3个区域。
图1(b)是放大了研磨试验晶片的一部分的示意剖面图。研磨试验晶片通过等离子体TEOS法在活性部以及沟槽部形成了氧化硅膜3,使得氧化硅膜3距离活性部表面的厚度为600nm()。在研磨试验中,对研磨试验晶片的氧化硅膜3进行研磨而进行平坦化。
图1(c)是放大了研磨氧化硅膜3后的研磨试验晶片的一部分的示意剖面图。在活性部的氮化硅膜2表面结束研磨,将这时研磨所需要的时间记为研磨时间,将由沟槽部的深度4减去沟槽部内的氧化硅膜3的厚度5所得的值作为碟陷量6。另外,研磨时间越短越好,碟陷量6越小越好。
在这样的研磨试验晶片的研磨中使用研磨装置(AMAT制造的Reflexion)。在贴附了基板安装用的吸附垫的支架上设置研磨试验晶片。在研磨装置的直径为600mm的研磨平台上,贴附多孔聚氨酯树脂制的研磨垫(沟槽形状=穿孔型:Rohm and Haas公司制造,型号IC1010)。进一步,使作为被研磨膜的绝缘膜(氧化硅被膜)面向下,将上述支架放置在研磨平台上,设定加工负荷为210gf/cm2(20.6kPa)。
一边将上述氧化铈研磨液以250毫升/分钟的速度滴在上述研磨垫上,一边使研磨平台与研磨试验晶片各自以130转/分钟工作,由此研磨研磨试验晶片。将100μm/100μm区域的活性部的氮化硅膜露出于表面时的研磨时间作为研磨结束时间。然而,关于平坦性的评价,对进行了超过该时间20%的研磨(例如,如果研磨结束时间为100秒,则从该时间追加研磨多于20秒的时间)的晶片进行。这是因为,从研磨工艺方面看,也具有工艺的尤度,是有利的,所以可以证明:通过过剩地研磨,评价项目的值容易出现差异,容易评价,另外即使过剩地研磨,数字也良好(特性良好)。研磨后的研磨试验晶片用纯水充分洗涤后进行干燥。
作为平坦性的评价项目,对以下的3项目进行评价。
项目1:100μm/100μm区域的沟槽部的碟陷(Dishing)量:使用触针式台阶仪(型号P16KLA-tencor制造)来测定。
项目2:100μm/100μm区域的活性部的SiN损耗:使用Nanometrics公司制造的干涉式膜厚测定装置NANOSPEC/AFT5100(商品名),测定通过研磨而除去的氮化硅膜(SiN膜)的厚度。
项目3:20μm/80μm区域以及80μm/20μm区域的沟槽部的SiO2残膜厚差(SiO2密度差):使用Nanometrics公司制造的干涉式膜厚测定装置NANOSPEC/AFT5100(商品名),测定各个区域中的氧化硅膜(SiO2膜)的残膜厚,求出其差。
(实施例1-2~6-9以及比较例1-1~6-9)
除了将研磨液的pH、有机酸A的种类以及使用量、或者高分子化合物B的使用量变更为表1~19所示的以外,与实施例1-1同样地制作氧化铈研磨液,并进行了绝缘膜的研磨。将结果示于同一表中。从表1~19可知,利用由本发明提供的研磨液,研磨速度和平坦性提高,可实现碟陷的减少。
[表1]
[表2]
[表3]
[表4]
[表5]
[表6]
[表7]
[表8]
[表9]
[表10]
[表11]
[表12]
[表13]
[表14]
[表15]
[表16]
[表17]
[表18]
[表19]
符号说明
1:晶片;2:氮化硅膜;3:通过等离子体TEOS法形成的氧化硅膜;4:沟槽部的深度;5:研磨后的沟槽部的氧化硅膜厚;6:碟陷量。
Claims (33)
1.一种研磨液,其是包含氧化铈粒子、有机酸A、具有羧酸基或羧酸盐基的高分子化合物B以及水的CMP用研磨液,
所述有机酸A为对甲苯磺酸,
所述有机酸A的含量相对于研磨液总质量为0.001~1质量%,
所述高分子化合物B的含量相对于研磨液总质量为0.01~0.50质量%,所述研磨液的pH为4.0以上7.0以下。
2.根据权利要求1所述的研磨液,其中,所述高分子化合物B是水溶性有机高分子。
3.根据权利要求1所述的研磨液,其中,所述有机酸A的含量相对于研磨液总质量为0.005质量%以上。
4.根据权利要求1所述的研磨液,其中,所述有机酸A的含量相对于研磨液总质量为0.01质量%以上。
5.根据权利要求1所述的研磨液,其中,所述有机酸A的含量相对于研磨液总质量为0.1质量%以下。
6.根据权利要求1所述的研磨液,其中,所述有机酸A的含量相对于研磨液总质量为0.05质量%以下。
7.根据权利要求1所述的研磨液,其中,所述氧化铈粒子是通过将选自碳酸盐的铈化合物、硝酸盐的铈化合物、硫酸盐的铈化合物、草酸盐的铈化合物氧化而得到的。
8.根据权利要求1所述的研磨液,其中,所述氧化铈粒子的平均粒径是10~500nm。
9.根据权利要求1所述的研磨液,其中,所述氧化铈粒子的平均粒径是20~400nm。
10.根据权利要求1所述的研磨液,其中,所述氧化铈粒子的平均粒径是50~300nm。
11.根据权利要求1所述的研磨液,其中,所述氧化铈粒子的含量为0.1质量%以上。
12.根据权利要求1所述的研磨液,其中,所述氧化铈粒子的含量为0.5质量%以上。
13.根据权利要求1所述的研磨液,其中,所述氧化铈粒子的含量为20质量%以下。
14.根据权利要求1所述的研磨液,其中,所述氧化铈粒子的含量为5质量%以下。
15.根据权利要求1所述的研磨液,其中,所述氧化铈粒子的含量为1.5质量%以下。
16.根据权利要求1所述的研磨液,其中,作为由包含所述氧化铈粒子和所述水的第1液体和包含所述有机酸A、所述高分子化合物B和所述水的第2液体构成的二液式研磨液保存。
17.根据权利要求16所述的研磨液,其中,所述第1液体进一步含有分散剂。
18.根据权利要求17所述的研磨液,其中,所述分散剂选自水溶性阴离子性分散剂、水溶性非离子性分散剂、水溶性阳离子性分散剂以及水溶性两性分散剂。
19.根据权利要求17所述的研磨液,其中,所述分散剂的含量以研磨液总质量基准计为0.001~10质量%的范围。
20.根据权利要求1所述的研磨液,其中,所述高分子化合物B选自:聚天冬氨酸、聚谷氨酸、聚赖氨酸、聚苹果酸、聚酰胺酸、聚酰胺酸铵盐、聚酰胺酸钠盐以及聚乙醛酸;选自丙烯酸、甲基丙烯酸、马来酸的具有羧酸基的单体的均聚物;所述均聚物的所述羧酸基部分为铵盐的均聚物;具有羧酸盐基的单体与羧酸的烷基酯的共聚物;以及聚(甲基)丙烯酸的羧酸基的一部分被取代成羧酸铵盐基的聚合物。
21.根据权利要求1所述的研磨液,其中,所述高分子化合物B的含量以研磨液总质量基准计为0.02质量%以上。
22.根据权利要求1所述的研磨液,其中,所述高分子化合物B的含量以研磨液总质量基准计为0.05质量%以上。
23.根据权利要求1所述的研磨液,其中,所述高分子化合物B的含量以研磨液总质量基准计为0.40质量%以下。
24.根据权利要求1所述的研磨液,其中,所述高分子化合物B的含量以研磨液总质量基准计为0.30质量%以下。
25.根据权利要求1所述的研磨液,其中,所述高分子化合物B的含量以研磨液总质量基准计为0.20质量%以下。
26.根据权利要求1所述的研磨液,其中,所述高分子化合物B的重均分子量为100000以下。
27.根据权利要求1所述的研磨液,其中,所述高分子化合物B的重均分子量为10000以下。
28.根据权利要求1所述的研磨液,其中,所述高分子化合物B的重均分子量为1000以上。
29.根据权利要求1所述的研磨液,其中,pH为4.0以上6.0以下。
30.根据权利要求1所述的研磨液,其中,pH为4.0以上5.5以下。
31.一种基板的研磨方法,使用权利要求1~30中任一项所述的研磨液来研磨在基板表面上形成的被研磨膜。
32.权利要求1~30中任一项所述的研磨液对于研磨在基板表面上形成的被研磨膜的应用。
33.根据权利要求32所述的应用,其中,所述基板选自形成有电路元件和线路图形的阶段的半导体基板、以及在形成有电路元件的阶段的半导体基板上形成有无机绝缘膜的基板。
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US20170133237A1 (en) | 2017-05-11 |
US20130260558A1 (en) | 2013-10-03 |
SG190765A1 (en) | 2013-07-31 |
JP2013149987A (ja) | 2013-08-01 |
KR101886464B1 (ko) | 2018-08-07 |
KR101389235B1 (ko) | 2014-04-24 |
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