CN1243370C - 用于金属布线的化学机械抛光的浆液组合物 - Google Patents
用于金属布线的化学机械抛光的浆液组合物 Download PDFInfo
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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 at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System 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
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/32115—Planarisation
- H01L21/3212—Planarisation by chemical mechanical polishing [CMP]
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
Abstract
本发明公开了一种在制造半导体设备中用于金属布线CMP(化学机械抛光)工艺的组合物,包括过氧化氢、无机酸、丙二胺四乙酸(PDTA)-金属络合物、羧酸、金属氧化物粉末和去离子水,其中PDTA-金属络合物通过防止研磨后的钨氧化物再粘附到抛光后的表面上,在全面改进抛光性能和抛光性能的可重复性方面以及在改进浆液组合物的分散稳定性方面起主要的作用。
Description
发明领域
总的来说,本发明涉及一种在制造半导体装置中用于化学机械抛光(CMP)工艺的浆液组合物,具体涉及一种用于装置晶片的钨层的平面化的CMP浆液组合物。
背景技术
金属包括钨在制造集成电路中有广泛的应用。例如,可以形成金属层来相互连接在硅晶片上的众多导电的设备或用来构成这些设备。目前,集成电路通过在硅晶片上和/或在硅晶片中安装合适的装置如二极管或晶体管而被制造出来。同时,反复进行在装置的整个表面上形成绝缘材料和导电材料的不同层的工艺。在集成电路中,接触孔或通道的特性依赖于绝缘材料的性能,并且通道被填充了导电材料以提供垂直接触,该垂直接触穿透了绝缘层并且接触到安装在晶片上的设备的适当的部位。当铝被用作布线材料时,完全填充通道的内部是不够的。典型的是,通道用能适于CVD(化学气相沉积)工艺的钨来填充。在化学气相沉积的过程中,钨不但能填充通道而且也能覆盖绝缘层的表面。在除去多余的钨之后,在电介质层和通道上就形成了铝线路。
以前,在传统的半导体工艺中,在钨除去步骤中使用RIE(活性离子蚀刻)工艺。然而,RIE工艺有关键性缺陷,因为它倾向于过度腐蚀钨层,甚至部分腐蚀了在通道中的钨,导致与在钨层上形成的铝线路的不良接触。而且,残留在晶片上的任何钨颗粒都能在形成的半导体集成电路中导致严重劣势。CMP(化学机械抛光)工艺已经被发展用来解决RIE工艺的这些问题。
相应于半导体集成电路层的集成性和数目的增加,CMP工艺已经被引入到现有技术中。在CMP工艺中,在半导体晶片同由聚氨酯制得的抛光垫和包括研磨剂和各种其它化合物的浆液组合物接触的同时,半导体晶片进行结合了旋转和平移的轨道移动,以平面化晶片的表面。通常,用在这样的CMP工艺(下文中,称为‘CMP浆液’)中的浆液组合物提供了化学和机械抛光作用,蚀刻剂、氧化剂、酸和分散剂起到化学抛光的作用,研磨剂、金属氧化物的微粒起到机械抛光的作用。这两种抛光作用使晶片的外表面的任何突出部分被选择性地蚀刻和抛光,得到最好的晶片平面化。
根据要抛光的基质,CMP浆液能被分类成用于绝缘层如SiO2层的氧化物抛光浆液和用于金属层如钨或铝层的金属抛光浆液。这两类CMP浆液在发挥化学抛光作用的组份方面不同。
同时,传统的金属抛光CMP浆液有几种典型的问题,具有代表性的问题有:因为在金属、屏蔽金属和电介质层中的抛光速率的不同,而引起氧化物磨耗;以及因为氧化剂成份对金属层的过分蚀刻而引起腐蚀。如果在CMP加工过程中发生磨耗或腐蚀,同其它沉积在抛光金属层上的接触变弱,于是得到的半导体集成电路可能不会正常工作。这些问题被认为主要来源于抛光浆液中所含的氧化剂的过多的氧化力。最近,主要通过增加加入到CMP浆液中的氧化剂的用量或增加它的强度,已经实现了传统半导体工艺所要求的抛光速率。所以,必然引起氧化物磨耗、腐蚀、凹点和凹坑等等。在附图1a和1b中图示说明了这样的氧化物磨耗和腐蚀。
而且,为了更有力地抛光钨,在酸性条件下制备金属CMP浆液,这样低的pH值通常降低研磨颗粒的可分散性,导致浆液抛光性能的可重复性显著变差。
发明内容
本发明涉及下面的发明:将丙二胺四乙酸金属络合物和羧酸加到含有少量过氧化物和无机酸作为氧化剂的非选择性的金属CMP浆液中能显著改进抛光速率、晶片内的不均匀性和晶片到晶片的不均匀性,以及浆液的分散稳定性。
本发明特性在于一种用在金属化学机械抛光中的浆液组合物,该组合物主要由过氧化物、无机酸、丙二胺四乙酸金属络合物、羧酸和金属氧化物粉末组成。
在本发明的优选实施方案中,通过在去离子水中分散以下物质来制备CMP浆液组合物:(i)过氧化物和无机酸,它们结合起来用作弱氧化剂,(ii)含有丙二胺四乙酸配体的金属络合物,其能防止被磨掉的钨氧化物颗粒重新粘合到抛光后的表面并改进分散稳定性,(iii)羧酸,其有助于提高抛光性能和分散稳定性的可重复性,以及(iv)用作研磨剂的金属氧化物粉末。
本发明的上述特性和其它特性都将从下文中描述的本发明中成功地获得。
附图说明
图1a和1b是分别说明在金属层的CMP工艺中氧化物磨耗和腐蚀的示意图。
图2是说明在使用根据本发明的浆液组合物的W-CMP工艺中PDTA-Fe的工作原理的示意图。
图3是说明抛光速率对PDTA-Fe的添加量的依赖性的图表。
图4是说明抛光可重复性对苹果酸的添加量的依赖性的图表。
具体实施方式
在本发明中,用于氧化将要被抛光的金属基质的氧化剂优选为过氧化剂如过氧化氢、过氧化苯甲酰、过氧化钙、过氧化钡和过氧化钠;考虑到所得的浆液的氧化能力和分散稳定性,最优选使用过氧化氢。过氧化氢有相对高的氧化电位,但氧化速率很低,以致于避免了由强氧化剂带来的各种问题(除非没有过量使用强氧化剂)。本发明的浆液组合物优选含有0.5~5wt%的过氧化物。
为了弥补浆液的氧化能力,除了过氧化物外使用至少一种无机酸。举例说明优选的无机酸:硝酸、硫酸、盐酸和磷酸。考虑到抛光后表面的污染,最优选硝酸。在本发明中,无机酸也起pH值控制剂的作用,用来促进钨的氧化。在本发明的浆液组合物中无机酸的含量优选为0.001~5.0wt%,更优选0.001~3.0wt%。
在这两种类型的氧化剂即过氧化物和无机酸分别被加入超过上述范围的上限的量的情况下,容易发生氧化物磨耗、腐蚀、凹点和凹坑等等,以及在相反的情况下,不能实现理想的抛光速率。
典型的是,包括少量弱氧化剂如过氧化物和无机酸的CMP浆液组合物能以足够小的速率抛光金属层和阻挡层(主要是Ti/TiN层)以防止氧化物磨耗,但因为过于低的抛光速率,它们对传统的半导体工艺来说是不合适的。虽然过量的氧化剂的加入能改进抛光速率,因为强酸性,这样会导致各种问题包括氧化物磨耗和腐蚀,进一步使控制浆液困难。作为这种方式的替换方式,我们使用特殊的金属络合物,以有效获得半导体工艺所要求的抛光速率。由丙二胺四乙酸(PDTA)配体和金属(M)原子组成的金属络合物,其中O-M的键能低于O-W的键能。下文中,这样的金属络合物称作‘PDTA-M络合物’,或简称为‘PDTA-M’。
PDTA-M络合物增强抛光速率的可能的机理可以被解释为:PDTA配体同在CMP工艺中从氧化后的钨层上被研磨下来的氧化钨WXOY形成络合物,并且将它们从反应体系中除去,使钨层的氧化反应变得容易。通常,虽然可以使用强的氧化剂,但它不能克服由根据抛光工艺的研磨后的金属氧化物的积累引起的抛光速率的降低,因为金属氧化物通过再粘附到将要被抛光的金属层的表面上,抑制了抛光。本发明目的在于解决该再粘附问题。PDTA配体是多齿配体,它有四个配体原子,于是很容易形成螯合物PDTA-M。有优势的是,通过选择金属原子使得O-M的键能低于O-W的键能,在抛光工艺过程中PDTA-M络合物能同时自发转变成PDTA-W络合物。例如,在使用PDTA-Fe络合物的情况下,O-Fe的键能为93.3kcal/mol,而O-W的键能为160kcal/mol,因而配位到PDTA配体上的Fe原子能容易地用W原子替换,也就是PDTA-Fe络合物转化成PDTA-W络合物。于是,通过使用PDTA-M络合物,氧化钨的再粘附被有效地阻挡,因此包括抛光速率的抛光性能的可重复性以及选择性也能被改进。
根据成本和抛光金属氧化物的吸收效率,虽然PDTA-Fe络合物是最优选的,但任何金属原子都能替代Fe,要有该金属原子能同PDTA配体形成配位键并且该金属原子键合到氧原子上比钨金属更弱。这样的PDTA-金属络合物的非限制性实例包括PDTA-Ni和PDTA-Co。图2图解说明了在使用本发明的浆液组合物抛光钨层的过程中,PDTA-Fe络合物的工作机理。
而且,PDTA-M络合物改进了本发明的浆液组合物的储存稳定性,于是在一段长时间后,以刮擦和抛光速率为代表的抛光性能是可重复的。在二氧化硅粉末作为研磨剂被加到浆液组合物的情况下,在通常的金属抛光工艺所需的酸性pH下,二氧化硅的分散性必然大幅降低,因为在pH2~4范围内,二氧化硅的等电位点有最小的绝对值。因而,随着时间的推移,二氧化硅颗粒的的再聚集自发地进行从而形成了大的聚集体,引起沉淀和擦伤。PDTA-M络合物防止了包括二氧化硅的研磨颗粒的这样的聚集,于是增强了本发明的浆液组合物的长期储存稳定性。
PDTA-M络合物优选以0.001~0.5wt%的量被添加到本发明的浆液组合物中,更优选0.05~0.3wt%。如果添加过量的PDTA-M络合物,在浆液组合物中金属杂质增加,于是所得的半导体产品的可靠性将变差。另一方面,如果PDTA-M络合物的量不足,捕捉氧化钨以及稳定研磨剂分散性的效率降低。
在本发明中当过氧化氢用作氧化剂的情况下,随着时间推移,因为过氧化氢降解成O2和H2O,浆液组合物的氧化能力变差。基于该观察,我们使用至少一种带有一个或多个羧基的羧酸来进一步增强本发明的浆液组合物的抛光性能可重复性和储存稳定性。这样的羧酸的非限制性实例包括乙酸、柠檬酸、戊二酸、乙醇酸、甲酸、乳酸、苹果酸、马来酸、草酸、邻苯二甲酸、琥珀酸和酒石酸,其中苹果酸是最优选的。在本发明的浆液组合物中羧酸的含量优选是0.1~10wt%,更优选是0.1~2wt%。超过10wt%的过量羧酸会进一步降低浆液组合物的分散稳定性,同时用不足量的羧酸不能获得理想的效果。
在本发明中,金属氧化物粉末如二氧化硅、氧化铝、二氧化铈和二氧化钛能被用作抛光被氧化剂氧化的钨膜的研磨剂,二氧化硅是最优选的,因为它提供了优良的分散性和擦伤的最小的可能性。在本发明的浆液组合物中,优选金属氧化物粉末为0.1~10wt%,更优选为1~7wt%。如果其超过10wt%,浆液组合物的分散稳定性变差,而且会发生擦伤和氧化物磨耗,如果其低于0.1wt%,不能获得对于通常的半导体工艺合适的抛光速率。
参考下面的实施例,本发明能被更清楚地理解。下面的实施例不以任何方式限制本发明的保护范围。每个实施例获得的各个浆液组合物的抛光性能被如下评价:
●抛光机:型号NO.6EC(STRASBAUGH,USA)
●抛光条件:
—垫块类型:IC1400/SubaIV Stacked(Rodel,USA)
—压板速度:75rpm
—主轴速度:35rpm
—压力:4psi
—反压:0psi
—温度:25℃
—浆液流速:250ml/min
●抛光基质:W均厚晶片(blanket wafers)被用作测试晶片,它们中的每一个通过在聚硅晶片上顺序沉淀1000的HTO层、1000的TiN层和10000的W层来制备。
实施例1:抛光速率对PDTA-Fe的添加量的依赖性
在烧瓶中添加50g的Aerosil 90G(Degussa AG,Germany),917.5g去离子水,10.0g苹果酸、0.3g硝酸和20.0g过氧化氢,然后在2000rpm下搅拌2小时,随后在1200psi下高压分散。所得的浆液用1μm的过滤器过滤,且0.0g、0.02g、4.0g或10.0g的PDTA-Fe被加入,获得抛光浆液组合物。在上述的条件下用各个浆液组合物进行测试晶片(W均厚晶片)的抛光,持续2分钟。所得的结果列在表1和图3。
表1
浆液 | PDTA-Fe | 对W*的抛光速率 | 对P-TEOS**的抛光速率 |
I | 0.0g | 863/min | 48/min |
II | 0.02g | 1006/min | 53/min |
III | 4.0g | 2445/min | 87/min |
IV | 10.0g | 2718/min | 105/min |
*W:钨
P-TEOS**:聚原硅酸四乙酯
实施例2:PDTA-Fe对氧化物磨耗和腐蚀的作用。
上述实施例1的浆液III以及有与浆液III相同组成(除了用Fe(NO3)3或KIO3替换PDTA-Fe)的其它浆液组合物,分别被用于在上述条件下抛光线宽0.2μm的图案晶片。结果列在表2中。
表2
试样 | PDTA-Fe | Fe(NO3)3 | KIO3 | 对W的抛光速率 | 氧化剂磨耗 | 腐蚀速度 |
1 | 4.0g | 0.0g | 0.0g | 2486/min | 85 | 10/min |
2 | 0.0g | 15.0g | 0.0g | 2445/min | 460 | 120/min |
3 | 0.0g | 0.0g | 20.0g | 2718/min | 328 | 150/min |
实施例3:抛光性能可重复性对苹果酸的添加量的依赖性
根据在上述实施例1的浆液III的制备中的相同方法制备一系列浆液组合物,除了改变苹果酸的量。在上述的条件下用各个浆液组合物进行测试晶片(W均厚晶片)的抛光,持续2分钟。所得的结果见图4。
实施例4:PDTA-Fe对浆液组合物的分散稳定性的作用
将上述实施例1的浆液III和有与浆液III相同组成(除了缺少PDTA-Fe)的对照浆液组合物,在它们制备后的0、30、60和120天时,进行抛光测试。结果连同通过ELS8000(Ostuka Co.,Japan)的方法测定的各个浆液组合物的平均颗粒尺寸一起列在表3中。
表3
试样 | PDTA-Fe | 制备后的天数 | 对W的抛光速率 | 平均颗粒尺寸 |
1 | 0.0g | 0 | 863/min | 185nm |
2 | 4.0g | 0 | 2445/min | 185nm |
3 | 0.0g | 30 | 425/min | 210nm |
4 | 4.0g | 30 | 2375/min | 186nm |
5 | 0.0g | 60 | 388/min | 248nm |
6 | 4.0g | 60 | 2485/min | 188nm |
7 | 0.0g | 120 | 376/min | 447nm |
8 | 4.0g | 120 | 2418/min | 188nm |
实施例5:抛光性能对过氧化氢和硝酸的添加量的依赖性
根据在上述实施例1的浆液III的制备中的相同方法制备一系列浆液组合物,除了改变过氧化氢或硝酸的量。在上述条件下用各个浆液组合物抛光线宽0.2μm的图案晶片2分钟。结果列在表4中。
表4
试样 | 过氧化氢 | 硝酸 | 对W的抛光速率 | 腐蚀速率 | 氧化物磨损 |
1 | 20g | 0.3g | 2486/min | 10/min | 85 |
2 | 60g | 0.3g | 3253/min | 130/min | 684 |
3 | 2g | 0.3g | 637/min | 4/min | 62 |
4 | 20g | 0.005g | 1204/min | 5/min | 47 |
5 | 20g | 0.8g | 2765/min | 8/min | 116 |
如上所述,根据本发明,在CMP工艺中实现最优化的抛光速率而没有典型的问题如氧化物磨耗、腐蚀、凹点和凹坑等等变得可能。而且,本发明的浆液组合物在分散稳定性方面已经被改进,它们适合长期的储存。
本领域技术人员很容易对本发明进行简单改进和改变,所有这些改进和改变都理解为包括在本发明的范围里。
Claims (8)
1.一种用于金属化学机械抛光的浆液组合物,包括过氧化氢、无机酸、丙二胺四乙酸-金属络合物、羧酸、金属氧化物粉末和去离子水,其中,丙二胺四乙酸-金属络合物中金属原子和氧原子间的键能低于O-W的键能。
2.根据权利要求1所述的组合物,其中所述组合物包括0.5~5wt%的过氧化物、0.001~5.0wt%的无机酸、0.001~0.5w%的丙二胺四乙酸-金属络合物、0.1~10wt%的羧酸和0.1~10wt%的金属氧化物粉末。
3.根据权利要求1所述的组合物,其中所述过氧化物是选自过氧化氢、过氧化苯甲酰、过氧化钙、过氧化钡和过氧化钠中的一种或多种。
4.根据权利要求1所述的组合物,其中所述无机酸是选自硝酸、硫酸、盐酸和磷酸中的一种或多种。
5.根据权利要求1所述的组合物,其中所述丙二胺四乙酸-金属是丙二胺四乙酸-Fe、丙二胺四乙酸-Ni或丙二胺四乙酸-Co。
6.根据权利要求1所述的组合物,其中所述羧酸是选自乙酸、柠檬酸、戊二酸、乙醇酸、甲酸、乳酸、苹果酸、马来酸、草酸、邻苯二甲酸、琥珀酸和酒石酸中的一种或多种。
7.根据权利要求1所述的组合物,其中所述金属氧化物是二氧化硅、氧化铝、二氧化铈、二氧化钛或它们的混合物。
8.根据权利要求2所述的组合物,其中所述组合物的丙二胺四乙酸-金属络合物的含量为0.05~0.3wt%。
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-
2002
- 2002-07-15 TW TW091115732A patent/TW591089B/zh not_active IP Right Cessation
- 2002-08-06 JP JP2003519982A patent/JP3987490B2/ja not_active Expired - Lifetime
- 2002-08-06 EP EP02755950A patent/EP1421610B1/en not_active Expired - Lifetime
- 2002-08-06 DE DE60215956T patent/DE60215956T2/de not_active Expired - Lifetime
- 2002-08-06 CN CN02815444.4A patent/CN1243370C/zh not_active Expired - Lifetime
- 2002-08-06 IL IL16018402A patent/IL160184A0/xx unknown
- 2002-08-06 WO PCT/KR2002/001492 patent/WO2003015148A1/en active IP Right Grant
- 2002-08-06 US US10/485,500 patent/US6930054B2/en not_active Expired - Lifetime
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2007
- 2007-04-18 JP JP2007109688A patent/JP2007243209A/ja active Pending
Also Published As
Publication number | Publication date |
---|---|
TW591089B (en) | 2004-06-11 |
EP1421610A1 (en) | 2004-05-26 |
JP2004538636A (ja) | 2004-12-24 |
US6930054B2 (en) | 2005-08-16 |
CN1539162A (zh) | 2004-10-20 |
EP1421610B1 (en) | 2006-11-08 |
DE60215956T2 (de) | 2007-05-10 |
JP2007243209A (ja) | 2007-09-20 |
JP3987490B2 (ja) | 2007-10-10 |
IL160184A0 (en) | 2004-07-25 |
US20040244911A1 (en) | 2004-12-09 |
WO2003015148A1 (en) | 2003-02-20 |
EP1421610A4 (en) | 2004-12-15 |
DE60215956D1 (de) | 2006-12-21 |
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