CN109251674B - 一种化学机械抛光液 - Google Patents
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- 238000005498 polishing Methods 0.000 title claims abstract description 84
- 239000000126 substance Substances 0.000 title claims abstract description 11
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 15
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229920000289 Polyquaternium Polymers 0.000 claims abstract 4
- 229920002553 poly(2-methacrylolyloxyethyltrimethylammonium chloride) polymer Polymers 0.000 claims description 30
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000003002 pH adjusting agent Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 38
- 229910052814 silicon oxide Inorganic materials 0.000 abstract description 22
- 239000002245 particle Substances 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 22
- 235000012431 wafers Nutrition 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000377 silicon dioxide Substances 0.000 description 8
- 229910052581 Si3N4 Inorganic materials 0.000 description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 7
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 7
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 3
- RRHXZLALVWBDKH-UHFFFAOYSA-M trimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)OCC[N+](C)(C)C RRHXZLALVWBDKH-UHFFFAOYSA-M 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
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- 239000000178 monomer Substances 0.000 description 2
- 238000010526 radical polymerization reaction Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- OCKGFTQIICXDQW-ZEQRLZLVSA-N 5-[(1r)-1-hydroxy-2-[4-[(2r)-2-hydroxy-2-(4-methyl-1-oxo-3h-2-benzofuran-5-yl)ethyl]piperazin-1-yl]ethyl]-4-methyl-3h-2-benzofuran-1-one Chemical compound C1=C2C(=O)OCC2=C(C)C([C@@H](O)CN2CCN(CC2)C[C@H](O)C2=CC=C3C(=O)OCC3=C2C)=C1 OCKGFTQIICXDQW-ZEQRLZLVSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- AKMJJGSUTRBWGW-UHFFFAOYSA-N pyridine-2-carboxylic acid Chemical compound OC(=O)C1=CC=CC=N1.OC(=O)C1=CC=CC=N1 AKMJJGSUTRBWGW-UHFFFAOYSA-N 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C09G—POLISHING COMPOSITIONS; SKI WAXES
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- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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- 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
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- 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
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- 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
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- 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
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Abstract
本发明提供了一种化学机械抛光液，包含氧化铈磨料颗粒、聚季铵盐及pH调节剂。本发明中的聚季铵盐可控制氧化硅的抛光速率，使得在高压下达到高的氧化硅抛光速率，在低压下实现低的氧化硅的抛光速率，从而取得较低碟形凹陷(dishing)。
Description
技术领域
本发明涉及化学机械抛光领域，尤其涉及一种化学机械抛光液。
背景技术
氧化铈是一种重要的CMP抛光液磨料，相比于传统硅溶胶磨料，氧化铈对二氧化硅材质具有更高效的抛光特性，已广泛应用于STI和ILD的CMP抛光。但是，在STI的CMP抛光应用中，通常要求具备高的二氧化硅介质层的抛光速率要高，而低的氮化硅介质层的抛光速率要低，最好氮化硅介质层的抛光速率可以接近于零。也就是说，要求高的二氧化硅对氮化硅的选择比。有机分子能够有效地抑制氮化硅的抛光速率已有许多报道，比如，Electrochemical and Solid-State Letter(vol 8(8),page G218-G221,year 2005)报道吡啶甲酸(picolinic acid)等化合物能够提高抛光液对二氧化硅介质层的抛光速率，同时抑制氮化硅的抛光速率，相比普通抛光液减小至少20倍，使得抛光液对二氧化硅和氮化硅的选择比超过200。
但是，在STI应用中，除了抑制氮化硅的抛光速率，同时还要控制碟形凹陷(dishing)。其中一种取得低碟形凹陷数值的方式是在高的压力下(比如，4psi或5psi下)，采用高的氧化硅的抛光速率，在低的压力下(比如，1.5psi下)，采用低的氧化硅的抛光速率。换言之，氧化硅的速率对压力的曲线，应该偏离传统的Prestonian线性方程。而在图形的晶圆抛光时，则需高点的地方要承受大的压力，低点(trench)承受的压力要比高点低很多，CMP的目的就是去除高点的材料，实现平整化。
有报道发现，带正电的季氨盐会对同样带正电的氧化铈摩擦颗粒产生强的电荷排斥作用，但是对带负电的氧化硅晶圆有强的吸引作用，从而达到控制氧化硅抛光速率的目的。但是不是所有的季铵盐都能很好的控制氧化硅的抛光速率。
发明内容
本发明发现聚季铵盐-37(PQ-37)有独特的控制氧化硅抛光速率的能力。聚季铵盐-6(PQ-6)也有独特的控制氧化硅抛光速率的能力。但是，聚季铵盐-6(PQ-6)的缺点是摩擦颗粒的固含量不能低于0.2wt％，如果低于该值，图形晶圆上的抛光速率就会显著降低。而聚季铵盐-37(PQ-37)没有这个问题。本发明用聚季铵盐-37(PQ-37)来控制氧化硅的抛光速率，使得在高压下达到高的氧化硅的抛光速率，在低压下实现低的氧化硅的抛光速率，从而取得较低的碟形凹陷(dishing)。
具体地，本发明提供一种化学机械抛光液。该抛光液包含氧化铈磨料、聚季铵盐-37及pH调节剂。该配方可以控制氧化硅的抛光速率，使得在高的压力下达到较高的氧化硅的抛光速率，在低的压力下达到较低的氧化硅的抛光速率，从而取得较低碟形凹陷(dishing)。
本发明在于提供一种化学机械抛光液，其包含氧化铈研磨颗粒、聚季铵盐-37及pH调节剂。
优选地，所述溶胶型氧化铈研磨颗粒浓度为0.1-1.0wt％。
优选地，所述的聚季铵盐-37浓度为100ppm～1000ppm。
优选地，所述化学机械抛光液的pH值为3.5-5.5。
优选地，所述pH调节剂为氢氧化钾(KOH)和/或硝酸(HNO3)。
与现有技术相比较，本发明的优势在于：本发明在抛光液添加溶胶型氧化铈磨料、聚季铵盐-37及pH调节剂，可以有效地控制氧化硅的抛光速率，使得在高的压力下达到较高的氧化硅的抛光速率，在低的压力下达到较低的氧化硅的抛光速率，从而取得较低碟形凹陷(dishing)。
具体实施方式
下面结合具体实施例详细阐述本发明的优势。
本发明中的聚季铵盐-37(PQ-37)是通过自由基聚合反应合成的，而聚季铵盐-37(PQ-37)的单体是甲基丙烯酰氧乙基三甲基氯化铵。其具体制备方法为，取200ppm双氧水，10ppm硝酸铁与80％的甲基丙烯酰氧乙基三甲基氯化铵水溶液混合几分钟直至混匀，然后加热到55℃，半个小时后自由基聚合反应开始，溶液维持在55度16小时，直到反应完成。具体反应原理如反应式Ⅰ所示。其中，单体甲基丙烯酰氧乙基三甲基氯化铵的分子结构如结构式Ⅰ所示：
Fe2++H2O2→Fe3++HO·+OH- (1)
Fe3++H2O2→Fe2++HOO·+H+ (2)
HO·+n CH2＝CHR-CH3→OH-+(-CH2-CHRCH3-)n (3)
R＝-COO-CH2CH2N(CH3)3Cl
反应式Ⅰ
结构式Ⅰ
本实施例中所选用合成PQ-37原料皆市售可得。具体按照表1中季铵盐和氧化铈的具体组分和含量混合均匀，用水补足质量百分比至100％，以氢氧化钾(KOH)或硝酸(HNO3)调节溶液pH，得到对比及具体实施例如下：
表1.对比例及实施例配比及具体实施结果
将上述实施例和对比例中配制的抛光液分别在不同压力条件下测量对TEOS空白晶圆的抛光速率。
具体抛光条件为，抛光机台为Mirra，IC1010抛光垫，Platten和Carrier转速分别为93rpm和87rpm，压力1.5psi，2psi、3psi、4psi和5psi，抛光液流速为150mL/min，抛光时间为60秒。
上述对比例和实施例的结果表示，聚季铵盐-37(PQ-37)的浓度变化对TEOS抛光速率具有显著的影响。从表1中可以看出，与空白基准样对比，如实施例1B，当聚季铵盐-37(PQ-37)浓度为250ppm时,在3psi到5psi压力区间内，氧化硅的抛光速率高于空白基准样；而，当聚季铵盐-37(PQ-37)的浓度在250ppm到500ppm时，在压力为5psi时，抛光液对氧化硅抛光速率逐渐降低，但降低强度在低压力区(1.5psi到2psi)加快。上述数据表明，在不同抛光液pH条件下，调节抛光液配方中氧化铈和聚季铵盐-7浓度，对应抛光速率与抛光压力条件间均表现出非线性关系。可见，聚季铵盐-37的添加，使氧化铈抛光液显示出典型的非普林斯顿压力-抛光速率曲线关系，对Dishing的出现有良好的抑制效果。如表2所示，对比例2A中含有0.4wt％氧化铈，5ppm PQ-6；对比例2B中含有0.2wt％氧化铈，5ppm PQ-6；实施例2C中含有0.2wt％氧化铈，475ppm PQ-37；将上述抛光液按照上述组分混合均匀，用水补足质量百分比至100％，以氢氧化钾(KOH)或硝酸(HNO3)调节pH至4.5。得到对比及具体实施例如下表所示：
表2对比抛光液和本发明抛光液的抛光效果列表
将上述实施例和对比例中配制的抛光液分别进行不同压力条件下测量TEOS空白晶圆及STI图形晶圆的抛光去除速率。
其抛光条件为，抛光机台为Mirra，IC1010抛光垫，Platten和Carrier转速分别为93rpm和87rpm，，抛光液流速为150mL/min，抛光时间为30秒。
TEOS和SiN膜厚是用NanoSpec膜厚测量系统(NanoSpec6100-300,ShanghaiNanospec Technology Corporation)测出的。从晶圆边缘10mm开始，在直径线上以同等间距测49个点。抛光速率是49点的平均值。图形晶圆的抛光速率测量设在500um/500um(线宽/空间)结构上。
表2的数据表明，含聚季铵盐-37(PQ-37)的抛光液，当其含量是0.4wt％时，在STI图形晶圆上TEOS的抛光速率与空白晶圆的抛光速率接近。在0.2wt％的固含量时，在STI图形晶圆上TEOS的抛光速率远远低于(10倍)空白晶圆的抛光速率。另一方面，含聚季铵盐-37(PQ-37)的抛光液，当其含量是0.2wt％时，抛光压力为2psi时，在STI图形晶圆上TEOS的抛光速率高于空白晶圆的抛光速率(1.37倍)。
综上可见，本发明在抛光液添加氧化铈磨料、聚季铵盐-37及pH调节剂，可以有效地控制氧化硅的抛光速率，使得在高的压力下达到较高的氧化硅的抛光速率，在低的压力下达到较低的氧化硅的抛光速率，从而取得较低碟形凹陷(dishing)。
以上对本发明的具体实施例进行了详细描述，但其只是作为范例，本发明并不限制于以上描述的具体实施例。对于本领域技术人员而言，任何对本发明进行的等同修改和替代也都在本发明的范畴之中。因此，在不脱离本发明的精神和范围下所作的均等变换和修改，都应涵盖在本发明的范围内。
Claims (2)
1.一种化学机械抛光液，由氧化铈磨料、聚季铵盐、水及pH调节剂组成；
所述的聚季铵盐选自聚季铵盐-37；
所述的聚季铵盐-37浓度为250ppm～1000ppm；
所述氧化铈磨料浓度为0.1-1.0wt％；
所述化学机械抛光液的pH值为3.5-5.5。
2.如权利要求1所述的化学机械抛光液，其特征在于，所述pH调节剂为氢氧化钾(KOH)和/或硝酸(HNO3)。
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| PCT/CN2018/095203 WO2019011254A1 (zh) | 2017-07-13 | 2018-07-10 | 一种化学机械抛光液 |
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| CN118222187A (zh) * | 2022-12-13 | 2024-06-21 | 安集微电子科技（上海）股份有限公司 | 一种氧化铈的表面处理方法、一种氧化铈及其用途 |
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| CN101724346A (zh) * | 2008-10-10 | 2010-06-09 | 安集微电子（上海）有限公司 | 一种化学机械抛光液 |
| CN102464947A (zh) * | 2010-11-19 | 2012-05-23 | 安集微电子（上海）有限公司 | 一种化学机械抛光液 |
| US9758697B2 (en) * | 2015-03-05 | 2017-09-12 | Cabot Microelectronics Corporation | Polishing composition containing cationic polymer additive |
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| CN107851568B (zh) * | 2015-07-13 | 2021-10-08 | Cmc材料股份有限公司 | 用于加工介电基板的方法及组合物 |
| KR20170076191A (ko) * | 2015-12-24 | 2017-07-04 | 주식회사 케이씨텍 | 연마입자-분산층 복합체 및 그를 포함하는 연마 슬러리 조성물 |
| CN106927495A (zh) * | 2015-12-31 | 2017-07-07 | 安集微电子科技(上海)有限公司 | 一种氧化铈的制备方法及其cmp应用 |
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| CN105393337A (zh) * | 2013-07-22 | 2016-03-09 | 嘉柏微电子材料股份公司 | 用于氧化硅、氮化硅、和多晶硅材料的化学机械抛光的组合物和方法 |
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