WO2015096629A1 - 一种应用于sti领域的化学机械抛光液及其使用方法 - Google Patents

一种应用于sti领域的化学机械抛光液及其使用方法 Download PDF

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WO2015096629A1
WO2015096629A1 PCT/CN2014/093678 CN2014093678W WO2015096629A1 WO 2015096629 A1 WO2015096629 A1 WO 2015096629A1 CN 2014093678 W CN2014093678 W CN 2014093678W WO 2015096629 A1 WO2015096629 A1 WO 2015096629A1
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polishing liquid
mechanical polishing
chemical mechanical
liquid according
polishing
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PCT/CN2014/093678
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French (fr)
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尹先升
房庆华
王雨春
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安集微电子（上海）有限公司
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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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
    • C08L5/16—Cyclodextrin; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • C09K3/1454—Abrasive powders, suspensions and pastes for polishing
    • C09K3/1472—Non-aqueous liquid suspensions
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • C08L33/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof

Definitions

  • the present invention relates to a chemical mechanical polishing liquid, and more particularly to a polishing liquid in which the abrasive particles are cerium oxide.
  • Shallow trench isolation is currently the primary method of device isolation in IC fabrication.
  • the first step is to create a number of trenches at predetermined locations on the substrate, typically using an anisotropic etch.
  • silicon dioxide is deposited in each of the trenches, and then the silicon dioxide is polished by CMP and polished down to the silicon nitride layer to form an STI structure. Polishing of STI requires not only a high removal rate of HDP oxide (silica) and a high selectivity to silicon nitride, but also requires very low surface defect indicators and polishing uniformity in different density regions, as this Directly determines the efficiency of device isolation.
  • Silica is currently the most widely used CMP abrasive, its silica polishing rate is generally low, and generally has a lower silica/silicon nitride polishing selectivity ratio.
  • patent 200510116191.9 discloses a silicon oxide At the end of the polishing solution, the polishing rate of silica is low, and the selection of silica/silicon nitride polishing is relatively low. Due to its special crystal structure and chemical activity, cerium oxide has high selective polishing characteristics for silicon oxide and silicon nitride under specific formulation conditions. It is the main abrasive used in STI polishing, but due to the surface morphology of cerium oxide. There are many corners, so it is easy to cause defects such as scratches during polishing.
  • Patent 101065458A uses yttrium oxide as an abrasive to achieve a high selectivity silica/silicon nitride polishing selectivity ratio under the synergistic effect of cationic polymers, but this patent does not consider scratch suppression of TEOS surfaces during polishing.
  • Patent 2005100884709 proposes the addition of polyvinylpyrrolidone to the polishing bath to improve polishing uniformity, but fails to give the effect of the addition of polyvinylpyrrolidone on the polishing selectivity.
  • the invention discloses a CMP polishing liquid for polishing silicon dioxide and silicon nitride, which is characterized in that nano cerium oxide is used as an abrasive, and nitriding can be effectively suppressed by adding an oligomeric cyclic saccharide compound.
  • the silicon polishing rate achieves a high silicon dioxide/silicon nitride polishing selectivity ratio (>30); by adding an organic high molecular polymer, defects such as pits and scratches during polishing are reduced or avoided.
  • the invention discloses an STI polishing liquid with cerium oxide as an abrasive.
  • a cyclic oligosaccharide compound and an organic high molecular polymer can be applied on STI, thereby making silicon dioxide (TEOS)/nitrogen.
  • TEOS silicon dioxide
  • the silicon (Si 3 N 4 ) polishing selection ratio is greater than 30, and the occurrence of defects such as dishing, scratch, and the like during polishing is avoided or reduced.
  • the STI polishing liquid contains: (a) 0.1% to 2% cerium oxide abrasive (b) 0.1% to 5% cyclic oligosaccharide compound (c) 0.05% to 2% organic high molecular polymer (d) 0.1% -1.0% organic polyacid.
  • the polishing solution has a polishing ratio of silicon dioxide (TEOS)/silicon nitride (Si 3 N 4 ) of more than 30, thereby avoiding or reducing the occurrence of defects such as dishing, scratch, etc. during polishing. .
  • the cerium oxide abrasive particles have an average particle diameter of 120 to 200 nm and an average grain size of 20 to 60 nm.
  • the cyclic oligosaccharide compound is selected from the group consisting of ⁇ -cyclodextrin ( ⁇ -CD, 6 glucose ring bonds), ⁇ -cyclodextrin ( ⁇ -CD, 7 glucose rings).
  • ⁇ -cyclodextrin ⁇ -CD, 8 glucose ring-bonds
  • ⁇ -cyclodextrin ⁇ -CD, 8 glucose ring-bonds
  • the constituent unit of the cyclic oligosaccharide-based compound is not particularly limited, and the manner of bonding is not particularly limited, and the cyclic oligosaccharide further includes structural isomers and stereoisomers.
  • the organic high molecular polymer may be one or more of the following polymers: polyacrylic acid and its salt compounds (such as sodium polyacrylate, ammonium polyacrylate) molecular weight of 3000-5000; polyethylene Pyrrolidone, molecular weight of 3000-10000; polyethylene glycol, molecular weight of 3000-5000.
  • polyacrylic acid and its salt compounds such as sodium polyacrylate, ammonium polyacrylate
  • polyethylene Pyrrolidone molecular weight of 3000-10000
  • polyethylene glycol molecular weight of 3000-5000.
  • the organic polybasic acid may be one or more of acetic acid, glycine, and citric acid.
  • the polishing liquid may further include deionized water and a pH adjuster.
  • the pH adjusting agent is KOH or H 2 SO 4 ;
  • the polishing liquid has a pH of 4.0 to 11.0, and a more optimized pH range of 4.5 to 10.0.
  • the positive progress of the invention is that the cyclic oligosaccharide compound, the organic high molecular polymer and the organic polybasic acid have a compounding effect, and the silica/silicon nitride polishing is adjusted by adjusting the content of each substance in combination.
  • the selection ratio is greater than 30, to avoid or reduce the occurrence of defects such as depressions and scratches during the polishing process, and the solution is more stable.
  • the reagents and starting materials used in the present invention are commercially available.
  • the particle size of the cerium oxide particles used in the polishing liquid is the average diameter of the average diameter, which is determined by Malvern's Nano ⁇ ZS90 laser particle size analyzer; the grain size of the cerium oxide particles used in the polishing liquid passes through Shimadzu LabX, Japan. XRD-6100 X-ray diffractometer.
  • the cerium oxide particles or silica particles, in Comparative Example 1-3
  • the components other than the abrasive particles are added according to the contents listed in the table.
  • the blank TEOS and Si3N4 were polished in the same conditions, and the polishing parameters were as follows: Logitech polishing pad, downward pressure 3 psi, turntable speed/polishing The head rotation speed was 60/80 rpm, the polishing time was 60 s, and the chemical mechanical polishing slurry flow rate was 100 mL/min.
  • the wafer slices used for polishing are all sliced from commercially available (for example, SVTC, USA) 8-inch coated wafers.
  • TEOS and Si3N4 thicknesses were measured by a NANO SPEC 6100 tester manufactured by Matrics.
  • the removal rate of TEOS and Si3N4 is obtained by dividing the difference in thickness measured before and after polishing by the time taken for polishing.
  • the polishing time is 1 minute.
  • TEOS scratch evaluation TEOS was observed for scratches under a light microscope after polishing.
  • Dishing defect evaluation STI3 mode wafer manufactured by SKW (STI3 patterned The wafer was subjected to a recess defect evaluation polishing experiment, and the depth of the pit defect was evaluated by AFM analysis.
  • a comparison of the polishing effects of the polishing liquids of Example 1-6 and Comparative Example 1-9 of the present invention in Table 4-6 shows that the corresponding polishing liquid in Example 1-6 shows a high polishing rate for TEOS, and also for TEOS.
  • the polishing selection ratio with Si3N4 is greater than 30, and there is no visible scratch on the TEOS surface.
  • Comparative Example 1-3 with silica as the abrasive, it can be seen that even at a solid content of 10%, the corresponding TEOS polishing rate is still lower than 1000 A/min, and the polishing selection ratio of TEOS and Si 3 N 4 can only be 6; Comparative Example 4-9, when the content of the cyclic oligosaccharide compound, the organic high molecular polymer or the organic polybasic acid was changed, it can be seen that the polishing selection ratio of TEOS and Si 3 N 4 was significantly reduced. TEOS scratches and dents have also increased dramatically, failing to meet polishing requirements.
  • wt% of the present invention refers to the mass percentage.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)

Abstract

本发明涉及一种应用于STI领域的化学机械抛光液，含有氧化铈磨料，环状低聚糖类化合物，有机高分子聚合物，有机多元酸。本发明中环状低聚糖类化合物、有机高分子聚合物和有机多元酸具有复配效果，通过调整各物质的含量，结合使用达到调整二氧化硅/氮化硅抛光的选择比大于30，避免或降低抛光过程中凹陷、划痕等缺陷的产生，溶液更稳定的效果。

Description

一种应用于STI领域的化学机械抛光液及其使用方法 技术领域
本发明涉及一种化学机械抛光液，尤其涉及一种研磨颗粒为二氧化铈的抛光液。
技术背景
浅槽隔离(STI)是目前IC制造中器件隔离的主要方法，在STI技术中，第一步是在基材的预定位置上生成若干槽，通常采用各向异性蚀刻法。其次，在各个槽中沉积二氧化硅，然后用CMP法抛光二氧化硅，向下抛光到氮化硅层就形成了STI结构。对STI的抛光不仅要求很高的HDP oxide(二氧化硅)的去除速率和很高的对氮化硅的选择比，而且要求非常低的表面缺陷指标以及不同密度区域的抛光均一性，因为这直接决定了器件隔离的效率。
二氧化硅是目前应用最广泛的CMP研磨剂，其二氧化硅抛光速率普遍较低，通常具有较低的二氧化硅/氮化硅抛光选择比，如专利200510116191.9公开了一种以氧化硅为末了得抛光液，二氧化硅抛光速率较低，其对二氧化硅/氮化硅抛光选择比较低。而氧化铈由于自身特殊的晶体结构和化学活性，在特定配方条件下对氧化硅和氮化硅具有高选择性的抛光特征，是目前STI抛光主要采用的磨料，但由于氧化铈表面形貌较多的棱角，因此在抛光过程中容易引起划伤(scratch)等缺陷。
专利101065458A采用氧化铈为磨料，在阳离子聚合物的协同作用下可实现高选择比二氧化硅/氮化硅抛光选择比，但该专利并未考虑抛光过程中TEOS表面的划伤抑制。专利2005100884709提出在抛光液中加入聚乙烯基吡咯烷酮以提高抛光均一性，但未能给出聚乙烯吡咯烷酮的加入，对抛光选择比有何影响。
本发明公开了一种用于抛光二氧化硅和氮化硅的CMP抛光液，其特征在于以纳米氧化铈为磨料，通过添加低聚环状糖类化合物，可有效抑制氮化 硅抛光速率，实现高的二氧化硅/氮化硅抛光选择比(>30)；通过添加有机高分子聚合物，降低或避免了抛光过程中凹陷、划痕等缺陷的出现。
发明概要
本发明公开了一种以氧化铈为磨料的STI抛光液，该抛光液中，环状低聚糖类化合物以及有机高分子聚合物可在STI上应用，从而使二氧化硅(TEOS)/氮化硅(Si3N4)抛光选择比大于30，并避免或降低了抛光过程中碟形凹槽(Dishing)、划痕(scratch)等缺陷的产生。
该STI抛光液含有：(a)0.1％-2％氧化铈磨料(b)0.1％-5％环状低聚糖类化合物(c)0.05％-2％有机高分子聚合物(d)0.1％-1.0％有机多元酸。该抛光液对二氧化硅(TEOS)/氮化硅(Si3N4)抛光选择比大于30，避免或降低了抛光过程中碟形凹槽(Dishing)、划痕(scratch)等缺陷的产生。
本发明中，所述氧化铈研磨颗粒的平均粒径为120-200纳米，平均晶粒尺寸为20-60纳米。
本发明中，所述环状低聚糖类化合物为选自α‐环糊精(α‐CD，6个葡萄糖环状键合)、β‐环糊精(β‐CD，7个葡萄糖环状键合)、γ‐环糊精(γ‐CD，8个葡萄糖环状键合)中一种或多种，优选β‐环糊精。所述环状低聚糖类化合物的构成单元没有特殊限定，而且键合的方式也没有特殊限定，并且环状低聚糖还包括结构异构体、立体异构体。
本发明中，所述有机高分子聚合物可以为下列聚合物中的一种或多种混合：聚丙烯酸及其盐类化合物(如聚丙烯酸钠、聚丙烯酸铵)分子量在3000-5000；聚乙烯基吡咯烷酮，分子量在3000-10000；聚乙二醇，分子量在3000-5000。
本发明中，所述有机多元酸可以为：醋酸、甘氨酸、柠檬酸中的一种或多种。
本发明中，抛光液中还可进一步包括去离子水和pH值调节剂。
本发明中，所述pH值调节剂为KOH或H2SO4；
本发明中，所述抛光液的pH值为4.0-11.0，更为优化的pH范围为4.5-10.0。
本发明的积极进步效果在于：环状低聚糖类化合物、有机高分子聚合物和有机多元酸具有复配效果，通过调整各物质的含量，结合使用达到调整二氧化硅/氮化硅抛光的选择比大于30，避免或降低抛光过程中凹陷、划痕等缺陷的产生，溶液更稳定的效果。
发明内容
下面通过具体实施例进一步阐述本发明的优点，但本发明的保护范围不仅仅局限于下述实施例。
本发明所用试剂及原料均市售可得。抛光液中使用的氧化铈颗粒的粒径为平均折合直径，其平均粒径由Malvern公司的Nano‐ZS90激光粒度分析仪测定；抛光液中使用的氧化铈颗粒的晶粒度通过日本岛津LabX XRD‐6100型X射线衍射仪测定。首先将氧化铈颗粒(或二氧化硅颗粒，对比例1‐3中)加入设定浓度有机分散剂溶液液中混合均匀，再将除研磨颗粒外的组分按照表中所列的含量，在去离子水中混合均匀，用KOH调节到所需pH值，然后加入有机分散剂分散的研磨颗粒分散液，若pH下降则用KOH调节到所需的pH值，并用去离子水补足百分含量至100wt％，即可制得化学机械抛光液。
表1 本发明的化学机械抛光液实施例配方
Figure PCTCN2014093678-appb-000001
表2 本发明的化学机械抛光液实施例对比例
Figure PCTCN2014093678-appb-000002
表3 本发明的化学机械抛光液实施例对比例
Figure PCTCN2014093678-appb-000003
效果实施例
分别用上述实施例中抛光液1‐6和对比例1‐9的化学机械抛光浆料对空白TEOS和Si3N4，抛光条件相同，抛光参数如下：Logitech抛光垫，向下压力3psi，转盘转速/抛光头转速＝60/80rpm，抛光时间60s，化学机械抛浆料流速100mL/min。抛光所用晶圆切片均由市售(例如美国SVTC公司生产的)8英寸镀膜晶圆切片而成。TEOS和Si3N4厚度由Matrics公司生产的NANO SPEC 6100测试仪测得。用抛光前后测得的厚度差值除以抛光耗用时间即得TEOS和Si3N4的去除速率。抛光时间为1分钟。
TEOS划痕(scratch)评价：抛光后TEOS在光学显微镜下观察划痕。
凹陷(Dishing)缺陷评价：采用SKW公司制造STI3模式晶片(STI3 patterned  wafer)进行凹陷缺陷评价抛光实验，通过AFM分析评价凹陷缺陷深度。
表4‐6中对本发明抛光液实施例1‐6和对比实施例1‐9的抛光效果比较表明，在实施例1‐6中对应抛光液，对TEOS显示了高的抛光速率，同时对TEOS和Si3N4的抛光选择比均大于30，并且TEOS表面无明显可见划痕。对比实施例1‐3以二氧化硅为磨料，可以看出，即使在固含量达到10％，对应TEOS抛光速率仍然低于1000A/min，并且TEOS和Si3N4的抛光选择比最大只能达到6；对比实施例4‐9，在改变了环状低聚糖类化合物、有机高分子聚合物或有机多元酸的含量，可以看出，TEOS和Si3N4的抛光选择比明显减少，TEOS划痕及凹陷也急剧增加，不能满足抛光要求。
表4 本发明的化学机械抛光液实施例抛光结果比较
Figure PCTCN2014093678-appb-000004
表5 本发明的化学机械抛光液对比实施例抛光结果比较
Figure PCTCN2014093678-appb-000005
表6 本发明的化学机械抛光液实施例和对比例抛光结果比较
Figure PCTCN2014093678-appb-000006
应当理解的是，本发明所述wt％均指的是质量百分含量。
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 (14)

  1. 一种应用于STI领域的化学机械抛光液，其特征在于，含有氧化铈磨料，环状低聚糖类化合物，有机高分子聚合物，有机多元酸。
  2. 如权利要求1所述的化学机械抛光液，其特征在于，所述氧化铈磨料的浓度为质量百分比0.1％-2％。
  3. 如权利要求1所述的化学机械抛光液，其特征在于，所述氧化铈磨料的平均粒径为120-200纳米，平均晶粒尺寸为20-60纳米。
  4. 如权利要求1所述的化学机械抛光液，其特征在于，所述环状低聚糖类化合物选自α‐环糊精(α‐CD，6个葡萄糖环状键合)、β‐环糊精(β‐CD，7个葡萄糖环状键合)、γ‐环糊精(γ‐CD，8个葡萄糖环状键合)中一种或多种。
  5. 如权利要求1所述的化学机械抛光液，其特征在于，所述环状低聚糖类化合物的浓度为质量百分比0.1％-5％。
  6. 如权利要求1所述的化学机械抛光液，其特征在于，所述有机高分子聚合物为下列聚合物中的一种或多种混合：聚丙烯酸及其盐类化合物，聚乙烯基吡咯烷酮，聚乙二醇。
  7. 如权利要求6所述的化学机械抛光液，其特征在于，所述聚丙烯酸盐类化合物为聚丙烯酸钠、聚丙烯酸铵。
  8. 如权利要求6所述的化学机械抛光液，其特征在于，所述聚丙烯酸及其盐类化合物的分子量为3000-5000；所述聚乙烯基吡咯烷酮的分子量为3000-10000；所述聚乙二醇的分子量为3000-5000。
  9. 如权利要求1所述的化学机械抛光液，其特征在于，所述有机高分子聚合物的浓度为质量百分比0.05％-2％。
  10. 如权利要求1所述的化学机械抛光液，其特征在于，所述有机多元酸为醋酸、甘氨酸、柠檬酸中的一种或多种。
  11. 如权利要求1所述的化学机械抛光液，其特征在于，所述有机多元酸的浓度为质量百分比0.1％-1.0％。
  12. 如权利要求1所述的化学机械抛光液，其特征在于，所述抛光液还含有pH调节剂和去离子水。
  13. 如权利要求1所述的化学机械抛光液，其特征在于，所述抛光液的pH值为4.0-11.0。
  14. 如权利要求13所述的化学机械抛光液，其特征在于，所述抛光液的pH值为4.5-10.0。
PCT/CN2014/093678 2013-12-26 2014-12-12 一种应用于sti领域的化学机械抛光液及其使用方法 WO2015096629A1 (zh)

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