WO2019011253A1 - Chemical-mechanical polishing slurry - Google Patents

Chemical-mechanical polishing slurry Download PDF

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WO2019011253A1
WO2019011253A1 PCT/CN2018/095201 CN2018095201W WO2019011253A1 WO 2019011253 A1 WO2019011253 A1 WO 2019011253A1 CN 2018095201 W CN2018095201 W CN 2018095201W WO 2019011253 A1 WO2019011253 A1 WO 2019011253A1
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mechanical polishing
polishing liquid
chemical mechanical
polyquaternium
polishing
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PCT/CN2018/095201
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French (fr)
Chinese (zh)
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李守田
尹先升
贾长征
王雨春
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安集微电子科技（上海）股份有限公司
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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

Definitions

  • the invention relates to the field of chemical mechanical polishing, in particular to a chemical mechanical polishing liquid applied in STI polishing.
  • Cerium oxide is an important CMP polishing liquid abrasive. Compared with traditional silica sol abrasives, cerium oxide has more efficient polishing properties for silica. It has been widely used in CMP polishing of STI and ILD. However, in STI CMP polishing applications, it is generally required to have a high polishing rate of the silicon dioxide dielectric layer, while the low silicon nitride dielectric layer has a low polishing rate, preferably the polishing rate of the silicon nitride dielectric layer. Can be close to zero. That is to say, the selection ratio of silicon dioxide to silicon nitride which is required to be high is preferably higher than 100:1. Organic molecules have been able to effectively inhibit the polishing rate of silicon nitride.
  • Electrochemical and Solid-State Letter (vol 8 (8), page G218-G221, year 2005) reported that compounds such as picolinic acid can Increasing the polishing rate of the polishing liquid to the silicon dioxide dielectric layer while suppressing the polishing rate of the silicon nitride is at least 20 times smaller than that of the ordinary polishing liquid, so that the selection ratio of the polishing liquid to silicon dioxide and silicon nitride exceeds 200.
  • the synergistic action of 4-hydroxybenzoic acid and polyquaternium-37 is used to increase the polishing rate of silica while controlling the generation of butterfly depressions, thereby obtaining an STI chemical mechanical polishing excellent in polishing effect. liquid.
  • the present invention provides a chemical mechanical polishing liquid applied to STI using sol type cerium oxide as abrasive particles while adding polyquaternium-37 and 4-hydroxybenzoic acid as additives in polyquaternium-37 Synergistic action with 4-hydroxybenzoic acid achieves a technical effect of increasing the polishing rate of silica while controlling the generation of butterfly depressions.
  • the present invention provides a chemical mechanical polishing liquid comprising sol type cerium oxide and polyquaternium-37 and 4-hydroxybenzoic acid.
  • the chemical mechanical polishing liquid further contains a pH adjuster.
  • the sol type cerium oxide is contained in an amount of 0.1 to 1.0% by weight.
  • the content of the polyquaternium-37 is 30-60 ppm, and the content of the 4-hydroxybenzoic acid is 200-600 ppm.
  • the pH adjusting agent is selected from the group consisting of potassium hydroxide (KOH) and/or nitric acid (HNO3).
  • the chemical mechanical polishing liquid also contains oligosaccharide molecules.
  • the oligosaccharide molecule is further selected from the group consisting of dextran and/or ⁇ -cyclodextrin.
  • the polishing liquid has a pH of from 4.0 to 5.0.
  • the technical advantage of the present invention is that the present invention uses sol type cerium oxide as the abrasive particles, while adding polyquaternium-37 and 4-hydroxybenzoic acid as additives in the polyquaternium-37 and Under the synergistic action of 4-hydroxybenzoic acid, the technical effect of improving the polishing rate of silica while controlling the generation of butterfly depression is achieved.
  • PQ-37 is synthesized by a radical polymerization in which the monomer is methacryloyloxyethyltrimethylammonium chloride.
  • 200 ppm of hydrogen peroxide, 10 ppm of ferric nitrate and 80% of methacryloyloxyethyltrimethylammonium chloride aqueous solution were mixed until homogeneously mixed, and then the mixture was heated to 55 ° C for 30 minutes, and radical polymerization was started. The solution was incubated at 55 ° C for 16 hours until the reaction was complete.
  • the molecular structure of the monomeric methacryloyloxyethyltrimethylammonium chloride and the polymerization principle are as follows:
  • the reference example is a composition containing 0.1-1.0% by weight of sol-type cerium oxide, 200 ppm of dextran or ⁇ -cyclodextrin; other examples and comparative examples are added with a certain amount based on the reference example.
  • Polyquaternium-37 (PQ-37) and/or 4-hydroxybenzoic acid (4-HBA) and the pH is adjusted to 4.0-5.0 with potassium hydroxide (KOH) or nitric acid (HNO3).
  • the TEOS blank wafer was polished using a Mirra polishing machine.
  • the corresponding polishing conditions included: IC1010 polishing pad, Platten and carrier rotation speeds of 93 rpm and 87 rpm, pressure 1.5 psi, 2 psi and 5 psi, polishing fluid flow rate of 150 mL/min, polishing.
  • the time is 60 seconds.
  • the TEOS film thickness was measured using a NanoSpec film thickness measuring system (NanoSpec 6100-300, Shanghai Nanospec Technology Corporation). Starting at 10 mm from the edge of the wafer, 49 points were measured at equal intervals on the diameter line. The polishing rate is an average of 49 points.
  • Table 1 The test results are shown in Table 1:
  • the data in Table 1 shows that the addition of 500 ppm 4-HBA in the reference solution reduces the polishing rate of TEOS, and the addition of 50 ppm PQ-37 increases the polishing rate of TEOS.
  • 500 ppm 4-HBA and 50 ppm PQ-37 were added simultaneously, the TEOS polishing rate increased more than the 50 ppm PQ-37 alone.
  • the comparative examples and the results of Examples 1E to 1H show that the addition amounts of 4-HBA and PQ-37 correspond to the range of 200-600 ppm and 30-60 ppm, respectively, and all show significant synergistic effects, pH and strontium oxide concentration. Adjustment does not change the above-mentioned synergistic characteristics. This shows that under the synergistic action of polyquaternium-37 and 4-hydroxybenzoic acid, the technical effect of increasing the polishing rate of silica while controlling the generation of butterfly depression is achieved.

Abstract

Provided is a chemical-mechanical polishing slurry, comprising sol-type cerium oxide and benzoic acid compounds. The chemical-mechanical polishing slurry can control the generation of dishing while increasing the polishing rate.

Description

一种化学机械抛光液Chemical mechanical polishing liquid 技术领域Technical field
本发明涉及化学机械抛光领域，尤其涉及一种应用于STI抛光中化学机械抛光液。The invention relates to the field of chemical mechanical polishing, in particular to a chemical mechanical polishing liquid applied in STI polishing.
背景技术Background technique
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，最好高于100∶1。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。Cerium oxide is an important CMP polishing liquid abrasive. Compared with traditional silica sol abrasives, cerium oxide has more efficient polishing properties for silica. It has been widely used in CMP polishing of STI and ILD. However, in STI CMP polishing applications, it is generally required to have a high polishing rate of the silicon dioxide dielectric layer, while the low silicon nitride dielectric layer has a low polishing rate, preferably the polishing rate of the silicon nitride dielectric layer. Can be close to zero. That is to say, the selection ratio of silicon dioxide to silicon nitride which is required to be high is preferably higher than 100:1. Organic molecules have been able to effectively inhibit the polishing rate of silicon nitride. For example, Electrochemical and Solid-State Letter (vol 8 (8), page G218-G221, year 2005) reported that compounds such as picolinic acid can Increasing the polishing rate of the polishing liquid to the silicon dioxide dielectric layer while suppressing the polishing rate of the silicon nitride is at least 20 times smaller than that of the ordinary polishing liquid, so that the selection ratio of the polishing liquid to silicon dioxide and silicon nitride exceeds 200.
发明内容Summary of the invention
研究表明，4-羟基苯甲酸，3-胺基苯甲酸和3，5-二胺基苯甲酸能够抑制氮化硅的抛光速率，而对氧化硅的速率影响很小，从而达到很高的选择比，同时不会引起氧化硅抛光速率不均匀的问题。但是，在STI的应用中，除了抑制氮化硅的速率同时，还要控制碟形凹陷(dishing)；聚季铵盐-37(PQ-37，poly(N，N，N-trimethyl-2-[(2-methylacryloyl)oxy]ethanaminium chloride))可控制 氧化硅的抛光速率，从而取得低碟形凹陷(dishing)。因此，本发明中，利用4-羟基苯甲酸和聚季铵盐-37的协同作用来提高二氧化硅的抛光速率，同时控制蝶形凹陷的产生，获得一种抛光效果优异的STI化学机械抛光液。Studies have shown that 4-hydroxybenzoic acid, 3-aminobenzoic acid and 3,5-diaminobenzoic acid can inhibit the polishing rate of silicon nitride, but have little effect on the rate of silicon oxide, thus achieving a high choice. The ratio does not cause the problem of uneven polishing rate of silicon oxide. However, in the application of STI, in addition to suppressing the rate of silicon nitride, it is also necessary to control dishing; polyquaternium-37 (PQ-37, poly(N, N, N-trimethyl-2-) [(2-methylacryloyl)oxy]ethanaminium chloride)) can control the polishing rate of silicon oxide, thereby achieving low dishing. Therefore, in the present invention, the synergistic action of 4-hydroxybenzoic acid and polyquaternium-37 is used to increase the polishing rate of silica while controlling the generation of butterfly depressions, thereby obtaining an STI chemical mechanical polishing excellent in polishing effect. liquid.
具体地，本发明提供一种应用于STI的化学机械抛光液，采用溶胶型氧化铈作为研磨颗粒，同时添加聚季铵盐-37和4-羟基苯甲酸作为添加剂，在聚季铵盐-37和4-羟基苯甲酸的协同作用下，实现提高二氧化硅的抛光速率，同时控制蝶形凹陷的产生的技术效果。Specifically, the present invention provides a chemical mechanical polishing liquid applied to STI using sol type cerium oxide as abrasive particles while adding polyquaternium-37 and 4-hydroxybenzoic acid as additives in polyquaternium-37 Synergistic action with 4-hydroxybenzoic acid achieves a technical effect of increasing the polishing rate of silica while controlling the generation of butterfly depressions.
本发明提供一种化学机械抛光液，包括溶胶型氧化铈以及聚季铵盐-37和4-羟基苯甲酸。The present invention provides a chemical mechanical polishing liquid comprising sol type cerium oxide and polyquaternium-37 and 4-hydroxybenzoic acid.
优选地，所述化学机械抛光液还含有pH调节剂。Preferably, the chemical mechanical polishing liquid further contains a pH adjuster.
优选地，所述溶胶型氧化铈的含量为0.1-1.0wt％。Preferably, the sol type cerium oxide is contained in an amount of 0.1 to 1.0% by weight.
优选地，所述聚季铵盐-37的含量为30-60ppm，所述4-羟基苯甲酸的含量为200-600ppm。Preferably, the content of the polyquaternium-37 is 30-60 ppm, and the content of the 4-hydroxybenzoic acid is 200-600 ppm.
优选地，所述pH调节剂选自氢氧化钾(KOH)和/或硝酸(HNO3)。Preferably, the pH adjusting agent is selected from the group consisting of potassium hydroxide (KOH) and/or nitric acid (HNO3).
所述化学机械抛光液还含有低聚糖分子。低聚糖分子进一步选自葡聚糖和/或β-环糊精。The chemical mechanical polishing liquid also contains oligosaccharide molecules. The oligosaccharide molecule is further selected from the group consisting of dextran and/or β-cyclodextrin.
优选地，所述抛光液的pH为4.0-5.0。Preferably, the polishing liquid has a pH of from 4.0 to 5.0.
与现有技术相比较，本发明的技术优势在于：本发明采用溶胶型氧化铈作为研磨颗粒，同时添加聚季铵盐-37和4-羟基苯甲酸作为添加剂，在聚季铵盐-37和4-羟基苯甲酸的协同作用下，实现提高二氧化硅的抛光速率，同时控制蝶形凹陷的产生的技术效果。Compared with the prior art, the technical advantage of the present invention is that the present invention uses sol type cerium oxide as the abrasive particles, while adding polyquaternium-37 and 4-hydroxybenzoic acid as additives in the polyquaternium-37 and Under the synergistic action of 4-hydroxybenzoic acid, the technical effect of improving the polishing rate of silica while controlling the generation of butterfly depression is achieved.
具体实施方式Detailed ways
下面结合具体实施例，详细阐述本发明的优势。Advantages of the present invention are explained in detail below in conjunction with specific embodiments.
PQ-37合成：PQ-37 synthesis:
PQ-37是通过自由基聚合反应合成的，其中，单体是甲基丙烯酰氧乙基三甲基氯化铵。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直至混合均匀，然后将混合液加热到55℃，恒温30分钟，自由基聚合反应开始。溶液在55℃下恒温16小时，直到反应完成。单体甲基丙烯酰氧乙基三甲基氯化铵的分子结构，以及聚合反应原理如下所示：PQ-37 is synthesized by a radical polymerization in which the monomer is methacryloyloxyethyltrimethylammonium chloride. 200 ppm of hydrogen peroxide, 10 ppm of ferric nitrate and 80% of methacryloyloxyethyltrimethylammonium chloride aqueous solution were mixed until homogeneously mixed, and then the mixture was heated to 55 ° C for 30 minutes, and radical polymerization was started. The solution was incubated at 55 ° C for 16 hours until the reaction was complete. The molecular structure of the monomeric methacryloyloxyethyltrimethylammonium chloride and the polymerization principle are as follows:
Figure PCTCN2018095201-appb-000001
Figure PCTCN2018095201-appb-000001
公式1.单体甲基丙烯酰氧乙基三甲基氯化铵的分子结构Formula 1. Molecular structure of monomeric methacryloyloxyethyltrimethylammonium chloride
Fe 2++H 2O 2→Fe 3++HO·+OH -     (1) Fe 2+ +H 2 O 2 →Fe 3+ +HO·+OH - (1)
Fe 3++H 2O 2→Fe 2++HOO·+H +     (2) Fe 3+ +H 2 O 2 →Fe 2+ +HOO·+H + (2)
HO·+n CH 2＝CHR-CH 3→OH -+(-CH 2-CHRCH 3-) n   (3) HO·+n CH 2 =CHR-CH 3 →OH - +(-CH 2 -CHRCH 3 -) n (3)
R＝-COO-CH 2CH 2N(CH 3) 3Cl R=-COO-CH 2 CH 2 N(CH 3 ) 3 Cl
公式2.自由基聚合反应制备PQ-37Formula 2. Free radical polymerization to prepare PQ-37
高分子的聚季铵盐-37和4-羟基苯甲酸的协同作用：Synergistic effect of polymeric polyquaternium-37 and 4-hydroxybenzoic acid:
本实施例中，基准例为含有0.1-1.0wt％溶胶型氧化铈，200ppm葡聚糖或β-环糊精的组合物；其他实施例及对比例则在基准例的基础上添加一定含量的聚季铵盐-37(PQ-37)和/或4-羟基苯甲酸(4-HBA)，并以氢氧化钾(KOH)或硝酸(HNO3)调节pH至4.0-5.0。In this embodiment, the reference example is a composition containing 0.1-1.0% by weight of sol-type cerium oxide, 200 ppm of dextran or β-cyclodextrin; other examples and comparative examples are added with a certain amount based on the reference example. Polyquaternium-37 (PQ-37) and/or 4-hydroxybenzoic acid (4-HBA), and the pH is adjusted to 4.0-5.0 with potassium hydroxide (KOH) or nitric acid (HNO3).
采用Mirra抛光机台对TEOS空白晶圆进行抛光测试，对应抛光条件包括：IC1010抛光垫，Platten和Carrier转速分别为93rpm和87rpm，压力1.5psi，2psi和5psi，抛光液流速为150mL/min，抛光时间为60秒。TEOS膜厚是用NanoSpec膜厚测量系统(NanoSpec6100-300，Shanghai Nanospec 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。测试结果如表1所示：The TEOS blank wafer was polished using a Mirra polishing machine. The corresponding polishing conditions included: IC1010 polishing pad, Platten and carrier rotation speeds of 93 rpm and 87 rpm, pressure 1.5 psi, 2 psi and 5 psi, polishing fluid flow rate of 150 mL/min, polishing. The time is 60 seconds. The TEOS film thickness was measured using a NanoSpec film thickness measuring system (NanoSpec 6100-300, Shanghai Nanospec Technology Corporation). Starting at 10 mm from the edge of the wafer, 49 points were measured at equal intervals on the diameter line. The polishing rate is an average of 49 points. The test results are shown in Table 1:
表1.聚季铵盐-37或4-羟基苯甲酸的浓度在不同压力下对TEOS速率影响Table 1. Effect of concentration of polyquaternium-37 or 4-hydroxybenzoic acid on TEOS at different pressures
Figure PCTCN2018095201-appb-000002
Figure PCTCN2018095201-appb-000002
表1的数据表明，在基准液中，加入500ppm 4-HBA，可降低TEOS的抛光速率，加入50ppm PQ-37，可增加TEOS的抛光速率。当500ppm 4-HBA和50ppm PQ-37同时加入时，TEOS的抛光速率增加的比单独的50ppm PQ-37还要高。另外，对比例及实施例1E～1H结果表明，4-HBA和PQ-37的添加量分别对应200-600ppm和30-60ppm范围内，均能显示出显著的协同效应，pH和氧化铈浓度的调节不改变上述协同特性。这说明在聚季铵盐-37和4-羟基苯甲酸的协同作用下，实现提高二氧化硅的抛光速率，同时控制蝶形凹陷的产生的技术效果。The data in Table 1 shows that the addition of 500 ppm 4-HBA in the reference solution reduces the polishing rate of TEOS, and the addition of 50 ppm PQ-37 increases the polishing rate of TEOS. When 500 ppm 4-HBA and 50 ppm PQ-37 were added simultaneously, the TEOS polishing rate increased more than the 50 ppm PQ-37 alone. In addition, the comparative examples and the results of Examples 1E to 1H show that the addition amounts of 4-HBA and PQ-37 correspond to the range of 200-600 ppm and 30-60 ppm, respectively, and all show significant synergistic effects, pH and strontium oxide concentration. Adjustment does not change the above-mentioned synergistic characteristics. This shows that under the synergistic action of polyquaternium-37 and 4-hydroxybenzoic acid, the technical effect of increasing the polishing rate of silica while controlling the generation of butterfly depression is achieved.
应当注意的是，本发明的实施例有较佳的实施性，且并非对本发明作任何形式的限制，任何熟悉该领域的技术人员可能利用上述揭示的技术内容变更或修饰为等同的有效实施例，但凡未脱离本发明技术方案的内容，依据本发明的技术实质对以上实施例所作的任何修改或等同变化及修饰，均仍属于本发明技术方案的范围内。It should be noted that the embodiments of the present invention are preferred embodiments, and are not intended to limit the scope of the present invention. Any one skilled in the art may use the above-disclosed technical contents to change or modify the equivalent embodiments. Any modification or equivalent changes and modifications of the above embodiments in accordance with the technical spirit of the present invention are still within the scope of the technical solutions of the present invention.

Claims (10)

  1. 一种化学机械抛光液，其特征在于，包括溶胶型氧化铈和苯甲酸类化合物。A chemical mechanical polishing liquid characterized by comprising a sol type cerium oxide and a benzoic acid compound.
  2. 如权利要求1所述的化学机械抛光液，其特征在于，所述苯甲酸类化合物为4-羟基苯甲酸。The chemical mechanical polishing liquid according to claim 1, wherein the benzoic acid compound is 4-hydroxybenzoic acid.
  3. 如权利要求1或2所述的化学机械抛光液，其特征在于，所述化学机械抛光液还含有聚季铵盐。The chemical mechanical polishing liquid according to claim 1 or 2, wherein the chemical mechanical polishing liquid further contains a polyquaternium.
  4. 如权利要求3所述的化学机械抛光液，其特征在于，所述聚季铵盐为聚季铵盐-37。The chemical mechanical polishing liquid according to claim 3, wherein the polyquaternium is polyquaternium-37.
  5. 如权利要求1所述的化学机械抛光液，其特征在于，所述溶胶型氧化铈的含量为0.1-1.0wt％。The chemical mechanical polishing liquid according to claim 1, wherein the sol type cerium oxide is contained in an amount of from 0.1 to 1.0% by weight.
  6. 如权利要求4所述的化学机械抛光液，其特征在于，所述聚季铵盐-37的含量为30-60ppm。The chemical mechanical polishing liquid according to claim 4, wherein the polyquaternium-37 is contained in an amount of from 30 to 60 ppm.
  7. 如权利要求2所述的化学机械抛光液，其特征在于，所述4-羟基苯甲酸的含量为200-600ppm。The chemical mechanical polishing liquid according to claim 2, wherein the 4-hydroxybenzoic acid is contained in an amount of from 200 to 600 ppm.
  8. 如权利要求1-3任一所述的化学机械抛光液，其特征在于，所述抛光液还含有低聚糖分子。The chemical mechanical polishing liquid according to any one of claims 1 to 3, wherein the polishing liquid further contains oligosaccharide molecules.
  9. 如权利要求8所述的化学机械抛光液，其特征在于，所述低聚糖分子选自葡聚糖和/或β-环糊精。The chemical mechanical polishing liquid according to claim 8, wherein the oligosaccharide molecule is selected from the group consisting of dextran and/or β-cyclodextrin.
  10. 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为4.0-5.0。The chemical mechanical polishing liquid according to claim 1, wherein the polishing liquid has a pH of from 4.0 to 5.0.
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