JP6396741B2 - Polishing composition, method for producing the same, and polishing method - Google Patents
Polishing composition, method for producing the same, and polishing method Download PDFInfo
- Publication number
- JP6396741B2 JP6396741B2 JP2014198547A JP2014198547A JP6396741B2 JP 6396741 B2 JP6396741 B2 JP 6396741B2 JP 2014198547 A JP2014198547 A JP 2014198547A JP 2014198547 A JP2014198547 A JP 2014198547A JP 6396741 B2 JP6396741 B2 JP 6396741B2
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- Prior art keywords
- polishing
- acid
- polishing composition
- heterocyclic compound
- composition according
- Prior art date
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- 238000005498 polishing Methods 0.000 title claims description 222
- 239000000203 mixture Substances 0.000 title claims description 111
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 238000000034 method Methods 0.000 title claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 54
- 239000008119 colloidal silica Substances 0.000 claims description 44
- 150000002391 heterocyclic compounds Chemical class 0.000 claims description 34
- 150000007524 organic acids Chemical class 0.000 claims description 34
- 238000000227 grinding Methods 0.000 claims description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 21
- 229910052710 silicon Inorganic materials 0.000 claims description 21
- 239000010703 silicon Substances 0.000 claims description 21
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 20
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 19
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 19
- 239000000758 substrate Substances 0.000 claims description 17
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 15
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 5
- GIWQSPITLQVMSG-UHFFFAOYSA-N 1,2-dimethylimidazole Chemical compound CC1=NC=CN1C GIWQSPITLQVMSG-UHFFFAOYSA-N 0.000 claims description 4
- JWYUFVNJZUSCSM-UHFFFAOYSA-N 2-aminobenzimidazole Chemical compound C1=CC=C2NC(N)=NC2=C1 JWYUFVNJZUSCSM-UHFFFAOYSA-N 0.000 claims description 4
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 4
- SDXAWLJRERMRKF-UHFFFAOYSA-N 3,5-dimethyl-1h-pyrazole Chemical compound CC=1C=C(C)NN=1 SDXAWLJRERMRKF-UHFFFAOYSA-N 0.000 claims description 4
- FYTLHYRDGXRYEY-UHFFFAOYSA-N 5-Methyl-3-pyrazolamine Chemical compound CC=1C=C(N)NN=1 FYTLHYRDGXRYEY-UHFFFAOYSA-N 0.000 claims description 4
- UQFQONCQIQEYPJ-UHFFFAOYSA-N N-methylpyrazole Chemical compound CN1C=CC=N1 UQFQONCQIQEYPJ-UHFFFAOYSA-N 0.000 claims description 4
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 claims description 4
- WTKZEGDFNFYCGP-UHFFFAOYSA-N Pyrazole Chemical compound C=1C=NNC=1 WTKZEGDFNFYCGP-UHFFFAOYSA-N 0.000 claims description 4
- 150000001735 carboxylic acids Chemical class 0.000 claims description 4
- 150000002460 imidazoles Chemical class 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 150000003217 pyrazoles Chemical class 0.000 claims description 4
- GLINCONFUZIMCN-UHFFFAOYSA-N 1h-pyrazole-3,5-dicarboxylic acid;hydrate Chemical compound O.OC(=O)C=1C=C(C(O)=O)NN=1 GLINCONFUZIMCN-UHFFFAOYSA-N 0.000 claims description 3
- 229940079865 intestinal antiinfectives imidazole derivative Drugs 0.000 claims description 3
- BUUPQKDIAURBJP-UHFFFAOYSA-N sulfinic acid Chemical compound OS=O BUUPQKDIAURBJP-UHFFFAOYSA-N 0.000 claims description 3
- -1 2-Nitrobenzyl Ester Chemical class 0.000 description 32
- 150000003839 salts Chemical class 0.000 description 19
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- 229910052757 nitrogen Inorganic materials 0.000 description 10
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- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 7
- 239000002585 base Substances 0.000 description 7
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 6
- 239000002609 medium Substances 0.000 description 6
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 6
- 239000011164 primary particle Substances 0.000 description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 5
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- 125000001453 quaternary ammonium group Chemical group 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
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- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 4
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 4
- 239000000908 ammonium hydroxide Substances 0.000 description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 4
- UCMIRNVEIXFBKS-UHFFFAOYSA-N beta-alanine Chemical compound NCCC(O)=O UCMIRNVEIXFBKS-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 4
- SUMDYPCJJOFFON-UHFFFAOYSA-N isethionic acid Chemical compound OCCS(O)(=O)=O SUMDYPCJJOFFON-UHFFFAOYSA-N 0.000 description 4
- FGKJLKRYENPLQH-UHFFFAOYSA-N isocaproic acid Chemical compound CC(C)CCC(O)=O FGKJLKRYENPLQH-UHFFFAOYSA-N 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 4
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- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 4
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 4
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- 230000003746 surface roughness Effects 0.000 description 4
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 239000006061 abrasive grain Substances 0.000 description 3
- 235000011054 acetic acid Nutrition 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 3
- 150000005215 alkyl ethers Chemical class 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
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- 229910021529 ammonia Inorganic materials 0.000 description 3
- 239000003429 antifungal agent Substances 0.000 description 3
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229960003080 taurine Drugs 0.000 description 1
- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical compound CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 description 1
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 1
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 1
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 1
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 1
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 description 1
- 229960002898 threonine Drugs 0.000 description 1
- 229940034208 thyroxine Drugs 0.000 description 1
- XUIIKFGFIJCVMT-UHFFFAOYSA-N thyroxine-binding globulin Natural products IC1=CC(CC([NH3+])C([O-])=O)=CC(I)=C1OC1=CC(I)=C(O)C(I)=C1 XUIIKFGFIJCVMT-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- OUYCCCASQSFEME-UHFFFAOYSA-N tyrosine Natural products OC(=O)C(N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-UHFFFAOYSA-N 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- AQLJVWUFPCUVLO-UHFFFAOYSA-N urea hydrogen peroxide Chemical compound OO.NC(N)=O AQLJVWUFPCUVLO-UHFFFAOYSA-N 0.000 description 1
- 239000004474 valine Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Description
本発明は研磨用組成物及びその製造方法並びに研磨方法に関する。 The present invention relates to a polishing composition, a method for producing the same, and a polishing method.
半導体デバイスの製造プロセスにおいては、単体シリコン(Si)、シリコン化合物、金属等の研磨対象物を研磨する工程があり、例えば、化学反応性に乏しい窒化ケイ素(Si3N4)を高研磨速度で研磨することが要求される。窒化ケイ素を研磨するために従来使用されている研磨用組成物の多くは、砥粒及び酸を含有している。例えば、特許文献1には、リン酸又はリン酸誘導体を含有する研磨用組成物が開示されている。また、特許文献2には、コロイダルシリカと、スルホン酸基又はホスホン酸基を有する有機酸とを含有する研磨用組成物が開示されている。さらに、特許文献3には、スルホン酸やカルボン酸のような有機酸を固定化したコロイダルシリカを含有する酸性の研磨用組成物が開示されている。しかしながら、これら従来の研磨用組成物は、窒化ケイ素の研磨速度に関するユーザーの要求を十分に満足するものではなかった。 In the manufacturing process of a semiconductor device, there is a step of polishing an object to be polished such as single silicon (Si), silicon compound, metal, etc. For example, silicon nitride (Si 3 N 4 ) having poor chemical reactivity is polished at a high polishing rate. Polishing is required. Many of the polishing compositions conventionally used for polishing silicon nitride contain abrasive grains and acids. For example, Patent Document 1 discloses a polishing composition containing phosphoric acid or a phosphoric acid derivative. Patent Document 2 discloses a polishing composition containing colloidal silica and an organic acid having a sulfonic acid group or a phosphonic acid group. Further, Patent Document 3 discloses an acidic polishing composition containing colloidal silica in which an organic acid such as sulfonic acid or carboxylic acid is immobilized. However, these conventional polishing compositions do not sufficiently satisfy the user's requirements regarding the polishing rate of silicon nitride.
そこで、本発明は上記のような従来技術が有する問題点を解決し、単体シリコン、シリコン化合物、金属等の研磨対象物、特に、窒化ケイ素を高研磨速度で研磨することが可能な研磨用組成物及びその製造方法並びに研磨方法を提供することを課題とする。 Therefore, the present invention solves the above-mentioned problems of the prior art, and a polishing composition capable of polishing an object to be polished such as single silicon, silicon compound, metal, etc., particularly silicon nitride at a high polishing rate. It is an object to provide an object, a manufacturing method thereof, and a polishing method.
前記課題を解決するため、本発明の一態様に係る研磨用組成物は、表面に有機酸を固定化したコロイダルシリカと、2個以上の窒素原子を環中に含む複素環化合物と、を含有することを要旨とする。
上記一態様に係る研磨用組成物においては、複素環化合物がイミダゾール誘導体及びピラゾール誘導体から選ばれる少なくとも1種であってもよい。また、複素環化合物が5員環の化合物であってもよい。さらに、複素環化合物が、イミダゾール、1,2−ジメチルイミダゾール、2−メチルイミダゾール、2−アミノベンゾイミダゾール、ピラゾール、1−メチルピラゾール、3,5−ジメチルピラゾール、3,5−ピラゾールジカルボン酸水和物、及び3−アミノ−5−メチルピラゾールから選ばれる少なくとも1種であってもよい。
In order to solve the above problems, a polishing composition according to one embodiment of the present invention contains colloidal silica having an organic acid immobilized on the surface, and a heterocyclic compound containing two or more nitrogen atoms in the ring. The gist is to do.
In the polishing composition according to the above aspect, the heterocyclic compound may be at least one selected from imidazole derivatives and pyrazole derivatives. The heterocyclic compound may be a 5-membered ring compound. Further, the heterocyclic compound is imidazole, 1,2-dimethylimidazole, 2-methylimidazole, 2-aminobenzimidazole, pyrazole, 1-methylpyrazole, 3,5-dimethylpyrazole, 3,5-pyrazole dicarboxylic acid hydration. And at least one selected from 3-amino-5-methylpyrazole.
さらに、上記一態様に係る研磨用組成物は、pHが7以下であってもよい。
さらに、上記一態様に係る研磨用組成物においては、有機酸がスルホン酸、カルボン酸、スルフィン酸、及びホスホン酸から選ばれる少なくとも1種であってもよい。
さらに、上記一態様に係る研磨用組成物においては、複素環化合物の含有量が0.01質量%以上1質量%以下であってもよい。
さらに、上記一態様に係る研磨用組成物は、窒化ケイ素の研磨に使用することができる。
Furthermore, the polishing composition according to the above aspect may have a pH of 7 or less.
Furthermore, in the polishing composition according to one aspect, the organic acid may be at least one selected from sulfonic acid, carboxylic acid, sulfinic acid, and phosphonic acid.
Furthermore, in the polishing composition according to the above aspect, the content of the heterocyclic compound may be 0.01% by mass or more and 1% by mass or less.
Furthermore, the polishing composition according to the above-described embodiment can be used for polishing silicon nitride.
また、本発明の他の態様に係る研磨方法は、上記一態様に係る研磨用組成物を用いて研磨対象物を研磨することを要旨とする。この研磨方法においては、研磨対象物が窒化ケイ素であってもよい。
さらに、本発明の他の態様に係る研磨用組成物の製造方法は、上記一態様に係る研磨用組成物を製造する方法であって、コロイダルシリカと複素環化合物と液状媒体とを混合することを含むことを要旨とする。
さらに、本発明の他の態様に係る基板は、上記一態様に係る研磨用組成物を用いて表面が研磨されたことを要旨とする。
さらに、本発明の他の態様に係る基板製造方法は、上記一態様に係る研磨用組成物を用いて基板の表面を研磨することを含むことを要旨とする。
Another aspect of the polishing method according to the present invention is to polish an object to be polished using the polishing composition according to the above aspect. In this polishing method, the object to be polished may be silicon nitride.
Furthermore, the manufacturing method of the polishing composition according to another aspect of the present invention is a method of manufacturing the polishing composition according to the above-described aspect, wherein the colloidal silica, the heterocyclic compound, and the liquid medium are mixed. It is made to include.
Furthermore, the gist of the substrate according to another aspect of the present invention is that the surface is polished using the polishing composition according to the above aspect.
Furthermore, the gist of the substrate manufacturing method according to another aspect of the present invention includes polishing the surface of the substrate using the polishing composition according to the above aspect.
本発明の研磨用組成物及び研磨方法は、単体シリコン、シリコン化合物、金属等の研磨対象物を高研磨速度で研磨することができる。また、本発明の研磨用組成物の製造方法は、単体シリコン、シリコン化合物、金属等の研磨対象物を高研磨速度で研磨する研磨用組成物を製造することができる。 The polishing composition and polishing method of the present invention can polish an object to be polished such as simple silicon, silicon compound, metal, etc. at a high polishing rate. Moreover, the manufacturing method of the polishing composition of this invention can manufacture the polishing composition which grind | polishes grinding | polishing objects, such as a single-piece | unit silicon, a silicon compound, a metal, at a high polishing rate.
本発明の実施の形態を詳細に説明する。本実施形態の研磨用組成物は、表面に有機酸を固定化したコロイダルシリカと、2個以上の窒素原子を環中に含む複素環化合物と、を含有する。この研磨用組成物は、表面に有機酸を固定化したコロイダルシリカと、2個以上の窒素原子を環中に含む複素環化合物と、水、有機溶剤等の液状媒体と、を混合することによって製造することができる。 Embodiments of the present invention will be described in detail. The polishing composition of the present embodiment contains colloidal silica having an organic acid immobilized on the surface and a heterocyclic compound containing two or more nitrogen atoms in the ring. This polishing composition is obtained by mixing colloidal silica having an organic acid immobilized on the surface, a heterocyclic compound containing two or more nitrogen atoms in the ring, and a liquid medium such as water or an organic solvent. Can be manufactured.
この研磨用組成物は、単体シリコン、シリコン化合物、金属等の研磨対象物を研磨する用途、例えば、半導体デバイスの製造プロセスにおいて半導体配線基板の単体シリコン、シリコン化合物、金属等を含んだ表面を研磨する用途に好適である。そして、窒化ケイ素を研磨する用途に特に好適である。この研磨用組成物を用いて研磨を行えば、単体シリコン、シリコン化合物、金属等の研磨対象物、特に窒化ケイ素を高研磨速度で研磨することができる。 This polishing composition is used for polishing an object to be polished such as single silicon, silicon compound, metal, etc., for example, polishing the surface of a semiconductor wiring substrate containing single silicon, silicon compound, metal, etc. in a semiconductor device manufacturing process. It is suitable for the use to do. And it is especially suitable for the use which grind | polishes a silicon nitride. When polishing is performed using this polishing composition, it is possible to polish an object to be polished such as single silicon, silicon compound, metal, etc., particularly silicon nitride, at a high polishing rate.
以下に、本実施形態の研磨用組成物について詳細に説明する。
1.表面に有機酸を固定化したコロイダルシリカについて
1−1 有機酸の固定化について
表面に有機酸を固定化したコロイダルシリカは、研磨用組成物において砥粒として機能する。コロイダルシリカの表面への有機酸の固定化は、例えば、コロイダルシリカの表面に有機酸の官能基を化学的に結合させることにより行われる。コロイダルシリカと有機酸を単に共存させただけでは、コロイダルシリカへの有機酸の固定化は果たされない。
Below, the polishing composition of this embodiment is demonstrated in detail.
1. About Colloidal Silica Immobilizing Organic Acid on Surface 1-1 Regarding Immobilization of Organic Acid Colloidal silica having an organic acid immobilized on its surface functions as abrasive grains in the polishing composition. For example, the organic acid is immobilized on the surface of the colloidal silica by chemically bonding a functional group of the organic acid to the surface of the colloidal silica. If the colloidal silica and the organic acid are simply allowed to coexist, the organic acid is not fixed to the colloidal silica.
有機酸の一種であるスルホン酸をコロイダルシリカに固定化するのであれば、例えば、“Sulfonic acid−functionalized silica through quantitative oxidation of thiol groups”,Chem. Commun.246−247(2003)に記載の方法で行うことができる。具体的には、3−メルカプトプロピルトリメトキシシラン等のチオール基を有するシランカップリング剤をコロイダルシリカの表面のヒドロキシ基に反応させてカップリングさせた後に、過酸化水素でチオール基を酸化することにより、スルホン酸が表面に固定化されたコロイダルシリカを得ることができる。 If sulfonic acid, which is a kind of organic acid, is immobilized on colloidal silica, see, for example, “Sulphonic acid-functionalized silica through quantitative oxides of thiol groups”, Chem. Commun. 246-247 (2003). Specifically, a silane coupling agent having a thiol group such as 3-mercaptopropyltrimethoxysilane is reacted with a hydroxy group on the surface of colloidal silica to be coupled, and then the thiol group is oxidized with hydrogen peroxide. Thus, colloidal silica having sulfonic acid immobilized on the surface can be obtained.
あるいは、カルボン酸をコロイダルシリカの表面に固定化するのであれば、例えば、“Novel Silane Coupling Agents Containing
a Photolabile 2−Nitrobenzyl Ester for Introduction of a Carboxy Group on the Surface of Silica Gel”,Chemistry Letters,3,228−229(2000)に記載の方法で行うことができる。具体的には、光反応性2−ニトロベンジルエステルを含むシランカップリング剤をコロイダルシリカの表面のヒドロキシ基に反応させてカップリングさせた後に、光照射することにより、カルボン酸が表面に固定化されたコロイダルシリカを得ることができる。
Alternatively, if the carboxylic acid is immobilized on the surface of colloidal silica, for example, “Novel Silene Coupling Agents Containing”
a Photolabile 2-Nitrobenzyl Ester for Induction of a Carboxy Group on the Surface of Silica Gel ”, Chemistry Letters, 3, 228-229. -Colloidal silica in which carboxylic acid is immobilized on the surface can be obtained by irradiating light after reacting a silane coupling agent containing nitrobenzyl ester with a hydroxy group on the surface of colloidal silica and coupling it. .
その他では、スルフィン酸、ホスホン酸等の有機酸をコロイダルシリカの表面に固定化してもよい。
通常のコロイダルシリカは、酸性条件下ではゼータ電位の値がゼロに近いため、酸性条件下ではコロイダルシリカの粒子同士が互いに電気的に反発せず、凝集を起こしやすい。これに対して、表面に有機酸を固定化したコロイダルシリカは、酸性条件下でもゼータ電位が比較的大きな負の値を有するように表面修飾されているため、酸性条件下においてもコロイダルシリカの粒子同士が互いに強く反発して良好に分散する。その結果、研磨用組成物の保存安定性が向上する。
In other cases, an organic acid such as sulfinic acid or phosphonic acid may be immobilized on the surface of colloidal silica.
Since normal colloidal silica has a zeta potential value close to zero under acidic conditions, the colloidal silica particles are not electrically repelled with each other under acidic conditions and are likely to agglomerate. In contrast, colloidal silica with an organic acid immobilized on the surface is surface-modified so that the zeta potential has a relatively large negative value even under acidic conditions. They repel each other strongly and disperse well. As a result, the storage stability of the polishing composition is improved.
1−2 アスペクト比について
表面に有機酸を固定化したコロイダルシリカのアスペクト比は、1.4未満であることが好ましく、1.3以下であることがより好ましく、1.25以下であることがさらに好ましい。そうすれば、砥粒の形状が原因となる研磨対象物の表面粗さを良好なものとすることができる。
なお、このアスペクト比は、コロイダルシリカ粒子に外接する最小の長方形の長辺の長さを同じ長方形の短辺の長さで除することにより得られる値の平均値であり、走査型電子顕微鏡によって得たコロイダルシリカ粒子の画像から、一般的な画像解析ソフトウエアを用いて求めることができる。
1-2 Aspect Ratio The aspect ratio of colloidal silica having an organic acid immobilized on the surface is preferably less than 1.4, more preferably 1.3 or less, and 1.25 or less. Further preferred. If it does so, the surface roughness of the grinding | polishing target object resulting from the shape of an abrasive grain can be made favorable.
This aspect ratio is an average value of values obtained by dividing the length of the longest side of the smallest rectangle circumscribing the colloidal silica particles by the length of the short side of the same rectangle, and is obtained by scanning electron microscope. It can obtain | require from the image of the obtained colloidal silica particle using general image analysis software.
1−3 平均一次粒子径について
表面に有機酸を固定化したコロイダルシリカの平均一次粒子径は、5nm以上であることが好ましく、7nm以上であることがより好ましく、10nm以上であることがさらに好ましい。また、表面に有機酸を固定化したコロイダルシリカの平均一次粒子径は、200nm以下であることが好ましく、150nm以下であることがより好ましく、100nm以下であることがさらに好ましい。
1-3 Average primary particle diameter The average primary particle diameter of colloidal silica having an organic acid immobilized on its surface is preferably 5 nm or more, more preferably 7 nm or more, and even more preferably 10 nm or more. . The average primary particle diameter of colloidal silica having an organic acid immobilized on the surface is preferably 200 nm or less, more preferably 150 nm or less, and even more preferably 100 nm or less.
このような範囲であれば、研磨用組成物による研磨対象物の研磨速度が向上する。また、研磨用組成物を用いて研磨した後の研磨対象物の表面にディッシングが生じることをより抑えることができる。
なお、コロイダルシリカの平均一次粒子径は、例えば、BET法で測定されるコロイダルシリカの比表面積に基づいて算出される。
If it is such a range, the grinding | polishing speed | rate of the grinding | polishing target object by polishing composition will improve. Moreover, it can suppress more that dishing arises on the surface of the grinding | polishing target object after grind | polishing using polishing composition.
In addition, the average primary particle diameter of colloidal silica is calculated based on the specific surface area of colloidal silica measured by BET method, for example.
1−4 平均二次粒子径について
表面に有機酸を固定化したコロイダルシリカの平均二次粒子径は、25nm以上であることが好ましく、30nm以上であることがより好ましく、35nm以上であることがさらに好ましい。また、表面に有機酸を固定化したコロイダルシリカの平均二次粒子径は、300nm以下であることが好ましく、260nm以下であることがより好ましく、220nm以下であることがさらに好ましい。
1-4 Average secondary particle diameter The average secondary particle diameter of colloidal silica having an organic acid immobilized on its surface is preferably 25 nm or more, more preferably 30 nm or more, and preferably 35 nm or more. Further preferred. The average secondary particle diameter of colloidal silica having an organic acid immobilized on the surface is preferably 300 nm or less, more preferably 260 nm or less, and even more preferably 220 nm or less.
このような範囲であれば、研磨用組成物による研磨対象物の研磨速度が向上する。また、研磨用組成物を用いて研磨した後の研磨対象物の表面に表面欠陥が生じることをより抑えることができる。
なお、ここでいう二次粒子とは、表面に有機酸を固定化したコロイダルシリカ(一次粒子)が研磨用組成物中で会合して形成する粒子をいい、この二次粒子の平均二次粒子径は、例えば動的光散乱法により測定することができる。
If it is such a range, the grinding | polishing speed | rate of the grinding | polishing target object by polishing composition will improve. Moreover, it can suppress more that a surface defect arises on the surface of the grinding | polishing target object after grind | polishing using a polishing composition.
The secondary particles referred to here are particles formed by colloidal silica (primary particles) having an organic acid immobilized on the surface in the polishing composition, and the average secondary particles of the secondary particles. The diameter can be measured, for example, by a dynamic light scattering method.
1−5 粒度分布について
表面に有機酸を固定化したコロイダルシリカの粒度分布において、微粒子側からの積算粒子質量が全粒子質量の90%に達したときの粒子の直径D90と、微粒子側からの積算粒子質量が全粒子質量の10%に達したときの粒子の直径D10との比D90/D10は、1.5以上であることが好ましく、1.8以上であることがより好ましく、2.0以上であることがさらに好ましい。また、この比D90/D10は、5.0以下であることが好ましく、3.0以下であることがより好ましい。
このような範囲であれば、研磨対象物の研磨速度が向上し、また、研磨用組成物を用いて研磨した後の研磨対象物の表面に表面欠陥が生じることをより抑えることができる。
なお、表面に有機酸を固定化したコロイダルシリカの粒度分布は、例えばレーザー回折散乱法により求めることができる。
1-5 Particle size distribution In the particle size distribution of colloidal silica having an organic acid immobilized on the surface, the particle diameter D90 when the accumulated particle mass from the fine particle side reaches 90% of the total particle mass, The ratio D90 / D10 with the particle diameter D10 when the accumulated particle mass reaches 10% of the total particle mass is preferably 1.5 or more, more preferably 1.8 or more. More preferably, it is 0 or more. Further, the ratio D90 / D10 is preferably 5.0 or less, and more preferably 3.0 or less.
If it is such a range, the grinding | polishing speed | rate of a grinding | polishing target object will improve, and it can suppress more that a surface defect arises on the surface of the grinding | polishing target object after grind | polishing using a polishing composition.
The particle size distribution of colloidal silica having an organic acid immobilized on the surface can be determined, for example, by a laser diffraction scattering method.
1−6 コロイダルシリカの含有量について
表面に有機酸を固定化したコロイダルシリカの研磨用組成物全体における含有量は、0.005質量%以上であることが好ましく、0.5質量%以上であることがより好ましく、1質量%以上であることがさらに好ましく、3質量%以上であることが特に好ましい。このような範囲であれば、研磨対象物の研磨速度が向上する。
1-6 Content of Colloidal Silica The content of colloidal silica having an organic acid immobilized on its surface in the entire polishing composition is preferably 0.005% by mass or more, and more preferably 0.5% by mass or more. More preferably, it is more preferably 1% by mass or more, and particularly preferably 3% by mass or more. If it is such a range, the grinding | polishing speed | rate of a grinding | polishing target object will improve.
また、表面に有機酸を固定化したコロイダルシリカの研磨用組成物全体における含有量は、50質量%以下であることが好ましく、30質量%以下であることがより好ましく、20質量%以下であることがさらに好ましい。このような範囲であれば、研磨用組成物のコストを抑えることができる。また、研磨用組成物を用いて研磨した後の研磨対象物の表面に表面欠陥が生じることをより抑えることができる。 Further, the content of the colloidal silica having the organic acid immobilized on the surface in the entire polishing composition is preferably 50% by mass or less, more preferably 30% by mass or less, and 20% by mass or less. More preferably. If it is such a range, the cost of polishing composition can be held down. Moreover, it can suppress more that a surface defect arises on the surface of the grinding | polishing target object after grind | polishing using a polishing composition.
2.2個以上の窒素原子を環中に含む複素環化合物について
2個以上の窒素原子を環中に含む複素環化合物は、研磨対象物の研磨速度の向上に寄与する。特に、窒化ケイ素の研磨速度の向上に有効である。研磨対象物が窒化ケイ素の場合は、複素環化合物が窒化ケイ素に接近すると、窒化ケイ素の共有結合が伸びて結合力が弱まるため、研磨速度が向上すると考えられる。
About the heterocyclic compound which contains a 2 or more nitrogen atom in a ring The heterocyclic compound which contains a 2 or more nitrogen atom in a ring contributes to the improvement of the grinding | polishing speed | rate of a grinding | polishing target object. In particular, it is effective for improving the polishing rate of silicon nitride. In the case where the object to be polished is silicon nitride, it is considered that when the heterocyclic compound approaches silicon nitride, the covalent bond of silicon nitride is extended and the bonding force is weakened, so that the polishing rate is improved.
イミダゾール等の複素環化合物は、研磨用組成物に防食剤(研磨対象物の表面の金属の溶解を抑制することにより、研磨対象物の表面の表面状態の悪化(面荒れ等)を抑える添加剤)として添加されることがあるが、研磨対象物の研磨速度の向上に寄与することは知られていない。なお、2個以上の窒素原子を環中に含む複素環化合物が、研磨用組成物において防食剤としても機能することは勿論である。 Heterocyclic compounds such as imidazole are anticorrosive agents for polishing compositions (additives that suppress deterioration of the surface condition (surface roughness, etc.) of the surface of the polishing object by suppressing dissolution of the metal on the surface of the polishing object) However, it is not known to contribute to the improvement of the polishing rate of the object to be polished. Of course, a heterocyclic compound containing two or more nitrogen atoms in the ring also functions as an anticorrosive agent in the polishing composition.
2個以上の窒素原子を環中に含む複素環化合物としては、イミダゾール誘導体、ピラゾール誘導体、トリアゾール誘導体、テトラゾール誘導体、ピラジン誘導体、ピリダジン誘導体、キノキサリン誘導体等があげられる。この複素環化合物の環員数は特に限定されるものではなく、5員環の化合物であってもよいし、6員環の化合物であってもよい。一実施態様としては、2個以上の窒素原子を環中に含む複素環化合物は5員環の化合物である。また、環中に2個以上の窒素原子を含んでいるならば、さらに環外にも窒素原子(例えばアミノ基、ニトロ基として)を含んでいてもよい。 Examples of the heterocyclic compound containing two or more nitrogen atoms in the ring include imidazole derivatives, pyrazole derivatives, triazole derivatives, tetrazole derivatives, pyrazine derivatives, pyridazine derivatives, quinoxaline derivatives, and the like. The number of ring members of this heterocyclic compound is not particularly limited, and it may be a 5-membered ring compound or a 6-membered ring compound. In one embodiment, the heterocyclic compound containing two or more nitrogen atoms in the ring is a 5-membered ring compound. Further, if the ring contains two or more nitrogen atoms, it may further contain a nitrogen atom (for example, as an amino group or a nitro group) outside the ring.
イミダゾール誘導体の具体例としては、イミダゾール、1−メチルイミダゾール、2−メチルイミダゾール、4−メチルイミダゾール、1,2−ジメチルイミダゾール、2−エチル−4−メチルイミダゾール、2−イソプロピルイミダゾール、ベンゾイミダゾール、5,6−ジメチルベンゾイミダゾール、2−アミノベンゾイミダゾール、2−クロロベンゾイミダゾール、2−メチルベンゾイミダゾール、2−(1−ヒドロキシエチル)ベンゾイミダゾール、2−ヒドロキシベンゾイミダゾール、2−フェニルベンゾイミダゾール、2,5−ジメチルベンゾイミダゾール、5−メチルベンゾイミダゾール、5−ニトロベンゾイミダゾールがあげられる。 Specific examples of the imidazole derivative include imidazole, 1-methylimidazole, 2-methylimidazole, 4-methylimidazole, 1,2-dimethylimidazole, 2-ethyl-4-methylimidazole, 2-isopropylimidazole, benzimidazole, 5 , 6-dimethylbenzimidazole, 2-aminobenzimidazole, 2-chlorobenzimidazole, 2-methylbenzimidazole, 2- (1-hydroxyethyl) benzimidazole, 2-hydroxybenzimidazole, 2-phenylbenzimidazole, 2, Examples thereof include 5-dimethylbenzimidazole, 5-methylbenzimidazole, and 5-nitrobenzimidazole.
また、ピラゾール誘導体の具体例としては、ピラゾール、4−ニトロ−3−ピラゾールカルボン酸、3,5−ピラゾールジカルボン酸水和物、3−アミノ−5−フェニルピラゾール、5−アミノ−3−フェニルピラゾール、3,4,5−トリブロモピラゾール、3−アミノピラゾール、3,5−ジメチルピラゾール、3,5−ジメチル−1−ヒドロキシメチルピラゾール、3−メチルピラゾール、1−メチルピラゾール、3−アミノ−5−メチルピラゾールがあげられる。
さらに、トリアゾール誘導体の具体例としては、1,2,3−トリアゾール、1,2,4−トリアゾール、1−メチル−1,2,4−トリアゾールがあげられる。
さらに、テトラゾール誘導体の具体例としては、テトラゾール、5−メチルテトラゾール、5−アミノテトラゾール、5−フェニルテトラゾールがあげられる。
Specific examples of the pyrazole derivative include pyrazole, 4-nitro-3-pyrazolecarboxylic acid, 3,5-pyrazole dicarboxylic acid hydrate, 3-amino-5-phenylpyrazole, and 5-amino-3-phenylpyrazole. 3,4,5-tribromopyrazole, 3-aminopyrazole, 3,5-dimethylpyrazole, 3,5-dimethyl-1-hydroxymethylpyrazole, 3-methylpyrazole, 1-methylpyrazole, 3-amino-5 -Methylpyrazole.
Furthermore, specific examples of the triazole derivative include 1,2,3-triazole, 1,2,4-triazole, and 1-methyl-1,2,4-triazole.
Furthermore, specific examples of tetrazole derivatives include tetrazole, 5-methyltetrazole, 5-aminotetrazole, and 5-phenyltetrazole.
これら2個以上の窒素原子を環中に含む複素環化合物は、1種を単独で用いてもよいし、2種以上を併用してもよい。
ただし、これらの複素環化合物の中でも、イミダゾール、1,2−ジメチルイミダゾール、2−メチルイミダゾール、2−アミノベンゾイミダゾール、ピラゾール、1−メチルピラゾール、3,5−ジメチルピラゾール、3,5−ピラゾールジカルボン酸水和物、及び3−アミノ−5−メチルピラゾールがより好ましい。
These heterocyclic compounds containing two or more nitrogen atoms in the ring may be used alone or in combination of two or more.
However, among these heterocyclic compounds, imidazole, 1,2-dimethylimidazole, 2-methylimidazole, 2-aminobenzimidazole, pyrazole, 1-methylpyrazole, 3,5-dimethylpyrazole, 3,5-pyrazoledicarboxylic Acid hydrate and 3-amino-5-methylpyrazole are more preferred.
2個以上の窒素原子を環中に含む複素環化合物の研磨用組成物全体における含有量は、0.01質量%以上であることが好ましく、0.05質量%以上であることがより好ましく、0.10質量%以上であることがさらに好ましい。このような範囲であれば、研磨対象物の研磨速度が向上する。
また、2個以上の窒素原子を環中に含む複素環化合物の研磨用組成物全体における含有量は、1.0質量%以下であることが好ましく、0.8質量%以下であることがより好ましく、0.5質量%以下であることがさらに好ましい。このような範囲であれば、研磨用組成物のコストを抑えることができる。
The total content of the heterocyclic compound containing two or more nitrogen atoms in the ring is preferably 0.01% by mass or more, more preferably 0.05% by mass or more, More preferably, it is 0.10% by mass or more. If it is such a range, the grinding | polishing speed | rate of a grinding | polishing target object will improve.
In addition, the content of the heterocyclic compound containing two or more nitrogen atoms in the ring in the entire polishing composition is preferably 1.0% by mass or less, and more preferably 0.8% by mass or less. Preferably, it is 0.5 mass% or less. If it is such a range, the cost of polishing composition can be held down.
3.液状媒体について
液状媒体は、研磨用組成物の各成分(表面に有機酸を固定化したコロイダルシリカ、2個以上の窒素原子を環中に含む複素環化合物、添加剤等)を分散又は溶解するための分散媒又は溶媒として機能する。液状媒体としては水、有機溶剤があげられ、1種を単独で用いることができるし、2種以上を混合して用いることができるが、水を含有することが好ましい。ただし、各成分の作用を阻害することを防止するという観点から、不純物をできる限り含有しない水を用いることが好ましい。具体的には、イオン交換樹脂にて不純物イオンを除去した後にフィルタを通して異物を除去した純水や超純水、あるいは蒸留水が好ましい。
3. Liquid medium The liquid medium disperses or dissolves each component of the polishing composition (colloidal silica with an organic acid immobilized on the surface, a heterocyclic compound containing two or more nitrogen atoms in the ring, additives, etc.). It functions as a dispersion medium or solvent for the purpose. Examples of the liquid medium include water and organic solvents. One kind can be used alone, or two or more kinds can be mixed and used, but it is preferable to contain water. However, it is preferable to use water containing as little impurities as possible from the viewpoint of preventing the action of each component from being inhibited. Specifically, pure water, ultrapure water, or distilled water from which foreign substances are removed through a filter after removing impurity ions with an ion exchange resin is preferable.
4.添加剤について
研磨用組成物には、その性能を向上させるために、pH調整剤、酸化剤、錯化剤、界面活性剤、水溶性高分子、防カビ剤等の各種添加剤を添加してもよい。
4−1 pH調整剤について
研磨用組成物のpHの値は、1.5以上であることが好ましく、2以上であることがより好ましい。研磨用組成物のpHの値が高いほど研磨対象物の溶解が生じやすいので、このような範囲であれば、研磨用組成物による研磨対象物の研磨速度が向上する。また、研磨用組成物のpHの値が低くなるにしたがって取扱いが容易になるので、研磨用組成物のpHの値は、12未満であることが好ましく、10以下であることがより好ましい。
研磨用組成物のpHの値は、pH調節剤の添加により調整することができる。研磨用組成物のpHの値を所望の値に調整するために必要に応じて使用されるpH調節剤は、酸及びアルカリのいずれであってもよく、また、無機化合物及び有機化合物のいずれであってもよい。
4). Additives In order to improve the performance of the polishing composition, various additives such as a pH adjuster, an oxidizing agent, a complexing agent, a surfactant, a water-soluble polymer, and an antifungal agent are added. Also good.
4-1 About pH adjuster The pH value of the polishing composition is preferably 1.5 or more, and more preferably 2 or more. The higher the pH value of the polishing composition, the easier the dissolution of the polishing object. In such a range, the polishing rate of the polishing object by the polishing composition is improved. Further, since the handling becomes easier as the pH value of the polishing composition becomes lower, the pH value of the polishing composition is preferably less than 12, and more preferably 10 or less.
The pH value of the polishing composition can be adjusted by adding a pH regulator. The pH adjuster used as necessary to adjust the pH value of the polishing composition to a desired value may be either acid or alkali, and any of inorganic compounds and organic compounds. There may be.
pH調整剤としての酸の具体例としては、無機酸や、カルボン酸、有機硫酸等の有機酸があげられる。無機酸の具体例としては、硫酸、硝酸、ホウ酸、炭酸、次亜リン酸、亜リン酸、リン酸等があげられる。また、カルボン酸の具体例としては、ギ酸、酢酸、プロピオン酸、酪酸、吉草酸、2−メチル酪酸、n−ヘキサン酸、3,3−ジメチル酪酸、2−エチル酪酸、4−メチルペンタン酸、n−ヘプタン酸、2−メチルヘキサン酸、n−オクタン酸、2−エチルヘキサン酸、安息香酸、グリコール酸、サリチル酸、グリセリン酸、シュウ酸、マロン酸、コハク酸、グルタル酸、アジピン酸、ピメリン酸、マレイン酸、フタル酸、リンゴ酸、酒石酸、クエン酸、乳酸等があげられる。さらに、有機硫酸の具体例としては、メタンスルホン酸、エタンスルホン酸、イセチオン酸等があげられる。これらの酸は、1種を単独で用いてもよいし、2種以上を組み合わせて用いてもよい。 Specific examples of the acid as the pH adjusting agent include inorganic acids, organic acids such as carboxylic acids and organic sulfuric acids. Specific examples of the inorganic acid include sulfuric acid, nitric acid, boric acid, carbonic acid, hypophosphorous acid, phosphorous acid, phosphoric acid and the like. Specific examples of the carboxylic acid include formic acid, acetic acid, propionic acid, butyric acid, valeric acid, 2-methylbutyric acid, n-hexanoic acid, 3,3-dimethylbutyric acid, 2-ethylbutyric acid, 4-methylpentanoic acid, n-heptanoic acid, 2-methylhexanoic acid, n-octanoic acid, 2-ethylhexanoic acid, benzoic acid, glycolic acid, salicylic acid, glyceric acid, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid Maleic acid, phthalic acid, malic acid, tartaric acid, citric acid, lactic acid and the like. Furthermore, specific examples of organic sulfuric acid include methanesulfonic acid, ethanesulfonic acid, isethionic acid and the like. These acids may be used individually by 1 type, and may be used in combination of 2 or more type.
pH調整剤としての塩基の具体例としては、アルカリ金属の水酸化物又はその塩、アルカリ土類金属の水酸化物又はその塩、水酸化第四級アンモニウム又はその塩、アンモニア、アミン等があげられる。
アルカリ金属の具体例としては、カリウム、ナトリウム等があげられる。また、アルカリ土類金属の具体例としては、カルシウム、ストロンチウム等があげられる。さらに、塩の具体例としては、炭酸塩、炭酸水素塩、硫酸塩、酢酸塩等があげられる。さらに、第四級アンモニウムの具体例としては、テトラメチルアンモニウム、テトラエチルアンモニウム、テトラブチルアンモニウム等があげられる。
Specific examples of the base as the pH adjusting agent include alkali metal hydroxides or salts thereof, alkaline earth metal hydroxides or salts thereof, quaternary ammonium hydroxide or salts thereof, ammonia, amines, and the like. It is done.
Specific examples of the alkali metal include potassium and sodium. Specific examples of the alkaline earth metal include calcium and strontium. Furthermore, specific examples of the salt include carbonate, hydrogen carbonate, sulfate, acetate, and the like. Furthermore, specific examples of quaternary ammonium include tetramethylammonium, tetraethylammonium, tetrabutylammonium and the like.
水酸化第四級アンモニウム化合物としては、水酸化第四級アンモニウム又はその塩を含み、具体例としては、水酸化テトラメチルアンモニウム、水酸化テトラエチルアンモニウム、水酸化テトラブチルアンモニウム等があげられる。
さらに、アミンの具体例としては、メチルアミン、ジメチルアミン、トリメチルアミン、エチルアミン、ジエチルアミン、トリエチルアミン、エチレンジアミン、モノエタノールアミン、N−(β−アミノエチル)エタノールアミン、ヘキサメチレンジアミン、ジエチレントリアミン、トリエチレンテトラミン、無水ピペラジン、ピペラジン六水和物、1−(2−アミノエチル)ピペラジン、N−メチルピペラジン、グアニジン等があげられる。
The quaternary ammonium hydroxide compound includes quaternary ammonium hydroxide or a salt thereof, and specific examples thereof include tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrabutylammonium hydroxide and the like.
Further, specific examples of the amine include methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, ethylenediamine, monoethanolamine, N- (β-aminoethyl) ethanolamine, hexamethylenediamine, diethylenetriamine, triethylenetetramine, Anhydrous piperazine, piperazine hexahydrate, 1- (2-aminoethyl) piperazine, N-methylpiperazine, guanidine and the like can be mentioned.
これらの塩基は、1種を単独で用いてもよいし、2種以上を組み合わせて用いてもよい。
これらの塩基の中でも、アンモニア、アンモニウム塩、アルカリ金属水酸化物、アルカリ金属塩、水酸化第四級アンモニウム化合物、及びアミンが好ましく、さらに、アンモニア、カリウム化合物、水酸化ナトリウム、水酸化第四級アンモニウム化合物、炭酸水素アンモニウム、炭酸アンモニウム、炭酸水素ナトリウム、及び炭酸ナトリウムがより好ましい。
また、研磨用組成物には、塩基として、金属汚染防止の観点からカリウム化合物を含むことがさらに好ましい。カリウム化合物としては、カリウムの水酸化物又はカリウム塩があげられ、具体的には水酸化カリウム、炭酸カリウム、炭酸水素カリウム、硫酸カリウム、酢酸カリウム、塩化カリウム等があげられる。
These bases may be used individually by 1 type, and may be used in combination of 2 or more type.
Among these bases, ammonia, ammonium salts, alkali metal hydroxides, alkali metal salts, quaternary ammonium hydroxide compounds, and amines are preferable, and ammonia, potassium compounds, sodium hydroxide, quaternary hydroxides are more preferable. More preferred are ammonium compounds, ammonium bicarbonate, ammonium carbonate, sodium bicarbonate, and sodium carbonate.
Moreover, it is more preferable that the polishing composition contains a potassium compound as a base from the viewpoint of preventing metal contamination. Examples of the potassium compound include potassium hydroxide or potassium salt, and specific examples include potassium hydroxide, potassium carbonate, potassium hydrogen carbonate, potassium sulfate, potassium acetate, and potassium chloride.
4−2 酸化剤について
金属を酸化して酸化膜を形成し、研磨しやすくするために、研磨用組成物に酸化剤を添加してもよい。酸化剤の具体例としては、過酸化水素、過酢酸、過炭酸塩、過酸化尿素、過塩素酸、過硫酸塩等があげられる。過硫酸塩の具体例としては、過硫酸ナトリウム、過硫酸カリウム、過硫酸アンモニウム等があげられる。これら酸化剤は、1種を単独で用いてもよいし、2種以上を組み合わせて用いてもよい。これらの酸化剤の中でも、過硫酸塩、過酸化水素が好ましく、特に好ましいのは過酸化水素である。
4-2 Oxidizing agent An oxidizing agent may be added to the polishing composition in order to oxidize a metal to form an oxide film and facilitate polishing. Specific examples of the oxidizing agent include hydrogen peroxide, peracetic acid, percarbonate, urea peroxide, perchloric acid, persulfate and the like. Specific examples of the persulfate include sodium persulfate, potassium persulfate, and ammonium persulfate. These oxidizing agents may be used individually by 1 type, and may be used in combination of 2 or more type. Among these oxidizing agents, persulfate and hydrogen peroxide are preferable, and hydrogen peroxide is particularly preferable.
研磨用組成物全体における酸化剤の含有量が多いほど、研磨用組成物による研磨対象物の研磨速度が向上する。よって、研磨用組成物全体における酸化剤の含有量は、0.01質量%以上であることが好ましく、0.05質量%以上であることがより好ましく、0.1質量%以上であることがさらに好ましい。
また、研磨用組成物全体における酸化剤の含有量が少ないほど、研磨用組成物の材料コストを抑えることができる。また、研磨使用後の研磨用組成物の処理、すなわち廃液処理の負荷を軽減することができる。さらに、酸化剤による研磨対象物の表面の過剰な酸化が起こりにくくなる。よって、研磨用組成物全体における酸化剤の含有量は、10質量%以下であることが好ましく、5質量%以下であることがより好ましく、3質量%以下であることがさらに好ましい。
The greater the content of the oxidizing agent in the entire polishing composition, the higher the polishing rate of the object to be polished by the polishing composition. Therefore, the content of the oxidizing agent in the entire polishing composition is preferably 0.01% by mass or more, more preferably 0.05% by mass or more, and more preferably 0.1% by mass or more. Further preferred.
Moreover, the material cost of polishing composition can be held down, so that there is little content of the oxidizing agent in the whole polishing composition. Moreover, the load of the processing of the polishing composition after polishing use, that is, the waste liquid processing can be reduced. Furthermore, excessive oxidation of the surface of the object to be polished by the oxidizing agent is less likely to occur. Therefore, the content of the oxidizing agent in the entire polishing composition is preferably 10% by mass or less, more preferably 5% by mass or less, and further preferably 3% by mass or less.
4−3 錯化剤について
研磨用組成物による研磨対象物の研磨速度を向上させるために、研磨用組成物に錯化剤を添加してもよい。錯化剤は、研磨対象物の表面を化学的にエッチングする作用を有する。錯化剤の具体例としては、無機酸又はその塩、有機酸又はその塩、ニトリル化合物、アミノ酸、キレート剤等があげられる。これらの錯化剤は、1種を単独で用いてもよいし、2種以上を組み合わせて用いてもよい。また、これらの錯化剤は、市販品を用いてもよいし合成品を用いてもよい。
4-3 Complexing Agent A complexing agent may be added to the polishing composition in order to improve the polishing rate of the object to be polished by the polishing composition. The complexing agent has a function of chemically etching the surface of the object to be polished. Specific examples of the complexing agent include inorganic acids or salts thereof, organic acids or salts thereof, nitrile compounds, amino acids, chelating agents and the like. These complexing agents may be used singly or in combination of two or more. These complexing agents may be commercially available products or synthetic products.
無機酸の具体例としては、塩酸、硫酸、硝酸、炭酸、ホウ酸、テトラフルオロホウ酸、次亜リン酸、亜リン酸、リン酸、ピロリン酸等があげられる。
また、有機酸の具体例としては、カルボン酸、スルホン酸等があげられる。カルボン酸の具体例としては、ギ酸、酢酸、プロピオン酸、酪酸、吉草酸、2−メチル酪酸、n−ヘキサン酸、3,3−ジメチル酪酸、2−エチル酪酸、4−メチルペンタン酸、n−ヘプタン酸、2−メチルヘキサン酸、n−オクタン酸、2−エチルヘキサン酸、乳酸、グリコール酸、グリセリン酸、安息香酸、サリチル酸等の一価カルボン酸や、シュウ酸、マロン酸、コハク酸、グルタル酸、グルコン酸、アジピン酸、ピメリン酸、マレイン酸、フタル酸、フマル酸、リンゴ酸、酒石酸、クエン酸等の多価カルボン酸があげられる。また、スルホン酸の具体例としては、メタンスルホン酸、エタンスルホン酸、イセチオン酸等があげられる。
Specific examples of the inorganic acid include hydrochloric acid, sulfuric acid, nitric acid, carbonic acid, boric acid, tetrafluoroboric acid, hypophosphorous acid, phosphorous acid, phosphoric acid, pyrophosphoric acid and the like.
Specific examples of the organic acid include carboxylic acid and sulfonic acid. Specific examples of the carboxylic acid include formic acid, acetic acid, propionic acid, butyric acid, valeric acid, 2-methylbutyric acid, n-hexanoic acid, 3,3-dimethylbutyric acid, 2-ethylbutyric acid, 4-methylpentanoic acid, n- Monovalent carboxylic acids such as heptanoic acid, 2-methylhexanoic acid, n-octanoic acid, 2-ethylhexanoic acid, lactic acid, glycolic acid, glyceric acid, benzoic acid, salicylic acid, oxalic acid, malonic acid, succinic acid, glutar Examples thereof include polyvalent carboxylic acids such as acid, gluconic acid, adipic acid, pimelic acid, maleic acid, phthalic acid, fumaric acid, malic acid, tartaric acid and citric acid. Specific examples of the sulfonic acid include methanesulfonic acid, ethanesulfonic acid, isethionic acid and the like.
錯化剤として、これらの無機酸又は有機酸の塩を用いることができるが、特に、弱酸と強塩基との塩、強酸と弱塩基との塩、又は弱酸と弱塩基との塩を用いた場合には、pHの緩衝作用を期待することができる。このような塩の例としては、塩化カリウム、硫酸ナトリウム、硝酸カリウム、炭酸カリウム、テトラフルオロホウ酸カリウム、ピロリン酸カリウム、シュウ酸カリウム、クエン酸三ナトリウム、(+)−酒石酸カリウム、ヘキサフルオロリン酸カリウム等があげられる。 As the complexing agent, salts of these inorganic acids or organic acids can be used, and in particular, salts of weak acid and strong base, salts of strong acid and weak base, or salts of weak acid and weak base are used. In some cases, a buffering effect on pH can be expected. Examples of such salts include potassium chloride, sodium sulfate, potassium nitrate, potassium carbonate, potassium tetrafluoroborate, potassium pyrophosphate, potassium oxalate, trisodium citrate, (+)-potassium tartrate, hexafluorophosphoric acid Examples include potassium.
また、ニトリル化合物の具体例としては、アセトニトリル、アミノアセトニトリル、プロピオニトリル、ブチロニトリル、イソブチロニトリル、ベンゾニトリル、グルタロジニトリル、メトキシアセトニトリル等があげられる。
さらに、アミノ酸の具体例としては、グリシン、α−アラニン、β−アラニン、N−メチルグリシン、N,N−ジメチルグリシン、2−アミノ酪酸、ノルバリン、バリン、ロイシン、ノルロイシン、イソロイシン、フェニルアラニン、プロリン、サルコシン、オルニチン、リシン、タウリン、セリン、トレオニン、ホモセリン、チロシン、ビシン、トリシン、3,5−ジヨードチロシン、β−(3,4−ジヒドロキシフェニル)アラニン、チロキシン、4−ヒドロキシプロリン、システイン、メチオニン、エチオニン、ランチオニン、シスタチオニン、シスチン、システイン酸、アスパラギン酸、グルタミン酸、S−(カルボキシメチル)システイン、4−アミノ酪酸、アスパラギン、グルタミン、アザセリン、アルギニン、カナバニン、シトルリン、δ−ヒドロキシリシン、クレアチン、ヒスチジン、1−メチルヒスチジン、3−メチルヒスチジン、トリプトファンがあげられる。
Specific examples of the nitrile compound include acetonitrile, aminoacetonitrile, propionitrile, butyronitrile, isobutyronitrile, benzonitrile, glutaronitrile, methoxyacetonitrile and the like.
Furthermore, specific examples of amino acids include glycine, α-alanine, β-alanine, N-methylglycine, N, N-dimethylglycine, 2-aminobutyric acid, norvaline, valine, leucine, norleucine, isoleucine, phenylalanine, proline, Sarcosine, ornithine, lysine, taurine, serine, threonine, homoserine, tyrosine, bicine, tricine, 3,5-diiodotyrosine, β- (3,4-dihydroxyphenyl) alanine, thyroxine, 4-hydroxyproline, cysteine, methionine , Ethionine, lanthionine, cystathionine, cystine, cysteic acid, aspartic acid, glutamic acid, S- (carboxymethyl) cysteine, 4-aminobutyric acid, asparagine, glutamine, azaserine, arginine, canavanine, cytosine Phosphorus, .delta.-hydroxylysine, creatine, histidine, 1-methylhistidine, 3-methylhistidine, tryptophan and the like.
さらに、キレート剤の具体例としては、ニトリロ三酢酸、ジエチレントリアミン五酢酸、エチレンジアミン四酢酸、N,N,N−トリメチレンホスホン酸、エチレンジアミン−N,N,N’,N’−テトラメチレンスルホン酸、トランスシクロヘキサンジアミン四酢酸、1,2−ジアミノプロパン四酢酸、グリコールエーテルジアミン四酢酸、エチレンジアミンオルトヒドロキシフェニル酢酸、エチレンジアミンジ琥珀酸(SS体)、N−(2−カルボキシラートエチル)−L−アスパラギン酸、β−アラニンジ酢酸、2−ホスホノブタン−1,2,4−トリカルボン酸、1−ヒドロキシエチリデン−1,1−ジホスホン酸、N,N’−ビス(2−ヒドロキシベンジル)エチレンジアミン−N,N’−ジ酢酸、1,2−ジヒドロキシベンゼン−4,6−ジスルホン酸等があげられる。 Furthermore, specific examples of the chelating agent include nitrilotriacetic acid, diethylenetriaminepentaacetic acid, ethylenediaminetetraacetic acid, N, N, N-trimethylenephosphonic acid, ethylenediamine-N, N, N ′, N′-tetramethylenesulfonic acid, Transcyclohexanediaminetetraacetic acid, 1,2-diaminopropanetetraacetic acid, glycol etherdiaminetetraacetic acid, ethylenediamine orthohydroxyphenylacetic acid, ethylenediamine disuccinic acid (SS form), N- (2-carboxylateethyl) -L-aspartic acid , Β-alanine diacetate, 2-phosphonobutane-1,2,4-tricarboxylic acid, 1-hydroxyethylidene-1,1-diphosphonic acid, N, N′-bis (2-hydroxybenzyl) ethylenediamine-N, N′— Diacetic acid, 1,2-dihydroxybenzene Such as 4,6-disulfonic acid and the like.
これらの中でも、無機酸又はその塩、カルボン酸又はその塩、及びニトリル化合物からなる群より選択される少なくとも1種が好ましく、研磨対象物に含まれる金属化合物との錯体構造の安定性の観点から、無機酸又はその塩がより好ましい。また、上述した各種の錯化剤として、pH調整機能を有するもの(例えば、各種の酸)を用いる場合には、当該錯化剤をpH調整剤の少なくとも一部として利用してもよい。 Among these, at least one selected from the group consisting of an inorganic acid or a salt thereof, a carboxylic acid or a salt thereof, and a nitrile compound is preferable, from the viewpoint of the stability of the complex structure with the metal compound contained in the object to be polished. An inorganic acid or a salt thereof is more preferable. Moreover, when using what has pH adjustment function (for example, various acids) as various complexing agents mentioned above, you may utilize the said complexing agent as at least one part of a pH adjusting agent.
研磨用組成物全体における錯化剤の含有量の下限値は、少量でも効果を発揮するため特に限定されるものではないが、錯化剤の含有量が多いほど研磨用組成物による研磨対象物の研磨速度が向上するので、研磨用組成物全体における錯化剤の含有量は、0.001g/L以上であることが好ましく、0.01g/L以上であることがより好ましく、1g/L以上であることがさらに好ましい。
また、研磨用組成物全体における錯化剤の含有量が少ないほど、研磨対象物の溶解が生じにくく段差解消性が向上する。よって、研磨用組成物全体における錯化剤の含有量は、20g/L以下であることが好ましく、15g/L以下であることがより好ましく、10g/L以下であることがさらに好ましい。
The lower limit value of the content of the complexing agent in the entire polishing composition is not particularly limited because the effect is exhibited even in a small amount, but the higher the content of the complexing agent, the more the polishing object by the polishing composition. Therefore, the content of the complexing agent in the entire polishing composition is preferably 0.001 g / L or more, more preferably 0.01 g / L or more, and 1 g / L. More preferably, it is the above.
Further, as the content of the complexing agent in the entire polishing composition is smaller, dissolution of the object to be polished is less likely to occur, and the step resolution is improved. Therefore, the content of the complexing agent in the entire polishing composition is preferably 20 g / L or less, more preferably 15 g / L or less, and even more preferably 10 g / L or less.
4−4 界面活性剤について
研磨用組成物には界面活性剤を添加してもよい。界面活性剤は、研磨後の研磨対象物の研磨表面に親水性を付与する作用を有しているので、研磨後の研磨対象物の洗浄効率を良好にし、汚れの付着等を抑制することができる。界面活性剤としては、陰イオン性界面活性剤、陽イオン性界面活性剤、両性界面活性剤、及び非イオン性界面活性剤のいずれも使用することができる。
4-4 Surfactant A surfactant may be added to the polishing composition. Since the surfactant has an action of imparting hydrophilicity to the polished surface of the polished object after polishing, it can improve the cleaning efficiency of the polished object after polishing and suppress the adhesion of dirt and the like. it can. As the surfactant, any of an anionic surfactant, a cationic surfactant, an amphoteric surfactant, and a nonionic surfactant can be used.
陰イオン性界面活性剤の具体例としては、ポリオキシエチレンアルキルエーテル酢酸、ポリオキシエチレンアルキル硫酸エステル、アルキル硫酸エステル、ポリオキシエチレンアルキル硫酸、アルキル硫酸、アルキルベンゼンスルホン酸、アルキルリン酸エステル、ポリオキシエチレンアルキルリン酸エステル、ポリオキシエチレンスルホコハク酸、アルキルスルホコハク酸、アルキルナフタレンスルホン酸、アルキルジフェニルエーテルジスルホン酸、又はこれらの塩があげられる。 Specific examples of the anionic surfactant include polyoxyethylene alkyl ether acetic acid, polyoxyethylene alkyl sulfuric acid ester, alkyl sulfuric acid ester, polyoxyethylene alkyl sulfuric acid, alkyl sulfuric acid, alkylbenzene sulfonic acid, alkyl phosphoric acid ester, polyoxyethylene Examples thereof include ethylene alkyl phosphates, polyoxyethylene sulfosuccinic acid, alkyl sulfosuccinic acid, alkyl naphthalene sulfonic acid, alkyl diphenyl ether disulfonic acid, and salts thereof.
また、陽イオン性界面活性剤の具体例としては、アルキルトリメチルアンモニウム塩、アルキルジメチルアンモニウム塩、アルキルベンジルジメチルアンモニウム塩、アルキルアミン塩があげられる。
さらに、両性界面活性剤の具体例としては、アルキルベタイン、アルキルアミンオキシドがあげられる。
さらに、非イオン性界面活性剤の具体例としては、ポリオキシエチレンアルキルエーテル、ポリオキシアルキレンアルキルエーテル、ソルビタン脂肪酸エステル、グリセリン脂肪酸エステル、ポリオキシエチレン脂肪酸エステル、ポリオキシエチレンアルキルアミン、アルキルアルカノールアミドがあげられる。
これらの界面活性剤は、1種を単独で用いてもよいし、2種以上を組み合わせて用いてもよい。
Specific examples of the cationic surfactant include alkyl trimethyl ammonium salt, alkyl dimethyl ammonium salt, alkyl benzyl dimethyl ammonium salt, and alkyl amine salt.
Furthermore, specific examples of amphoteric surfactants include alkyl betaines and alkyl amine oxides.
Furthermore, specific examples of the nonionic surfactant include polyoxyethylene alkyl ether, polyoxyalkylene alkyl ether, sorbitan fatty acid ester, glycerin fatty acid ester, polyoxyethylene fatty acid ester, polyoxyethylene alkylamine, and alkylalkanolamide. can give.
These surfactants may be used individually by 1 type, and may be used in combination of 2 or more type.
研磨用組成物全体における界面活性剤の含有量が多いほど、研磨後の研磨対象物の洗浄効率がより向上するので、研磨用組成物全体における界面活性剤の含有量は0.0001g/L以上であることが好ましく、0.001g/L以上であることがより好ましい。
また、研磨用組成物全体における界面活性剤の含有量が少ないほど、研磨後の研磨対象物の研磨面への界面活性剤の残存量が低減され、洗浄効率がより向上するので、研磨用組成物全体における界面活性剤の含有量は10g/L以下であることが好ましく、1g/L以下であることがより好ましい。
As the surfactant content in the entire polishing composition increases, the cleaning efficiency of the polishing object after polishing is further improved. Therefore, the surfactant content in the entire polishing composition is 0.0001 g / L or more. It is preferable that it is 0.001 g / L or more.
Further, the smaller the surfactant content in the polishing composition as a whole, the less surfactant remains on the polished surface of the polished object after polishing, and the cleaning efficiency is further improved. The surfactant content in the whole product is preferably 10 g / L or less, and more preferably 1 g / L or less.
4−5 水溶性高分子について
研磨用組成物には水溶性高分子を添加してもよい。研磨用組成物に水溶性高分子を添加すると、研磨後の研磨対象物の表面粗さがより低減する(平滑となる)。
水溶性高分子の具体例としては、ポリスチレンスルホン酸塩、ポリイソプレンスルホン酸塩、ポリアクリル酸塩、ポリマレイン酸、ポリイタコン酸、ポリ酢酸ビニル、ポリビニルアルコール、ポリグリセリン、ポリビニルピロリドン、イソプレンスルホン酸とアクリル酸の共重合体、ポリビニルピロリドンポリアクリル酸共重合体、ポリビニルピロリドン酢酸ビニル共重合体、ナフタレンスルホン酸ホルマリン縮合物の塩、ジアリルアミン塩酸塩二酸化硫黄共重合体、カルボキシメチルセルロース、カルボキシメチルセルロースの塩、ヒドロキシエチルセルロース、ヒドロキシプロピルセルロース、プルラン、キトサン、及びキトサン塩類があげられる。これらの水溶性高分子は、1種を単独で用いてもよいし、2種以上を組み合わせて用いてもよい。
4-5 Water-soluble polymer A water-soluble polymer may be added to the polishing composition. When a water-soluble polymer is added to the polishing composition, the surface roughness of the polished object after polishing is further reduced (smoothed).
Specific examples of water-soluble polymers include polystyrene sulfonate, polyisoprene sulfonate, polyacrylate, polymaleic acid, polyitaconic acid, polyvinyl acetate, polyvinyl alcohol, polyglycerin, polyvinyl pyrrolidone, isoprene sulfonic acid and acrylic. Acid copolymer, polyvinylpyrrolidone polyacrylic acid copolymer, polyvinylpyrrolidone vinyl acetate copolymer, naphthalenesulfonic acid formalin condensate salt, diallylamine hydrochloride sulfur dioxide copolymer, carboxymethylcellulose, carboxymethylcellulose salt, hydroxy Examples include ethyl cellulose, hydroxypropyl cellulose, pullulan, chitosan, and chitosan salts. These water-soluble polymers may be used alone or in combination of two or more.
研磨用組成物全体における水溶性高分子の含有量が多いほど、研磨対象物の研磨面の表面粗さがより低減するので、研磨用組成物全体における水溶性高分子の含有量は、0.0001g/L以上であることが好ましく、0.001g/L以上であることがより好ましい。
また、研磨用組成物全体における水溶性高分子の含有量が少ないほど、研磨対象物の研磨面への水溶性高分子の残存量が低減され洗浄効率がより向上するので、研磨用組成物全体における水溶性高分子の含有量は、10g/L以下であることが好ましく、1g/L以下であることがより好ましい。
As the content of the water-soluble polymer in the entire polishing composition is larger, the surface roughness of the polishing surface of the object to be polished is further reduced, so that the content of the water-soluble polymer in the entire polishing composition is 0. It is preferably 0001 g / L or more, and more preferably 0.001 g / L or more.
Further, as the content of the water-soluble polymer in the entire polishing composition is smaller, the remaining amount of the water-soluble polymer on the polishing surface of the object to be polished is reduced and the cleaning efficiency is further improved. The water-soluble polymer content in is preferably 10 g / L or less, more preferably 1 g / L or less.
4−6 防カビ剤、防腐剤について
研磨用組成物には防カビ剤、防腐剤を添加してもよい。防カビ剤、防腐剤の具体例としては、イソチアゾリン系防腐剤(例えば2−メチル−4−イソチアゾリン−3−オン、5−クロロ−2−メチル−4−イソチアゾリン−3−オン)、パラオキシ安息香酸エステル類、フェノキシエタノールがあげられる。これらの防カビ剤、防腐剤は、1種を単独で用いてもよいし、2種以上を組み合わせて用いてもよい。
4-6 Antifungal Agent and Antiseptic Agent An antifungal agent and an antiseptic agent may be added to the polishing composition. Specific examples of fungicides and preservatives include isothiazoline preservatives (for example, 2-methyl-4-isothiazolin-3-one, 5-chloro-2-methyl-4-isothiazolin-3-one), paraoxybenzoic acid Examples include esters and phenoxyethanol. One of these fungicides and preservatives may be used alone, or two or more thereof may be used in combination.
5.研磨用組成物の製造方法について
本実施形態の研磨用組成物の製造方法は特に限定されるものではなく、表面に有機酸を固定化したコロイダルシリカと、2個以上の窒素原子を環中に含む複素環化合物と、所望により各種添加剤とを、水等の液状媒体中で攪拌、混合することによって製造することができる。
混合時の温度は特に限定されるものではないが、10℃以上40℃以下が好ましく、溶解速度を向上させるために加熱してもよい。また、混合時間も特に限定されない。
5. About the manufacturing method of polishing composition The manufacturing method of the polishing composition of this embodiment is not specifically limited, Colloidal silica which fixed the organic acid on the surface, and two or more nitrogen atoms in a ring It can manufacture by stirring and mixing the heterocyclic compound containing and various additives as needed in liquid media, such as water.
Although the temperature at the time of mixing is not specifically limited, 10 to 40 degreeC is preferable and you may heat in order to improve a dissolution rate. Further, the mixing time is not particularly limited.
6.研磨対象物について
研磨対象物の種類は特に限定されるものではないが、単体シリコン、シリコン化合物、金属等があげられる。単体シリコン及びシリコン化合物は、シリコン含有材料を含む層を有する研磨対象物である。
単体シリコンとしては、例えば単結晶シリコン、多結晶シリコン(ポリシリコン)、アモルファスシリコン等があげられる。また、シリコン化合物としては、例えば窒化ケイ素、二酸化ケイ素、炭化ケイ素等があげられる。シリコン化合物膜には、比誘電率が3以下の低誘電率膜が含まれる。
さらに、金属としては、例えば、タングステン、銅、アルミニウム、ハフニウム、コバルト、ニッケル、チタン、タンタル、金、銀、白金、パラジウム、ロジウム、ルテニウム、イリジウム、オスミウム等があげられる。これらの金属は、合金又は金属化合物の形態で含まれていてもよい。これらの金属の中では銅が好ましい。
6). Regarding the polishing object The type of the polishing object is not particularly limited, and examples thereof include simple silicon, silicon compounds, and metals. The simple silicon and the silicon compound are polishing objects having a layer containing a silicon-containing material.
Examples of the single silicon include single crystal silicon, polycrystalline silicon (polysilicon), and amorphous silicon. Examples of the silicon compound include silicon nitride, silicon dioxide, and silicon carbide. The silicon compound film includes a low dielectric constant film having a relative dielectric constant of 3 or less.
Furthermore, examples of the metal include tungsten, copper, aluminum, hafnium, cobalt, nickel, titanium, tantalum, gold, silver, platinum, palladium, rhodium, ruthenium, iridium, and osmium. These metals may be contained in the form of an alloy or a metal compound. Of these metals, copper is preferred.
7.研磨方法について
研磨装置の構成は特に限定されるものではないが、例えば、研磨対象物を有する基板等を保持するホルダーと、回転速度を変更可能なモータ等の駆動部と、研磨パッド(研磨布)を貼り付け可能な研磨定盤と、を備える一般的な研磨装置を使用することができる。
研磨パッドとしては、一般的な不織布、ポリウレタン、多孔質フッ素樹脂等を特に制限なく使用することができる。研磨パッドには、液状の研磨用組成物が溜まるような溝加工が施されているものを使用することができる。
7). Polishing Method The configuration of the polishing apparatus is not particularly limited. For example, a holder for holding a substrate having a polishing object, a driving unit such as a motor capable of changing the rotation speed, and a polishing pad (polishing cloth) A general polishing apparatus provided with a polishing surface plate that can be attached).
As the polishing pad, a general nonwoven fabric, polyurethane, porous fluororesin, or the like can be used without particular limitation. As the polishing pad, a polishing pad that has been grooved so as to accumulate a liquid polishing composition can be used.
研磨条件は特に制限はなく、例えば、研磨定盤の回転速度は、10min−1以上500min−1以下とすることができる。また、研磨対象物を有する基板に負荷する圧力(研磨圧力)は、0.7kPa以上69kPa以下とすることができる。
また、研磨パッドに研磨用組成物を供給する方法も特に限定されるものではなく、例えば、ポンプ等で連続的に供給する方法が採用される。研磨用組成物の供給量に制限はないが、研磨パッドの表面が常に研磨用組成物で覆われていることが好ましい。なお、研磨対象物の研磨においては、本実施形態の研磨用組成物の原液をそのまま用いて研磨を行ってもよいが、原液を水等の希釈液で例えば10倍以上に希釈した研磨用組成物の希釈物を用いて研磨を行ってもよい。
The polishing conditions are not particularly limited, for example, the rotational speed of the polishing platen may be a 10min -1 or 500 min -1 or less. Further, the pressure (polishing pressure) applied to the substrate having the object to be polished can be 0.7 kPa or more and 69 kPa or less.
Moreover, the method of supplying polishing composition to a polishing pad is not specifically limited, For example, the method of supplying continuously with a pump etc. is employ | adopted. The supply amount of the polishing composition is not limited, but it is preferable that the surface of the polishing pad is always covered with the polishing composition. In the polishing of the object to be polished, polishing may be performed using the stock solution of the polishing composition of the present embodiment as it is, but the polishing composition is diluted 10 times or more with a diluent such as water. Polishing may be performed using a diluted product.
研磨終了後、基板を例えば流水で洗浄し、スピンドライヤ等により基板上に付着した水滴を払い落として乾燥させることにより、例えばシリコン含有材料を含む層を有する基板が得られる。
このように、本実施形態の研磨用組成物は、基板の研磨の用途に用いることができる。すなわち、本実施形態の研磨用組成物を用いて基板の表面を研磨することを含む方法により、基板の表面を高研磨速度で研磨して、基板を製造することができる。基板としては、例えば、単体シリコン、シリコン化合物、金属等を含む層を有するシリコンウェーハがあげられる。
After polishing, the substrate is washed with, for example, running water, and water droplets adhering to the substrate are removed by a spin dryer or the like and dried to obtain a substrate having a layer containing, for example, a silicon-containing material.
Thus, the polishing composition of this embodiment can be used for polishing a substrate. That is, the substrate can be manufactured by polishing the surface of the substrate at a high polishing rate by a method including polishing the surface of the substrate using the polishing composition of the present embodiment. Examples of the substrate include a silicon wafer having a layer containing single silicon, a silicon compound, a metal, or the like.
〔実施例〕
以下に実施例及び比較例を示し、本発明をさらに具体的に説明する。
表面にスルホン酸を固定化したコロイダルシリカと、各種の含窒素複素環化合物と、pH調整剤である乳酸と、液状媒体である水とを混合して、実施例1〜9及び比較例1,2の研磨用組成物を製造した。この際、表1に示されるように、実施例1〜9においては、各種の2個の窒素原子を環中に含む複素環化合物を使用し、比較例1においては、複素環化合物を使用せず、比較例2においては、1個の窒素原子を環中に含む複素環化合物(ピロール)を使用した。
〔Example〕
Hereinafter, the present invention will be described more specifically with reference to examples and comparative examples.
Colloidal silica having sulfonic acid immobilized on the surface, various nitrogen-containing heterocyclic compounds, lactic acid as a pH adjuster, and water as a liquid medium were mixed, and Examples 1 to 9 and Comparative Example 1, 2 polishing composition was manufactured. At this time, as shown in Table 1, in Examples 1 to 9, a heterocyclic compound containing various two nitrogen atoms in the ring was used, and in Comparative Example 1, a heterocyclic compound was used. In Comparative Example 2, a heterocyclic compound (pyrrole) containing one nitrogen atom in the ring was used.
表面にスルホン酸を固定化したコロイダルシリカの平均一次粒子径は、実施例1〜9及び比較例1,2のいずれにおいても32nmであり、平均二次粒子径はいずれにおいても70nmである。また、表面にスルホン酸を固定化したコロイダルシリカの研磨用組成物全体における含有量は、実施例1〜9及び比較例1,2のいずれにおいても4質量%である。さらに、pH調整剤により調整した研磨用組成物のpHの値は、実施例1〜9及び比較例1,2のいずれにおいても4.2である。さらに、複素環化合物の研磨用組成物全体における含有量は、比較例1が0g/kg(含有しない)であり、それ以外はいずれも1g/kg(0.1質量%)である。 The average primary particle diameter of colloidal silica having sulfonic acid immobilized on the surface is 32 nm in each of Examples 1 to 9 and Comparative Examples 1 and 2, and the average secondary particle diameter is 70 nm in both cases. Moreover, content in the whole polishing composition of the colloidal silica which fix | immobilized the sulfonic acid on the surface is 4 mass% in any of Examples 1-9 and Comparative Examples 1 and 2. Furthermore, the pH value of the polishing composition adjusted with the pH adjuster is 4.2 in any of Examples 1 to 9 and Comparative Examples 1 and 2. Further, the content of the heterocyclic compound in the entire polishing composition is 0 g / kg (not contained) in Comparative Example 1, and 1 g / kg (0.1% by mass) in all other cases.
実施例1〜9及び比較例1,2の研磨用組成物を用いて、下記の研磨条件で直径200mmのウェーハの研磨を行った。
研磨装置:200mmウェーハ用片面CMP研磨機
研磨圧力:12.4kPa
研磨定盤の回転速度:97min−1
キャリアの回転速度:92min−1
研磨用組成物の供給量:200mL/min
研磨時間:60秒
Using the polishing compositions of Examples 1 to 9 and Comparative Examples 1 and 2, a wafer having a diameter of 200 mm was polished under the following polishing conditions.
Polishing machine: 200 mm wafer single-side CMP polisher Polishing pressure: 12.4 kPa
Rotating speed of polishing surface plate: 97 min −1
Carrier rotation speed: 92 min −1
Supply amount of polishing composition: 200 mL / min
Polishing time: 60 seconds
研磨に供したウェーハは、二酸化ケイ素膜(テトラエトキシシラン膜)付シリコンウェーハ、多結晶シリコン膜付きシリコンウェーハ、及び窒化ケイ素膜付きシリコンウェーハである。なお、下記の表1においては、二酸化ケイ素膜(テトラエトキシシラン膜)付シリコンウェーハを「TEOS」、多結晶シリコン膜付きシリコンウェーハを「Poly−Si」、窒化ケイ素膜付きシリコンウェーハを「SiN」と示した。
各ウェーハについては、光干渉式膜厚測定装置を用いて、研磨前と研磨後の各膜の膜厚をそれぞれ測定した。そして、膜厚差と研磨時間から、二酸化ケイ素、多結晶シリコン、窒化ケイ素の研磨速度をそれぞれ算出した。結果を表1に示す。
The wafers subjected to polishing are a silicon wafer with a silicon dioxide film (tetraethoxysilane film), a silicon wafer with a polycrystalline silicon film, and a silicon wafer with a silicon nitride film. In Table 1 below, a silicon wafer with a silicon dioxide film (tetraethoxysilane film) is “TEOS”, a silicon wafer with a polycrystalline silicon film is “Poly-Si”, and a silicon wafer with a silicon nitride film is “SiN”. It showed.
About each wafer, the film thickness of each film | membrane before grinding | polishing was measured using the optical interference type film thickness measuring apparatus, respectively after grinding | polishing. Then, polishing rates of silicon dioxide, polycrystalline silicon, and silicon nitride were calculated from the film thickness difference and polishing time, respectively. The results are shown in Table 1.
表1に示す結果から、実施例1〜9の研磨用組成物を用いて研磨を行うと、いずれのウェーハにおいても、比較例1,2の研磨用組成物を用いた場合よりも高研磨速度で研磨を行うことができることが分かる。特に、比較例2の研磨用組成物の結果から、1個の窒素原子を環中に含む複素環化合物を含有する研磨用組成物では、実施例1〜9に比較して研磨速度が劣り、2個以上の窒素原子を環中に含む複素環化合物を使用することが重要であることが分かる。また、実施例1〜9の研磨用組成物は、比較例1及び2に比べて、特に、窒化ケイ素の研磨速度が大きいことが分かる。 From the results shown in Table 1, when polishing is performed using the polishing composition of Examples 1 to 9, the polishing rate is higher than that in the case of using the polishing composition of Comparative Examples 1 and 2 in any wafer. It can be seen that polishing can be performed. In particular, from the result of the polishing composition of Comparative Example 2, in the polishing composition containing a heterocyclic compound containing one nitrogen atom in the ring, the polishing rate is inferior compared to Examples 1 to 9, It can be seen that it is important to use a heterocyclic compound containing two or more nitrogen atoms in the ring. Moreover, it turns out that the polishing composition of Examples 1-9 has especially large polishing rate of silicon nitride compared with Comparative Examples 1 and 2.
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