JP7414437B2 - 研磨用組成物、研磨用組成物の製造方法、研磨方法および半導体基板の製造方法 - Google Patents
研磨用組成物、研磨用組成物の製造方法、研磨方法および半導体基板の製造方法 Download PDFInfo
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- JP7414437B2 JP7414437B2 JP2019167314A JP2019167314A JP7414437B2 JP 7414437 B2 JP7414437 B2 JP 7414437B2 JP 2019167314 A JP2019167314 A JP 2019167314A JP 2019167314 A JP2019167314 A JP 2019167314A JP 7414437 B2 JP7414437 B2 JP 7414437B2
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- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 125000005385 peroxodisulfate group Chemical group 0.000 description 1
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- 235000011056 potassium acetate Nutrition 0.000 description 1
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- 238000000790 scattering method Methods 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 description 1
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- 239000000741 silica gel Substances 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- RAHZWNYVWXNFOC-UHFFFAOYSA-N sulfur dioxide Inorganic materials O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 125000001302 tertiary amino group Chemical group 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N tetrahydrofuran Substances C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 1
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical class C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 1
- UAXOELSVPTZZQG-UHFFFAOYSA-N tiglic acid Natural products CC(C)=C(C)C(O)=O UAXOELSVPTZZQG-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 150000003628 tricarboxylic acids Chemical class 0.000 description 1
- AQZSPJRLCJSOED-UHFFFAOYSA-M trimethyl(octyl)azanium;chloride Chemical compound [Cl-].CCCCCCCC[N+](C)(C)C AQZSPJRLCJSOED-UHFFFAOYSA-M 0.000 description 1
- CEYYIKYYFSTQRU-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)C CEYYIKYYFSTQRU-UHFFFAOYSA-M 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
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- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/31051—Planarisation of the insulating layers
- H01L21/31053—Planarisation of the insulating layers involving a dielectric removal step
-
- 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
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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Description
で表される第4級アンモニウム化合物と、を含有し、pHが4.0未満であり、前記コロイダルシリカのゼータ電位が、-60mV以上-35mV以下である、研磨用組成物により、上記課題が解決することを見出した。
本発明は、研磨対象物を研磨するために用いられる研磨用組成物であって、コロイダルシリカと、下記式(1):
R1~R4のうち1または2の基は、それぞれ独立して、炭素数3以上20以下のアルキル基、炭素数3以上20以下のアルケニル基または炭素数6~20のアリール基である第1の基であり、
R1~R4のうち前記第1の基以外の残りの3または2の基は、それぞれ独立して、炭素数1または2のアルキル基または炭素数2のアルケニル基である第2の基であり、
A-は、一価のアニオンである、
で表される第4級アンモニウム化合物と、を含有し、pHが4.0未満であり、前記コロイダルシリカのゼータ電位が、-60mV以上-35mV以下である、研磨用組成物である。当該研磨用組成物によれば、SiOCを高い研磨速度で研磨することができる。
本発明の研磨用組成物により研磨される研磨対象物は、SiOC(炭素含有酸化ケイ素)を含むことが好ましい。すなわち、本発明の研磨用組成物は、SiOCを含む研磨対象物を研磨する用途で用いられるのが好ましい。研磨対象物は、SiOC以外の材料を含んでいてもよく、研磨対象物に含まれるSiOC以外の材料としては、特に制限されず、例えば、酸化ケイ素、窒化ケイ素、炭窒化ケイ素(SiCN)、多結晶シリコン(ポリシリコン)、非晶質シリコン(アモルファスシリコン)、金属、SiGe等が挙げられる。
本発明の研磨用組成物は、砥粒としてコロイダルシリカを含む。本発明の研磨用組成物に使用されるコロイダルシリカは、pH4.0未満で-60mV以上-35mV以下のゼータ電位を示すものである。コロイダルシリカのゼータ電位は、-55mV以上-38mV以下であるのが好ましく、-50mV以上-40mV以下であるのがより好ましい。コロイダルシリカがこのような範囲のゼータ電位を有していることにより、SiOCに対する研磨速度をより向上させることができる。
本発明の研磨用組成物は、下記式(1)で表される第4級アンモニウム化合物(以下、単に「第4級アンモニウム化合物」とも称する。)を含む。
本発明の研磨用組成物のpHは4.0未満である。仮に、pH4.0以上となると、研磨対象物の研磨速度を向上させることができない。本発明の研磨用組成物のpHは4.0未満であればよいが、より好ましくは3.9以下である。pHが4.0未満であると、研磨対象物、特にSiOCの研磨速度が向上する有利な効果がある。pHの下限は、1.0以上であることが好ましく、1.5以上であることがより好ましい。
本発明の研磨用組成物は、必要に応じて、分散媒、無機塩類、式(1)で表される第4級アンモニウム化合物以外の界面活性剤、水溶性高分子、防腐剤、防カビ剤、酸化剤等の他の成分をさらに含んでもよい。以下、他の成分である、分散媒、無機塩類、界面活性剤、水溶性高分子、防腐剤および防カビ剤、ならびに酸化剤について説明する。
研磨用組成物は、研磨用組成物を構成する各成分の分散のために分散媒(溶媒)を含んでもよい。分散媒は、各成分を分散または溶解させる機能を有する。分散媒としては、有機溶媒、水が挙げられるが、水を含むことが好ましく、水であることがより好ましい。
本発明の研磨用組成物は、無機塩類を含んでもよい。本発明で添加される無機塩類の具体例としては、例えば硫酸アンモニウム、塩化マグネシウム、酢酸カリウム、および硝酸アルミニウム等が挙げられる。
本発明の研磨用組成物は、式(1)で表される第4級アンモニウム化合物以外の界面活性剤を含んでもよい。本発明で添加される界面活性剤は、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、および非イオン性界面活性剤のいずれであってもよい。
本発明の研磨用組成物は、水溶性高分子を含んでもよい。本発明で添加される水溶性高分子の具体例としては、例えば、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との共重合体、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、およびキトサン塩類が挙げられる。
本発明で用いられる防腐剤および防カビ剤としては、例えば、2-メチル-4-イソチアゾリン-3-オンや5-クロロ-2-メチル-4-イソチアゾリン-3-オン等のイソチアゾリン系防腐剤、パラオキシ安息香酸エステル類、およびフェノキシエタノール等が挙げられる。これら防腐剤および防カビ剤は、単独でもまたは2種以上混合して用いてもよい。
本発明の研磨用組成物は、酸化剤を含むことが好ましい。酸化剤は、研磨対象物の表面を酸化する作用を有し、研磨用組成物による研磨対象物の研磨速度をより向上させうる。
本発明の研磨用組成物は、典型的には該研磨用組成物を含む研磨液の形態で研磨対象物に供給されて、その研磨対象物の研磨に用いられる。本発明の研磨用組成物は、例えば、希釈(典型的には、水により希釈)して研磨液として使用されるものであってもよく、そのまま研磨液として使用されるものであってもよい。すなわち、本発明に係る技術における研磨用組成物の概念には、研磨対象物に供給されて該研磨対象物の研磨に用いられる研磨用組成物(ワーキングスラリー)と、希釈して研磨に用いられる濃縮液(ワーキングスラリーの原液)との双方が包含される。上記濃縮液の濃縮倍率は、例えば、体積基準で2倍~100倍程度とすることができ、通常は5倍~50倍程度が適当である。
本発明の研磨用組成物の製造方法は、特に制限されず、例えば、コロイダルシリカ、第4級アンモニウム化合物および必要に応じてpH調整剤等の他の添加剤を、分散媒中で攪拌混合することにより得ることができる。各成分の詳細は上述した通りである。したがって、本発明は、コロイダルシリカと、上記式(1)で表される第4級アンモニウム化合物と、を混合する工程を含み、pHが4.0未満であり、コロイダルシリカのゼータ電位が、-60mV以上-35mV以下である、研磨用組成物の製造方法を提供する。
本発明は、本発明の研磨用組成物または本発明の製造方法により製造されてなる研磨用組成物を用いて研磨対象物を研磨する工程を含む研磨方法を提供する。また、本発明は、上記研磨方法を有する、半導体基板の製造方法を提供する。
下記で調製した各研磨用組成物を大塚電子株式会社製ELS-Z2に供し、測定温度25℃でフローセルを用い、レーザードップラー法(電気泳動光散乱測定法)により測定を行った。得られたデータをSmoluchowskiの式で解析することにより、研磨用組成物中のスルホン酸修飾コロイダルシリカまたは未修飾コロイダルシリカのゼータ電位を算出した。
(表面修飾コロイダルシリカの準備)
コロイダルシリカとして、平均一次粒子径12nm、平均二次粒子径24nm、平均会合度2のスルホン酸修飾コロイダルシリカを、“Sulfonic acid-functionalized silica through quantitative oxidation of thiol groups”, Chem. Commun. 246-247 (2003)に記載の方法で作製したものを準備した。
砥粒として上記で得られたスルホン酸修飾コロイダルシリカ(平均一次粒子径12nm、平均二次粒子径24nm、平均会合度2)を4質量%、および第4級アンモニウム化合物としてドデシルトリメチルアンモニウムクロリドを0.05質量%の最終濃度となるように、分散媒であるイオン交換水に室温(25℃)で加え、混合液を得た。
砥粒の種類、および第4級アンモニウム化合物の種類を表1のように変更したこと以外は実施例1と同様にして、実施例2、4、6および比較例1、3に係る研磨用組成物を調製した。なお、下記表1において「-」と表示されているものは、その剤を含んでいないことを示す。得られた研磨用組成物のpH、およびスルホン酸修飾コロイダルシリカまたは未修飾コロイダルシリカのゼータ電位は、下記表1に示す。
表1に記載のpHとなるようにpH調整剤の種類および含有量を変更したこと以外は実施例1と同様にして、実施例3および比較例2に係る研磨用組成物を調製した。なお、実施例3では、pH調整剤としてマレイン酸を研磨用組成物のpHが3.8となるように添加し、比較例2では、pH調整剤としてマレイン酸を研磨用組成物のpHが6.0となるように添加した。得られた研磨用組成物のpHおよび研磨用組成物中のスルホン酸修飾コロイダルシリカのゼータ電位は、下記表1に示す。
スルホン酸修飾コロイダルシリカおよび第4級アンモニウム化合物に加えて、酸化剤として過酸化水素を1質量%の最終濃度となるように添加した以外は、実施例1と同様にして、研磨用組成物を調製した。得られた研磨用組成物のpHおよび研磨用組成物中のスルホン酸修飾コロイダルシリカのゼータ電位は、下記表1に示す。
研磨用組成物中のコロイダルシリカの平均二次粒子径は、レーザー光を用いた光散乱法によって測定し、測定機器としては日機装株式会社製、動的光散乱式粒度分布計UPA-UT151を用いた。
研磨対象物として、表面に厚さ450ÅのSiOC膜をFCVD(Flowable CVD)法で形成したシリコンウェーハ(300mm、ブランケットウェーハ)及び表面に厚さ5000ÅのSiOC膜をSOG(Spin on glass)法で形成したシリコンウェーハを準備した。それぞれのシリコンウェーハを30mm×30mmのチップに切断したクーポンを試験片とし、上記で得られた各研磨用組成物を用いて、基板を以下の研磨条件で研磨した。
研磨機としてEJ-380IN-CH(日本エンギス株式会社製)を、研磨パッドとして硬質ポリウレタンパッドIC1010(ロームアンドハース社製)を、それぞれ用いた。研磨圧力3.8psi(21.0kPa)、定盤回転数60rpm、キャリア回転数60rpm、研磨用組成物の供給速度100ml/minの条件で、研磨時間は60秒で研磨を実施した。
研磨速度(Removal Rate;RR)は、以下の式により計算した。
Claims (8)
- コロイダルシリカと、下記式(1):
ここで、
R1~R4のうち1または2の基は、それぞれ独立して、炭素数3以上20以下のアルキル基、炭素数3以上20以下のアルケニル基または炭素数6~20のアリール基である第1の基であり、
R1~R4のうち前記第1の基以外の残りの3または2の基は、それぞれ独立して、炭素数1または2のアルキル基または炭素数2のアルケニル基である第2の基であり、
A-は、一価のアニオンである、
で表される第4級アンモニウム化合物と、を含有し、
pHが4.0未満であり、
前記コロイダルシリカのゼータ電位が、-60mV以上-35mV以下であり、
SiOCを含む研磨対象物を研磨する用途で使用される、研磨用組成物。 - コロイダルシリカと、下記式(1):
ここで、
R1~R4のうち1または2の基は、それぞれ独立して、炭素数3以上20以下のアルキル基、炭素数3以上20以下のアルケニル基または炭素数6~20のアリール基である第1の基であり、
R1~R4のうち前記第1の基以外の残りの3または2の基は、それぞれ独立して、炭素数1または2のアルキル基または炭素数2のアルケニル基である第2の基であり、
A-は、一価のアニオンである、
で表される第4級アンモニウム化合物と、を含有し、
鉄化合物を含有せず、
pHが4.0未満であり、
前記コロイダルシリカのゼータ電位が、-60mV以上-35mV以下であり、
SiOCを含む研磨対象物を研磨する用途で使用される、研磨用組成物。 - 前記式(1)において、前記第1の基は、炭素数が8以上13以下のアルキル基、炭素数8以上13以下のアルケニル基、または炭素数6以上13以下のアリール基である、請求項1または2に記載の研磨用組成物。
- 前記コロイダルシリカが、有機酸を表面に固定化したコロイダルシリカである、請求項1~3のいずれか1項に記載の研磨用組成物。
- 酸化剤をさらに含む、請求項1~4のいずれか1項に記載の研磨用組成物。
- コロイダルシリカと、下記式(1):
ここで、
R1~R4のうち1または2の基は、それぞれ独立して、炭素数3以上20以下のアルキル基、炭素数3以上20以下のアルケニル基または炭素数6~20のアリール基である第1の基であり、
R1~R4のうち前記第1の基以外の残りの3または2の基は、それぞれ独立して、炭素数1または2のアルキル基または炭素数2のアルケニル基である第2の基であり、
A-は、一価のアニオンである、
で表される第4級アンモニウム化合物と、を混合する工程を含み、
pHが4.0未満であり、
前記コロイダルシリカのゼータ電位が、-60mV以上-35mV以下である、SiOCを含む研磨対象物を研磨する用途で使用される研磨用組成物の製造方法。 - 請求項1~5のいずれか1項に記載の研磨用組成物または請求項6に記載の製造方法により製造されてなる研磨用組成物を用いて、研磨対象物を研磨する工程を含む、研磨方法。
- 請求項7に記載の研磨方法を有する、半導体基板の製造方法。
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
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JP2019167314A JP7414437B2 (ja) | 2019-09-13 | 2019-09-13 | 研磨用組成物、研磨用組成物の製造方法、研磨方法および半導体基板の製造方法 |
KR1020200109046A KR20210031822A (ko) | 2019-09-13 | 2020-08-28 | 연마용 조성물, 연마용 조성물의 제조 방법, 연마 방법 및 반도체 기판의 제조 방법 |
US17/008,872 US20210079264A1 (en) | 2019-09-13 | 2020-09-01 | Polishing composition, method for producing polishing composition, polishing method, and method for producing semiconductor substrate |
TW109131096A TW202116966A (zh) | 2019-09-13 | 2020-09-10 | 研磨用組合物、研磨用組合物的製造方法、研磨方法及半導體基板的製造方法 |
CN202010953542.6A CN112500798A (zh) | 2019-09-13 | 2020-09-11 | 研磨用组合物、研磨用组合物的制造方法、研磨方法及半导体基板的制造方法 |
JP2023182296A JP2024008946A (ja) | 2019-09-13 | 2023-10-24 | 研磨用組成物、研磨用組成物の製造方法、研磨方法および半導体基板の製造方法 |
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US20220348788A1 (en) * | 2021-04-27 | 2022-11-03 | Rohm And Haas Electronic Materials Cmp Holdings, Inc. | Polishing composition and method of polishing a substrate having enhanced defect reduction |
KR20240049278A (ko) * | 2021-08-20 | 2024-04-16 | 가부시키가이샤 후지미인코퍼레이티드 | 연마용 조성물, 연마용 조성물의 제조 방법, 연마 방법, 반도체 기판의 제조 방법 |
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TW202116966A (zh) | 2021-05-01 |
US20210079264A1 (en) | 2021-03-18 |
JP2021042343A (ja) | 2021-03-18 |
KR20210031822A (ko) | 2021-03-23 |
CN112500798A (zh) | 2021-03-16 |
JP2024008946A (ja) | 2024-01-19 |
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