WO2020009054A1 - 研磨用組成物 - Google Patents
研磨用組成物 Download PDFInfo
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- WO2020009054A1 WO2020009054A1 PCT/JP2019/026040 JP2019026040W WO2020009054A1 WO 2020009054 A1 WO2020009054 A1 WO 2020009054A1 JP 2019026040 W JP2019026040 W JP 2019026040W WO 2020009054 A1 WO2020009054 A1 WO 2020009054A1
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- polishing
- polyalkylene oxide
- independently
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- 238000005498 polishing Methods 0.000 title claims abstract description 96
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- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 29
- 125000002947 alkylene group Chemical group 0.000 claims abstract description 17
- 239000010954 inorganic particle Substances 0.000 claims abstract description 17
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 15
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- 125000001183 hydrocarbyl group Chemical group 0.000 claims abstract description 8
- -1 dimethylphenylene group Chemical group 0.000 claims description 18
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
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- C08G18/246—Catalysts containing metal compounds of tin tin salts of carboxylic acids containing also tin-carbon bonds
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- C—CHEMISTRY; METALLURGY
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- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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Definitions
- R 1 each independently (that is, the same or different) represents a group represented by R 11 — (O—R 12 ) x —.
- R 11 is each independently (that is, the same or different), and has 1 to 24 carbon atoms (1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23 or 24), and preferably an alkyl group having 8 to 24 carbon atoms.
- the alkyl group may be linear or branched, and is preferably linear.
- (B) is particularly preferably a compound of the following formula (III) R 11 -[(OCH 2 CH 2 ) a -ran- (OCH 2 CH (CH 3 )) b ] -OH (III)
- R 11 in the formula is more preferably R 11z , for example.
- formula (III) represents R 11 —OH.
- R 11z is a straight-chain alkyl group having 15 to 24 carbon atoms as described above, preferably a straight-chain alkyl group having 16 to 22 carbon atoms, and more preferably a straight-chain alkyl group having 16 to 20 carbon atoms. Group.
- the reaction temperature is preferably from 70 to 210 ° C, more preferably from 90 to 180 ° C, and still more preferably from 100 to 160 ° C.
- the reaction time can be appropriately set so that the reaction is completed according to the reaction temperature, the type of the polyalkylene oxide compound, the polyether monoalcohol, and the diisocyanate compound to be used.
- the reaction time refers to an average residence time obtained by the following method in a multi-screw extruder. The average residence time is determined by feeding a trace amount of a colorant (eg, crushed red chalk, blue No.
- the surface roughness of the oxide film on the silicon wafer surface 20 (the center point of the polishing amount measurement points 1 to 39) before and after the surface roughness polishing was measured by AFM (AFM5400L manufactured by Hitachi High-Tech Science Corporation).
- Example 2 A polishing slurry was prepared in the same manner as in Example 1 except that the concentration of the aqueous solution of the modified polyalkylene oxide obtained in Production Example 1 was changed to 0.1%, and the polishing characteristics were evaluated.
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Abstract
Description
項1.
無機粒子、
水、及び
式(1):
で表されるポリアルキレンオキシド変性物
を含有する、研磨用組成物(好ましくは、集積回路形成用基板研磨用組成物)。
項2.
式(1)中、R2が、それぞれ独立に、メチルジフェニレン基、ヘキサメチレン基、メチルジシクロヘキシレン基、3-メチル-3,5,5-トリメチルシクロヘキシレン基、ジメチルフェニレン基またはトリレン基を示す、
項1に記載の組成物。
項3.
式(1)中、xが0~30の整数を示す、
項1又は2に記載の組成物。
項4.
式(1)中、nが100~700の整数を示す、
項1~3のいずれかに記載の組成物。
項5.
式(1)中、mが1~10の整数を示す、
項1~4のいずれかに記載の組成物。
項6.
式(1)中、
R2が、それぞれ独立に、メチルジフェニレン基、ヘキサメチレン基、メチルジシクロヘキシレン基、3-メチル-3,5,5-トリメチルシクロヘキシレン基、ジメチルフェニレン基またはトリレン基を示し、
xが0~30の整数を示し、nが100~700の整数を示し、mが1~10の整数を示す、
項1に記載の組成物。
項7.
無機粒子が、遷移金属酸化物、酸化アルミニウム、シリカ、酸化チタン、炭化珪素、及びダイヤモンドから選択される少なくとも1種である、項1~6のいずれかに記載の組成物。
項8.
式(1):
で表されるポリアルキレンオキシド変性物
を含有する、研磨用助剤(好ましくは、集積回路形成用基板研磨用助剤)。
[-NH-R2-NH-CO-(OR3)n-]
で示される単位はm個存在するところ、m個の各単位は同一又は異なってよく、さらに当該1つの単位には(OR3)はn個存在するところ、n個の各(OR3)は同一又は異なってよい。付け加えれば、当該1つの単位にはR2はn個存在するところ、前記の通りn個の各R2は同一又は異なってよい。
(A)は、式(II):
HO-(CH2CH2O)n-H (II)
(式中、nは前記に同じ)で表されるポリエチレンオキシドである。
数平均分子量=(56,100×2)/O1
R11-[(OCH2CH2)a -ran-(OCH2CH(CH3))b]-OH (III)
で表すことができる。当該式における R11は、例えばR11zであることがさらに好ましい。なお、上記の通り、a及びbは、いずれも0若しくは正の数であって、a+b=xを満たす。a=b=0のとき、式(III)はR11-OHを示す。
(B)は、例えば、R11-OHで表されるアルキルアルコール(好ましくは直鎖の1価飽和アルコール)にエチレンオキシドおよびプロピレンオキシドを付加重合させることにより得ることができる。当該R11-OHで表されるアルキルアルコールは、炭素数1~24(好ましくは、炭素数15~24、より好ましくは炭素数16~22、さらに好ましくは炭素数16~20)の直鎖状の飽和アルコールである。
本開示の研磨用組成物の効果が奏される限り特に制限はされないが、(B)の使用量は、(A)1モルに対して1~2モルの割合が好ましく、1.1~2モルがより好ましく、1.5~2モルがさらに好ましい。
O=C=N-R2-N=C=O (IV)
で表されるジイソシアネート化合物である。R2は前記に同じであり、前記の通りメチルジフェニレン基、ヘキサメチレン基、メチルジシクロヘキシレン基、3-メチル-3,5,5-トリメチルシクロヘキシレン基、ジメチルフェニレン基またはトリレン基を示すことが好ましい。
研磨パッド(ニッタ・ハース製IC1400 K-XY Grv)を研磨装置(不二越機械工業製RDP-500)に設置し、ダイヤモンドドレッサー(旭ダイヤモンド工業製番手:#100)を用い、8.5kgf、ドレッサー回転数100回転/分にて10分間研磨パッド表面を研削した。次に、プラテン回転数90rpm、ヘッド回転数90rpm、研磨圧力280g/cm2、研磨時間60秒の条件で、各実施例または比較例で製造した研磨用スラリーを150ml/分の速度で供給しつつ直径8インチの酸化膜表面(1000nm)を有するシリコンウェハーを研磨した。
研磨前後のシリコンウェハー表面の酸化膜の膜厚を非接触光学式膜厚計(ナノメトリックス社製Nanospec 5100)により測定して研磨量を求めた。シリコンウェハー上の39点(図1参照)において研磨量を測定し、その平均値を研磨速度とした。また当該測定結果の標準偏差を平坦性とした。
研磨前後のシリコンウェハー表面20(上記研磨量測定点1~39の中央の点)の酸化膜の表面粗さをAFM(株式会社日立ハイテクサイエンス社製AFM5400L)により測定した。
乾式篩分け法(JIS Z8815)により、中位粒子径を求めた。具体的には、樹脂50gを秤量し、これをJIS標準篩(JIS Z8801)を使用して篩分けした後に篩毎に秤量し、その結果に基づいて積算質量が50%になる点の粒子径を求めた。
カラム :TOSOH TSKgel MultiporeHxL-M ×3本 (排除限界2000000:ポリスチレン)
ポンプ流量:0.6mL/min
80℃に保温された攪拌機のついた貯蔵タンクAに、十分に脱水した数平均分子量8,000のポリエチレンオキシド100質量部とデシルアルコールCH3-(CH2)9-OH 3質量部およびジオクチルスズジラウレート0.1質量部の割合で投入し、窒素ガス雰囲気下で攪拌して均一な混合物とした。
80℃に保温された攪拌機のついた貯蔵タンクAに、十分に脱水した数平均分子量20,000のポリエチレンオキシド100質量部とポリエーテルステアリルアルコール ポリエーテルステアリルアルコール CH3(CH2)17O-[(CH2CH2O)8-ran-(CH2CH(CH3)O)6]-H (青木油脂株式会社製 ブラウノン SA50/50 数平均分子量 1,000)7.4質量部およびジオクチルスズジラウレート0.2質量部の割合で投入し、窒素ガス雰囲気下で攪拌して均一な混合物とした。
80℃に保温された攪拌機のついた貯蔵タンクAに、十分に脱水した数平均分子量20,000のポリエチレンオキシド100質量部とポリオキシエチレンラウリルエーテルCH3-(CH2)11-(OCH2CH2)n-HO(n=5、12、又は20)3質量部およびジオクチルスズジラウレート0.1質量部の割合で投入し、窒素ガス雰囲気下で攪拌して均一な混合物とした。
80℃に保温された攪拌機のついた貯蔵タンクAに、十分に脱水した数平均分子量20,000のポリエチレンオキシド100質量部とステアリルアルコールCH3-(CH2)17-HO 3質量部およびジオクチルスズジラウレート0.1質量部の割合で投入し、窒素ガス雰囲気下で攪拌して均一な混合物とした。
80℃に保温された攪拌機のついた貯蔵タンクAに、十分に脱水した数平均分子量11,000のポリエチレンオキシド100質量部とポリエーテルステアリルアルコール CH3(CH2)17O-[(CH2CH2O)8-ran-(CH2CH(CH3)O)6]-H(青木油脂株式会社製 ブラウノン SA50/50 数平均分子量 1,000) 14.0質量部およびジオクチルスズジラウレート0.2質量部の割合で投入し、窒素ガス雰囲気下で攪拌して均一な混合物とした。
80℃に保温された攪拌機のついた貯蔵タンクAに、十分に脱水した数平均分子量20,000のポリエチレンオキシド100質量部とポリエーテルセチルアルコール CH3(CH2)15O-[(CH2CH2O)10-ran-(CH2CH(CH3)O)8]-H(日油株式会社製 ユニセーフ10P-8 数平均分子量 1,150) 8.3質量部およびジオクチルスズジラウレート0.2質量部の割合で投入し、窒素ガス雰囲気下で攪拌して均一な混合物とした。
80℃に保温された攪拌機のついた貯蔵タンクAに、十分に脱水した数平均分子量20,000のポリエチレンオキシド100質量部とポリエーテルステアリルアルコール CH3(CH2)17O-[ (CH2CH2O)4-ran-(CH2CH(CH3)O)7]-H(青木油脂株式会社製 ブラウノン SA30/70 数平均分子量 900) 6.7質量部およびジオクチルスズジラウレート0.2質量部の割合で投入し、窒素ガス雰囲気下で攪拌して均一な混合物とした。
80℃に保温された攪拌機のついた貯蔵タンクAに、十分に脱水した数平均分子量11,000のポリエチレンオキシド100質量部とポリエーテルベヘニルアルコール CH3(CH2)21O-[(CH2CH2O)15-ran-(CH2CH(CH3)O)1]-H(東邦化学株式会社製 ベポール BEP-0115 数平均分子量 1,040)13.6質量部およびジオクチルスズジラウレート0.2質量部の割合で投入し、窒素ガス雰囲気下で攪拌して均一な混合物とした。
80℃に保温された攪拌機のついた貯蔵タンクAに、十分に脱水した数平均分子量20,000のポリエチレンオキシド100質量部とポリエーテルステアリルエーテル C18H37O-(CH2CH2O)20-H(日油株式会社製 ノニオンS-220 分子量 1,150)3.2質量部およびジオクチルスズジラウレート0.2質量部の割合で投入し、窒素ガス雰囲気下で攪拌して均一な混合物とした。
80℃に保温された攪拌機のついた貯蔵タンクAに、十分に脱水した数平均分子量4,000のポリエチレンオキシド100質量部とポリエーテルステアリルアルコール CH3(CH2)17O-[(CH2CH2O)8-ran-(CH2CH(CH3)O)6]-H(青木油脂株式会社製 ブラウノン SA50/50 数平均分子量 1,000) 36.0質量部およびジオクチルスズジラウレート0.2質量部の割合で投入し、窒素ガス雰囲気下で攪拌して均一な混合物とした。
製造例1で得られた変性ポリアルキレンオキシドの0.05%水溶液1kgに、pH10.7に調製したキャボット社製スラリーSS25[ヒュームドシリカ(平均粒子径:0.16μm)25質量%、純水とからなる]1kgを添加して混合し研磨用スラリーを得た。この研磨用スラリーを用いて上記の方法により研磨特性評価を行った。なお、変性ポリアルキレンオキシド水溶液濃度を示す%は質量(wt/wt)%である(以下も同じ)。
製造例1で得られた変性ポリアルキレンオキシドの水溶液濃度を0.1%に変えた以外は、実施例1と同様にして研磨用スラリーを調製し、研磨性特性評価を行った。
製造例1で得られた変性ポリアルキレンオキシドの水溶液濃度を0.6%に変えた以外は、実施例1と同様にして研磨用スラリーを調製し、研磨性特性評価を行った。
製造例1で得られた変性ポリアルキレンオキシドの水溶液濃度を1%に変えた以外は、実施例1と同様にして研磨用スラリーを調製し、研磨性特性評価を行った。
変性ポリアルキレンオキシドの水溶液を、製造例2で得られた変性ポリアルキレンオキシドの0.1%水溶液1kgに変えた以外は、実施例1と同様にして研磨用スラリーを調製し、研磨性特性評価を行った。
製造例2で得られた変性ポリアルキレンオキシドの水溶液濃度を0.6%に変えた以外は、実施例5と同様にして研磨用スラリーを調製し、研磨性特性評価を行った。
変性ポリアルキレンオキシド水溶液を、純水に変えた以外は、実施例1と同様にして研磨用スラリーを調製し、研磨性特性評価を行った。
変性ポリアルキレンオキシド水溶液を、0.6質量%カルボキシメチルセルロース(第一工業製薬社製セロゲンF-AG)水溶液に変えた以外は、実施例1と同様にして研磨用スラリーを調製し、研磨性特性評価を行った。
Claims (8)
- 式(1)中、R2が、それぞれ独立に、メチルジフェニレン基、ヘキサメチレン基、メチルジシクロヘキシレン基、3-メチル-3,5,5-トリメチルシクロヘキシレン基、ジメチルフェニレン基またはトリレン基を示す、
請求項1に記載の組成物。 - 式(1)中、xが0~30の整数を示す、
請求項1又は2に記載の組成物。 - 式(1)中、nが100~700の整数を示す、
請求項1~3のいずれかに記載の組成物。 - 式(1)中、mが1~10の整数を示す、
請求項1~4のいずれかに記載の組成物。 - 式(1)中、
R2が、それぞれ独立に、メチルジフェニレン基、ヘキサメチレン基、メチルジシクロヘキシレン基、3-メチル-3,5,5-トリメチルシクロヘキシレン基、ジメチルフェニレン基またはトリレン基を示し、
xが0~30の整数を示し、nが100~700の整数を示し、mが1~10の整数を示す、
請求項1に記載の組成物。 - 無機粒子が、遷移金属酸化物、酸化アルミニウム、シリカ、酸化チタン、炭化珪素、及びダイヤモンドから選択される少なくとも1種である、請求項1~6のいずれかに記載の組成物。
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JP2020528848A JPWO2020009054A1 (ja) | 2018-07-04 | 2019-07-01 | 研磨用組成物 |
EP19829862.2A EP3819352A4 (en) | 2018-07-04 | 2019-07-01 | POLISHING COMPOSITION |
US17/257,428 US20210277281A1 (en) | 2018-07-04 | 2019-07-01 | Polishing composition |
CN201980041965.6A CN112384591A (zh) | 2018-07-04 | 2019-07-01 | 研磨用组合物 |
KR1020217000229A KR20210031454A (ko) | 2018-07-04 | 2019-07-01 | 연마용 조성물 |
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JP2003342556A (ja) * | 2002-05-30 | 2003-12-03 | Fujimi Inc | 研磨用組成物 |
JP2013140984A (ja) * | 2011-12-30 | 2013-07-18 | Cheil Industries Inc | Cmpスラリー組成物及びそれを用いた研磨方法 |
JP2013541194A (ja) * | 2010-09-02 | 2013-11-07 | キャボット マイクロエレクトロニクス コーポレイション | 高速及び低欠陥性のシリコン研磨組成物 |
WO2014007366A1 (ja) | 2012-07-06 | 2014-01-09 | 住友精化株式会社 | ポリアルキレンオキシド変性物 |
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JP2714411B2 (ja) | 1988-12-12 | 1998-02-16 | イー・アイ・デュポン・ドゥ・ヌムール・アンド・カンパニー | ウェハーのファイン研摩用組成物 |
JP4115562B2 (ja) | 1997-10-14 | 2008-07-09 | 株式会社フジミインコーポレーテッド | 研磨用組成物 |
WO2012096124A1 (ja) * | 2011-01-13 | 2012-07-19 | 住友精化株式会社 | 水溶性ポリアルキレンオキシド変性物 |
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2019
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- 2019-07-01 WO PCT/JP2019/026040 patent/WO2020009054A1/ja active Application Filing
- 2019-07-01 EP EP19829862.2A patent/EP3819352A4/en not_active Withdrawn
- 2019-07-01 JP JP2020528848A patent/JPWO2020009054A1/ja active Pending
- 2019-07-01 US US17/257,428 patent/US20210277281A1/en not_active Abandoned
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JP2003342556A (ja) * | 2002-05-30 | 2003-12-03 | Fujimi Inc | 研磨用組成物 |
JP2013541194A (ja) * | 2010-09-02 | 2013-11-07 | キャボット マイクロエレクトロニクス コーポレイション | 高速及び低欠陥性のシリコン研磨組成物 |
JP2013140984A (ja) * | 2011-12-30 | 2013-07-18 | Cheil Industries Inc | Cmpスラリー組成物及びそれを用いた研磨方法 |
WO2014007366A1 (ja) | 2012-07-06 | 2014-01-09 | 住友精化株式会社 | ポリアルキレンオキシド変性物 |
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US20210277281A1 (en) | 2021-09-09 |
JPWO2020009054A1 (ja) | 2021-08-05 |
CN112384591A (zh) | 2021-02-19 |
KR20210031454A (ko) | 2021-03-19 |
EP3819352A1 (en) | 2021-05-12 |
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