JP2013505191A - 炭酸セリウム系化合物の製造方法、酸化セリウムの製造方法及び結晶性酸化セリウム - Google Patents
炭酸セリウム系化合物の製造方法、酸化セリウムの製造方法及び結晶性酸化セリウム Download PDFInfo
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- -1 cerium carbonate compound Chemical class 0.000 title claims abstract description 103
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 73
- 229910000420 cerium oxide Inorganic materials 0.000 title claims description 148
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims description 147
- 239000013078 crystal Substances 0.000 claims abstract description 69
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 65
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 60
- 238000000034 method Methods 0.000 claims abstract description 42
- NKCVNYJQLIWBHK-UHFFFAOYSA-N carbonodiperoxoic acid Chemical compound OOC(=O)OO NKCVNYJQLIWBHK-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims description 70
- GHLITDDQOMIBFS-UHFFFAOYSA-H cerium(3+);tricarbonate Chemical compound [Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GHLITDDQOMIBFS-UHFFFAOYSA-H 0.000 claims description 46
- 239000002245 particle Substances 0.000 claims description 43
- 239000002002 slurry Substances 0.000 claims description 40
- WMOHXRDWCVHXGS-UHFFFAOYSA-N [La].[Ce] Chemical compound [La].[Ce] WMOHXRDWCVHXGS-UHFFFAOYSA-N 0.000 claims description 38
- 150000001875 compounds Chemical class 0.000 claims description 33
- 239000007788 liquid Substances 0.000 claims description 23
- 239000000843 powder Substances 0.000 claims description 22
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- 239000002270 dispersing agent Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000003125 aqueous solvent Substances 0.000 claims description 11
- 238000010304 firing Methods 0.000 claims description 11
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- NAFHKBCKZMZCTP-UHFFFAOYSA-K [Ce+3].OOC([O-])=O.OOC([O-])=O.OOC([O-])=O Chemical compound [Ce+3].OOC([O-])=O.OOC([O-])=O.OOC([O-])=O NAFHKBCKZMZCTP-UHFFFAOYSA-K 0.000 claims description 5
- 229920000642 polymer Polymers 0.000 claims description 5
- 238000005498 polishing Methods 0.000 description 30
- 239000002243 precursor Substances 0.000 description 30
- 238000000635 electron micrograph Methods 0.000 description 24
- 238000010298 pulverizing process Methods 0.000 description 14
- 238000002441 X-ray diffraction Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 13
- 230000000704 physical effect Effects 0.000 description 13
- 230000035484 reaction time Effects 0.000 description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 11
- 239000004202 carbamide Substances 0.000 description 11
- 239000010419 fine particle Substances 0.000 description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- 150000000703 Cerium Chemical class 0.000 description 8
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 8
- 239000011324 bead Substances 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
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- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 230000009257 reactivity Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
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- 239000002699 waste material Substances 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- CLSZAABBVGFUJA-UHFFFAOYSA-N O.C1(OOO1)=O.[Ce] Chemical compound O.C1(OOO1)=O.[Ce] CLSZAABBVGFUJA-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 229920006318 anionic polymer Polymers 0.000 description 2
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- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
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- 229910052746 lanthanum Inorganic materials 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
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- 229920001223 polyethylene glycol Polymers 0.000 description 2
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- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000012429 reaction media Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 102100035472 DNA polymerase iota Human genes 0.000 description 1
- 101001094672 Homo sapiens DNA polymerase iota Proteins 0.000 description 1
- 238000003991 Rietveld refinement Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- JYYOBHFYCIDXHH-UHFFFAOYSA-N carbonic acid;hydrate Chemical compound O.OC(O)=O JYYOBHFYCIDXHH-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 150000001785 cerium compounds Chemical class 0.000 description 1
- DRVWBEJJZZTIGJ-UHFFFAOYSA-N cerium(3+);oxygen(2-) Chemical class [O-2].[O-2].[O-2].[Ce+3].[Ce+3] DRVWBEJJZZTIGJ-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000000223 laser vaporisation method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/224—Oxides or hydroxides of lanthanides
- C01F17/235—Cerium oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/247—Carbonates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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Abstract
【解決手段】前記炭酸セリウム系化合物の製造方法は、昇温下で、ランタナイトセリウムを反応させて、斜方晶系セリウムオキシカーボネートハイドレート(Ce2O(CO3)2・H2O)または六方晶系セリウムヒドロキシカーボネート(Ce(OH)・(CO3))を含む炭酸セリウム系化合物を形成する工程を含む。
【選択図】 図1
Description
本発明によると、炭酸セリウム系化合物の結晶構造、大きさまたは形状などの容易な調節が可能であり、前記炭酸セリウム系化合物を経済的かつ効率的に製造できるようにする炭酸セリウム系化合物の製造方法が提供される。
[実施例1]
常圧(1atm)及び常温(RT)下で、ランタナイトセリウムを蒸溜水に分散させた。分散液を反応器に投入し、攪拌しながら、反応器の温度を昇温した。目標反応温度に昇温した後、一定時間維持してから、温度を低くして、反応を終了させた。反応が終了されると、生成物を乾燥することで炭酸セリウム系化合物を得た。このような炭酸セリウム系化合物の製造工程で、反応温度、反応時間、蒸溜水及びランタナイトセリウムの使用量の反応条件は、下記表1に記載された通りである。
下記表1に記載されたように、反応温度、反応時間、蒸溜水及びランタナイトセリウムの使用量の反応条件を変化させたことを除いては、実施例1と同様な方法で炭酸セリウム系化合物を製造した。
常圧(1atm)下で、セリウム硝酸塩(Cerium nitrate)を3mol/Lの濃度、ウレアを9mol/Lの濃度で、それぞれ、蒸溜水に溶解した後、前記2つの水溶液を混合して、180℃で2時間反応を行った。反応中に内部圧力が40bar以上上昇すると、安全上自動的に圧力を排出して、内部圧力が常時40barに維持されるようにした。自動排出を行わなければ、90barを越えられるため、危険であると確認された。反応が終了されると、反応器の温度を冷却して、圧力を排出し、1barになるようにした。
[実施例13〜23]
上記実施例で製造された炭酸セリウム系化合物を連続式加熱炉を用いて、表2に示した多様な条件下で焼成することによって、酸化セリウムを製造した。
上記比較例1で製造された炭酸セリウム系化合物を連続式加熱炉を用いて、900℃で熱処理することによって、酸化セリウムを製造した。
[実施例24]
実施例14〜17及び実施例20で製造された酸化セリウム100gを水900g及び分散剤(LG化学社製、酸化セリウムに対して2重量%)と混合した後、ビードミルを用いて、所望の粒度に粉砕分散して、スラリーを製造した。
CMP用スラリーの製造及び研磨評価
実施例14〜17の酸化セリウムをそれぞれ用いて実施例24で製造された10%固体含有量スラリーに、水を1000g及び高選択比の添加剤を用いて、5%CMP用スラリーを製造した。このようなCMP用スラリーに対して POLI 500 Polisherで研磨評価を進め、結果を表3に示した。
ランタナイトセリウムを別途の反応なしに実施例15と同様な方法で焼成して、酸化セリウムに転換した。このような酸化セリウムに対して実施例24及び25と同様な方法を適用して、CMP用スラリーを製造した。これに対して、実施例25と同様な方法で研磨評価を進め、その結果を表3に記載した。
Claims (21)
- 50℃以上の温度でランタナイトセリウムを反応させて、斜方晶系セリウムオキシカーボネートハイドレート(Ce2O(CO3)2・H2O)、六方晶系セリウムヒドロキシカーボネート(Ce(OH)・(CO3))またはこれらの混合物を形成する工程を含むことを特徴とする炭酸セリウム系化合物の製造方法。
- 前記ランタナイトセリウムの反応は、液状媒質内で行われることを特徴とする請求項1に記載の炭酸セリウム系化合物の製造方法。
- 前記液状媒質は、水、エタノール、メタノール、ジメチルホルムアミド(DMF)及びジメチルスルホキシド(DMSO)からなる群より選ばれた1種以上の溶媒を含むことを特徴とする請求項2に記載の炭酸セリウム系化合物の製造方法。
- 前記ランタナイトセリウムの反応は、水溶媒に分散したランタナイトセリウムを用いることにより行われることを特徴とする請求項3に記載の炭酸セリウム系化合物の製造方法。
- 前記ランタナイトセリウムの反応は、50〜300℃の温度で行われることを特徴とする請求項1に記載の炭酸セリウム系化合物の製造方法。
- 前記ランタナイトセリウムの反応は、1乃至100barの圧力で開始されることを特徴とする請求項1に記載の炭酸セリウム系化合物の製造方法。
- 前記ランタナイトセリウムの反応は、0.5〜100時間行われることを特徴とする請求項1に記載の炭酸セリウム系化合物の製造方法。
- 前記ランタナイトセリウムの反応は、ランタナイトセリウム:液状媒質の重量比が1:0.5〜1:20になる量の液状媒質内で行われることを特徴とする請求項2に記載の炭酸セリウム系化合物の製造方法。
- 前記ランタナイトセリウムの反応は、50〜130℃の温度で行われ、斜方晶系セリウムオキシカーボネートハイドレート(Ce2O(CO3)2・H2O)を含む炭酸セリウム系化合物を形成することを特徴とする請求項1に記載の炭酸セリウム系化合物の製造方法。
- 前記ランタナイトセリウムの反応は、110〜300℃の温度で行われ、六方晶系セリウムヒドロキシカーボネート(Ce(OH)・(CO3))を含む炭酸セリウム系化合物を形成することを特徴とする請求項1に記載の炭酸セリウム系化合物の製造方法。
- 前記ランタナイトセリウムの反応は、50℃以上110℃未満の温度で行われ、50体積%以上の斜方晶系セリウムオキシカーボネートハイドレート(Ce2O(CO3)2・H2O)を含む炭酸セリウム系化合物を形成することを特徴とする請求項1に記載の炭酸セリウム系化合物の製造方法。
- 前記ランタナイトセリウムの反応は、130℃超過300℃以下の温度で行われ、50体積%以上の六方晶系セリウムヒドロキシカーボネート(Ce(OH)・(CO3))を含む炭酸セリウム系化合物を形成することを特徴とする請求項1に記載の炭酸セリウム系化合物の製造方法。
- 第1項乃至第12項のいずれか1項に記載の方法で得られることを特徴とする炭酸セリウム系化合物。
- 前記炭酸セリウム系化合物に、斜方晶系セリウムオキシカーボネートハイドレート(Ce2O(CO3)2・H2O)または六方晶系セリウムヒドロキシカーボネート(Ce(OH)・(CO3))が50体積%以上含まれていることを特徴とする請求項13に記載の炭酸セリウム系化合物。
- 第1項乃至第12項のいずれか1項に記載の方法で炭酸セリウム系化合物を製造する工程、及び前記炭酸セリウム系化合物を焼成する工程を含むことを特徴とする酸化セリウムの製造方法。
- 前記焼成工程は、300乃至1500℃で行われることを特徴とする請求項15に記載の酸化セリウムの製造方法。
- 複数の酸化セリウム粒子を含み、
それぞれの酸化セリウム粒子上には、複数の結晶粒(crystal grain)を定義する境界(boundary)が形成されており、
それぞれの結晶粒は、一つ以上の酸化セリウム結晶を含むことを特徴とする結晶性酸化セリウム。 - 前記結晶粒は、20乃至300nmの大きさを有し、前記酸化セリウム結晶は、10乃至300nmの結晶サイズを有することを特徴とする請求項17に記載の結晶性酸化セリウム。
- 水溶媒に分散した状態で0.5〜5μmの体積平均粒径を有することを特徴とする請求項17に記載の結晶性酸化セリウム。
- 第17項乃至第19項のいずれか1項による結晶性酸化セリウムの粉末を研磨材として含むことを特徴とするCMP用スラリー。
- 水溶媒に分散した研磨材及び高分子分散剤を含むことを特徴とする請求項20に記載のCMP用スラリー。
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CA3172282A1 (en) * | 2020-03-20 | 2021-09-23 | James C. Bohling | Aqueous dispersion of cerium (iii) carbonate particles |
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