JP2022534203A - 表面突起が形成された球状無機粒子及びその製造方法 - Google Patents
表面突起が形成された球状無機粒子及びその製造方法 Download PDFInfo
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Classifications
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- C—CHEMISTRY; METALLURGY
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Abstract
Description
しかし、これは、本発明を特定の実施形態に限定しようとするものではなく、本発明の技術思想及び範囲に含まれる変形物、均等物または代替物をいずれも含むものと理解しなければならない。
本発明による球状突起無機粒子は、下記の段階を含む方法で製造可能である。
(a)溶媒に自己組立性界面活性剤を溶解させる段階;(b)前記(a)段階を実施する前、後、または同時に、無機物前駆体を前記溶媒に溶解または分散させて無機物前駆体溶液を製造する段階;及び(c)前記無機物前駆体と前記界面活性剤との自己組立反応を通じて界面活性剤が形成するシェルの中で結晶性相と無定形相とが混在された素粒子を形成し、複数個の素粒子が凝集されて無機粒子を形成する段階。
まず、製造しようとする無機物の前駆体溶液を製造する。無機物前駆体と自己組立性界面活性剤、溶媒とを混合して製造し、この際、溶媒に界面活性剤を先に溶解させた後に無機物前駆体を入れても、溶媒に無機物前駆体を先に溶解した後、界面活性剤を入れて混合しても、または、溶媒に無機物前駆体と自己組立性界面活性剤とを同時に添加して混合しても良い。この過程で無機物前駆体と界面活性剤との間の弱い結合がなされる。
自己組立を形成する界面活性剤としては、陰イオン性、陽イオン性及び両性界面活性剤いずれもが使われ、無機物前駆体と結合することができ、溶媒に溶けながら、(+)または(-)、あるいは2種の電荷をいずれも有しながら、架橋反応によって粒子形成反応を誘導することができる官能基を保有したものである。このような官能基としては、アミド基、ニトロ基、アルデヒド基、カルボニル基などを例として挙げられる。
球状突起無機粒子の合成反応に使われる溶媒は、水または水と相溶性を有する溶媒と水との混合溶媒である。
球状突起無機粒子の合成段階では、前記製造された無機物前駆体溶液を反応器に流入し、自己組立界面活性剤との合成反応を進行する。球状突起無機粒子の合成は、1~24時間、60~250℃の温度範囲でなされる。望ましくは、2時間以上、3時間以上、または4時間以上、そして、20時間以下、10時間以下、または8時間以下の間、70℃以上、80℃以上または90℃以上、そして、220℃以下、200℃以下、180℃以下、または160℃以下の範囲で進行しうる。
本発明によれば、前記合成反応で得た無機粒子を酸及び/または塩基で処理して無機粒子の表面電荷を制御することができる。
<実施例1>
エチレングリコール(99%)と水とを体積比100:100に混合した溶媒160mlに、自己組立性界面活性剤としてPoly(N-isopropylacrylamide)(アルドリッチ社、Mw:30,000)を2g入れ、マグネチック撹拌機で撹拌した。完全に溶解されたことを確認した後にセリウム前駆体としてアルドリッチ社(Aldrich社)のCerium nitrate hexahydrate(Ce(NO3)3・6H2O)2gを入れ、溶解させてセリウム前駆体溶液を製造した。
水180mlにCerium chloride 2.4gを溶解させた水溶液に実施例1で使用したものとは分子量が異なるPoly(N-isopropylacrylamide)(アルドリッチ社、Mw:85,000)を2.4g添加して70~90℃で6時間撹拌して反応させた。以後、前記の実施例1と同じ方法で分離及び洗浄して球状突起を有するセリア粒子を得た。
フローライト六角構造のCeO2粒子(製造社:Solvay、製品名:HC60)を準備した。
水160mlにセリウム前駆体としてアルドリッチ社のCerium nitrate hexahydrate(Ce(NO3)3・6H2O)8gを入れ、溶解させてセリウム前駆体溶液を作り、マグネチック撹拌機で撹拌した。完全に溶解されたことを確認した後にSodium hydroxide(NaOH)4gを入れて、塩基状態の溶液で製造した。約1時間撹拌して沈澱法で合成されたCeO2粒子を準備した。
実施例1及び実施例2と比較例1とのセリア粒子に対するモルフォロジー及び構造を走査電子顕微鏡(FE-SEM、JEOL JSM 7401F)、高解像度透過電子顕微鏡(HR-TEM、JEM-2100F)、X線回折分析器(Rigaku SmartLab SE X-ray diffractometer with Cu Kα radiation)及びX線光電子分光分析器(XPS、Thermo ESCALAB 250)を使用して分析した。
[Ce4+]=v1+v3+v4+u1+u3+u4
実施例1及び実施例2と比較例1及び比較例2とによるCeO2無機粒子の密度をTAP密度測定法(ASTM B527)で測定した。
ゼータ電位は、Malvern社のzeta potential analyzer(Nano ZS)を用いて測定した。
脱イオン水に実施例1及び比較例1のセリア粒子を他の添加剤なしに、それぞれ0.1、0.2、0.3、0.4、0.5、0.6、0.7、0.8、0.9、1.0、2.0及び3重量%の濃度で分散させたスラリーを製造した。
Claims (15)
- 複数個の素粒子が凝集されて形成された無機粒子であって、前記素粒子は、結晶性相と無定形相とが混在されており、結晶化度が90%以下である、無機粒子。
- 前記素粒子は、粒径が10nm以下である、請求項1に記載の無機粒子。
- 前記無機粒子は、密度が3.0~5.0g/mlであり、平均粒径が30~1000nmであり、粒径の標準偏差が20以下である、請求項1に記載の無機粒子。
- 前記無機粒子は、等電点がpH5~7である、請求項1に記載の無機粒子。
- 前記無機粒子は、pH4の水分散液の状態で表面電荷が+30~+50mVまたは-30~-50mVのゼータ電位を有する、請求項1に記載の無機粒子。
- 前記無機粒子は、Ga、Sn、As、Sb、Ce、Si、Al、Co、Fe、Li、Mn、Ba、Ti、Sr、V、Zn、La、Hf、Ni、及びZrからなる群から選択される1つ以上の元素の酸化物からなる、請求項1に記載の無機粒子。
- 前記無機粒子は、CeO2粒子であり、Ce3+/Ce4+イオン比が40~60である、請求項1に記載の無機粒子。
- (a)自己組立性界面活性剤を溶媒に溶解させる段階と、
(b)前記(a)段階を実施する前、後、または同時に、無機物前駆体を前記溶媒に溶解または分散させて無機物前駆体溶液を製造する段階と、
(c)前記無機物前駆体と前記界面活性剤との自己組立反応を通じて界面活性剤が形成するシェルの中で結晶性相と無定形相とが混在された素粒子を形成し、複数個の素粒子が凝集されて無機粒子を形成する段階と、を含む、請求項1~7の何れか一項に記載の無機粒子の製造方法。 - 前記(c)段階で得た無機粒子を酸と塩基とで処理して表面電荷が制御された無機粒子を得る段階をさらに含む、請求項8に記載の無機粒子の製造方法。
- 前記自己組立性界面活性剤は、前記無機物前駆体と結合することができる電荷を有する陽イオン性界面活性剤、陰イオン性界面活性剤及び両性界面活性剤から選択される1つ以上であって、縮合反応ないし架橋反応が可能な官能基を保有する、請求項8に記載の無機粒子の製造方法。
- 前記縮合反応ないし架橋反応が可能な官能基は、アミド基、ニトロ基、アルデヒド基、及びカルボニル基からなる群から選択される1つ以上である、請求項10に記載の無機粒子の製造方法。
- 前記溶媒は、水または水と相溶性を有する溶媒と水との混合溶媒である、請求項8に記載の無機粒子の製造方法。
- 請求項1~7の何れか一項に記載の無機粒子が水に分散されている、水分散液。
- 前記水分散液は、CMP用スラリーである、請求項14に記載の水分散液。
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