JP5403956B2 - 研磨液組成物 - Google Patents
研磨液組成物 Download PDFInfo
- Publication number
- JP5403956B2 JP5403956B2 JP2008172697A JP2008172697A JP5403956B2 JP 5403956 B2 JP5403956 B2 JP 5403956B2 JP 2008172697 A JP2008172697 A JP 2008172697A JP 2008172697 A JP2008172697 A JP 2008172697A JP 5403956 B2 JP5403956 B2 JP 5403956B2
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- JP
- Japan
- Prior art keywords
- polishing
- peak
- acid
- substrate
- region
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
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- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 1
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 description 1
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- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Description
第1の研磨材粒子と、分散剤と、第2の研磨材粒子と、水系媒体とを含む研磨液組成物であって、
前記第1の研磨材粒子がセリウムとジルコニウムとを含む複合酸化物粒子であり、
CuKα1線(λ=0.154050nm)を照射することにより得られる前記複合酸化物粒子の粉末X線回折スペクトル中に、
回折角2θ(θはブラック角)領域28.61〜29.67°内に頂点があるピーク(第1ピーク)、
回折角2θ領域33.14〜34.53°内に頂点があるピーク(第2ピーク)、
回折角2θ領域47.57〜49.63°内に頂点があるピーク(第3ピーク)、
回折角2θ領域56.45〜58.91°内に頂点があるピーク(第4ピーク)、が存在し、
前記第1ピークの半値幅が0.8°以下である。
第1の研磨材粒子と、分散剤と、第2の研磨材粒子と、水系媒体とを含む研磨液組成物であって、
前記第1の研磨材粒子がセリウムとジルコニウムとを含む複合酸化物粒子であり、
前記複合酸化物粒子は、酸化数が4のセリウム化合物と酸化数が4のジルコニウム化合物とを含む溶液と、沈殿剤とを混合することにより、前記セリウム化合物と前記ジルコニウム化合物とを加水分解させ、生じた沈殿物を分離し、次いで、焼成し、得られた焼成物を粉砕して得られる複合酸化物粒子である。
第1の研磨材粒子である複合酸化物粒子は、例えば、下記組成式によって表される。
CeXZr1-XO2
ただし、xは、条件式0<x<1、好ましくは0.50<x<0.97、より好ましくは0.55<x<0.95、さらに好ましくは0.60<x<0.90、さらにより好ましくは0.65<x<0.90、よりいっそう好ましくは0.70<x<0.90を満たす数である。
ピーク(第3ピーク)、および、回折角2θ領域56.45〜58.91°内に頂点があるピーク(第4ピーク)が観察される。
とよりいっそう好ましい。
平均一次粒子径(nm)=820/S
殿が生じるpH領域が異なるため、両者の混合状態が不十分な沈殿物が得られる。この沈殿物を熱処理すると、酸化セリウムあるいは酸化ジルコニウムが分離した部分が生じる。
本実施形態の研磨液組成物に含まれる第2の研磨材粒子としては、例えば、アルミナ粒子、シリカ粒子、ジルコニア粒子、酸化チタン粒子、セリア粒子等が挙げられ、シリカ粒子としては、コロイダルシリカ、ヒュームドシリカ、表面修飾したシリカ等が挙げられる。これらの中でも、研磨速度を向上させる観点およびスクラッチ低減の観点から、コロイダルシリカが好ましい。なお、コロイダルシリカ粒子は、例えば、ケイ酸水溶液から生成させる製法により得ることができる。
本実施形態の研磨液組成物に含まれる水系媒体としては、水、または水と溶媒との混合媒体等が挙げられ、上記溶媒としては、水と混合可能な溶媒(例えば、エタノール等のアルコール)が好ましい。水系媒体としては、なかでも、水が好ましく、イオン交換水がより好ましい。
本実施形態の研磨液組成物に含まれる分散剤は水溶性であると好ましい。水溶性の分散剤としては、カチオン性界面活性剤、アニオン性界面活性剤、非イオン性界面活性剤、およびアクリル酸系重合体からなる群から選ばれる少なくとも1種が好ましい。上記分散剤は、アニオン性界面活性剤、非イオン性界面活性剤、およびアクリル酸系重合体からなる群から選ばれる少なくとも1種であるとより好ましい。上記分散剤は、アクリル酸系重合体であるとさらに好ましい。分散剤は、水系媒体と混合される前に、複合酸化物粒子の表面に物理吸着されていてもよいし、または、複合酸化物粒子の表面に化学的に結合されていてもよい。
カラム:G4000PWXL+G2500PWXL(東ソー株式会社)
溶離液:(0.2Mリン酸バッファー)/(CH3CN)=9/1(容量比)
流量:1.0mL/min
カラム温度:40℃
検出器:RI検出器
標準物質:ポリアクリル酸換算
本実施形態の研磨液組成物は、高い表面平坦性を有する研磨表面の形成に寄与する、水溶性有機化合物を含むことが好ましい。
ガラス基板の製造過程の研磨工程で用いられる研磨パッドの材質について特に制限はなく、従来から公知のものを用いることができる。
本実施形態の研磨液組成物は、例えば、半導体基板の一方の主面がわに配置された薄膜の研磨にも用いることができる。
熱酸化膜付きシリコンウエハ
直径20.32cm(8インチ)のシリコンウエハ上に形成された、厚さ2000nmの二酸化ケイ素膜を用意した。二酸化ケイ素膜(熱酸化膜)は、シリコンウエハを、酸化炉内に入れて酸素ガスやスチームに晒し、シリコンウエハ中のシリコンと酸素を反応させることにより形成できる。
研磨試験機:片面研磨機(品番:LP−541、ラップマスターSFT(株)製、定盤径540mm)
研磨パッド:IC1000(硬質ウレタンパッド)とsuba400(不織布タイプパッド)との積層パッド(ニッタ・ハース(株)製)
定盤回転数:100rpm
へッド回転数:110rpm(回転方向は定盤と同じ)
研磨時間:1min
研磨荷重:30kPa(設定値)
研磨液組成物供給量:200ml/min
実施例1〜16、比較例1〜4の研磨液組成物(表1〜表2参照)を用いて、研磨対象基板の二酸化ケイ素膜を研磨した後、イオン交換水を用いて流水洗浄し、次いで、イオン交換水中に浸漬した状態で超音波洗浄(100kHz、3min)し、更に、イオン交換水で流水洗浄し、最後に、スピンドライ法により乾燥させた。
(1)スラリーA、B
分散剤(ポリアクリル酸アンモニウム、重量平均分子量6000)が添加された水中で、体積中位径が各々表1に記載の値となるよう、ビーズミルにより焼成物a(Ce0.75Zr0.25O2粒子)が湿式粉砕されることにより得られたCe0.75Zr0.25O2粒子スラリー(Ce0.75Zr0.25O2粒子:25重量%)をスラリーA、Bとして用意した。焼成物aは、未焼成Ce0.75Zr0.25O2粒子(商品名Actalys9320、ローディア社製)が1160℃で6時間、連続式焼成炉で焼成されることにより得られたものである。なお、焼成物aは、セリウム(IV)化合物とジルコニウム(IV)化合物とを原料として用いて得られたものである。
分散剤(ポリアクリル酸アンモニウム、重量平均分子量6000)が添加された水中で、体積中位径が表1に記載の値となるよう、ビーズミルにより焼成物b(Ce0.75Zr0.25O2粒子)が湿式粉砕されることにより得られたCe0.75Zr0.25O2粒子スラリー(Ce0.75Zr0.25O2粒子:25重量%)をスラリーCとして用意した。焼成物bは、未焼成Ce0.75Zr0.25O2粒子(商品名Actalys9320、ローディア社製)が1090℃で6時間、連続式焼成炉で焼成されることにより得られたものである。なお、焼成物bは、セリウム(IV)化合物とジルコニウム(IV)化合物とを原料として用いて得られたものである。
分散剤(ポリアクリル酸アンモニウム、重量平均分子量6000)が添加された水中で、体積中位径が表2に記載の値となるよう、ビーズミルにより焼成物c(Ce0.62Zr0.38O2粒子)が湿式粉砕されることにより得られたCe0.62Zr0.38O2粒子スラリー(Ce0.62Zr0.38O2粒子:25重量%)をスラリーDとして用意した。焼成物cは、未焼成Ce0.62Zr0.38O2粒子(商品名Actalys9330、ローディア社製)が1240℃で6時間、連続式焼成炉で焼成されることにより得られたものである。なお、焼成物cは、セリウム(IV)化合物とジルコニウム(IV)化合物とを原料として用いて得られたものである。
分散剤(ポリアクリル酸アンモニウム、重量平均分子量6000)が添加された水中で、体積中位径が表2に記載の値となるよう、ビーズミルにより焼成物d(Ce0.74Zr0.26O2粒子)が湿式粉砕されることにより得られたCe0.74Zr0.26O2粒子スラリー(Ce0.74Zr0.26O2粒子:25重量%)をスラリーEとして用意した。なお、焼成物dは、セリウム(III)化合物とジルコニウム(IV)化合物とを原料として用いて得られたものである。
分散剤(ポリアクリル酸アンモニウム、重量平均分子量6000)が添加された水中で、体積中位径が表2に記載の値となるよう、ビーズミルにより焼成物であるCeO2粒子(バイコウスキー社製、純度99.9%)が湿式粉砕されることにより得られたCeO2粒子スラリー(CeO2粒子:40重量%)をスラリーFとして用意した。なお、CeO2粒子は、セリウム(IV)化合物を原料として用いて得られたものである。
下記記載のコロイダルシリカを含む市販のスラリーをスラリーG〜Iとして用意した。
スラリーG:触媒化成工業(株)製、カタロイドSI-50、固形分濃度50(重量%)
スラリーH:触媒化成工業(株)製、カタロイドSI-45P、固形分濃度40(重量%)
スラリーI:触媒化成工業(株)製、カタロイドSI-80P、固形分濃度40(重量%)
上記のようにして調整されたスラリーA〜Fの何れかと、スラリーG〜Iの何れかと、水と、pH調整剤として硝酸とを、各々の濃度が夫々表2に記載の濃度となるように混合して、研磨液組成物を得た。
複合酸化物粒子の平均一次粒子径(nm)は、BET(窒素吸着)法によって算出される比表面積S(m2/g)を用いて下記式で算出される粒径(真球換算)を意味し、下記式により算出される。
平均一次粒子径(nm)=820/S
なお、前記比表面積は、スラリー10gを110℃で減圧乾燥して水分を除去したものをメノウ乳鉢で解砕し、得られた粉末を流動式比表面積自動測定装置フローソーブ2300(島津製作所製)を用いてを測定することにより求めた。
複合酸化物粒子の体積中位径(D50)は、以下の条件で測定した。
測定機器 :堀場製作所製 レーザー回折/散乱式粒度分布測定装置LA920
循環強度 :4
超音波強度:4
コロイダルシリカの一次粒子の体積中位粒径(D50)は、以下の方法により求めた。コロイダルシリカを日本電子製透過型電子顕微鏡(TEM)(商品名「JEM−2000FX」、80kV、1〜5万倍)で観察した写真をパソコンにスキャナで画像データとして取込む。そして、解析ソフト「WinROOF」(販売元:三谷商事)を用いて1000個以上のコロイダルシリカの1個1個のコロイダルシリカの円相当径を求めた。それを直径とし、表計算ソフト「EXCEL」(マイクロソフト社製)にて、コロイダルシリカの粒径分布データを得、全粒子中における、ある粒径の粒子の割合(体積基準%)を小粒径側からの累積体積頻度(%)として算出した。得られたコロイダルシリカの粒径及び累積体積頻度データに基づき、粒径に対して累積体積頻度をプロットすることにより、粒径対累積体積頻度グラフを得た。このグラフにおいて、小粒径側からの累積体積頻度が50%となる粒径をコロイダルシリカの体積中位粒径として求めた。
(測定条件)
装置:(株)リガク製、粉末X線解析装置 RINT2500VC
X線発生電圧:40kV
放射線 :Cu−Kα1線(λ=0.154050nm)
電流 :120mA
Scan Speed:10度/min
測定ステップ:0.02度/min
13133E02、理学電機株式会社)に基づいてなされている。
研磨前後の熱酸化膜の厚みを光干渉式膜厚計(商品名:VM−1000、大日本スクリーン製造(株)製)を用いて測定し、これらの値から下記の通り研磨速度を算出した。
研磨速度(nm/min)=(研磨前の膜の厚み)―(研磨後の膜の厚み)
直径5cm(2インチ)のシリコンウエハ上に形成された、厚さ1000nmの二酸化ケイ素膜を用意した。二酸化ケイ素膜は、シリコンウエハを、酸化炉内に入れて酸素ガスやスチームに晒し、シリコンウエハ中のシリコンと酸素を反応させることにより形成できる。
研磨試験機:ムサシノ電子社製、MA−300片面研磨機、定盤直径300mm、
研磨パッド:IC1000(硬質ウレタンパッド)とsuba400(不織布タイプパッド)との積層パッド(ニッタ・ハース(株)製)、
定盤回転数:90r/min、
キャリア回転数:90r/min、強制駆動式、
研磨液組成物供給速度:50g/min(約1.5mL/min/cm2)、
研磨時間:1min
研磨荷重:300g/cm2(錘による一定荷重)
ドレス条件:研磨前にイオン交換水を1分間供給して、ダイヤモンドリングでドレスした。
測定機器:VISION PSYTEC製、MicroMax VMX−2100
(Micromaxの測定条件)
光源:2Sλ(250W)及び3Pλ(250W)、共に光量が100%
チルド角:−9°
倍率:最大(視野範囲:研磨された面の全面積の35分の1)
観察領域:研磨された面の全面積(2インチ熱酸化膜ウエハ基板)
アイリス:notch
Claims (7)
- セリウムとジルコニウムとを含む複合酸化物粒子と、分散剤と、コロイダルシリカと、水系媒体とを含む研磨液組成物であって、
CuKα1線(λ=0.154050nm)を照射することにより得られる前記複合酸化物粒子の粉末X線回折スペクトル中に、
回折角2θ(θはブラック角)領域28.731〜28.911°内に頂点があるピーク(第1ピーク)、
回折角2θ領域33.273〜33.491°内に頂点があるピーク(第2ピーク)、
回折角2θ領域47.752〜48.143°内に頂点があるピーク(第3ピーク)、
回折角2θ領域56.717〜57.084°内に頂点があるピーク(第4ピーク)、が存在し、
前記第1ピークの半値幅が0.330〜0.433°であり、
前記粉末X線回折スペクトル中に、酸化ジルコニウムに由来し、その頂点が回折角2θ領域29.69〜31.60°に存在するピークa 2 が存在する場合、前記ピークa 2 の頂点の高さが前記第1ピークの頂点の高さの6.4%以下であり、
前記粉末X線回折スペクトル中に、酸化セリウムに由来し、その頂点が回折角2θ領域28.40〜28.59°に存在するピークa 1 は存在しない、研磨液組成物。 - 前記粉末X線回折スペクトル中に、前記ピークa2 が存在する場合、前記ピークa2の頂点の高さが前記第1ピークの頂点の高さの6.0%以下である、請求項1に記載の研磨液組成物。
- CuKα1線(λ=0.154050nm)を照射することにより得られる前記複合酸化物粒子の粉末X線回折スペクトル中に、
回折角2θ(θはブラック角)領域28.822〜28.911°内に頂点があるピーク(第1ピーク)、
回折角2θ領域33.406〜33.491°内に頂点があるピーク(第2ピーク)、
回折角2θ領域47.996〜48.143°内に頂点があるピーク(第3ピーク)、
回折角2θ領域56.971〜57.084°内に頂点があるピーク(第4ピーク)、が存在する、請求項2に記載の研磨液組成物。 - 前記複合酸化物粒子の体積中位径は、30〜1000nmである請求項1〜3のいずれかの項に記載の研磨液組成物。
- 前記コロイダルシリカの一次粒子の体積中位径(D50)は、50〜120nmである請求項1〜4のいずれかの項に記載の研磨液組成物。
- 研磨対象基板と研磨パッドとの間に、請求項1〜5のいずれかの項に記載の研磨液組成物を供給し、前記研磨対象基板と前記研磨パッドとが接した状態で、前記研磨パッドを前記研磨対象基板に対して相対運動させることにより、前記研磨対象基板を研磨する工程を含む研磨方法。
- 研磨対象基板の両主面のうちの少なくとも一方の主面を請求項1〜5のいずれかの項に記載の研磨液組成物を用いて研磨する研磨工程を含む精密部品用基板の製造方法。
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