JP2003342554A - Abrasive composition - Google Patents
Abrasive compositionInfo
- Publication number
- JP2003342554A JP2003342554A JP2002151422A JP2002151422A JP2003342554A JP 2003342554 A JP2003342554 A JP 2003342554A JP 2002151422 A JP2002151422 A JP 2002151422A JP 2002151422 A JP2002151422 A JP 2002151422A JP 2003342554 A JP2003342554 A JP 2003342554A
- Authority
- JP
- Japan
- Prior art keywords
- silica
- slurry
- particles
- silica particles
- polishing composition
- 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.)
- Pending
Links
Landscapes
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、硬度の異なるシリ
カ粒子を混合することによって研磨性能を高めた研磨組
成物に関する。本発明の研磨組成物は濃度４０％以上の
高濃度シリカスラリーにした場合でも低粘性で取り扱い
性がよく、化学的研磨(CMP)に適する。TECHNICAL FIELD The present invention relates to a polishing composition having improved polishing performance by mixing silica particles having different hardness. The polishing composition of the present invention has low viscosity and good handleability even when made into a high-concentration silica slurry having a concentration of 40% or more, and is suitable for chemical polishing (CMP).
【０００２】[0002]
【従来の技術】化学的研磨(CMP)において、フュームド
シリカやコロイダルシリカの分散液スラリーが用いられ
ている。研磨用分散液のフュームドシリカは研磨速度が
速い反面、精度面で劣ると言われており、一方、コロイ
ダルシリカは研磨速度が遅いが精度面で優れている。何
れの分散液についても、ハンドリング面では高濃度で取
り扱うほうが好ましいが、従来の分散液は高濃度スラリ
ーの経時安定性に問題があった。また、コロイダルシリ
カをベース研磨剤として、これに粒子径の異なるフュー
ムドシリカやフュームドアルミナを分散ないし含有せし
めた研磨剤も開示されているが（特開２００１−３４２
４５５）、スラリー濃度を高めようとすると分散状態が
不安定になるため、スラリー濃度の上限は５０％程度に
過ぎず、高濃度スラリーが得られないと云う問題があ
る。2. Description of the Related Art In chemical polishing (CMP), a dispersion slurry of fumed silica or colloidal silica is used. The fumed silica of the polishing dispersion has a high polishing rate, but is inferior in accuracy. On the other hand, colloidal silica has a low polishing rate but is excellent in accuracy. It is preferable to handle each of the dispersions at a high concentration in terms of handling, but the conventional dispersions have a problem in stability with time of the high-concentration slurry. Also disclosed is an abrasive in which colloidal silica is used as a base abrasive and fumed silica or fumed alumina having different particle diameters is dispersed or contained therein (JP-A-2001-342).
455), when the slurry concentration is increased, the dispersed state becomes unstable, so the upper limit of the slurry concentration is only about 50%, and there is a problem that a high concentration slurry cannot be obtained.
【０００３】[0003]
【発明が解決しようとする課題】本発明は従来のシリカ
スラリーにおける上記問題を解決したものであり、ドー
プ元素を導入して硬度を高めたシリカ粒子Ａとドープ元
素を含まないシリカ粒子Ｂとの混合粒子を用いることに
よって、研磨速度と研磨精度の両方の性能に優れた研磨
組成物を達成したものであり、この混合粒子はシリカ濃
度４０％以上、好ましくはシリカ濃度６０％以上の高濃
度スラリーにしても粘性が低く、経時安定性に優れる。DISCLOSURE OF THE INVENTION The present invention solves the above problems in conventional silica slurries, and comprises a silica particle A having a hardness increased by introducing a doping element and a silica particle B containing no doping element. By using the mixed particles, a polishing composition excellent in both polishing speed and polishing accuracy is achieved, and the mixed particles have a silica concentration of 40% or more, preferably a silica concentration of 60% or more. However, it has low viscosity and excellent stability over time.
【０００４】[0004]
【課題を解決する手段】すなわち、本発明は、（１）ド
ープ元素を導入して硬度を増強したシリカ粒子Ａと、ド
ープ元素を導入しないシリカ粒子Ｂとの混合粒子からな
ることを特徴とする研磨組成物に関する。本発明の研磨
組成物は、（２）シリカ粒子Ａとシリカ粒子Ｂの混合比
が０.５〜２.０である研磨組成物、（３）アルミニウム
またはカリウムを導入して硬度を高めたシリカ粒子Ａを
用いる研磨組成物、（４）シリカ粒子Ａの平均一次粒子
径が５〜６０nmであり、シリカ粒子Ｂの平均一次粒子径
が１〜１００nmである研磨組成物、（５）シリカ粒子Ａ
とシリカ粒子Ｂの混合粒子において、凝集粒子の平均粒
子径が０.０５〜１.０μmであり、この粒子径範囲に９
５％以上の凝集粒子が一山に分布している研磨組成物を
含む。Means for Solving the Problems That is, the present invention is characterized by comprising (1) mixed particles of silica particles A having a hardness enhanced by introducing a doping element and silica particles B having no doping element introduced therein. A polishing composition. The polishing composition of the present invention is (2) a polishing composition in which the mixing ratio of silica particles A and silica particles B is 0.5 to 2.0, and (3) silica in which aluminum or potassium is introduced to increase hardness. Polishing composition using particles A, (4) Polishing composition in which silica particles A have an average primary particle diameter of 5 to 60 nm, and silica particles B have an average primary particle diameter of 1 to 100 nm, (5) silica particles A
In the mixed particles of silica particles and silica particles B, the average particle size of the agglomerated particles is 0.05 to 1.0 μm, and the average particle size is 9
The polishing composition contains 5% or more of aggregated particles distributed in a mountain.
【０００５】さらに、本発明は、（６）上記何れかのシ
リカ粒子Ａとシリカ粒子Ｂの混合粒子を溶媒に分散させ
てなる高シリカ濃度シリカスラリーからなる研磨組成物
に関し、また（７）フュームドシリカからなるシリカ粒
子Ａを、コロイダルシリカからなるシリカ粒子Ｂに添加
して分散させたシリカスラリーからなる研磨組成物に関
する。このスラリー状の研磨組成物は、（８）シリカ濃
度４０wt％以上であって、スラリー粘度が６００mPa・s
以下である研磨組成物、（９）シリカ濃度６０wt％以上
であって、スラリー粘度が５００mPa・s以下である研磨
組成物、（１０）スラリー調製時の粘度と１ヶ月経過後
のスラリー粘度との比が１.５以下である研磨組成物を
含む。Further, the present invention relates to (6) a polishing composition comprising a silica slurry having a high silica concentration obtained by dispersing the mixed particles of any one of the above silica particles A and silica particles in a solvent, and (7) fumes. The present invention relates to a polishing composition composed of silica slurry in which silica particles A made of do silica are added to and dispersed in silica particles B made of colloidal silica. This slurry type polishing composition (8) has a silica concentration of 40 wt% or more and a slurry viscosity of 600 mPa · s.
The following polishing composition, (9) a silica concentration of 60 wt% or more and a slurry viscosity of 500 mPa · s or less, (10) a viscosity at the time of preparing the slurry and a slurry viscosity after one month has passed. The polishing composition has a ratio of 1.5 or less.
【０００６】本発明の研磨組成物は、ドープ元素を導入
して硬度を増強したシリカ粒子Ａとドープ元素を導入し
ないシリカ粒子Ｂの混合粒子を用いており、異なった硬
度のシリカ粒子が研磨作用を発揮するので、研磨速度と
研磨精度の両方の性能に優れている。また、シリカ粒子
Ａをフュームドシリカによって形成し、シリカ粒子Ｂを
コロイダルシリカによって形成すれば、シリカ濃度４０
％以上、好ましくはシリカ濃度６０wt％以上の高濃度ス
ラリーでも低粘性であって、しかも粘度の経時変化が少
ないスラリーを得ることができる。The polishing composition of the present invention uses a mixed particle of silica particles A having a hardness enhanced by introducing a doping element and silica particles B not having a doping element introduced therein, and silica particles having different hardness are used for polishing. Therefore, it excels in both polishing rate and polishing accuracy. If the silica particles A are made of fumed silica and the silica particles B are made of colloidal silica, the silica concentration is 40%.
% Or more, preferably a high-concentration slurry having a silica concentration of 60 wt% or more, it is possible to obtain a slurry having a low viscosity and a small viscosity change with time.
【０００７】[0007]
【発明の実施の形態】以下、本発明を実施形態に基づい
て具体的に説明する。なお、％は特に示さない限り重量
％である。本発明の研磨組成物は、ドープ元素を導入し
て硬度を増強したシリカ粒子Ａとドープ元素を導入しな
いシリカ粒子Ｂとの混合粒子からなる研磨組成物であ
り、好ましくは、シリカ粒子Ａとシリカ粒子Ｂの混合比
が０.５〜２.０であり、シリカ粒子Ａの平均一次粒子径
が５〜６０nm、シリカ粒子Ｂの平均一次粒子径が１〜１
００nmのものである。BEST MODE FOR CARRYING OUT THE INVENTION The present invention will be specifically described below based on embodiments. In addition,% is weight% unless otherwise indicated. The polishing composition of the present invention is a polishing composition composed of mixed particles of silica particles A having a hardness enhanced by introducing a doping element and silica particles B having no doping element introduced therein, preferably the silica particles A and silica. The mixing ratio of the particles B is 0.5 to 2.0, the average primary particle diameter of the silica particles A is 5 to 60 nm, and the average primary particle diameter of the silica particles B is 1 to 1
00 nm.
【０００８】シリカ粒子Ａに導入するドープ元素はシリ
カ粒子の硬度を高めるものが用いられる。具体的には、
例えば、アルミニウムやカリウムなどをドープすること
によってシリカ粒子の硬度を高めることができる。一般
にアルミニウムをドープしたシリカ粒子を製造する方法
としては、アルミニウム化合物、例えば塩化アルミニウ
ム(AlCl3)を含む溶液中にシリカ粒子を入れて、その表
面に溶液をコーティングし、その後、乾燥、焼成する方
法（溶液法）やアルミニウムおよびケイ素の化合物をガ
ス化し、その混合ガスを火炎（フレーム）中で反応させ
て混合酸化物を得る方法（火炎加水分解法）が知られて
いるが、本発明のアルミニウムドープシリカ粒子は、例
えば、ＥＰ第０８０８７６号、特開平１０−１６７７１
７号、特開平１２−１２７６１８号、特開２０００−１
６９１３２号で示される火炎加水分解法による熱分解に
基づき、本発明が意図するアルミニウムドープシリカが
得られる条件下で製造することによって得ることができ
る。このような方法でアルミニウムドープシリカを製造
することにより、シリカ粒子の表面層のみがアルミニウ
ムでドープされたシリカ粒子を得ることができ、しかも
微量のアルミニウムを均一にドープすることができる。The doping element introduced into the silica particles A is one that increases the hardness of the silica particles. In particular,
For example, the hardness of the silica particles can be increased by doping with aluminum or potassium. In general, as a method of producing silica particles doped with aluminum, a method of depositing silica particles in a solution containing an aluminum compound, for example, aluminum chloride (AlCl 3 ), coating the surface with the solution, and then drying and firing the solution. (Solution method) and a method of gasifying a compound of aluminum and silicon and reacting the mixed gas in a flame (flame) to obtain a mixed oxide (flame hydrolysis method) are known. Doped silica particles are described, for example, in EP No. 080876, JP-A-10-16771.
7, JP-A-12-127618, JP-A-2000-1
It can be obtained by producing under the conditions where the aluminum-doped silica intended by the present invention is obtained, based on the thermal decomposition by the flame hydrolysis method shown in No. 69132. By producing aluminum-doped silica by such a method, it is possible to obtain silica particles in which only the surface layer of the silica particles is doped with aluminum, and it is possible to uniformly dope a trace amount of aluminum.
【０００９】本発明の製造方法は、ガス化したケイ素化
合物（典型的には、SiCl4などのハロゲン化物）をフレ
ーム（火炎）中に送り、エアロゾルと反応させる。この
際、エアロゾルとしてアルミニウム化合物、例えば塩化
アルミニウム(AlCl3)を含むエアロゾルを用意する。こ
のようなエアロゾルは、アルミニウム化合物を含む溶液
または分散液を、エアロゾル発生器を用い、好適には超
音波法により噴霧状にすることにより調製する。このエ
アロゾルとケイ素化合物を含むガス混合物とを均一に混
合した状態で、フレーム中で反応させる。これにより表
面がアルミニウムでドープされたシリカが生成するの
で、これを常法によりガスから分離する。In the production method of the present invention, a gasified silicon compound (typically, a halide such as SiCl 4 ) is sent into a flame (flame) to react with an aerosol. At this time, an aerosol containing an aluminum compound, for example, aluminum chloride (AlCl 3 ) is prepared as the aerosol. Such an aerosol is prepared by atomizing a solution or dispersion containing an aluminum compound using an aerosol generator, preferably by an ultrasonic method. The aerosol and the gas mixture containing the silicon compound are allowed to react in a flame in a uniformly mixed state. This produces silica whose surface is doped with aluminum, which is separated from the gas by conventional methods.
【００１０】このような方法により製造されたアルミニ
ウムドープシリカ粒子は、アルミナ粒子とシリカ粒子が
混合したものとは異なり、シリカ粒子の表面層にアルミ
ニウムがドープされた粒子になる。また塩化アルミニウ
ム(AlCl3)の代わりに塩化カリウム(KCl)を用いるとシリ
カ粒子表面がカリウムでドープされたシリカを得ること
ができる。これらのシリカ粒子のBET比表面積は概ね５
〜４００m2/gである。このようにして得たシリカ粒子の
アルミニウムないしカリウムのドープ量は酸化物換算で
２.０重量％以下のものが適当であり、１×１０-2〜０.
５重量％がより好ましい。ドープ量が２.０重量％より
多いと大きなサイズの粒子ができやすくなるので経時的
に沈降等の問題を生じる。The aluminum-doped silica particles produced by such a method are particles in which the surface layer of the silica particles is doped with aluminum, unlike particles in which alumina particles and silica particles are mixed. When potassium chloride (KCl) is used instead of aluminum chloride (AlCl 3 ), silica whose surface is doped with potassium can be obtained. The BET specific surface area of these silica particles is approximately 5
~ 400 m 2 / g. The doping amount of aluminum or potassium in the silica particles thus obtained is preferably 2.0% by weight or less in terms of oxide, and 1 × 10 -2 to 0.
5% by weight is more preferred. If the dope amount is more than 2.0% by weight, large-sized particles are likely to be formed, which causes problems such as sedimentation over time.
【００１１】表面層にアルミニウムやカリウムがドープ
されたシリカ粒子Ａは、これらをドープしないシリカ粒
子Ｂよりも硬度が大きく、この混合粒子からなる研磨組
成物は異なった硬度のシリカ粒子Ａ、Ｂがおのおの研磨
作用を発揮するので、研磨速度と研磨精度の両方の性能
に優れている。さらに、単にアルミナ粒子やシリカ粒子
を混合したものでは得られない特性、例えば、優れた液
流動性や分散性を有する。The silica particles A whose surface layer is doped with aluminum or potassium have a higher hardness than the silica particles B not doped with aluminum or potassium, and the polishing composition comprising the mixed particles has silica particles A and B having different hardnesses. Since each exerts a polishing action, it excels in both polishing speed and polishing accuracy. Furthermore, it has characteristics that cannot be obtained by simply mixing alumina particles and silica particles, for example, excellent liquid flowability and dispersibility.
【００１２】シリカ粒子Ａの平均一次粒子径は５〜６０
nmが好ましく、シリカ粒子Ｂの平均一次粒子径は１〜１
００nmが好ましい。シリカ粒子Ａをフュームドシリカに
よって形成し、シリカ粒子Ｂをコロイダルシリカによっ
て形成する場合、一次粒子径５nm以下のフュームドシリ
カ粒子は製造が困難であり、６０nm以上のフュームドシ
リカ粒子はスラリーの経時変化に影響を起こしやすくな
り、粘度の経時変化やスラリー沈降物を生じさせる。ま
た、一次粒子径が１nm以下のコロイダルシリカ粒子は製
造が困難であり、１００nm以上のコロイダルシリカ粒子
はスラリー粘度の経時変化を生じやすくなり、またスラ
リーに沈降物を生じさせる。The average primary particle diameter of the silica particles A is 5 to 60.
nm is preferable, and the average primary particle diameter of the silica particles B is 1 to 1
00 nm is preferred. When the silica particles A are formed of fumed silica and the silica particles B are formed of colloidal silica, it is difficult to produce fumed silica particles having a primary particle size of 5 nm or less, and fumed silica particles having a particle size of 60 nm or more are used in the slurry over time. It tends to affect the change and causes a change in viscosity with time and a slurry sediment. Further, it is difficult to produce colloidal silica particles having a primary particle diameter of 1 nm or less, and colloidal silica particles having a primary particle diameter of 100 nm or more tend to cause a change in slurry viscosity with time, and also to cause sediment in the slurry.
【００１３】シリカ粒子Ａとシリカ粒子Ｂの混合比は
０.５〜２.０が好ましい。何れか一方が０.５倍未満あ
るいは２.０倍を上回ると、各々の特性が乏しくなり、
またシリカスラリーをを調製したときに高濃度化および
経時安定性が低下する。The mixing ratio of silica particles A and silica particles B is preferably 0.5 to 2.0. If either one is less than 0.5 times or more than 2.0 times, each characteristic becomes poor,
Further, when a silica slurry is prepared, the concentration becomes high and the stability with time decreases.
【００１４】また、シリカ粒子Ａとシリカ粒子Ｂの混合
粒子は、その凝集粒子の平均粒子径が０.０５〜１.０μ
mであり、この粒子径範囲に９５％以上の凝集粒子が一
山に分布しているものが好ましい。この混合シリカの凝
集粒子の分布ピークが一山９５％以下であると、スラリ
ーの経時変化に影響を起こしやすくなる。また、この分
布ピークにある凝集粒子の平均粒子径が１.０μmより大
きいとスラリー粘度が経時的に不安定である。一方、こ
の凝集粒子の平均粒子径が０.０５μmより小さいと十分
な効果が得られない。The mixed particles of the silica particles A and the silica particles B have an average particle diameter of the agglomerated particles of 0.05 to 1.0 μm.
It is m, and it is preferable that 95% or more of aggregated particles are distributed in a mountain in this particle size range. When the distribution peak of the aggregated particles of this mixed silica is 95% or less for one peak, the change over time of the slurry tends to be affected. If the average particle size of the aggregated particles at this distribution peak is larger than 1.0 μm, the slurry viscosity becomes unstable over time. On the other hand, if the average particle size of the aggregated particles is smaller than 0.05 μm, a sufficient effect cannot be obtained.
【００１５】本発明の研磨組成物は、上記シリカ粒子Ａ
とシリカ粒子Ｂの混合粒子を溶媒に分散させてなる高シ
リカ濃度シリカスラリーからなる研磨組成物として用い
ることができる。この場合、フュームドシリカからなる
シリカ粒子Ａをコロイダルシリカからなるシリカ粒子Ｂ
に添加して分散させればシリカ濃度の高いシリカスラリ
ーを容易に得ることができる。具体的には、フュームド
シリカからなるシリカ粒子Ａを、コロイダルシリカから
なるシリカ粒子Ｂに添加して分散させることにより、シ
リカ濃度４０％以上、好ましくはシリカ濃度６０％以上
の高濃度スラリーであって、しかも粘性が低く、かつ粘
性の経時変化が少ないスラリーを得ることができる。The polishing composition of the present invention comprises the above silica particles A.
It can be used as a polishing composition comprising a silica slurry having a high silica concentration obtained by dispersing mixed particles of silica particles B with a silica particle in a solvent. In this case, the silica particles A made of fumed silica are replaced by the silica particles B made of colloidal silica.
A silica slurry having a high silica concentration can be easily obtained by adding it to and dispersing it. Specifically, a silica particle A made of fumed silica is added to and dispersed in a silica particle B made of colloidal silica to obtain a high-concentration slurry having a silica concentration of 40% or more, preferably a silica concentration of 60% or more. Moreover, it is possible to obtain a slurry having a low viscosity and a small change in viscosity over time.
【００１６】因みに、一般にはコロイダルシリカスラリ
ーのシリカ濃度は２０〜４０％程度であり、５０％以上
の高濃度スラリーを得るのは難しい。また、通常、フュ
ームドシリカのスラリー濃度は蒸留水中で２０%程度が
限度であるが、本発明において、アルミナや酸化カリウ
ムをドープしたフュームドシリカは蒸留水中で４０%程
度まで分散させることが可能であり、このフュームドシ
リカをコロイダルシリカスラリーに添加することによっ
て、シリカ濃度４０％以上、好ましくはシリカ濃度６０
％以上の高濃度シリカスラリーを得ることができる。Incidentally, the silica concentration of colloidal silica slurry is generally about 20 to 40%, and it is difficult to obtain a high concentration slurry of 50% or more. Further, usually, the concentration of the fumed silica slurry is limited to about 20% in distilled water, but in the present invention, fumed silica doped with alumina or potassium oxide can be dispersed up to about 40% in distilled water. By adding this fumed silica to the colloidal silica slurry, the silica concentration is 40% or more, preferably the silica concentration is 60%.
It is possible to obtain a high-concentration silica slurry having a concentration of at least%.
【００１７】また、アルミニウムおよび/またはカリウ
ムをドープしたフュームドシリカを用いることによっ
て、シリカスラリーの粘度が安定し、ｐＨ４.５以下な
いしｐＨ８以上のシリカスラリーについて、粘度が１０
０/ｓのせん断速度で６００mPa・s以下、好ましくは５０
０mPa・s以下の低粘性シリカスラリーを得ることができ
る。しかも、このシリカスラリーはスラリー調製時の粘
度と１ヶ月経過後のスラリー粘度との比が１.５以下で
あり、経時安定性に優れたものである。The use of fumed silica doped with aluminum and / or potassium stabilizes the viscosity of the silica slurry, and the viscosity of silica slurries having a pH of 4.5 or less to a pH of 8 or more has a viscosity of 10 or less.
600 mPa · s or less at a shear rate of 0 / s, preferably 50
A low-viscosity silica slurry having a viscosity of 0 mPa · s or less can be obtained. Moreover, this silica slurry has a ratio of the viscosity at the time of slurry preparation to the viscosity of the slurry after one month is 1.5 or less, and is excellent in stability over time.
【００１８】[0018]
【実施例】以下、実施例および比較例によって本発明を
具体的に示す。なお、各例において粘度はHAAKE社のRhe
oStress計を用いて測定し、粒子径はHORIBA社のレーザ
ー散乱式粒度分布計を用いて測定した。粘度は１００ｓ
-1のせん断速度での値、経時変化粘度はスラリー調製時
から１ヶ月経過後の粘度である。EXAMPLES The present invention will be specifically described below with reference to Examples and Comparative Examples. In each case, the viscosity is Rhe of HAAKE.
The particle size was measured using a laser scattering type particle size distribution meter manufactured by HORIBA. Viscosity is 100s
The value at a shear rate of -1 and the viscosity with time change are the viscosities after one month has elapsed from the time of slurry preparation.
【００１９】〔実施例１〕市販のコロイダルシリカスラ
リー（日産化学社製品:スノーテックス#30）にフュームドシリ
カ（商品名VP3375、比表面積70m2/g、アルミナ0.2％含有、テ
゛ク゛サ社製品）を４０％添加し、攪拌分散させてスラリー
化し、ｐＨ９.１に調整し、シリカ濃度７０％のスラリ
ーを調製した。このスラリーの粘度と粒子径を測定し
た。またスラリー中の凝集粒子径および凝集一山率を測
定した。この結果をスラリー化条件と共に表１に示し
た。Example 1 A commercially available colloidal silica slurry (Nissan Chemical Co., Ltd .: Snowtex # 30) was mixed with fumed silica (trade name VP3375, specific surface area 70 m 2 / g, alumina 0.2% content, manufactured by Debugger). 40% was added and dispersed by stirring to make a slurry, and the pH was adjusted to 9.1 to prepare a slurry having a silica concentration of 70%. The viscosity and particle size of this slurry were measured. In addition, the aggregate particle size and the aggregate peak rate in the slurry were measured. The results are shown in Table 1 together with the slurry conditions.
【００２０】〔実施例２〕市販のコロイダルシリカスラ
リー（日産化学社製品:スノーテックス#20）にフュームドシリ
カ（商品名VP3375、比表面積70m2/g、アルミナ0.2％含有、テ
゛ク゛サ社製品）を４０％添加し、攪拌分散させてスラリー
化し、ｐＨ３.４に調整し、シリカ濃度６０％のスラリ
ーを調製した。このスラリーの粘度と粒子径を測定し
た。またスラリー中の凝集粒子径および凝集一山率を測
定した。この結果をスラリー化条件と共に表１に示し
た。Example 2 A commercially available colloidal silica slurry (Nissan Chemical Co., Ltd .: Snowtex # 20) was mixed with fumed silica (trade name VP3375, specific surface area 70 m 2 / g, alumina 0.2% content, manufactured by Debugger). 40% was added, and the mixture was stirred and dispersed to form a slurry, which was adjusted to pH 3.4 to prepare a slurry having a silica concentration of 60%. The viscosity and particle size of this slurry were measured. In addition, the aggregate particle size and the aggregate peak rate in the slurry were measured. The results are shown in Table 1 together with the slurry conditions.
【００２１】〔実施例３〕市販のコロイダルシリカスラ
リー（日産化学社製品:スノーテックス#40）にフュームドシリ
カ（商品名VP3375、比表面積70m2/g、アルミナ0.2％含有、テ
゛ク゛サ社製品）を２０％添加し、攪拌分散させてスラリー
化し、ｐＨ９.４に調整し、シリカ濃度６０％のスラリ
ーを調製した。このスラリーの粘度と粒子径を測定し
た。またスラリー中の凝集粒子径および凝集一山率を測
定した。この結果をスラリー化条件と共に表１に示し
た。Example 3 A commercially available colloidal silica slurry (Nissan Chemical Co., Ltd .: Snowtex # 40) was mixed with fumed silica (trade name VP3375, specific surface area 70 m 2 / g, alumina 0.2% content, manufactured by Debugger). 20% was added and dispersed by stirring to make a slurry, and the pH was adjusted to 9.4 to prepare a slurry having a silica concentration of 60%. The viscosity and particle size of this slurry were measured. In addition, the aggregate particle size and the aggregate peak rate in the slurry were measured. The results are shown in Table 1 together with the slurry conditions.
【００２２】〔実施例４〕市販のコロイダルシリカスラ
リー（日産化学社製品:スノーテックス#20）にフュームドシリ
カ（商品名VP3375、比表面積70m2/g、アルミナ0.2％含有、テ
゛ク゛サ社製品）を４０％添加し、湿式ジェットミルで分散
させてスラリー化し、ｐＨ３.１に調整し、シリカ濃度
６０％のスラリーを調製した。このスラリーの粘度と粒
子径を測定した。またスラリー中の凝集粒子径および凝
集一山率を測定した。この結果をスラリー化条件と共に
表１に示した。[Example 4] A commercially available colloidal silica slurry (Nissan Chemical Co., Ltd. product: Snowtex # 20) was mixed with fumed silica (trade name VP3375, specific surface area 70 m 2 / g, alumina 0.2% content, manufactured by Debugger Company). 40% was added and dispersed by a wet jet mill to form a slurry, and the pH was adjusted to 3.1 to prepare a slurry having a silica concentration of 60%. The viscosity and particle size of this slurry were measured. In addition, the aggregate particle size and the aggregate peak rate in the slurry were measured. The results are shown in Table 1 together with the slurry conditions.
【００２３】〔実施例５〕市販のコロイダルシリカスラ
リー（日産化学社製品:スノーテックス#30）にフュームドシリ
カ(商品名VP3779、比表面積300m2/g、酸化カリウム0.2％含
有、テ゛ク゛サ社製品)を４０％添加し、攪拌分散させてスラ
リー化し、ｐＨ１.３に調整し、シリカ濃度７０％のス
ラリーを調製した。このスラリーの粘度と粒子径を測定
した。またスラリー中の凝集粒子径および凝集一山率を
測定した。この結果をスラリー化条件と共に表１に示し
た。Example 5 Fumed silica (trade name VP3779, specific surface area 300 m 2 / g, containing 0.2% potassium oxide, product of Debugger Co.) in commercially available colloidal silica slurry (Nissan Chemical Co., Ltd. product: Snowtex # 30). Was added to 40%, stirred and dispersed to form a slurry, and the pH was adjusted to 1.3 to prepare a slurry having a silica concentration of 70%. The viscosity and particle size of this slurry were measured. In addition, the aggregate particle size and the aggregate peak rate in the slurry were measured. The results are shown in Table 1 together with the slurry conditions.
【００２４】〔実施例６〕市販のコロイダルシリカスラ
リー（日産化学社製品:スノーテックス#40）にフュームドシリ
カ（商品名VP3375、比表面積70m2/g、アルミナ0.2％含有、テ
゛ク゛サ社製品）を４０％添加し、攪拌分散させてスラリー
化し、ｐＨ８.９に調整し、シリカ濃度８０％のスラリ
ーを調製した。このスラリーの粘度と粒子径を測定し
た。またスラリー中の凝集粒子径および凝集一山率を測
定した。この結果をスラリー化条件と共に表１に示し
た。Example 6 A commercially available colloidal silica slurry (Nissan Chemical Co., Ltd .: Snowtex # 40) was mixed with fumed silica (trade name VP3375, specific surface area 70 m 2 / g, alumina 0.2% content, manufactured by Debugger). 40% was added, stirred and dispersed to form a slurry, and the pH was adjusted to 8.9 to prepare a slurry having a silica concentration of 80%. The viscosity and particle size of this slurry were measured. In addition, the aggregate particle size and the aggregate peak rate in the slurry were measured. The results are shown in Table 1 together with the slurry conditions.
【００２５】〔比較例１〕蒸留水にフュームドシリカ
（商品名VP3375、比表面積70m2/g、アルミナ0.2％含有、テ゛ク゛
サ社製品）を７０％添加し、攪拌分散させてスラリー化
し、ｐＨ９.１に調整し、シリカ濃度７０％のスラリー
を調製した。このスラリーの粘度と粒子径を測定した。
またスラリー中の凝集粒子径および凝集一山率を測定し
た。この結果をスラリー化条件と共に表２に示した。[Comparative Example 1] 70% of fumed silica (trade name VP3375, specific surface area 70 m 2 / g, containing 0.2% alumina, product of DGEA Co., Ltd.) was added to distilled water, stirred and dispersed to form a slurry, and pH was adjusted to 9. The slurry was adjusted to 1 to prepare a slurry having a silica concentration of 70%. The viscosity and particle size of this slurry were measured.
In addition, the aggregate particle size and the aggregate peak rate in the slurry were measured. The results are shown in Table 2 together with the slurry conditions.
【００２６】〔比較例２〕市販のコロイダルシリカスラ
リー（日産化学社製品:スノーテックス#40）にアルミナ（商品
名:酸化アルミニウムC、比表面積100m2/g、アルミナ100％、
テ゛ク゛サ社製品）を６％添加し、ｐＨ９.８に調整し、シリ
カ・アルミナ濃度４６％のスラリーを調製した。このス
ラリーの粘度と粒子径を測定した。またスラリー中の凝
集粒子径および凝集一山率を測定した。この結果をスラ
リー化条件と共に表２に示した。Comparative Example 2 A commercially available colloidal silica slurry (Nissan Chemical Co., Ltd .: Snowtex # 40) was added to alumina (trade name: aluminum oxide C, specific surface area 100 m 2 / g, alumina 100%,
6% of a product manufactured by Degsa Co., Ltd. was added to adjust the pH to 9.8 to prepare a slurry having a silica / alumina concentration of 46%. The viscosity and particle size of this slurry were measured. In addition, the aggregate particle size and the aggregate peak rate in the slurry were measured. The results are shown in Table 2 together with the slurry conditions.
【００２７】〔比較例３〕市販のコロイダルシリカスラ
リー（日産化学社製品:スノーテックス#20）にフュームドシリ
カ(商品名VP3375、比表面積70０m2/g、アルミナ0.2％含有、
テ゛ク゛サ社製品)を６０％添加し、ｐＨ９.４に調整し、シ
リカ濃度８０％のスラリーを調製した。このスラリーの
粘度と粒子径を測定した。またスラリー中の凝集粒子径
および凝集一山率を測定した。この結果をスラリー化条
件と共に表２に示した。Comparative Example 3 A commercially available colloidal silica slurry (Nissan Chemical Co., Ltd .: Snowtex # 20) containing fumed silica (trade name VP3375, specific surface area 700 m 2 / g, alumina 0.2%,
60% of a product manufactured by Degsa Co., Ltd. was added to adjust the pH to 9.4 to prepare a slurry having a silica concentration of 80%. The viscosity and particle size of this slurry were measured. In addition, the aggregate particle size and the aggregate peak rate in the slurry were measured. The results are shown in Table 2 together with the slurry conditions.
【００２８】〔比較例４〕市販のコロイダルシリカスラ
リー（日産化学社製品:スノーテックス#40）にフュームドシリ
カ（商品名Aerosil#200、比表面積200m2/g、日本アエロシ゛ル
社製品）を１６％添加し、攪拌分散させてスラリー化
し、ｐＨ３.１に調整し、シリカ濃度５６％のスラリー
を調製した。このスラリーの粘度と粒子径を測定した。
またスラリー中の凝集粒子径および凝集一山率を測定し
た。この結果をスラリー化条件と共に表２に示した。[Comparative Example 4] 16% of commercially available colloidal silica slurry (Nissan Chemical Co., Ltd. product: Snowtex # 40) with fumed silica (trade name Aerosil # 200, specific surface area 200 m 2 / g, product of Nippon Aerogel Co., Ltd.) The mixture was added, stirred and dispersed to form a slurry, and the pH was adjusted to 3.1 to prepare a slurry having a silica concentration of 56%. The viscosity and particle size of this slurry were measured.
In addition, the aggregate particle size and the aggregate peak rate in the slurry were measured. The results are shown in Table 2 together with the slurry conditions.
【００２９】〔比較例５〕市販のコロイダルシリカスラ
リー（日産化学社製品:スノーテックス#20）にフュームドシリ
カ(商品名VP3375、比表面積70m2/g、アルミナ0.2％含有、テ゛
ク゛サ社製品)を５０％添加し、ｐＨ１０.０に調整し、シ
リカ濃度７０％のスラリーを調製した。このスラリーの
粘度と粒子径を測定した。またスラリー中の凝集粒子径
および凝集一山率を測定した。この結果をスラリー化条
件と共に表２に示した。[Comparative Example 5] A commercially available colloidal silica slurry (Nissan Chemical's product: Snowtex # 20) was mixed with fumed silica (trade name VP3375, specific surface area 70 m 2 / g, alumina 0.2% content, manufactured by Debugger). 50% was added and the pH was adjusted to 10.0 to prepare a slurry having a silica concentration of 70%. The viscosity and particle size of this slurry were measured. In addition, the aggregate particle size and the aggregate peak rate in the slurry were measured. The results are shown in Table 2 together with the slurry conditions.
【００３０】[0030]
【発明の効果】本発明の研磨組成物は硬度の異なるシリ
カ粒子Ａ、Ｂがおのおの研磨作用を発揮するので両方の
利点を併せ持つ。また高濃度のシリカスラリーを得るこ
とができ、このスラリーは高濃度でありながら粘性が低
く、粘度の経時変化も小さい。従って、化学的研磨(CM
P)などにおいて、研磨速度が比較的速く、しかも研磨精
度も優れる。EFFECTS OF THE INVENTION The polishing composition of the present invention has both advantages because silica particles A and B having different hardnesses exert polishing effects. Further, a high-concentration silica slurry can be obtained, and this slurry has a low viscosity while having a high concentration, and its viscosity changes little with time. Therefore, chemical polishing (CM
In P) and the like, the polishing rate is relatively fast and the polishing accuracy is excellent.
【００３１】[0031]
【表１】 [Table 1]
【００３２】[0032]
【表２】 [Table 2]
───────────────────────────────────────────────────── フロントページの続き (72)発明者 城野 博州 三重県四日市市三田町３番地 日本アエロ ジル株式会社四日市工場内 (72)発明者 落合 満 東京都新宿区西新宿２丁目３番１号 新宿 モノリス13階 日本アエロジル株式会社内 Ｆターム(参考） 3C058 AA07 CB01 CB03 DA02 DA12 ─────────────────────────────────────────────────── ─── Continued front page (72) Inventor Jono Hakushu 3 Mita-cho, Yokkaichi-shi, Mie Japan Aero Jill Co., Ltd. Yokkaichi factory (72) Inventor Mitsuru Ochiai 2-3-1, Nishi-Shinjuku, Shinjuku-ku, Tokyo Shinjuku Monolith 13th floor, within Aerosil Japan F term (reference) 3C058 AA07 CB01 CB03 DA02 DA12
Claims (10)
リカ粒子Ａと、ドープ元素を導入しないシリカ粒子Ｂと
の混合粒子からなることを特徴とする研磨組成物。1. A polishing composition comprising mixed particles of silica particles A having a hardness enhanced by introducing a doping element and silica particles B having no doping element introduced therein.
０.５〜２.０である請求項１の研磨組成物。2. The polishing composition according to claim 1, wherein the mixing ratio of the silica particles A and the silica particles B is 0.5 to 2.0.
硬度を高めたシリカ粒子Ａを用いる請求項１または２の
研磨組成物。3. The polishing composition according to claim 1, wherein silica particles A having an increased hardness by introducing aluminum or potassium are used.
０nmであり、シリカ粒子Ｂの平均一次粒子径が１〜１０
０nmである請求項１、２または３に記載する研磨組成
物。4. The silica particles A have an average primary particle diameter of 5 to 6.
0 nm, and the average primary particle diameter of the silica particles B is 1 to 10
The polishing composition according to claim 1, 2 or 3, which has a thickness of 0 nm.
において、凝集粒子の平均粒子径が０.０５〜１.０μm
であり、この粒子径範囲に９５％以上の凝集粒子が一山
に分布している請求項１〜請求項４の何れかに記載する
研磨組成物。5. A mixed particle of silica particle A and silica particle B, wherein the average particle diameter of the agglomerated particles is 0.05 to 1.0 μm.
The polishing composition according to any one of claims 1 to 4, wherein 95% or more of the aggregated particles are distributed in one peak in this particle size range.
シリカ粒子Ｂの混合粒子を溶媒に分散させてなる高シリ
カ濃度シリカスラリーからなる研磨組成物。6. A polishing composition comprising a high-silica-concentration silica slurry obtained by dispersing the mixed particles of the silica particles A and the silica particles B according to claim 1 in a solvent.
を、コロイダルシリカからなるシリカ粒子Ｂに添加して
分散させたシリカスラリーからなる請求項１〜６の何れ
かに記載する研磨組成物。7. Silica particles A made of fumed silica
7. The polishing composition according to any one of claims 1 to 6, which comprises a silica slurry in which is added to and dispersed in silica particles B made of colloidal silica.
リー粘度が６００mPa・s以下である請求項１〜７の何れ
かに記載する研磨組成物。8. The polishing composition according to claim 1, which has a silica concentration of 40 wt% or more and a slurry viscosity of 600 mPa · s or less.
リー粘度が５００mPa・s以下である請求項８に記載する
研磨組成物。9. The polishing composition according to claim 8, which has a silica concentration of 60 wt% or more and a slurry viscosity of 500 mPa · s or less.
のスラリー粘度との比が１.５以下である請求項１〜９
の何れかに記載する研磨組成物。10. The ratio of the viscosity at the time of preparing the slurry to the viscosity of the slurry after one month has elapsed is 1.5 or less.
The polishing composition as described in any one of 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002151422A JP2003342554A (en) | 2002-05-24 | 2002-05-24 | Abrasive composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002151422A JP2003342554A (en) | 2002-05-24 | 2002-05-24 | Abrasive composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2003342554A true JP2003342554A (en) | 2003-12-03 |
Family
ID=29769018
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2002151422A Pending JP2003342554A (en) | 2002-05-24 | 2002-05-24 | Abrasive composition |
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| Country | Link |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006256913A (en) * | 2005-03-17 | 2006-09-28 | Admatechs Co Ltd | Spherical silica particle, resin composition and semiconductor liquid sealing material |
| JP2009279720A (en) * | 2008-05-23 | 2009-12-03 | Jgc Catalysts & Chemicals Ltd | Particle-dispersed fluid for polishing, and manufacturing method thereof |
| JP2010036290A (en) * | 2008-08-04 | 2010-02-18 | Jsr Corp | Aqueous dispersing element for chemical mechanical polishing to be used for manufacturing circuit board, method of manufacturing circuit board, circuit board, and multilayer circuit board |
| CN101970589A (en) * | 2007-11-30 | 2011-02-09 | 安集微电子（上海）有限公司 | A chemical-mechanical polishing liquid |
| JP2018104547A (en) * | 2016-12-26 | 2018-07-05 | ニッタ・ハース株式会社 | Slurry for polishing |
-
2002
- 2002-05-24 JP JP2002151422A patent/JP2003342554A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006256913A (en) * | 2005-03-17 | 2006-09-28 | Admatechs Co Ltd | Spherical silica particle, resin composition and semiconductor liquid sealing material |
| CN101970589A (en) * | 2007-11-30 | 2011-02-09 | 安集微电子（上海）有限公司 | A chemical-mechanical polishing liquid |
| JP2009279720A (en) * | 2008-05-23 | 2009-12-03 | Jgc Catalysts & Chemicals Ltd | Particle-dispersed fluid for polishing, and manufacturing method thereof |
| JP2010036290A (en) * | 2008-08-04 | 2010-02-18 | Jsr Corp | Aqueous dispersing element for chemical mechanical polishing to be used for manufacturing circuit board, method of manufacturing circuit board, circuit board, and multilayer circuit board |
| JP2018104547A (en) * | 2016-12-26 | 2018-07-05 | ニッタ・ハース株式会社 | Slurry for polishing |
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