JP2002329688A - Polishing suspension containing moisture holding agent - Google Patents
Polishing suspension containing moisture holding agentInfo
- Publication number
- JP2002329688A JP2002329688A JP2001378040A JP2001378040A JP2002329688A JP 2002329688 A JP2002329688 A JP 2002329688A JP 2001378040 A JP2001378040 A JP 2001378040A JP 2001378040 A JP2001378040 A JP 2001378040A JP 2002329688 A JP2002329688 A JP 2002329688A
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- Japan
- Prior art keywords
- polishing
- polishing suspension
- ethylene
- suspension
- abrasive
- 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.)
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、シリコンウエハー
等の精密電子部品や光学部品の表面を仕上げ研磨するた
めに使用される研磨用懸濁液に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a polishing suspension used for finish-polishing surfaces of precision electronic components and optical components such as silicon wafers.
【０００２】[0002]
【従来の技術】半導体集積回路用のシリコンウエハーの
表面は、精巧なパターンが形成されるため、精密な研磨
仕上げを施してある。2. Description of the Related Art The surface of a silicon wafer for a semiconductor integrated circuit is precisely polished to form a fine pattern.
【０００３】ウエハー表面の研磨仕上げは、従来汎用さ
れていたコロイダルシリカよりもさらに微細な研磨材で
あるヒュームドシリカが分散している研磨用懸濁液を用
いた化学的機械的研磨（chemical mechanical polishin
g：ＣＭＰ）により行われる。[0003] The polishing finish of the wafer surface is performed by a chemical mechanical polishing (chemical mechanical polishing) using a polishing suspension in which fumed silica, which is a finer abrasive material than conventional colloidal silica, is dispersed. polishin
g: CMP).
【０００４】研磨機のターンテーブルに載せたシリコン
ウエハーへこの懸濁液をかけながらウレタンパッドで研
磨する。このとき懸濁液の一部は滴となって飛び散り、
ターンテーブルを取り巻く外壁に付着する。この付着し
た滴が外壁上で乾燥すると、滴中のヒュームドシリカが
不可逆的に凝集して大きな凝集塊を形成する。研磨の途
中にこの凝集塊が剥離してウエハー表面に付着すると傷
をつけてしまう。また研磨後にウエハーや外壁を水で洗
浄してもその表面に凝集塊が懸濁液の跡となって残る。
これが剥離すると、研磨の途中のウエハー表面に傷をつ
けてしまう。研磨用懸濁液の跡や傷の付いたウエハー
は、不良品である。The suspension is applied to a silicon wafer placed on a turntable of a polishing machine and polished with a urethane pad. At this time, part of the suspension scatters as drops,
It adheres to the outer wall surrounding the turntable. When the attached droplets dry on the outer wall, the fumed silica in the droplets irreversibly aggregates to form large aggregates. If the aggregates are separated during the polishing and adhere to the surface of the wafer, they will be damaged. Further, even if the wafer and the outer wall are washed with water after polishing, agglomerates remain on the surface as traces of the suspension.
If this peels off, the surface of the wafer being polished will be damaged. Wafers with traces or scratches of the polishing suspension are defective.
【０００５】[0005]
【発明が解決しようとする課題】本発明は前記の課題を
解決するためになされたもので、シリコンウエハー等を
精密に研磨する際に用いられ、研磨後の水での洗浄の際
に残留物を残すことなく確実に洗い流すことのできる研
磨用懸濁液を提供することを目的とする。DISCLOSURE OF THE INVENTION The present invention has been made to solve the above-mentioned problems, and is used for precisely polishing a silicon wafer or the like. It is an object of the present invention to provide a polishing suspension that can be surely washed away without leaving.
【０００６】[0006]
【課題を解決するための手段】前記の目的を達成するた
めになされた本発明の研磨用懸濁液は、ヒュームドシリ
カ、ヒュームドアルミナ、高純度酸化セリウムから選ば
れる少なくとも一種類の研磨材がアルカリ水溶液に分散
し、エチレングリコール、ポリエチレングリコール、グ
リセリン、プロピレングリコール、ポリグリセリン、グ
リセリンのエチレンオキサイド付加物、エチレン−プロ
ピレンブロック共重合物から選ばれる少なくとも一種類
の保湿剤を含有している。In order to achieve the above-mentioned object, the polishing suspension of the present invention comprises at least one abrasive selected from fumed silica, fumed alumina and high-purity cerium oxide. Is dispersed in an aqueous alkali solution and contains at least one humectant selected from ethylene glycol, polyethylene glycol, glycerin, propylene glycol, polyglycerin, an ethylene oxide adduct of glycerin, and an ethylene-propylene block copolymer.
【０００７】ポリエチレングリコール、グリセリンのエ
チレンオキサイド付加物、エチレン−プロピレンブロッ
ク共重合物は平均分子量２００〜１００００のものが好
適に用いられる。ポリグリセリンは、ジグリセリンまた
はトリグリセリンであってもよい。保湿剤は、親水性で
あって水への溶解性が高く、常温における蒸気圧が低く
て揮発し難いものである。As the polyethylene glycol, an ethylene oxide adduct of glycerin, and an ethylene-propylene block copolymer, those having an average molecular weight of 200 to 10,000 are preferably used. The polyglycerin may be diglycerin or triglycerin. The humectant is hydrophilic, has high solubility in water, has a low vapor pressure at normal temperature, and is difficult to volatilize.
【０００８】保湿剤が、該研磨材１重量部に対し、０．
１〜１．０重量部であることが好ましい。この範囲より
も少ないと水で洗浄したときに研磨材が残存してしま
い、一方この範囲より多いとスラリーが増粘し作業性が
悪くなってしまう。A humectant is used in an amount of 0.1 to 1 part by weight of the abrasive.
It is preferably from 1 to 1.0 part by weight. If it is less than this range, the abrasive will remain when washed with water, while if it is more than this range, the slurry will thicken and the workability will deteriorate.
【０００９】研磨用懸濁液がアルカリ性であるので、研
磨材の分散が安定化している。研磨用懸濁液は、アルカ
リ水溶液が水酸化カリウム水溶液、アンモニア水、トリ
エチルアミン水溶液であることにより好適に実施され
る。特に水酸化カリウム水溶液であると、アミン臭がな
く作業し易いので一層好ましい。Since the polishing suspension is alkaline, the dispersion of the abrasive is stabilized. The polishing suspension is preferably performed when the aqueous alkaline solution is an aqueous potassium hydroxide solution, aqueous ammonia, or an aqueous triethylamine solution. In particular, an aqueous solution of potassium hydroxide is more preferable because it is easy to work without amine odor.
【００１０】ヒュームドシリカは、例えば酸水素火炎中
でテトラクロロシランを気相加水分解させると得られる
ものである。その粒径が１６〜２０ｎｍ、比表面積が９
０〜１３０ｍ２／ｇであることが好ましい。具体的には
ＡＥＲＯＳＩＬ ９０Ｇまたは同１３０（いずれも日本
アエロジル(株)社製の商品名）が挙げられる。[0010] Fumed silica is obtained, for example, by subjecting tetrachlorosilane to gas phase hydrolysis in an oxyhydrogen flame. Its particle size is 16-20 nm, specific surface area is 9
It is preferably from 0 to 130 m 2 / g. Specific examples include AEROSIL 90G and AEROSIL 130 (both are trade names manufactured by Nippon Aerosil Co., Ltd.).
【００１１】ヒュームドアルミナは、例えば、酸水素火
炎中で塩化アルミニウムを気相加水分解することにより
得られるものである。その粒径が約１３ｎｍ、比表面積
が８５〜１１５ｍ２／ｇであることが好ましい。具体的
には酸化アルミニウムＣ（日本アエロジル社製の商品
名）が挙げられる。Fumed alumina is obtained, for example, by subjecting aluminum chloride to gas phase hydrolysis in an oxyhydrogen flame. It is preferable that the particle size is about 13 nm and the specific surface area is 85 to 115 m 2 / g. Specific examples include aluminum oxide C (trade name, manufactured by Nippon Aerosil Co., Ltd.).
【００１２】高純度酸化セリウムは、溶媒抽出精製の
後、炭酸セリウム、シュウ酸セリウムとして焼成するこ
とにより得られるものである。その粒径が２００〜３０
０ｎｍ、比表面積が２０〜３０ｍ２／ｇであることが好
ましい。具体的にはＣｅＯ２ＫＫ（阿南化成社製の商品
名）が挙げられる。[0012] High-purity cerium oxide is obtained by calcination as cerium carbonate or cerium oxalate after solvent extraction and purification. Its particle size is 200-30
The specific surface area is preferably 0 nm and the specific surface area is 20 to 30 m 2 / g. Specific examples include CeO 2 KK (trade name of Anan Kasei Co., Ltd.).
【００１３】高圧ホモジナイザーにより、研磨材は分散
されている。高圧ホモジナイザーは、例えば攪拌してい
るアルカリ水溶液にヒュームドシリカ等の研磨材が加え
られて得られたスラリーを、高圧に加圧しつつ硬い面に
あけられた微細な孔へ強制的に通過させて、乱流による
衝撃や超音波の発生を利用して、研磨材の粉砕および分
散を行うものである。The abrasive is dispersed by the high-pressure homogenizer. The high-pressure homogenizer is, for example, forcibly passing a slurry obtained by adding an abrasive such as fumed silica to a stirred alkaline aqueous solution to fine holes drilled on a hard surface while applying high pressure. In this method, the abrasive is crushed and dispersed using the impact of turbulence and the generation of ultrasonic waves.
【００１４】この研磨用懸濁液は、そのまま研磨に用い
てもよいが、水で希釈して用いてもよい。The polishing suspension may be used for polishing as it is, or may be used after being diluted with water.
【００１５】この研磨用懸濁液を用いて、シリコンウエ
ハーを研磨すると、アルカリがウエハーを化学的に研磨
し、一方、分散している非常に細かなヒュームドシリカ
等の研磨材を介してウレタンパッドがウエハーと擦れ合
って機械的に研磨する。その結果、ウエハー表面は短時
間で精密に研磨される。When a silicon wafer is polished using this polishing suspension, the alkali chemically polishes the wafer, while the urethane passes through a very fine abrasive such as fumed silica dispersed. The pads rub against the wafer and are polished mechanically. As a result, the wafer surface is precisely polished in a short time.
【００１６】研磨の際に、飛散して外壁に付着した研磨
用懸濁液の滴からは、水分が多少蒸発する。しかし、揮
発し難い保湿剤はこの滴中の水分子と水素結合するの
で、滴中の水が完全に蒸発してしまうことはない。その
ため、滴中の研磨材は、凝集することがなく、さらに外
壁の表面との間に保湿剤や水が保持されているので、こ
れらの表面にこびりつくことはない。At the time of polishing, water is slightly evaporated from the droplets of the polishing suspension which are scattered and adhere to the outer wall. However, since the humectant which is hardly volatilized forms a hydrogen bond with the water molecule in the droplet, the water in the droplet does not completely evaporate. Therefore, the abrasive in the droplets does not agglomerate, and since the humectant and water are held between the abrasive and the surface of the outer wall, the abrasive does not stick to these surfaces.
【００１７】研磨終了後直ちに、ウエハーに付いた研磨
用懸濁液とともに、外壁に付いた研磨用懸濁液の滴を水
で洗浄する。すると研磨用懸濁液中の研磨材は、水へ迅
速に溶解する保湿剤とともに、研磨材の液跡を残すこと
なく確実に洗い流される。そのため研磨後のシリコンウ
エハーは、凝集塊による傷や研磨用懸濁液の跡がついて
いない。Immediately after the polishing is completed, the polishing suspension droplets on the outer wall are washed with water together with the polishing suspension on the wafer. Then, the abrasive in the polishing suspension, together with the humectant that quickly dissolves in water, is reliably washed off without leaving any trace of the abrasive. Therefore, the silicon wafer after polishing has no scratches due to agglomerates and no trace of polishing suspension.
【００１８】この研磨用懸濁液を用いて研磨すると、半
導体集積回路用のシリコンウエハー、コンピュータのハ
ードディスク用の基板をはじめ種々の精密電子部品の表
面や、光学部品の表面を精密に仕上げ研磨することがで
きる。When polishing is performed using this polishing suspension, the surfaces of various precision electronic components such as a silicon wafer for a semiconductor integrated circuit and a substrate for a hard disk of a computer, and the surfaces of optical components are precisely finished and polished. be able to.
【００１９】この研磨用懸濁液は、ゲル化や沈降を誘発
することなく、長期間安定して保存することが可能であ
る。This polishing suspension can be stably stored for a long period of time without inducing gelation or sedimentation.
【００２０】[0020]
【実施例】以下、本発明の研磨用懸濁液の実施例を詳細
に説明する。実施例は本発明を適用する研磨用懸濁液を
試作した例であり、比較例は本発明を適用外の研磨用懸
濁液を試作した例である。Hereinafter, embodiments of the polishing suspension of the present invention will be described in detail. The example is an example in which a polishing suspension to which the present invention is applied is trial manufactured, and the comparative example is an example in which a polishing suspension to which the present invention is not applied is trially manufactured.
【００２１】（実施例）先ず、イオン交換水６５重量部
に４８％水酸化カリウム水溶液を加え、ｐＨ９．５〜１
０．０に調整する。この液をホモミキサーで攪拌しなが
ら、ヒュームドシリカＡＥＲＯＳＩＬ９０Ｇ（日本アエ
ロジル(株)社製の商品名）の１２．５重量部を加える。
このとき液のｐＨが低下し粘度が上昇するので、４８％
水酸化カリウム水溶液でｐＨを９．５近傍に調整する
と、粘度は再び低下する。(Example) First, an aqueous solution of 48% potassium hydroxide was added to 65 parts by weight of ion-exchanged water, and the pH was adjusted to 9.5 to 1%.
Adjust to 0.0. While stirring this solution with a homomixer, 12.5 parts by weight of fumed silica AEROSIL90G (trade name, manufactured by Nippon Aerosil Co., Ltd.) is added.
At this time, since the pH of the liquid decreases and the viscosity increases, 48%
When the pH is adjusted to around 9.5 with an aqueous solution of potassium hydroxide, the viscosity decreases again.
【００２２】この液を高圧ホモジナイザーにより９８Ｍ
Ｐａに加圧して微細な孔へ強制的に通過させると、ヒュ
ームドシリカの分散された粘度の一層低いスラリーが得
られる。さらに、ＡＥＲＯＳＩＬ９０Ｇの１２．５重量
部を加え、４８％水酸化カリウム水溶液で、ｐＨを１
０．５に調整する。このとき水酸化カリウム水溶液は合
計で約０．３５重量部加えられている。これにプロピレ
ングリコール１０重量部を加え、高圧ホモジナイザーで
同様にして再度分散を行うと、研磨用懸濁液が得られ
る。This solution was subjected to 98M by a high-pressure homogenizer.
Pressing to Pa and forcibly passing through fine pores results in a slurry of fumed silica dispersed with lower viscosity. Further, 12.5 parts by weight of AEROSIL90G was added, and the pH was adjusted to 1 with a 48% aqueous potassium hydroxide solution.
Adjust to 0.5. At this time, about 0.35 parts by weight of the potassium hydroxide aqueous solution was added in total. To this, 10 parts by weight of propylene glycol is added, and the mixture is dispersed again by a high-pressure homogenizer in the same manner to obtain a polishing suspension.
【００２３】（比較例）プロピレングリコールを用いて
いないこと以外は実施例と同様にして研磨用懸濁液を得
た。(Comparative Example) A polishing suspension was obtained in the same manner as in Example except that propylene glycol was not used.
【００２４】実施例および比較例の研磨用懸濁液を用
い、平面研磨機により夫々、シリコンウエハーを研磨
し、その評価を行った。Using the polishing suspensions of the examples and comparative examples, a silicon wafer was polished by a plane polishing machine, respectively, and its evaluation was performed.
【００２５】周囲を外壁で取り囲まれたターンテーブル
に、酸化膜厚１１０００Åで直径６インチのシリコンウ
エハーを載せ、テーブルとヘッドとを４０ｒｐｍで回転
させる。このウエハーに実施例または比較例の研磨用懸
濁液を１２０ｍＬ／分の流量でかけ、５００ｇ／ｃｍ２
の圧力でポリウレタン製のパッドであるＩＣ１０００／
ＳＵＢＡ４００ ０．８ｔ（ロデールニッタ社製の商品
名）によりウエハーを押し付けつつ、９０秒間研磨し
た。研磨後、ウエハーとターンテーブルと外壁とを直ち
に水で洗浄した。得られたウエハーについて評価した。A 6 inch diameter silicon wafer having an oxide film thickness of 11000 ° is placed on a turntable surrounded by an outer wall, and the table and the head are rotated at 40 rpm. The polishing suspension of the example or the comparative example was applied to the wafer at a flow rate of 120 mL / min, and the polishing suspension was 500 g / cm 2.
IC1000 / pad made of polyurethane at a pressure of
The wafer was polished for 90 seconds while pressing the wafer with SUBA400 0.8t (trade name, manufactured by Rodel Nitta). After polishing, the wafer, the turntable and the outer wall were immediately washed with water. The obtained wafer was evaluated.
【００２６】実施例の研磨用懸濁液を用いて研磨したウ
エハーは、５枚の平均の研磨速度が３１．９Å／秒であ
り、表面粗さ測定器（テーラーホブソン社製）で測定し
た最大高さＲｙが０．０３５μｍであり、スラリー安定
性測定器 タービスキャン（英弘精機社製の商品名）で
測定した変化量が０％と安定しており、目視によるスク
ラッチ観察においてもスクラッチがゼロであった。The wafers polished using the polishing suspensions of the examples had an average polishing rate of 51.9 ° / sec for the five wafers, and the maximum was measured by a surface roughness measuring instrument (manufactured by Taylor Hobson). The height Ry is 0.035 μm, the change amount measured with a slurry stability measuring instrument Turbiscan (trade name, manufactured by Eiko Seiki Co., Ltd.) is stable at 0%, and scratches are zero even in visual scratch observation. there were.
【００２７】実施例の研磨用懸濁液の飛散した滴が、少
なくとも約２時間放置されて乾燥した場合であっても、
水で洗浄すると滴跡を残さずに確実に洗い流すことがで
きた。この時間は、１枚のシリコンウエハーを長くとも
数分間で研磨の終了する毎に直ちに水で洗浄する通常の
研磨において十分である。Even if the scattered droplets of the polishing suspension of the example are left to dry for at least about 2 hours,
When washed with water, it could be washed off without leaving any droplets. This time is sufficient for ordinary polishing in which one silicon wafer is immediately washed with water every time polishing is completed within several minutes at most.
【００２８】実施例の研磨用懸濁液は少なくとも６箇月
間はゲル化や沈降を起こさずに長期間安定である。The polishing suspensions of the examples are stable for a long period without gelation or sedimentation for at least 6 months.
【００２９】一方、比較例の研磨用懸濁液を用いて研磨
したウエハーは、５枚の平均の研磨速度が３０．２Å／
秒であり、表面粗さ測定器で測定したＲｙが０．０３７
μｍであり、スラリー安定性測定器 タービスキャンで
の変化量が０％と安定しており、目視によるスクラッチ
観察においてもスクラッチがゼロであった。しかしこの
懸濁液の飛散した滴は、約２時間放置されて乾燥する
と、水で洗浄しても完全には洗い流すことができなかっ
た。On the other hand, five wafers polished using the polishing suspension of the comparative example had an average polishing rate of 30.2 ° /
And Ry measured by a surface roughness measuring device is 0.037.
μm, and the change in the slurry stability measuring instrument Turbiscan was stable at 0%, and the scratch was zero even by visual scratch observation. However, when the scattered droplets of the suspension were left to dry for about 2 hours, they could not be completely washed away with water.
【００３０】[0030]
【発明の効果】以上、詳細に説明したように、本発明の
研磨用懸濁液を用いると、シリコンウエハーをはじめと
する種々の精密電子部品の表面や光学部品の表面を精密
に研磨することができる。研磨後に水で洗浄すると、残
留物が残らず、研磨用懸濁液が確実に洗い流される。そ
のため研磨されたシリコンウエハー等に、ヒュームドシ
リカ等の凝集塊が付着したり傷がついたりすることはな
い。研磨されたシリコンウエハー等は、高品質であり、
その生産性も高い。この研磨用懸濁液は、ゲル化や沈降
を起こさないので長期間保存が可能である。As described in detail above, when the polishing suspension of the present invention is used, the surfaces of various precision electronic components such as silicon wafers and the surfaces of optical components can be precisely polished. Can be. Washing with water after polishing leaves no residue and ensures that the polishing suspension is washed away. Therefore, no aggregates such as fumed silica adhere to the polished silicon wafer or the like and are not damaged. Polished silicon wafers are of high quality,
Its productivity is also high. Since this polishing suspension does not cause gelation or sedimentation, it can be stored for a long period of time.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 福岡 重範 東京都千代田区神田淡路町１丁目２番３号 共栄社化学株式会社内 Ｆターム(参考） 3C058 AA07 AC04 CB01 DA17 ──────────────────────────────────────────────────続 き Continued on the front page (72) Inventor Shigenori Fukuoka 1-3-2 Kanda Awaji-cho, Chiyoda-ku, Tokyo F-term in Kyoeisha Chemical Co., Ltd. 3C058 AA07 AC04 CB01 DA17
Claims (3)
ナ、高純度酸化セリウムから選ばれる少なくとも一種類
の研磨材がアルカリ水溶液に分散し、エチレングリコー
ル、ポリエチレングリコール、グリセリン、プロピレン
グリコール、ポリグリセリン、グリセリンのエチレンオ
キサイド付加物、エチレン−プロピレンブロック共重合
物から選ばれる少なくとも一種類の保湿剤を含有してい
ることを特徴とする研磨用懸濁液。At least one abrasive selected from fumed silica, fumed alumina, and high-purity cerium oxide is dispersed in an aqueous alkaline solution, and ethylene glycol, polyethylene glycol, glycerin, propylene glycol, polyglycerin, and ethylene of glycerin are dispersed. A polishing suspension comprising at least one humectant selected from an oxide adduct and an ethylene-propylene block copolymer.
０．１〜１．０重量部であることを特徴とする請求項１
に記載の研磨用懸濁液。2. The polishing composition according to claim 1, wherein the humectant is used in an amount of 0.1 to 1.0 part by weight based on 1 part by weight of the abrasive.
3. The polishing suspension according to item 1.
溶液であることを特徴とする請求項１に記載の研磨用懸
濁液。3. The polishing suspension according to claim 1, wherein the aqueous alkaline solution is an aqueous potassium hydroxide solution.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001378040A JP2002329688A (en) | 2001-02-28 | 2001-12-12 | Polishing suspension containing moisture holding agent |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001053873 | 2001-02-28 | ||
| JP2001-53873 | 2001-02-28 | ||
| JP2001378040A JP2002329688A (en) | 2001-02-28 | 2001-12-12 | Polishing suspension containing moisture holding agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2002329688A true JP2002329688A (en) | 2002-11-15 |
Family
ID=26610273
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2001378040A Pending JP2002329688A (en) | 2001-02-28 | 2001-12-12 | Polishing suspension containing moisture holding agent |
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| Country | Link |
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| JP (1) | JP2002329688A (en) |
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| JPWO2005029563A1 (en) * | 2003-09-24 | 2007-11-15 | 日本化学工業株式会社 | Silicon wafer polishing composition and polishing method |
| CN103620747A (en) * | 2011-06-14 | 2014-03-05 | 福吉米株式会社 | Polishing composition |
| JP2014130958A (en) * | 2012-12-28 | 2014-07-10 | Kao Corp | Polishing liquid composition for silicon wafer |
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|---|---|---|---|---|
| JPWO2005029563A1 (en) * | 2003-09-24 | 2007-11-15 | 日本化学工業株式会社 | Silicon wafer polishing composition and polishing method |
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| JP2014130966A (en) * | 2012-12-28 | 2014-07-10 | Kao Corp | Polishing liquid composition for silicon wafer |
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