JP2008055591A - Machining speed improver, and water soluble polish/grind agent including machining speed improver - Google Patents
Machining speed improver, and water soluble polish/grind agent including machining speed improver Download PDFInfo
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本発明は、金属材料用加工油及び脆性材料用加工油、これらを含む加工油用組成物に関し、更に詳細には鋳鉄、合金鋼、銅、銅合金、アルミ、アルミ合金、超硬合金等の金属材料及びシリコンウェハ、セラミック、水晶、ガラス等の脆性材料の平面研削、円筒研削、内面研削、ホーニング、センタレス、スライシング、ラッピング、ポリッシング等において好適に使用される加工速度向上剤、及び該加工速度向上剤を含有した水溶性研磨・研削加工液に関するものである。 The present invention relates to a processing oil for metal materials and a processing oil for brittle materials, and a composition for processing oil containing these, and more specifically, cast iron, alloy steel, copper, copper alloy, aluminum, aluminum alloy, cemented carbide, etc. Processing speed improver suitably used in surface grinding, cylindrical grinding, internal grinding, honing, centerless, slicing, lapping, polishing, etc. of brittle materials such as metal materials and silicon wafers, ceramics, quartz, glass, and the like The present invention relates to a water-soluble polishing / grinding fluid containing an improver.
金属材料及び脆性材料の加工液として、防錆剤、界面活性剤、分散剤、油脂、脂肪酸、脂肪酸エステルの組成成分を被加工材、加工条件等に対応して適宜配合したものが広く使用されている（特許文献１）。
これら加工液の研磨加工速度を向上させるためには、より大きな粒子径の砥粒を使用する、若しくはスラリーの潤滑摩擦特性を低下させる必要がある。しかし、これらの方法では研磨速度の向上に伴い、研磨面の品質が劣化するといった問題点があった。
Widely used as processing fluids for metal materials and brittle materials are appropriately blended with rust preventives, surfactants, dispersants, fats and oils, fatty acids, fatty acid esters corresponding to the materials to be processed, processing conditions, etc. (Patent Document 1).
In order to improve the polishing speed of these working fluids, it is necessary to use abrasive grains having a larger particle diameter or to reduce the lubricating friction characteristics of the slurry. However, these methods have a problem that the quality of the polished surface deteriorates as the polishing rate increases.
そこで、添加剤により加工速度を向上させる試みがなされおり、加工速度向上効果が報告されている添加剤としては、ポリオール又はポリオールアルキレンオキサイド付加物の脂肪酸エステル等の非イオン界面活性剤（特許文献２）、ポリエーテル及びそのリン酸エステルカリウム塩（特許文献３）等がある。しかしながら、これらの添加物は多量添加しないと速度が向上しないという欠点があると共に、発泡を伴う場合があるという問題があった。 Therefore, attempts have been made to improve the processing speed with additives, and additives that have been reported to have an effect of improving the processing speed include nonionic surfactants such as polyols or fatty acid esters of polyol alkylene oxide adducts (Patent Document 2). ), Polyether and phosphate potassium salt thereof (Patent Document 3). However, these additives have a drawback that the speed is not improved unless a large amount is added, and there is a problem that foaming may occur.
一方、ポリアクリルアミド誘導体は、金属用研磨液の保護膜形成剤として用いられる事（特許文献４）、研磨・研削加工液の粘度低下を防止し加工精度あるいは工具の寿命等の低下を改善できる事（特許文献５）は知られていが、加工速度を向上させる効果を有しているとの報告は無い。
本発明は、かかる従来の技術の欠点を有しない、少量の添加濃度で研磨速度を向上させ、研磨・研削加工液が有する防錆剤、消泡剤、防腐剤、酸化防止剤、金属封鎖剤等の作用を阻害しない加工速度向上剤、更に沈降した砥粒の再分散性にも優れた加工速度向上剤、及び研磨速度が向上した、更に砥粒の再分散性に優れた、水溶性研磨・研削加工液を提供することを課題とする。 The present invention does not have the disadvantages of the prior art, improves the polishing rate with a small amount of addition, and has a rust inhibitor, antifoaming agent, preservative, antioxidant, and metal sequestering agent in the polishing / grinding fluid. A processing speed improver that does not impede the action of, etc., a processing speed improver that is also excellent in redispersibility of settled abrasive grains, and a water-soluble polishing that is improved in polishing speed and excellent in redispersibility of abrasive grains・ Provide grinding fluid.
本発明者らは、かかる課題を解決するため、鋭意研究の結果、ポリアクリルアミド誘導体を用いることにより、更にカチオン性水溶性高分子を添加することにより、課題が解決できることを見いだし、本発明を完成した。
すなわち発明は、
（１）ポリアクリルアミド誘導体を有効成分とする加工速度向上剤、
（２）ポリアクリルアミド誘導体が、Ｎ，Ｎ−ジメチルアクリルアミドの単独重合物、又はＮ，Ｎ−ジメチルアクリルアミドとイオン性モノマーとの共重合物である上記（１）記載の加工速度向上剤、
（３）さらに、カチオン性水溶性高分子を含む上記（１）乃至（２）のいずれか一に記載の加工速度向上剤、
（４）カチオン性水溶性高分子が、ポリエチレンイミン等のポリアルキレンイミン、ポリN,N-ジメチルアミノエチルアクリレートメチルクロライド、ポリN,N-ジメチルアミノプロピルアクリルアミドメチルクロライド等の四級化アクリルアミド誘導体、ヒドロキシエチルセルロース／ジメチルジアリルアンモニウムクロライド共重合体、ポリアリルアミン及びその共重合体、ポリアリルアミン塩酸塩及びその共重合体、ポリジアリルジメチルアンモニウムクロライド及びその共重合体、ヒドロキシエチルセルロース／ヒドロキシプロピルトリメチルアンモニウムクロリド等のカチオン化セルロース、ビニルピロリドン／ジメチルアミノエチルアクリル酸共重合体のカチオン化物等の四級化ポリビニルピロリドン誘導体であり、望ましくはポリエチレンイミン、N,N-ジメチルアミノエチルアクリレートメチルクロライド、N,N-ジメチルアミノプロピルアクリルアミドメチルクロライド等の四級化アクリルアミド誘導体、さらに望ましくはポリエチレンイミンである上記（３）記載の加工速度向上剤、
（５）上記（１）乃至（４）のいずれか一に記載の加工速度向上剤を含有した水溶性研磨・研削加工液、
を提供するものである。
As a result of intensive research, the present inventors have found that the problem can be solved by using a polyacrylamide derivative and further adding a cationic water-soluble polymer to complete the present invention. did.
That is, the invention
(1) A processing speed improver comprising a polyacrylamide derivative as an active ingredient,
(2) The processing speed improver according to (1), wherein the polyacrylamide derivative is a homopolymer of N, N-dimethylacrylamide, or a copolymer of N, N-dimethylacrylamide and an ionic monomer,
(3) The processing speed improver according to any one of (1) to (2), further comprising a cationic water-soluble polymer,
(4) The cationic water-soluble polymer is a quaternized acrylamide derivative such as polyalkyleneimine such as polyethyleneimine, poly N, N-dimethylaminoethyl acrylate methyl chloride, poly N, N-dimethylaminopropyl acrylamide methyl chloride, Hydroxyethylcellulose / dimethyldiallylammonium chloride copolymer, polyallylamine and its copolymer, polyallylamine hydrochloride and its copolymer, polydiallyldimethylammonium chloride and its copolymer, hydroxyethylcellulose / hydroxypropyltrimethylammonium chloride, etc. Quaternized polyvinylpyrrolidone derivatives such as cationized cellulose and cationized vinylpyrrolidone / dimethylaminoethylacrylic acid copolymer, preferably polyester Ren'imin, N, N-dimethylaminoethyl acrylate methyl chloride, N, N-dimethylaminopropyl quaternized acrylamide derivatives such as acrylamide methyl chloride, more preferably a polyethyleneimine above (3), wherein the processing speed enhancers,
(5) A water-soluble polishing / grinding fluid containing the processing speed improver according to any one of (1) to (4) above,
Is to provide.
本発明によると、水溶性の研磨・研削加工液及び加工スラリーの各成分の作用を阻害することなく、少量の添加量で、研磨加工速度を向上させることができるという作用効果を奏する。
更に、カチオン性水溶性高分子を添加したものは、沈降した砥粒の再分散性が良好であると共に、研磨速度が相乗的に向上する、特にスラリー供給量が低い場合においても研磨速度向上の相乗効果が見られ、経済的、生産性に優れる、という作用効果を奏する。
According to the present invention, there is an effect that the polishing processing speed can be improved with a small amount of addition without inhibiting the action of each component of the water-soluble polishing / grinding fluid and the processing slurry.
Furthermore, the addition of the cationic water-soluble polymer has good redispersibility of the precipitated abrasive grains and improves the polishing rate synergistically, especially when the slurry supply amount is low. Synergistic effect is seen, and there is an effect of being economical and excellent in productivity.
本発明は、ポリアクリルアミド誘導体を有効成分とする加工速度向上剤である。
なお、本発明のいう「加工速度向上」とは、シリコンウェハ、セラミック、金属、ガラス等の研磨・研削加工における加工速度の向上させることをいう。
The present invention is a processing speed improver comprising a polyacrylamide derivative as an active ingredient.
In the present invention, “improving the processing speed” means improving the processing speed in polishing / grinding of silicon wafers, ceramics, metals, glass, and the like.
本発明に用いられるポリアクリルアミド誘導体としては、（メタ）アクリルアミド、Ｎ−メチル（メタ）アクリルアミド、Ｎ，Ｎ−ジメチル（メタ）アクリルアミド、Ｎ−アクリロイルモルホリンのアクリルアミド誘導体の単独重合体、あるいはこれらアクリルアミド誘導体とイオン性モノマー（例えば（メタ）アクリル酸又はそのアルカリ金属塩、アンモニウム塩、等）との共重合物が挙げられる。
中でも、Ｎ，Ｎ−ジ置換アクリルアミドの単独重合体、あるいはそれとアクリル酸（塩）との共重合体が好ましく、特に、Ｎ，Ｎ−ジメチルアクリルアミドの単独重合体あるいはそれとアクリル酸（塩）との共重合体が好ましい。
The polyacrylamide derivatives used in the present invention include (meth) acrylamide, N-methyl (meth) acrylamide, N, N-dimethyl (meth) acrylamide, homopolymers of acrylamide derivatives of N-acryloylmorpholine, or these acrylamide derivatives. And a copolymer of ionic monomer (for example, (meth) acrylic acid or its alkali metal salt, ammonium salt, etc.).
Among them, a homopolymer of N, N-disubstituted acrylamide or a copolymer thereof with acrylic acid (salt) is preferable, and in particular, a homopolymer of N, N-dimethylacrylamide or it and acrylic acid (salt). A copolymer is preferred.
ポリアクリルアミド誘導体は、上述したアクリルアミド誘導体、あるいはアクリル酸（塩）とを、公知の方法に準じて（共）重合する事により製造することができる。
重合方法は任意であるが、水溶性の研磨・研削加工液に添加する目的においては、水系での重合が好ましい。
The polyacrylamide derivative can be produced by (co) polymerizing the above-described acrylamide derivative or acrylic acid (salt) according to a known method.
The polymerization method is arbitrary, but for the purpose of adding to a water-soluble polishing / grinding liquid, polymerization in an aqueous system is preferable.
本発明において、加工速度向上剤として、カチオン性水溶性高分子を併用することができる。
カチオン性水溶性高分子を併用することにより、沈降した砥粒の再分散性が良好となるばかりでなく、研磨速度が、特に加工時のスラリーの供給が低流量時に、相乗的に向上する。
用いられるカチオン性水溶性高分子としては、ポリエチレンイミン、ポリアリルアミン、ポリビニルアミンが挙げられる。中でも、ポリエチレンイミンが好ましく、原液や加工液（希釈後の使用状態）への溶解性から３００〜１０００００の分子量のものが好ましい。
In the present invention, a cationic water-soluble polymer can be used in combination as a processing speed improver.
By using the cationic water-soluble polymer in combination, not only the redispersibility of the precipitated abrasive grains is improved, but also the polishing rate is improved synergistically, particularly when the slurry is supplied at a low flow rate during processing.
Examples of the cationic water-soluble polymer used include polyethyleneimine, polyallylamine, and polyvinylamine. Among these, polyethyleneimine is preferable, and one having a molecular weight of 300 to 100,000 is preferable from the viewpoint of solubility in a stock solution and a processing solution (use state after dilution).
本発明の加工速度向上剤は、水溶性研磨・研削加工液に添加して用いられ、ポリアクリルアミド誘導体の添加量は、加工液１００重量部に対して、０．００００１〜０．１重量部、好ましくは０．０００１〜０．１重量部、更に好ましくは０．０００５〜０．０５重量部である。添加が０．００００１重量部未満であると研磨速度の向上がみられず、一方０．１重量部を超えると研磨面の品質が劣化する場合がある。
また、カチオン性水溶性高分子を併用する場合のカチオン性水溶性高分子の添加量は、加工液１００重量部に対して、０．０００１〜０．１重量部、好ましくは０．００１〜０．１重量部、更に好ましくは０．００４〜０．０２重量部が添加される。添加量が０．０００１重量部未満であると加工速度の相乗的な向上はなく、さらに沈降した砥粒の再分散性の向上が見られない。一方０．１重量部を超えても研磨速度、再分散性の効果のさらなる向上は見られない。
The processing speed improver of the present invention is used by being added to a water-soluble polishing / grinding processing liquid, and the addition amount of the polyacrylamide derivative is 0.00001 to 0.1 parts by weight with respect to 100 parts by weight of the processing liquid, Preferably it is 0.0001-0.1 weight part, More preferably, it is 0.0005-0.05 weight part. If the addition is less than 0.00001 part by weight, the polishing rate is not improved, whereas if it exceeds 0.1 part by weight, the quality of the polished surface may be deteriorated.
In addition, when the cationic water-soluble polymer is used in combination, the addition amount of the cationic water-soluble polymer is 0.0001 to 0.1 parts by weight, preferably 0.001 to 0 parts per 100 parts by weight of the processing liquid. 0.1 part by weight, more preferably 0.004 to 0.02 part by weight is added. When the addition amount is less than 0.0001 part by weight, there is no synergistic improvement in the processing speed, and further no improvement in the redispersibility of the precipitated abrasive grains. On the other hand, even if it exceeds 0.1 parts by weight, no further improvement in the polishing rate and redispersibility effect is observed.
本発明では、更に、該加工速度向上剤を含有した水溶性研磨・研削加工液が提供される。
加工液としては、水溶性のもので、防錆剤、酸化防止剤、防腐剤、金属イオン封鎖剤、界面活性剤、油脂、脂肪酸、脂肪酸エステルの組成成分を、被加工材、加工条件等に対応して適宜配合した公知のものが用いられ、研磨速度向上剤の含有量は、上述した添加量の範囲が好ましい。
なお、加工速度向上剤の添加は粉末、溶液状（希釈状態を含む）のいずれでも良く、研磨・研削加工液に添加されるか、その原液に添加してもよく、また加工スラリー（砥粒添加後）に添加することもできる。
The present invention further provides a water-soluble polishing / grinding fluid containing the processing speed improver.
The processing fluid is water-soluble, and the rust inhibitor, antioxidant, preservative, sequestering agent, surfactant, oil, fat, fatty acid, fatty acid ester are used as the processing material, processing conditions, etc. The well-known thing mix | blended suitably correspondingly is used, and the range of the addition amount mentioned above is preferable for content of a polishing rate improvement agent.
The processing speed improver may be added in either powder or solution form (including diluted state), added to the polishing / grinding processing liquid, or added to the stock solution, and processed slurry (abrasive grains). It can also be added after).
水溶性高分子である、ポリアクリル酸及びその塩、ポリアクリルアミド等は水中で親水性ゾル体を形成することはよく知られているところである。本発明者らは、その水中でのゾル体の有する諸特性が研磨加工液の加工速度向上に有用であるところに着目し試験を重ねたところ、ポリアクリルアミド誘導体が研磨・研削加工液の加工速度を向上させるという新たな作用を見出し、さらに、カチオン性水溶性高分子を併用添加することで、加工速度が相乗的に向上すると共に、沈殿した砥粒の再分散が容易に行えるという知見を得、本発明を完成させたものである。 It is well known that water-soluble polymers such as polyacrylic acid and salts thereof, polyacrylamide and the like form a hydrophilic sol in water. The inventors of the present invention have repeatedly conducted tests focusing on the fact that various properties of the sol body in water are useful for improving the processing speed of the polishing liquid, and found that the polyacrylamide derivative has a processing speed of the polishing / grinding liquid. In addition, the addition of a cationic water-soluble polymer combined with the addition of a cationic water-soluble polymer synergistically improves the processing speed, and the knowledge that the precipitated abrasive grains can be easily redispersed. The present invention has been completed.
以下実施例により本発明を詳細に説明するが、本発明はこれに限定されるものではない。
製造例１ ポリＮ，Ｎ−ジメチルアクリルアミドの合成
１Ｌ容量のセパラブルフラスコに、Ｎ，Ｎ−ジメチルアクリルアミド１２０ｇ、脱イオン水６００ｇを加えて、攪拌しながら５重量％の硫酸水溶液を徐々に添加し、溶液のｐＨを７．３０に合わせ、中和操作を行った後、モノマー水溶液の濃度が１５重量％になるように、脱イオン水を補填した。その後、モノマー調製液を、２０℃の恒温槽に入れ、マグネチックスターラーで攪拌しながら窒素ガスを、１時間通気、恒温した。本溶液に、重合開始剤として２，２'−アゾビス［２−（２−イミダゾリン−２−イル）プロパン］ジハイドロクロライド（ＶＡ−０４４）の５重量％水溶液を２．１６ｇ、ナトリウムホルムアルデヒドスルホキシート２水和物（ロンガリット）の１０重量％水溶液を２．２０ｇ、ｔｅｒｔ−ブチルヒドロペルオキシド（ｔ−ＢＨＰＯ）の５重量％水溶液を２．５７ｇ順次投入し、重合反応を開始させた。５分後、攪拌並びに窒素ガスの通気を止め、密閉状態で室温下１６時間重合反応を続けた後、８５重量％の水を含む水あめ状のポリＮ，Ｎ−アクリルアミドを得た。
得られた水あめ状のポリＮ，Ｎ−アクリルアミドを裁断し、脱イオン水に溶解させ、本発明の加工速度向上剤を２重量％の水溶液として調製した。
Hereinafter, the present invention will be described in detail by way of examples, but the present invention is not limited thereto.
Production Example 1 Synthesis of Poly N, N-dimethylacrylamide To a 1 L separable flask, add 120 g of N, N-dimethylacrylamide and 600 g of deionized water, and gradually add 5% by weight sulfuric acid aqueous solution with stirring. After adjusting the pH of the solution to 7.30 and performing a neutralization operation, deionized water was supplemented so that the concentration of the aqueous monomer solution was 15% by weight. Thereafter, the monomer preparation solution was placed in a constant temperature bath at 20 ° C., and nitrogen gas was aerated for 1 hour while stirring with a magnetic stirrer. To this solution was added 2.16 g of a 5 wt% aqueous solution of 2,2′-azobis [2- (2-imidazolin-2-yl) propane] dihydrochloride (VA-044) as a polymerization initiator, 2.20 g of a 10 wt% aqueous solution of sheet dihydrate (Longalite) and 2.57 g of a 5 wt% aqueous solution of tert-butyl hydroperoxide (t-BHPO) were sequentially added to initiate the polymerization reaction. After 5 minutes, stirring and aeration of nitrogen gas were stopped, and the polymerization reaction was continued for 16 hours at room temperature in a sealed state. After that, water-like poly N, N-acrylamide containing 85% by weight of water was obtained.
The resulting candy-like poly N, N-acrylamide was cut and dissolved in deionized water to prepare the processing speed improver of the present invention as a 2% by weight aqueous solution.
実施例１
加工液（Ａ）として、水媒体１００重量部に、ジエタノールアミン０．４重量部、セバチン酸 ０．１５重量部、サーフィノール４８５（信越化学工業株式会社製）０．０５重量部、ＴＳＡ７３０（ＧＥ東芝シリコーン株式会社製）０．００２重量部を溶解したものを用いた。
加工液（Ａ）に、製造例１で得られたポリＮ，Ｎ−ジメチルアクリルアミドを０．００１重量部（純分換算）添加し、本発明の水溶性研磨・研削加工液を得た。
Example 1
As a working fluid (A), 100 parts by weight of an aqueous medium, 0.4 parts by weight of diethanolamine, 0.15 parts by weight of sebacic acid, 0.05 parts by weight of Surfinol 485 (Shin-Etsu Chemical Co., Ltd.), TSA730 (GE Toshiba) What dissolved 0.002 weight part (made by Silicone Co., Ltd.) was used.
To the working fluid (A), 0.001 part by weight (in terms of pure content) of the poly N, N-dimethylacrylamide obtained in Production Example 1 was added to obtain the water-soluble polishing / grinding fluid of the present invention.
実施例２
実施例１において、ポリＮ，Ｎ−ジメチルアクリルアミドの添加量を０．００５重量部（純分換算）とした以外は実施例１と同様に実施し、本発明の水溶性研磨・研削加工液を得た。
Example 2
The same procedure as in Example 1 was performed except that the amount of poly N, N-dimethylacrylamide added was 0.005 parts by weight (in terms of pure content) in Example 1, and the water-soluble polishing / grinding fluid of the present invention was used. Obtained.
実施例３
実施例１において、ポリＮ，Ｎ−ジメチルアクリルアミドの添加量を０．０１５重量部（純分換算）とした以外は実施例１と同様に実施し、本発明の水溶性研磨・研削加工液を得た。
Example 3
The same procedure as in Example 1 was performed except that the amount of poly N, N-dimethylacrylamide added was 0.015 parts by weight (in terms of pure content) in Example 1, and the water-soluble polishing / grinding fluid of the present invention was used. Obtained.
実施例４
実施例１において、ポリＮ，Ｎ−ジメチルアクリルアミドにかえてポリエチレンイミン（和光純薬製、平均分子量１８００）を用い、添加量を０．０１重量部（純分換算）とした以外は実施例１と同様に実施し、本発明の水溶性研磨・研削加工液を得た。
Example 4
In Example 1, polyethyleneimine (manufactured by Wako Pure Chemical Industries, average molecular weight 1800) was used instead of poly N, N-dimethylacrylamide, and the amount added was 0.01 parts by weight (pure component conversion). The water-soluble polishing / grinding fluid of the present invention was obtained.
実施例５
実施例２において、更にポリエチレンイミン（和光純薬製、平均分子量１８００）を０．０１重量部（純分換算）添加した以外は実施例２と同様に実施し、本発明の水溶性研磨・研削加工液を得た。
Example 5
In Example 2, the same procedure as in Example 2 was performed except that 0.01 part by weight (in terms of pure component) of polyethyleneimine (manufactured by Wako Pure Chemical Industries, average molecular weight 1800) was added. A working fluid was obtained.
評価例１ 研磨速度評価（シリコンウェハーのラッピング加工）
実施例１〜３及び加工液（Ａ）を用い、それぞれの加工液７２重量部に対し酸化アルミナ砥粒２８重量部（ＦＯ＃１２００、株式会社フジミインコーポレーテッド製）を混合し加工スラリー液とした。
この加工スラリー液を使用して、不二越機械工業社製ＵＳＰ−９Ｂを用い、表１に示した装置条件下、加工スラリー供給量２００ｍｌ／ｍｉｎ、４ｉｎｃｈシリコンウェハ、研磨枚数５枚を研磨した。
研磨速度は、研磨後のシリコンウェハの研磨除去量（シリコンウェハの厚みの減少量）を加工時間で除したものであり、結果を表２に示した。
Evaluation Example 1 Polishing speed evaluation (silicon wafer lapping)
Using Examples 1 to 3 and the processing liquid (A), 28 parts by weight of alumina oxide abrasive grains (FO # 1200, manufactured by Fujimi Incorporated) was mixed with 72 parts by weight of each processing liquid to obtain a processing slurry liquid. .
Using this processing slurry liquid, USP-9B manufactured by Fujikoshi Machine Industry Co., Ltd. was used to polish a processing slurry supply amount of 200 ml / min, a 4-inch silicon wafer, and 5 polishing sheets under the apparatus conditions shown in Table 1.
The polishing rate was obtained by dividing the polishing removal amount of the silicon wafer after polishing (the reduction amount of the thickness of the silicon wafer) by the processing time, and the results are shown in Table 2.
評価例２ 研磨速度評価（シリコンウェハーのラッピング加工）
実施例２、４、５及び加工液（Ａ）を用い、それぞれの加工液７２重量部に対し酸化アルミナ砥粒２８重量部（ＦＯ＃１２００、株式会社フジミインコーポレーテッド製）を混合し加工スラリー液とした。
この加工スラリー液を使用して、評価例１において、加工スラリー供給量を５０ｍｌ／ｍｉｎにかえた以外は評価例１と同様に実施した。
研磨速度は、研磨後のシリコンウェハの研磨除去量（シリコンウェハの厚みの減少量）を加工時間で除したものであり、結果を表３に示した。
Evaluation Example 2 Polishing rate evaluation (silicon wafer lapping)
Using Examples 2, 4, and 5 and the processing liquid (A), 28 parts by weight of alumina oxide abrasive grains (FO # 1200, manufactured by Fujimi Incorporated) are mixed with 72 parts by weight of each processing liquid, and a processing slurry liquid is used. It was.
Using this processing slurry liquid, the same processing as in Evaluation Example 1 was performed except that the processing slurry supply amount was changed to 50 ml / min in Evaluation Example 1.
The polishing rate was obtained by dividing the polishing removal amount of the silicon wafer after polishing (the reduction amount of the thickness of the silicon wafer) by the processing time, and the results are shown in Table 3.
評価例３ 砥粒再分散性評価
評価例２で調整した加工スラリー液を、良く攪拌し均一な状態にした後、外形３５ｍｍ×高さ７８ｍｍのガラス製透明サンプル瓶に５０ｇ入れ、７日間静置し、砥粒を完全に沈降させた後、ミキサーにて５分間振とうして砥粒が再分散するかどうか観察した。
砥粒の再分散の状態を目視したところ、実施例２及び加工液（Ａ）を用いた加工スラリー液では砥粒塊が少量残った（５％未満程度）が、実施例４及び実施例５を用いた加工スラリー液では砥粒塊は認められなかった。
Evaluation Example 3 Abrasive Grain Redispersibility Evaluation After the processing slurry liquid prepared in Evaluation Example 2 was stirred well and made uniform, 50 g was put into a glass transparent sample bottle having an outer shape of 35 mm × height of 78 mm and left for 7 days. Then, after the abrasive grains were completely settled, the mixture was shaken with a mixer for 5 minutes to observe whether the abrasive grains were redispersed.
When the state of re-dispersion of the abrasive grains was visually observed, a small amount of abrasive grain lump remained in the processing slurry liquid using Example 2 and the processing liquid (A) (less than about 5%), but Example 4 and Example 5 No abrasive lump was observed in the processing slurry liquid using No. 1.
以上の結果から、加工スラリー供給量にかかわらずポリＮ，Ｎ−ジメチルアクリルアミドを添加した場合に研磨速度が向上すること、ポリＮ，Ｎ−ジメチルアクリルアミドとポリエチレンイミンを併用することで研磨速度の相乗的な向上が見られること、また、沈降した砥粒の再分散効果が優れていること、が確認された。 From the above results, the polishing rate is improved when poly N, N-dimethylacrylamide is added regardless of the amount of processing slurry supplied, and the synergy of polishing rate is achieved by using poly N, N-dimethylacrylamide and polyethyleneimine together. It has been confirmed that there is a general improvement and that the redispersion effect of the settled abrasive grains is excellent.
評価例３ 研削速度評価（硬質ガラス棒の円筒研削加工）
実施例２及び加工液(A)を用い、砥石として#170ダイヤモンド砥石（メタルボンド）を使用し、回転速度２４００ｒｐｍ、圧力３５N下に於いて、硬質ガラス棒φ10mmの円筒研削加工を行った場合の加工速度を測定した。加工速度は、加工後の硬質ガラス棒直径減少量を加工時間で除したものであり、結果を表４に示した。
Evaluation Example 3 Grinding speed evaluation (cylindrical grinding of hard glass rod)
Example 2 and machining fluid (A) were used, and a # 170 diamond grindstone (metal bond) was used as a grindstone, and cylindrical grinding of a hard glass rod φ10 mm was performed at a rotational speed of 2400 rpm and a pressure of 35 N. The processing speed was measured. The processing speed was obtained by dividing the amount of hard glass rod diameter reduction after processing by the processing time, and the results are shown in Table 4.
全ての条件下で被加工材の割れ・カケの発生は見られなかった。図１より、加工加重一定条件下に於いて、ポリＮ，Ｎ−ジメチルアクリルアミドを添加した場合に加工速度が向上することが分かる。さらに、加工圧力、粒度を上げることなく、加工速度を向上することが可能であることから、被加工部材の割れ、カケを抑制することができる。 There was no cracking or chipping of the workpiece under all conditions. FIG. 1 shows that the processing speed is improved when poly N, N-dimethylacrylamide is added under a constant processing load. Furthermore, since it is possible to improve the processing speed without increasing the processing pressure and particle size, it is possible to suppress cracking and chipping of the workpiece.
以上述べてきたように、本発明によると、研磨速度が向上する、更に沈降した砥粒の再分散効果に優れる研磨速度向上剤、及び該研磨速度向上剤を含有した水溶性研磨・研削加工液が提供され、シリコンウェハ、セラミック、金属、ガラス等の研磨・研削加工において好適に用いることができる。 As described above, according to the present invention, the polishing rate is improved, the polishing rate improver excellent in the redispersion effect of the settled abrasive grains, and the water-soluble polishing / grinding fluid containing the polishing rate improver Can be suitably used in polishing and grinding of silicon wafers, ceramics, metals, glasses, and the like.
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| JP2011077115A (en) * | 2009-09-29 | 2011-04-14 | Jsr Corp | Aqueous dispersion for chemical mechanical polishing and chemical mechanical polishing method |
| WO2015068672A1 (en) * | 2013-11-08 | 2015-05-14 | 東亞合成株式会社 | Wetting agent and polishing composition for semiconductor |
| JP2015189806A (en) * | 2014-03-27 | 2015-11-02 | 株式会社フジミインコーポレーテッド | Composition for polishing, usage of the same and substrate production method |
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| JP2000323444A (en) * | 1999-05-10 | 2000-11-24 | Kao Corp | Polishing solution composition |
| JP2002164308A (en) * | 2000-11-24 | 2002-06-07 | Nec Corp | Slurry for chemical-mechanical polishing |
| WO2004107429A1 (en) * | 2003-05-28 | 2004-12-09 | Hitachi Chemical Co., Ltd. | Abrasive and method of polishing |
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| JP2000323444A (en) * | 1999-05-10 | 2000-11-24 | Kao Corp | Polishing solution composition |
| JP2002164308A (en) * | 2000-11-24 | 2002-06-07 | Nec Corp | Slurry for chemical-mechanical polishing |
| WO2004107429A1 (en) * | 2003-05-28 | 2004-12-09 | Hitachi Chemical Co., Ltd. | Abrasive and method of polishing |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2011077115A (en) * | 2009-09-29 | 2011-04-14 | Jsr Corp | Aqueous dispersion for chemical mechanical polishing and chemical mechanical polishing method |
| WO2015068672A1 (en) * | 2013-11-08 | 2015-05-14 | 東亞合成株式会社 | Wetting agent and polishing composition for semiconductor |
| JP2015189806A (en) * | 2014-03-27 | 2015-11-02 | 株式会社フジミインコーポレーテッド | Composition for polishing, usage of the same and substrate production method |
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