JP5429397B2 - Lubricating composition for polishing glass substrate and polishing slurry - Google Patents

Lubricating composition for polishing glass substrate and polishing slurry Download PDF

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JP5429397B2
JP5429397B2 JP2012539790A JP2012539790A JP5429397B2 JP 5429397 B2 JP5429397 B2 JP 5429397B2 JP 2012539790 A JP2012539790 A JP 2012539790A JP 2012539790 A JP2012539790 A JP 2012539790A JP 5429397 B2 JP5429397 B2 JP 5429397B2
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polishing
acid
glass substrate
lubricating composition
weight
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JPWO2012053660A1 (en
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秀和 稲垣
有志 南
研太郎 浜島
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Moresco Corp
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1409Abrasive particles per se
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1454Abrasive powders, suspensions and pastes for polishing
    • C09K3/1463Aqueous liquid suspensions

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Manufacturing Of Magnetic Record Carriers (AREA)

Description

本発明は、ガラス基板研磨用潤滑組成物(以下、研磨用潤滑組成物)及びそれを用いた研磨スラリーに関する。更に詳しくは、ガラス基板の研磨加工において、加工レートの向上及び仕上げ面粗さの改善に優れた研磨用潤滑組成物並びに研磨スラリーに関する。   The present invention relates to a lubricating composition for polishing a glass substrate (hereinafter, a lubricating composition for polishing) and a polishing slurry using the same. More specifically, the present invention relates to a polishing lubricating composition and polishing slurry excellent in improving a processing rate and finishing surface roughness in polishing a glass substrate.

近年、電子機器、光学機器、エネルギーデバイスなどの開発が積極的に行われている。それらを開発する上で重要な素材の一つにガラスがある。例えば、電子材料では、ハードディスクドライブのハードディスクガラス基板、液晶ディスプレーや有機ELディスプレーのフラットパネルガラス、光学機器では、光転写装置のフォトマスク用ガラス、カメラのレンズ、LED照明のガラス、エネルギーデバイスでは太陽光発電用ガラスパネルなどがある。このように最先端の様々な機器にガラス基板が用いられている。
これらガラス基板は種々の工程を経て作り上げられている、製造工程で重要なのが研磨工程である。目的の形状、精度に仕上げるためにはガラス表面を精密に研磨する必要がある。精密に研磨されたガラス基板によって最先端の技術が支えられている。
具体的な例としては、昨今、ハードディスクドライブの記録密度を向上させるために、磁気ヘッドと磁気ディスクの間隙より狭くする必要がある。ハードディスクドライブの記録密度の向上を達成するために、ハードディスクガラス基板の加工において、研磨速度の向上、仕上げ面粗さの改善及び表面残渣の低減が課題となっている。更には、フラットパネルガラス、フォトマスクガラスや光学レンズなども、光透過性など様々な要求に合わせて表面は研磨されている。
一般にガラスの主成分はケイ酸(SiO)であるが、求められる品質によって種々の元素を加えて目的の機能となるように調整されている。具体的にはホウ酸、アルミナ、酸化ナトリウム、酸化カリウム、酸化カルシウム、酸化マグネシウム等が添加されている。
この高記録密度化の流れは年々加速しており、ディスク基板加工用研磨スラリーへの要求は、より複雑化し高性能なものとなっている。その要求項目は研磨速度に始まり、低面粗度化、微小ピット、微小突起、微小スクラッチ等の表面欠陥が無いことなど、多岐にわたっている。
上記研磨用潤滑組成物としては、研磨速度を向上させ、しかも、高品質の表面を得るための研磨用組成物が、種々提案されている。
「研磨痕」や「研磨スクラッチ」の除去、及び仕上げ面粗さをより小さく仕上げる研磨用潤滑組成物として、例えば特許文献1には、炭素数10〜22の脂肪酸と各種アルコールからなる研磨用潤滑組成物が提案されている。しかし特許文献1で用いられる炭素数10〜22の脂肪酸は飽和、不飽和の脂肪酸であり、水酸基を含有する脂肪酸は全く記載されていない。更に上述の高能率で且つ高い研磨速度を与える組成物として、例えば特許文献2にはフェニル基を含有しないリン系界面活性剤、グリコール系溶剤、炭素数16〜40のカルボン酸、又は、ジカルボン酸、及び、アルカノールアミンからなる研磨用潤滑組成物が提案されている。
しかし、従来技術を用いた研磨液組成物では十分な研磨速度が得られない他、高記録密度化に適合する、仕上げ面粗さの低い高品質なハードディスクガラス基板を得ることが出来ない。
In recent years, electronic devices, optical devices, energy devices and the like have been actively developed. One of the important materials for developing them is glass. For example, in the case of electronic materials, a hard disk glass substrate of a hard disk drive, a flat panel glass of a liquid crystal display or an organic EL display, in an optical device, a glass for a photomask of a light transfer device, a camera lens, a glass of LED lighting, or a solar in an energy device There are glass panels for photovoltaic power generation. Thus, glass substrates are used in various state-of-the-art devices.
These glass substrates are manufactured through various processes, and an important process in the manufacturing process is a polishing process. In order to finish the target shape and accuracy, it is necessary to polish the glass surface precisely. State-of-the-art technology is supported by a precisely polished glass substrate.
As a specific example, in recent years, in order to improve the recording density of a hard disk drive, it is necessary to make it narrower than the gap between the magnetic head and the magnetic disk. In order to achieve an improvement in the recording density of the hard disk drive, in the processing of the hard disk glass substrate, improvement of the polishing rate, improvement of the finished surface roughness and reduction of the surface residue are problems. Furthermore, the surfaces of flat panel glass, photomask glass, optical lenses, and the like are polished to meet various requirements such as light transmittance.
In general, the main component of glass is silicic acid (SiO 2 ), but it is adjusted so as to have a desired function by adding various elements depending on the required quality. Specifically, boric acid, alumina, sodium oxide, potassium oxide, calcium oxide, magnesium oxide and the like are added.
This trend toward higher recording density has been accelerating year by year, and the demand for polishing slurry for disk substrate processing has become more complex and higher performance. The required items start from the polishing rate and range from low surface roughness, absence of surface defects such as fine pits, fine protrusions, and fine scratches.
As the above-mentioned polishing composition, various polishing compositions for improving the polishing rate and obtaining a high quality surface have been proposed.
As a lubricating composition for polishing which removes “polishing marks” and “polishing scratches” and finishes the finished surface with a smaller roughness, for example, Patent Document 1 discloses a polishing lubricant comprising a fatty acid having 10 to 22 carbon atoms and various alcohols. Compositions have been proposed. However, the C10-22 fatty acid used in Patent Document 1 is a saturated or unsaturated fatty acid, and no fatty acid containing a hydroxyl group is described. Furthermore, as a composition which gives the above-mentioned high efficiency and a high polishing rate, for example, Patent Document 2 discloses a phosphorus surfactant not containing a phenyl group, a glycol solvent, a carboxylic acid having 16 to 40 carbon atoms, or a dicarboxylic acid. And a polishing lubricating composition comprising alkanolamine has been proposed.
However, a polishing composition using a conventional technique cannot provide a sufficient polishing rate, and cannot obtain a high-quality hard disk glass substrate with low finished surface roughness that is suitable for high recording density.

特表2004−515609号公報JP-T-2004-515609 特開2004−306248号公報JP 2004-306248 A

本発明の課題は、ガラス基板の加工において、特に研磨速度の向上、仕上げ面粗さの改善に有効で、更には表面残渣を低減できる研磨スラリー並びに該研磨スラリーを調製するための研磨用潤滑組成物を提供することにある。
本発明者は、特定の研磨用潤滑組成物及び研磨砥粒を含む研磨スラリーが上記課題を解決することを見出し、本発明を完成するに至った。
SUMMARY OF THE INVENTION An object of the present invention is to provide a polishing slurry that is effective in improving the polishing rate and improving the finished surface roughness, and further reducing the surface residue, and a lubricating composition for polishing for preparing the polishing slurry. To provide things.
The present inventor has found that a polishing slurry containing a specific polishing lubricating composition and abrasive grains solves the above problems, and has completed the present invention.

本発明は、 本発明は、下記の発明に係る。
1.(A)及び(B)の成分を含むガラス基板研磨用潤滑組成物。
(A)環状オリゴ糖
(B)水
2.(A)、(B)及び(C)の成分を含むガラス基板研磨用潤滑組成物。
(A)環状オリゴ糖
(B)水
(C)アルカノールアミン
3.(A)、(B)、(C)及び(D)の成分を含むガラス基板研磨用潤滑組成物。
(A)環状オリゴ糖
(B)水
(C)アルカノールアミン
(D)炭素数6〜24の脂肪族カルボン酸
4.環状オリゴ糖が、αシクロデキストリンである上記のいずれかに記載の潤滑組成物。
5.(A)を0.1〜40重量%、(C)を1〜90重量%、(D)を0.1〜30重量%、(B)を残部、からなる上記のいずれかに記載の潤滑組成物。
6.上記のいずれかに記載の研磨用潤滑組成物及び研磨砥粒を含む研磨スラリー。
The present invention relates to the following invention.
1. A lubricating composition for polishing a glass substrate comprising the components (A) and (B).
(A) Cyclic oligosaccharide (B) Water A lubricating composition for polishing a glass substrate comprising the components (A), (B) and (C).
(A) cyclic oligosaccharide (B) water (C) alkanolamine 3. (A), (B), (C) and the lubricating composition for glass substrate polishing containing the component of (D).
(A) cyclic oligosaccharide (B) water (C) alkanolamine (D) aliphatic carboxylic acid having 6 to 24 carbon atoms The lubricating composition according to any one of the above, wherein the cyclic oligosaccharide is α-cyclodextrin.
5. The lubrication according to any one of the above, comprising (A) 0.1 to 40% by weight, (C) 1 to 90% by weight, (D) 0.1 to 30% by weight, and (B) the balance. Composition.
6). A polishing slurry comprising the lubricating composition for polishing according to any one of the above and abrasive grains.

本発明の研磨スラリーは、ガラス基板の加工において、特に研磨速度の向上、仕上げ面粗さの改善に有効な加工特性を示す。更には表面残渣の低減が出来る。   The polishing slurry of the present invention exhibits processing characteristics that are particularly effective in improving the polishing rate and finishing surface roughness in processing glass substrates. Furthermore, the surface residue can be reduced.

本発明のガラス基板研磨用潤滑組成物の各成分について以下に詳しく説明する。
(A)環状オリゴ糖として、例えば、α−シクロデキストリン(α−CD,6個のグルコース環状結合)、β−シクロデキストリン(β−CD,7個のグルコース環状結合)、γ−シクロデキストリン(γ−CD,8個のグルコース環状結合)等があげられる。これら環状オリゴ糖の中でも、αシクロデキストリンが好ましい。ただし、環状オリゴ糖の構成単位は特に限定せず、更には結合の仕方に関しても特に限定しない。また構造異性体、立体異性体も含む。
(B)水としては、イオン交換水もしくは純水等の精製水が好ましい。
(C)アルカノールアミンとしては、特に限定されないが、例えば、一般式
(R)mN(−R−OH)n
(Rは炭素数2〜5の直鎖又は分岐のアルキレン基であり、Rは水素原子又は炭素数1〜3のアルキル基を示す。n、mは1以上の整数であり、n+m=3である。)で表わされるアミンを挙げることができる。具体的にはモノエタノールアミン、ジエタノールアミン、トリエタノールアミン、モノイソプロパノールアミン、ジイソプロパノールアミン、トリイソプロパノールアミン、N,N−ジメチルエタノールアミン、N−メチルモノエタノールアミン、N−メチルジエタノールアミン、n−ブタノールアミン、イソブタノールアミン、tert−ブタノールアミン、2−アミノ−2−メチル−1−プロパノール、ジエチルエタノールアミン、エチルジエタノールアミン等が挙げられる。
(D)脂肪族カルボン酸としては、炭素数6〜24の脂肪族カルボン酸が好ましく、炭化水素鎖が直鎖でも分岐でも環状でも良く、不飽和結合や水酸基を有していても良い、更にはそれらの重縮合物や二塩基酸であってもよい。例えば、カプロン酸、ヘプチリック酸、カプリル酸、ペラゴニン酸、カプリン酸、ウンデシリン酸、ヘンデカン酸、ラウリン酸、トリデシリン酸、ミリスチン酸、ペンタデシリン酸、パルミチン酸、マルガリン酸、ステアリン酸、ノナデシリン酸、アラキジン酸、ベヘン酸、リグノセリン酸等の飽和脂肪酸、ソルビン酸、ウンデシレン酸、オレイン酸、リノール酸、リノレン酸、エルカ酸等の不飽和脂肪酸、イソヘプタン酸、イソノナン酸、イソミリスチン酸、イソパルミチン酸、イソステアリン酸、イソアラキン酸等の分岐鎖脂肪酸、アジピン酸、アゼライン酸、セバシン酸、ドデカン二酸等の二塩基脂肪酸、12ヒドロキシステアリン酸ダイマー、12ヒドロキシステアリン酸トライマー、12ヒドロキシステアリン酸テトラマー等の重縮合脂肪酸、リシノレイン酸、ラクトビオン酸、パントイン酸、メバロン酸、2,2−ビス(ヒドロキシメチル)プロピオン酸、2,2−ビス(ヒドロキシメチル)酪酸、デオキシコール酸、アロイリット酸、ガラクツロン酸、グルコン酸、キナ酸、シキミ酸、コール酸、ラクトン酸等のヒドロキシ脂肪酸などが挙げられる。ここで炭素数はカルボニル炭素を含む炭素数である。これら脂肪族カルボン酸のなかでも炭素数8〜22、更には炭素数12〜18の脂肪族カルボン酸が好ましい。
更に、これら組成物に加え、多価アルコール類を適宜用いても良い。多価アルコール類としては多価アルコール及び多価アルコールのアルキルエーテルを例示でき、例えばエチレングリコール、ジエチレングリコール、トリエチレングリコール、プロピレングリコール、ジプロピレングリコール、トリプロピレングリコール、ブチルカルビトール、ヘキシレングリコール、ブタンジオール、ブチルジグリコール、グリセリン、エチレングリコールモノメチルエーテル、ジエチレングリコールジメチルエーテル、エチレングリコールモノイソプロピルエーテル、エチレングリコールモノブチルエーテル、エチレングリコールジメチルエーテル、プロピレングリコールモノメチルエーテル、ジプロピレングリコールモノメチルエーテル、プロピレングリコールモノブチルエーテル、ジエチレングリコールジメチルエーテル、ジエチレングリコールジエチルエーテル、ソルビトール、スクロース等が挙げられる。
潤滑組成物における成分(A)〜(D)の含有量は特に限定されないが、環状オリゴ糖(A)の含有量としては0.1〜40重量%が好ましく、0.5〜30重量%がより好ましく、1〜15重量%が最も好ましい。成分(A)の含有量が上記範囲であれば、加工時に十分な研磨速度の向上と仕上げ面粗さの改善効果が得られる。更には、表面残渣も低減する。
アルカノールアミン(C)の含有量としては1〜90重量%が好ましく、5〜85重量%がより好ましく、10〜80重量%が最も好ましい。
脂肪族カルボン酸(D)の含有量としては0.1〜30重量%が好ましく、1〜15重量%がより好ましい。成分(D)の含有量を上記範囲とすれば、ハードディスクガラス基板表面に十分に吸着する量であり、加工時に十分な潤滑性が得られる。また潤滑組成物の安定性も良好となる。
水(B)の含有量は、残部である。
本発明の潤滑組成物に研磨砥粒を分散させることにより本発明の研磨スラリーを得ることができる。研磨砥粒としては、例えば、ダイヤモンド、酸化アルミニウム、酸化チタン、酸化ジルコニウム、酸化ゲルマニウム、酸化ケイ素、酸化セリウム、酸化タンタルなどの種々公知の研磨砥粒に適用できる。研磨砥粒の大きさとしては、一般に平均粒子径0.001〜30μm、好ましくは0.003〜20μm、より好ましくは0.005〜10μm程度が良い。なかでも研磨砥粒としてはダイヤモンド砥粒が好ましく、その大きさとしては、平均粒子径0.01〜1μm程度が好ましい。研磨スラリー中のダイヤモンド砥粒の含有量は特に限定されないが、通常1重量%以下、好ましくは0.001〜0.5重量%が良い。
本発明のガラス基板研磨用潤滑組成物及び研磨スラリーによって研磨されるガラス基板はとくに限定しないが、例えば珪酸、アルミナ、酸化ナトリウム、酸化カリウム等を主な組成物としたガラス基板が挙げられる。例えば、ハードディスクガラス基板、光学レンズ用ガラス基板、光学レンズ、薄膜トランジスタ(TFT)型LCDなどの液晶用ガラス基板、液晶TV用カラーフィルター、LSIフォトマスク用ガラス基板などを例示することができる。
本発明の研磨スラリーは、ガラス基板加工用の研磨スラリーであって、NiP合金基板加工用の研磨スラリーや、通常の鉄やアルミ材料の水溶性切削加工、水溶性研削加工、水溶性研磨加工液とは、区別されるものである。上記通常の加工においては、循環使用が一般的であり、防腐、消泡、防錆などの二次性能等において要求性能が大きく異なる。
Each component of the lubricating composition for polishing a glass substrate of the present invention will be described in detail below.
(A) As cyclic oligosaccharides, for example, α-cyclodextrin (α-CD, 6 glucose cyclic bonds), β-cyclodextrin (β-CD, 7 glucose cyclic bonds), γ-cyclodextrin (γ -CD, 8 glucose cyclic bonds) and the like. Among these cyclic oligosaccharides, α cyclodextrin is preferable. However, the structural unit of the cyclic oligosaccharide is not particularly limited, and further, the binding method is not particularly limited. Also includes structural isomers and stereoisomers.
(B) The water is preferably purified water such as ion exchange water or pure water.
The (C) an alkanolamine, but are not limited to, for example, the general formula (R 2) mN (-R 1 -OH) n
(R 1 is a linear or branched alkylene group having 2 to 5 carbon atoms, R 2 is a hydrogen atom or an alkyl group having 1 to 3 carbon atoms. N and m are integers of 1 or more, and n + m = 3)). Specifically, monoethanolamine, diethanolamine, triethanolamine, monoisopropanolamine, diisopropanolamine, triisopropanolamine, N, N-dimethylethanolamine, N-methylmonoethanolamine, N-methyldiethanolamine, n-butanolamine , Isobutanolamine, tert-butanolamine, 2-amino-2-methyl-1-propanol, diethylethanolamine, ethyldiethanolamine and the like.
(D) The aliphatic carboxylic acid is preferably an aliphatic carboxylic acid having 6 to 24 carbon atoms, and the hydrocarbon chain may be linear, branched or cyclic, and may have an unsaturated bond or a hydroxyl group. May be a polycondensate or dibasic acid thereof. For example, caproic acid, hepteric acid, caprylic acid, pelagonic acid, capric acid, undecylic acid, hedecanoic acid, lauric acid, tridecyric acid, myristic acid, pentadecylic acid, palmitic acid, margaric acid, stearic acid, nonadecylic acid, arachidic acid, Saturated fatty acids such as behenic acid and lignoceric acid, unsaturated fatty acids such as sorbic acid, undecylenic acid, oleic acid, linoleic acid, linolenic acid, and erucic acid, isoheptanoic acid, isononanoic acid, isomristic acid, isopalmitic acid, isostearic acid, Branched chain fatty acids such as isoarachidic acid, dibasic fatty acids such as adipic acid, azelaic acid, sebacic acid and dodecanedioic acid, heavy compounds such as 12 hydroxystearic acid dimer, 12 hydroxystearic acid trimer and 12 hydroxystearic acid tetramer Combined fatty acids, ricinoleic acid, lactobionic acid, pantoic acid, mevalonic acid, 2,2-bis (hydroxymethyl) propionic acid, 2,2-bis (hydroxymethyl) butyric acid, deoxycholic acid, alloyitic acid, galacturonic acid, gluconic acid And hydroxy fatty acids such as quinic acid, shikimic acid, cholic acid, and lactone acid. Here, the carbon number is a carbon number including a carbonyl carbon. Among these aliphatic carboxylic acids, aliphatic carboxylic acids having 8 to 22 carbon atoms, and more preferably 12 to 18 carbon atoms are preferable.
Furthermore, in addition to these compositions, polyhydric alcohols may be used as appropriate. Examples of polyhydric alcohols include polyhydric alcohols and alkyl ethers of polyhydric alcohols, such as ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, dipropylene glycol, tripropylene glycol, butyl carbitol, hexylene glycol, butane. Diol, butyl diglycol, glycerin, ethylene glycol monomethyl ether, diethylene glycol dimethyl ether, ethylene glycol monoisopropyl ether, ethylene glycol monobutyl ether, ethylene glycol dimethyl ether, propylene glycol monomethyl ether, dipropylene glycol monomethyl ether, propylene glycol monobutyl ether, diethylene glycol dimethyl ether Ether, diethylene glycol diethyl ether, sorbitol, sucrose and the like.
Although content of component (A)-(D) in a lubricating composition is not specifically limited, As content of cyclic oligosaccharide (A), 0.1 to 40 weight% is preferable and 0.5 to 30 weight% is preferable. More preferred is 1 to 15% by weight. If content of a component (A) is the said range, the improvement effect of the grinding | polishing speed | rate sufficient at the time of a process and the finishing surface roughness will be acquired. Furthermore, surface residues are also reduced.
The content of alkanolamine (C) is preferably 1 to 90% by weight, more preferably 5 to 85% by weight, and most preferably 10 to 80% by weight.
The content of the aliphatic carboxylic acid (D) is preferably 0.1 to 30% by weight, and more preferably 1 to 15% by weight. If the content of the component (D) is in the above range, the amount is sufficiently adsorbed on the hard disk glass substrate surface, and sufficient lubricity can be obtained during processing. Also, the stability of the lubricating composition is improved.
The content of water (B) is the balance.
The polishing slurry of the present invention can be obtained by dispersing abrasive grains in the lubricating composition of the present invention. As the abrasive grains, for example, various known abrasive grains such as diamond, aluminum oxide, titanium oxide, zirconium oxide, germanium oxide, silicon oxide, cerium oxide, and tantalum oxide can be applied. The size of the abrasive grains is generally about 0.001 to 30 μm, preferably 0.003 to 20 μm, more preferably about 0.005 to 10 μm. Among these, diamond abrasive grains are preferable as the abrasive grains, and the average particle diameter is preferably about 0.01 to 1 μm. The content of diamond abrasive grains in the polishing slurry is not particularly limited, but is usually 1% by weight or less, preferably 0.001 to 0.5% by weight.
The glass substrate polished with the lubricating composition for polishing a glass substrate and the polishing slurry of the present invention is not particularly limited, and examples thereof include a glass substrate mainly composed of silicic acid, alumina, sodium oxide, potassium oxide and the like. Examples thereof include a hard disk glass substrate, an optical lens glass substrate, an optical lens, a liquid crystal glass substrate such as a thin film transistor (TFT) type LCD, a liquid crystal TV color filter, and an LSI photomask glass substrate.
The polishing slurry of the present invention is a polishing slurry for processing a glass substrate, and is a polishing slurry for processing a NiP alloy substrate, a water-soluble cutting process of a normal iron or aluminum material, a water-soluble grinding process, a water-soluble polishing process liquid Is a distinction. In the above-mentioned normal processing, circulation is generally used, and the required performance differs greatly in secondary performance such as antiseptic, antifoaming, and rust prevention.

以下に示す実施例、及び、比較例においては、以下に示す研磨評価を行った。ただし、本発明は実施例に限定されるものではない。
研磨特性評価
ウレタンパッド(ニッタ・ハース製IC1000)を研磨装置(ナノファクター製NF−300)に設置し、プラテン回転数230回転/分、ヘッド回転数170回転/分、研磨圧力7.2PSIの条件で研磨スラリーを20ml/分の速度で供給しつつ、直径2.5インチのハードディスクガラス基板(ケイ酸、アルミナ、酸化ナトリウム、酸化カリウム等含むガラス)を研磨時間15分(研磨速度評価)、及び、1分(表面粗さ評価)で研磨評価を行った。研磨時の研磨速度、及び、研磨後の表面粗さを評価することによって研磨評価を行った。なお、研磨速度、及び、表面粗さの測定方法は以下の方法で測定した。
研磨速度
研磨前後のガラス基板の重量変化を電子天秤(ザルトリウス社製LE225D)により測定して研磨量を求め研磨速度を求めた。
表面粗さ
研磨後の表面粗さは走査プローブ顕微鏡(エスアイアイ・ナノテクノロジー製SPA−400)を用いて、AFMモードにより測定した。
表面残渣
研磨後の表面残渣は光学表面分析装置(Candela製OSA−5100)により測定した。
実施例1〜8及び比較例1〜8
下記表1〜4に示す成分(数値は重量%)を配合してハードディスクガラス基板用潤滑液を調製した。水は精製水を用いた。比較例2のリシノレイン酸は特開2004−306248号公報(特許文献2)で用いられる炭素数16〜40のカルボン酸、比較例5のオレイン酸は特表2004−515609号公報(特許文献1)で用いられる炭素数10〜22の脂肪酸である。なお、シクロデキストリン以外の糖として、比較例1でグルコース1,1グリコシド結合二糖を使用した。
ハードディスクガラス基板用研磨スラリーは、潤滑組成物17.5gを純水321.5gで希釈後、ダイヤモンド濃度:1.5重量%及び平均粒子径:30nm〔動的光散乱法(大塚電子株式会社製DLS−6000HL)で測定〕のダイヤモンドスラリーを10.9g添加することによりダイヤモンド砥粒の含有量が0.05重量%の研磨スラリーを調製した。この研磨スラリーを使用し、ハードディスクガラス基板の研磨評価を行った。結果を表1〜3に示す。表4に研磨後のガラス基板上に残る表面残渣を示す。

Figure 0005429397
Figure 0005429397
Figure 0005429397
Figure 0005429397
表1の実施例1は研磨速度は低いが、優れた表面粗さの改善を示し、最終段階での研磨工程に使用することができる。実施例2〜3及び比較例1〜2より環状オリゴ糖は十分な研磨速度と表面粗さの改善の両立が可能である事が確認できる。更には、実施例1〜2のαシクロデキストリンが最も好適である。
表2より比較例3〜5は研磨速度と表面粗さの両立が困難であるのに対し、実施例4は十分な研磨速度と表面粗さの改善の両立が可能である事が確認できる。
表3の、比較例6〜7の従来技術であるプロピレングリコールでは、研磨速度と表面粗さの両立が困難であるのに対し、実施例4〜7では十分な研磨速度と表面粗さの改善の両立が可能である。更に脂肪族カルボン酸を変えても、その効果は発揮され、十分な研磨速度と表面粗さの両立が可能である事が確認できる。
表4より、本発明を用いる事によって研磨後のガラス基板上に残る物理残渣及び有機残渣の低減が可能である事が確認できる。
実施例9〜12及び比較例9〜16
下記表5〜6に示す成分(数値は重量%)を配合してガラス基板用潤滑液を調製した以外は実施例1と同様にして研磨スラリーを調製した。この研磨スラリーを用いて、含有成分の違う各種ガラス基板を用いた研磨評価を行い、その結果を表5〜6に示す。
Figure 0005429397
Figure 0005429397
ガラス基板A:ケイ酸(SiO)を主成分とし、酸化ナトリウム、アルミナ、酸化カリウムを副成分として含有するガラス基板。
ガラス基板B:ケイ酸(SiO)を主成分とし、酸化ナトリウム、アルミナ、酸化カリウム、Pを副成分として含有するガラス基板。
ガラス基板C:ケイ酸(SiO)を主成分とし、アルミナ、酸化カリウムを副成分として含有するガラス基板。
ガラス基板D:ケイ酸(SiO)を主成分とし、アルミナを副成分として含有するガラス基板。In the following examples and comparative examples, the following polishing evaluation was performed. However, the present invention is not limited to the examples.
Polishing characteristic evaluation Urethane pad (Nitta Haas IC1000) is installed in a polishing apparatus (NF-300 manufactured by Nano Factor), conditions of platen rotation speed 230 rpm, head rotation speed 170 rpm, polishing pressure 7.2 PSI While supplying the polishing slurry at a rate of 20 ml / min, a hard disk glass substrate having a diameter of 2.5 inches (glass containing silicic acid, alumina, sodium oxide, potassium oxide, etc.) is polished for 15 minutes (polishing rate evaluation), and Polishing evaluation was performed in 1 minute (surface roughness evaluation). Polishing evaluation was performed by evaluating the polishing rate during polishing and the surface roughness after polishing. In addition, the measuring method of the grinding | polishing speed | rate and surface roughness was measured with the following method.
Polishing rate The weight change of the glass substrate before and after polishing was measured with an electronic balance (LE225D manufactured by Sartorius) to determine the polishing amount, and the polishing rate was determined.
Surface Roughness Surface roughness after polishing was measured by AFM mode using a scanning probe microscope (SP-400 manufactured by SII Nanotechnology).
Surface residue The surface residue after polishing was measured by an optical surface analyzer (OSA-5100 manufactured by Candela).
Examples 1-8 and Comparative Examples 1-8
Components shown in the following Tables 1 to 4 (numerical values are% by weight) were blended to prepare a lubricating liquid for a hard disk glass substrate. Purified water was used as the water. The ricinoleic acid of Comparative Example 2 is a carboxylic acid having 16 to 40 carbon atoms used in JP-A-2004-306248 (Patent Document 2), and the oleic acid of Comparative Example 5 is JP-T-2004-515609 (Patent Document 1). Is a fatty acid having 10 to 22 carbon atoms. In addition, as a sugar other than cyclodextrin, glucose 1,1 glycoside-linked disaccharide was used in Comparative Example 1.
The polishing slurry for hard disk glass substrate was prepared by diluting 17.5 g of the lubricating composition with 321.5 g of pure water, then diamond concentration: 1.5 wt% and average particle size: 30 nm [dynamic light scattering method (manufactured by Otsuka Electronics Co., Ltd.) 10.9 g of a diamond slurry measured in DLS-6000HL) was added to prepare a polishing slurry having a diamond abrasive grain content of 0.05% by weight. Polishing evaluation of the hard disk glass substrate was performed using this polishing slurry. The results are shown in Tables 1-3. Table 4 shows surface residues remaining on the polished glass substrate.
Figure 0005429397
Figure 0005429397
Figure 0005429397
Figure 0005429397
Although Example 1 of Table 1 has a low polishing rate, it shows excellent surface roughness improvement and can be used in the final polishing step. From Examples 2-3 and Comparative Examples 1-2, it can be confirmed that the cyclic oligosaccharide can achieve both a sufficient polishing rate and improved surface roughness. Furthermore, the α cyclodextrins of Examples 1 and 2 are most suitable.
From Table 2, it can be confirmed that Comparative Examples 3 to 5 are difficult to achieve both the polishing rate and the surface roughness, whereas Example 4 can achieve both a sufficient polishing rate and improvement of the surface roughness.
In propylene glycol, which is the prior art of Comparative Examples 6 to 7 in Table 3, it is difficult to achieve both the polishing rate and the surface roughness, whereas in Examples 4 to 7, the polishing rate and the surface roughness are sufficiently improved. Is possible. Furthermore, even if the aliphatic carboxylic acid is changed, the effect is exhibited, and it can be confirmed that both a sufficient polishing speed and surface roughness can be achieved.
From Table 4, it can be confirmed that by using the present invention, it is possible to reduce physical residues and organic residues remaining on the polished glass substrate.
Examples 9-12 and Comparative Examples 9-16
A polishing slurry was prepared in the same manner as in Example 1 except that the components shown in the following Tables 5 to 6 (the numerical values are% by weight) were blended to prepare a glass substrate lubricating liquid. Using this polishing slurry, polishing evaluation using various glass substrates having different components was performed, and the results are shown in Tables 5-6.
Figure 0005429397
Figure 0005429397
Glass substrate A: A glass substrate containing silicic acid (SiO 2 ) as a main component and sodium oxide, alumina and potassium oxide as subcomponents.
Glass substrate B: A glass substrate containing silicic acid (SiO 2 ) as a main component and sodium oxide, alumina, potassium oxide, and P 2 O 5 as subcomponents.
Glass substrate C: A glass substrate containing silicic acid (SiO 2 ) as a main component and alumina and potassium oxide as subcomponents.
Glass substrate D: A glass substrate containing silicic acid (SiO 2 ) as a main component and alumina as a subcomponent.

本発明によれば、研磨時の研磨速度に優れ、研磨後のガラス基板の仕上げ表面粗さの改善に有効な加工特性に優れた研磨スラリーが提供される。更に本発明の付帯効果として研磨後のガラス基板表面残渣の低減が出来る。
また、本発明のガラス基板研磨用潤滑組成物及び研磨スラリーは、光学レンズ用ガラス基板や光学レンズ、薄膜トランジスタ(TFT)型LCDなどの液晶用ガラス基板、液晶TV用カラーフィルター、LSIフォトマスク用ガラス基板の研磨、研削及び切断等にも適用できる。
ADVANTAGE OF THE INVENTION According to this invention, the grinding | polishing slurry which was excellent in the grinding | polishing speed | rate at the time of grinding | polishing, and excellent in the processing characteristic effective for improvement of the finishing surface roughness of the glass substrate after grinding | polishing is provided. Furthermore, as an incidental effect of the present invention, the glass substrate surface residue after polishing can be reduced.
The lubricating composition and polishing slurry for polishing a glass substrate of the present invention are a glass substrate for an optical lens, a glass substrate for an optical lens, a liquid crystal glass substrate such as a thin film transistor (TFT) type LCD, a color filter for a liquid crystal TV, and an LSI photomask glass. It can also be applied to substrate polishing, grinding and cutting.

Claims (7)

(A)、(B)及び(C)の成分を含むガラス基板研磨用潤滑組成物(ただしポリアクリル酸、ポリメタクリル酸、及びそれらの塩からなる群より選ばれる水溶性高分子を含まない)。
(A)環状オリゴ糖
(B)水
(C)アルカノールアミン
(A), (B) and a lubricating composition for polishing a glass substrate comprising the components (C) (however, it does not include a water-soluble polymer selected from the group consisting of polyacrylic acid, polymethacrylic acid, and salts thereof) .
(A) Cyclic oligosaccharide (B) Water (C) Alkanolamine
(A)、(B)、(C)及び(D)の成分を含むガラス基板研磨用潤滑組成物(ただしポリアクリル酸、ポリメタクリル酸、及びそれらの塩からなる群より選ばれる水溶性高分子を含まない)。
(A)環状オリゴ糖
(B)水
(C)アルカノールアミン
(D)炭素数6〜24の脂肪族カルボン酸
(A), (B), (C) and (D) lubricating composition for glass substrate polishing (however, a water-soluble polymer selected from the group consisting of polyacrylic acid, polymethacrylic acid, and salts thereof) Not included).
(A) Cyclic oligosaccharide (B) Water (C) Alkanolamine (D) Aliphatic carboxylic acid having 6 to 24 carbon atoms
環状オリゴ糖が、αシクロデキストリンである請求項1〜のいずれか1項に記載の潤滑組成物。 Cyclic oligosaccharides, alpha lubricating composition according to any one of claims 1-2 cyclodextrin. アルカノールアミンが、一般式
(R)mN(−R−OH)n
(Rは炭素数2〜5の直鎖又は分岐のアルキレン基であり、Rは水素原子又は炭素数1〜3のアルキル基を示す。n、mは1以上の整数であり、n+m=3である。)で表わされるアミンである請求項のいずれか1項に記載の潤滑組成物。
The alkanolamine is represented by the general formula (R 2 ) mN (—R 1 —OH) n
(R 1 is a linear or branched alkylene group having 2 to 5 carbon atoms, R 2 is a hydrogen atom or an alkyl group having 1 to 3 carbon atoms. N and m are integers of 1 or more, and n + m = 3 is.) lubricating composition according to any one of claims 1-2 which is an amine represented by.
(A)を0.1〜40重量%、(C)を1〜90重量%、(B)を残部、からなる請求項に記載の潤滑組成物。 The lubricating composition according to claim 1 , comprising (A) 0.1 to 40% by weight, (C) 1 to 90% by weight, and (B) the balance. (A)を0.1〜40重量%、(C)を1〜90重量%、(D)を0.1〜30重量%、(B)を残部、からなる請求項に記載の潤滑組成物。 The lubricating composition according to claim 2 , comprising (A) 0.1 to 40% by weight, (C) 1 to 90% by weight, (D) 0.1 to 30% by weight, and (B) the balance. object. 請求項1〜のいずれか1項に記載の研磨用潤滑組成物及び研磨砥粒を含む研磨スラリー。 Abrasive slurry comprising abrasive lubricating composition and abrasive grains according to any one of claims 1-6.
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