JP7158889B2 - Polishing liquid composition for glass hard disk substrate - Google Patents
Polishing liquid composition for glass hard disk substrate Download PDFInfo
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- JP7158889B2 JP7158889B2 JP2018091696A JP2018091696A JP7158889B2 JP 7158889 B2 JP7158889 B2 JP 7158889B2 JP 2018091696 A JP2018091696 A JP 2018091696A JP 2018091696 A JP2018091696 A JP 2018091696A JP 7158889 B2 JP7158889 B2 JP 7158889B2
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C19/00—Surface treatment of glass, not in the form of fibres or filaments, by mechanical means
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
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- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
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- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Surface Treatment Of Glass (AREA)
Description
本開示は、ガラスハードディスク基板用研磨液組成物、ガラスハードディスク基板の製造方法、及び、ガラス基板の研磨方法に関する。 TECHNICAL FIELD The present disclosure relates to a polishing liquid composition for glass hard disk substrates, a method for producing a glass hard disk substrate, and a method for polishing a glass substrate.
ハードディスクドライブに搭載されるハードディスクは高速で回転するため消費電力が高く、近年では環境への配慮から、低消費電力化が求められている。消費電力を低減するためには、ハードディスク１枚あたりの記録容量を増大させ、ドライブに搭載されるハードディスクの枚数を減らし、軽量化する方法がある。基板１枚の重量を軽量化するためには、基板の厚さを薄くする必要があり、この観点から、アルミ基板に比べて機械的強度が高いガラス基板の需要が高まり、近年の伸張は著しい。また、基板１枚あたりの記録容量を向上させるためには、単位記録面積を縮小する必要がある。しかし、単位記録面積を縮小すると磁気信号が弱くなる問題が発生する。そこで磁気信号の検出感度を向上するため、磁気ヘッドの浮上高さをより低くするための技術開発が進められている。ハードディスク基板の研磨においては、この磁気ヘッドの低浮上化に対応するため、表面欠陥や残留物の低減に対する要求が厳しくなっている。 Since the hard disk mounted on the hard disk drive rotates at high speed, it consumes a lot of power. In order to reduce power consumption, there is a method of increasing the recording capacity of each hard disk, reducing the number of hard disks mounted on the drive, and reducing the weight. In order to reduce the weight of each substrate, it is necessary to reduce the thickness of the substrate. From this point of view, the demand for glass substrates, which have higher mechanical strength than aluminum substrates, has increased, and the growth in recent years has been remarkable. . Also, in order to improve the recording capacity per substrate, it is necessary to reduce the unit recording area. However, when the unit recording area is reduced, there arises a problem that the magnetic signal becomes weaker. Therefore, in order to improve the detection sensitivity of magnetic signals, technological development is underway to lower the flying height of the magnetic head. In the polishing of hard disk substrates, there is an increasing demand for reducing surface defects and residues in order to cope with the reduction in flying height of magnetic heads.
このような要求に対し、例えば、特許文献１では、特定のグレイン径及び特定のゼータ電位を有するシリカ粒子を含む酸性の研磨液組成物が提案されている。
また、特許文献２では、（ａ）水、（ｂ）リン酸エステル化合物、（ｃ）研磨促進剤、（ｄ）研磨材を含む研磨液組成物が提案されている。
さらに、特許文献３では、（Ａ）リン酸、リン酸塩及びリン酸化合物から選ばれる少なくとも１種、（Ｂ）シリカ、（Ｃ）水を含む研磨液組成物が提案されている。
In response to such demands, for example, Patent Document 1 proposes an acidic polishing composition containing silica particles having a specific grain diameter and a specific zeta potential.
Further, Patent Document 2 proposes a polishing liquid composition containing (a) water, (b) a phosphate ester compound, (c) a polishing accelerator, and (d) an abrasive.
Furthermore, Patent Document 3 proposes a polishing composition containing (A) at least one selected from phosphoric acid, phosphates and phosphoric acid compounds, (B) silica, and (C) water.
ガラスハードディスク基板の研磨においては、酸性の研磨液組成物でガラス基板を研磨する方法が採用されている。酸性の研磨液組成物を用いることで、研磨中にガラス基板に含有されるアルカリイオンが溶出するリーチング作用が起こり、基板表面の硬度が低下して研磨速度が向上するという利点がある。しかしながら、酸性の研磨液組成物でガラス基板を研磨する方法は、ｐＨが低いとリーチング作用が大きく働くため、脆いリーチング層が深くまで生成し、研磨工程後のアルカリ洗浄工程におけるアルカリエッチングにより表面粗さが著しく悪化するという問題がある。また、一般的に、研磨速度と表面粗さとはトレードオフの関係にあり、一方が改善すれば一方が悪化するという問題がある。 In the polishing of glass hard disk substrates, a method of polishing the glass substrate with an acidic polishing liquid composition is employed. By using an acidic polishing liquid composition, a leaching effect occurs in which alkali ions contained in the glass substrate are eluted during polishing, and there is an advantage that the hardness of the substrate surface is lowered and the polishing speed is improved. However, in the method of polishing a glass substrate with an acidic polishing liquid composition, the leaching action acts strongly when the pH is low, so that a brittle leaching layer is formed deep and the surface is roughened by alkali etching in the alkali washing step after the polishing step. However, there is a problem that the noise level is remarkably deteriorated. Moreover, there is generally a trade-off relationship between the polishing rate and the surface roughness, and there is a problem that if one is improved, the other is deteriorated.
本開示は、一又は複数の実施形態において、ガラス基板を酸性研磨液で研磨する工程と洗浄する工程を有するガラスハードディスク基板の製造方法において、研磨工程において研磨速度を維持しつつ、洗浄工程においてガラス基板の表面粗さの悪化を抑制できるガラスハードディスク基板用研磨液組成物、並びにこれを用いたガラスハードディスク基板の製造方法及びガラス基板の研磨方法を提供する。 In one or a plurality of embodiments, the present disclosure provides a method for manufacturing a glass hard disk substrate, which includes a step of polishing a glass substrate with an acidic polishing liquid and a step of washing, in which the polishing speed is maintained in the polishing step, and the glass is polished in the washing step. Provided are a polishing liquid composition for glass hard disk substrates capable of suppressing deterioration of the surface roughness of a substrate, a method for producing a glass hard disk substrate and a method for polishing a glass substrate using the same.
本開示は、一態様において、砥粒、スルファミン酸、リン酸塩、及び水を含有する、ガラスハードディスク基板用研磨液組成物に関する。 In one aspect, the present disclosure relates to a polishing liquid composition for glass hard disk substrates, containing abrasive grains, sulfamic acid, phosphate, and water.
本開示は、その他の態様において、本開示の研磨液組成物を用いて被研磨ガラス基板を研磨する工程を含む、ガラスハードディスク基板の製造方法に関する。 In another aspect, the present disclosure relates to a method for manufacturing a glass hard disk substrate, comprising polishing a glass substrate to be polished using the polishing composition of the present disclosure.
本開示は、その他の態様において、本開示の研磨液組成物を用いて被研磨ガラス基板を研磨することを含む、ガラス基板の研磨方法に関する。 In another aspect, the present disclosure relates to a method for polishing a glass substrate, comprising polishing a glass substrate to be polished using the polishing composition of the present disclosure.
本開示によれば、一又は複数の実施形態において、研磨工程において研磨速度を維持しつつ、洗浄工程においてガラス基板の表面粗さの悪化を抑制できる。 According to the present disclosure, in one or a plurality of embodiments, deterioration of the surface roughness of the glass substrate can be suppressed in the cleaning process while maintaining the polishing rate in the polishing process.
本開示は、ガラス基板を酸性研磨液で研磨した後にアルカリ洗浄した場合であっても、研磨液組成物中にスルファミン酸とリン酸塩とが含まれていると、酸性研磨液による研磨速度を維持しつつ、洗浄によるガラス基板の表面粗さの悪化を抑制できるという知見に基づく。 According to the present disclosure, even when a glass substrate is polished with an acidic polishing liquid and then washed with an alkali, if the polishing liquid composition contains sulfamic acid and a phosphate, the polishing rate of the acidic polishing liquid is reduced. It is based on the knowledge that deterioration of the surface roughness of the glass substrate due to cleaning can be suppressed while maintaining the surface roughness.
すなわち、本開示は、一態様において、砥粒、スルファミン酸、リン酸塩、及び水を含有する、ガラスハードディスク基板用研磨液組成物（以下、「本開示の研磨液組成物」ともいう）に関する。 That is, in one aspect, the present disclosure relates to a polishing liquid composition for glass hard disk substrates (hereinafter also referred to as "polishing liquid composition of the present disclosure") containing abrasive grains, sulfamic acid, phosphate, and water. .
本開示の効果発現のメカニズムは明らかではないが、以下のように推察される。
一般に、ガラス基板を酸性研磨すると、ガラス基板表面から金属イオンが溶出して、ガラス基板表面が脆弱化し、研磨されやすくなることが知られている。
本開示では、スルファミン酸とリン酸塩とを研磨液組成物中に含有させることで、金属イオンの溶出が促進され、研磨速度の向上と表面粗さの悪化抑制とを両立できると考えられる。
但し、本開示はこれらのメカニズムに限定して解釈されなくてもよい。
Although the mechanism by which the effect of the present disclosure manifests is not clear, it is speculated as follows.
It is generally known that when a glass substrate is acid-polished, metal ions are eluted from the surface of the glass substrate, weakening the surface of the glass substrate and making it easier to polish.
In the present disclosure, it is believed that by including sulfamic acid and a phosphate in the polishing liquid composition, the elution of metal ions is promoted, and it is possible to both improve the polishing rate and suppress the deterioration of the surface roughness.
However, the present disclosure need not be construed as being limited to these mechanisms.
［砥粒（成分Ａ）］
本開示の研磨液組成物に含まれる砥粒（以下、「成分Ａ」ともいう）としては、研磨用に一般的に使用されている砥粒を使用することができ、金属、金属若しくは半金属の炭化物、窒化物、酸化物、又はホウ化物、ダイヤモンド等が挙げられる。金属又は半金属元素は、周期律表（長周期型）の２Ａ、２Ｂ、３Ａ、３Ｂ、４Ａ、４Ｂ、５Ａ、６Ａ、７Ａ又は８族由来のものである。成分Ａの具体例としては、酸化珪素（以下、シリカという）、酸化アルミニウム（以下、アルミナという）、炭化珪素、ダイヤモンド、酸化マンガン、酸化マグネシウム、酸化亜鉛、酸化チタン、酸化セリウム（以下、セリアという）、酸化ジルコニウム等が挙げられ、これらの１種以上を使用することは研磨速度を向上させる観点から好ましい。中でも、研磨速度を維持しつつ表面粗さの悪化を抑制する観点から、成分Ａとしては、シリカ粒子、セリア粒子が好ましく、シリカ粒子がより好ましい。シリカ粒子としては、コロイダルシリカ、ヒュームドシリカ、粉砕シリカ、及びそれらを表面修飾したシリカ等が挙げられ、コロイダルシリカが好ましい。成分Ａは、１種単独で用いてもよいし、２種以上を併用してもよい。
[Abrasive grain (component A)]
As the abrasive grains contained in the polishing composition of the present disclosure (hereinafter also referred to as “component A”), abrasive grains commonly used for polishing can be used, and metal, metal or semi-metal carbides, nitrides, oxides, borides, diamonds, and the like. The metal or metalloid element is from group 2A, 2B, 3A, 3B, 4A, 4B, 5A, 6A, 7A or 8 of the periodic table (long period type). Specific examples of component A include silicon oxide (hereinafter referred to as silica), aluminum oxide (hereinafter referred to as alumina), silicon carbide, diamond, manganese oxide, magnesium oxide, zinc oxide, titanium oxide, and cerium oxide (hereinafter referred to as ceria). ), zirconium oxide, etc., and it is preferable to use one or more of these from the viewpoint of improving the polishing rate. Among them, silica particles and ceria particles are preferable as component A, and silica particles are more preferable, from the viewpoint of suppressing deterioration of surface roughness while maintaining the polishing rate. Examples of silica particles include colloidal silica, fumed silica, pulverized silica, and silica obtained by surface modification thereof, and colloidal silica is preferred. Component A may be used alone or in combination of two or more.
前記シリカ粒子は、例えば、珪酸アルカリ水溶液を原料とした粒子成長による方法（以下、「水ガラス法」ともいう）、及び、アルコキシシランの加水分解物の縮合による方法（以下、「ゾルゲル法」）ともいう）により得たものが挙げられ、製造容易性及び経済性の観点から、好ましくは水ガラス法により得たものである。水ガラス法及びゾルゲル法により得られるシリカ粒子は、従来から公知の方法によって製造できる。シリカ粒子の形状は、特に限定されなくてもよく、球状でも非球状でもよい。 The silica particles are produced by, for example, a method by particle growth using an aqueous alkali silicate solution as a raw material (hereinafter also referred to as "water glass method"), and a method by condensation of a hydrolyzate of alkoxysilane (hereinafter, "sol-gel method"). from the standpoint of ease of production and economy, preferably by the water glass method. Silica particles obtained by the water glass method and the sol-gel method can be produced by conventionally known methods. The shape of the silica particles is not particularly limited, and may be spherical or non-spherical.
成分Ａの平均粒径は、研磨速度を維持しつつ表面粗さの悪化を抑制する観点から、１ｎｍ以上が好ましく、５ｎｍ以上がより好ましく、１０ｎｍ以上が更に好ましく、そして、同様の観点から、１００ｎｍ以下が好ましく、７０ｎｍ以下がより好ましく、４０ｎｍ以下が更に好ましい。より具体的には、成分Ａの平均粒径は、１ｎｍ以上１００ｎｍ以下が好ましく、５ｎｍ以上７０ｎｍ以下がより好ましく、１０ｎｍ以上４０ｎｍ以下が更に好ましい。成分Ａの平均粒径は、例えば、実施例に記載の方法により求めることができる。 The average particle size of component A is preferably 1 nm or more, more preferably 5 nm or more, still more preferably 10 nm or more, from the viewpoint of suppressing deterioration of surface roughness while maintaining the polishing rate, and from the same viewpoint, 100 nm. The following is preferable, 70 nm or less is more preferable, and 40 nm or less is even more preferable. More specifically, the average particle diameter of component A is preferably 1 nm or more and 100 nm or less, more preferably 5 nm or more and 70 nm or less, and even more preferably 10 nm or more and 40 nm or less. The average particle size of Component A can be determined, for example, by the method described in Examples.
本開示の研磨液組成物中における成分Ａの含有量は、研磨速度向上の観点から、０．１質量％以上が好ましく、１質量％以上がより好ましく、３質量％以上が更に好ましく、そして、表面粗さの悪化抑制の観点から、２０質量％以下が好ましく、１５質量％以下がより好ましく、１０質量％以下が更に好ましい。より具体的には、成分Ａの含有量は、０．１質量％以上２０質量％以下が好ましく、１質量％以上１５質量％以下が更に好ましい。成分Ａが２種以上の組合せである場合、成分Ａの含有量は、それらの合計含有量をいう。 The content of component A in the polishing composition of the present disclosure is preferably 0.1% by mass or more, more preferably 1% by mass or more, and even more preferably 3% by mass or more, from the viewpoint of improving the polishing rate, and From the viewpoint of suppressing deterioration of surface roughness, it is preferably 20% by mass or less, more preferably 15% by mass or less, and even more preferably 10% by mass or less. More specifically, the content of component A is preferably 0.1% by mass or more and 20% by mass or less, and more preferably 1% by mass or more and 15% by mass or less. When component A is a combination of two or more, the content of component A refers to their total content.
本開示の一実施形態において、成分Ａ、成分Ｂ、成分Ｃ、水、及び／又はその他の成分の含有量は、研磨液組成物の全量（１００質量％）に対する各成分の配合量とみなすことができる。一又は複数の実施形態において、「含有量」は「配合量」に読み替えることができ、Ｘを「含有する」はＸが「配合された」に読み替えることができる。 In one embodiment of the present disclosure, the content of component A, component B, component C, water, and/or other components is regarded as the blending amount of each component with respect to the total amount (100% by mass) of the polishing composition. can be done. In one or more embodiments, "content" can be read as "compound amount", and "containing" X can be read as "combined with" X.
［スルファミン酸（成分Ｂ）］
本開示の研磨液組成物は、研磨速度を維持しつつ表面粗さの悪化を抑制する観点から、スルファミン酸（以下、「成分Ｂ」ともいう）を含む。
[Sulfamic acid (component B)]
The polishing composition of the present disclosure contains sulfamic acid (hereinafter also referred to as “component B”) from the viewpoint of suppressing deterioration of surface roughness while maintaining polishing rate.
本開示の研磨液組成物中の成分Ｂの含有量は、研磨速度を維持しつつ表面粗さの悪化を抑制する観点から、０．０５質量％以上が好ましく、０．１質量％以上がより好ましく、０．１５質量％以上が更に好ましく、そして、同様の観点から、１０質量％以下が好ましく、７質量％以下がより好ましく、５質量％以下が更に好ましい。より具体的には、成分Ｂの含有量は、０．０５質量％以上１０質量％以下が好ましく、０．１質量％以上７質量％以下がより好ましく、０．１５質量％以上５質量％以下が更に好ましい。 The content of component B in the polishing composition of the present disclosure is preferably 0.05% by mass or more, more preferably 0.1% by mass or more, from the viewpoint of suppressing deterioration of surface roughness while maintaining the polishing rate. It is preferably 0.15% by mass or more, more preferably 0.15% by mass or less, and from the same viewpoint, preferably 10% by mass or less, more preferably 7% by mass or less, and even more preferably 5% by mass or less. More specifically, the content of component B is preferably 0.05% by mass or more and 10% by mass or less, more preferably 0.1% by mass or more and 7% by mass or less, and 0.15% by mass or more and 5% by mass or less. is more preferred.
本開示の研磨液組成物中の成分Ａと成分Ｂとの質量比Ａ／Ｂ（成分Ａの含有量／成分Ｂの含有量）は、研磨速度を維持しつつ表面粗さの悪化を抑制する観点から、１以上が好ましく、１．５以上がより好ましく、２以上が更に好ましく、そして、同様の観点から、１００以下が好ましく、９０以下がより好ましく、８０以下が更に好ましい。より具体的には、質量比Ａ／Ｂは、１以上１００以下が好ましく、１．５以上９０以下がより好ましく、２以上８０以下が更に好ましい。 The mass ratio A/B (content of component A/content of component B) of component A and component B in the polishing composition of the present disclosure suppresses deterioration of surface roughness while maintaining the polishing rate. From a viewpoint, it is preferably 1 or more, more preferably 1.5 or more, still more preferably 2 or more, and from the same viewpoint, it is preferably 100 or less, more preferably 90 or less, and even more preferably 80 or less. More specifically, the mass ratio A/B is preferably 1 or more and 100 or less, more preferably 1.5 or more and 90 or less, and even more preferably 2 or more and 80 or less.
［リン酸塩（成分Ｃ）］
本開示の研磨液組成物は、研磨速度を維持しつつ表面粗さの悪化を抑制する観点から、リン酸塩（以下、「成分Ｃ」ともいう）を含む。成分Ｃは、研磨速度を維持しつつ表面粗さの悪化を抑制する観点から、ｐＨ２の水性媒体中で完全には遊離せず（完全にはＨ3ＰＯ4（ａｑ）とならず）、塩の形態（イオン）で存在するリン酸塩が好ましい。一又は複数の実施形態において、ｐＨ２の水性媒体中で塩の形態（イオン）で存在する成分Ｃの割合は、ｐＨ２の水性媒体中に添加された成分Ｃの全量（１００質量％）に対し、好ましくは１０質量％以上、より好ましくは２０質量％以上、更に好ましくは３０質量％以上である。例えば、成分Ｃがリン酸二水素ナトリウムの場合、ｐＨ２の水性媒体に添加した成分Ｃの４３質量％が塩の形態（イオン）で存在する。成分Ｃがピロリン酸二水素二ナトリウムの場合、ｐＨ２の水性媒体に添加した成分Ｃの９６質量％が塩の形態（イオン）で存在する。
[Phosphate (Component C)]
The polishing composition of the present disclosure contains a phosphate (hereinafter also referred to as “component C”) from the viewpoint of suppressing deterioration of surface roughness while maintaining polishing rate. From the viewpoint of suppressing deterioration of surface roughness while maintaining the polishing rate, component C is not completely liberated (incompletely converted to H 3 PO 4 (aq)) in an aqueous medium of pH 2, and is a salt. Phosphate present in the form (ion) of is preferred. In one or more embodiments, the proportion of component C present in the form of a salt (ion) in the pH 2 aqueous medium is It is preferably 10% by mass or more, more preferably 20% by mass or more, and still more preferably 30% by mass or more. For example, when Component C is sodium dihydrogen phosphate, 43% by weight of Component C added to the pH 2 aqueous medium is present in the salt form (ion). When Component C is disodium dihydrogen pyrophosphate, 96% by weight of Component C added to the pH 2 aqueous medium is present in the salt form (ion).
成分Ｃのリン酸塩としては、研磨速度を維持しつつ表面粗さの悪化を抑制する観点から、アルカリ金属リン酸塩が好ましく、アルカリ金属リン酸水素塩がより好ましい。アルカリ金属リン酸水素塩の具体例としては、リン酸水素二カリウム、リン酸水素二ナトリウム、リン酸水素二アンモニウム、リン酸二水素カリウム、リン酸二水素ナトリウム、リン酸二水素アンモニウム、ピロリン酸二水素二ナトリウム（酸性ピロリン酸ソーダ）、ピロリン酸ナトリウム、ヘキサメタリン酸ナトリウム、トリポリリン酸ナトリウム等が挙げられる。成分Ｃは、１種単独で用いてもよいし、２種以上を併用してもよい。 The phosphate of component C is preferably an alkali metal phosphate, more preferably an alkali metal hydrogen phosphate, from the viewpoint of suppressing deterioration of surface roughness while maintaining the polishing rate. Specific examples of alkali metal hydrogen phosphate include dipotassium hydrogen phosphate, disodium hydrogen phosphate, diammonium hydrogen phosphate, potassium dihydrogen phosphate, sodium dihydrogen phosphate, ammonium dihydrogen phosphate, pyrophosphate Disodium dihydrogen (acidic sodium pyrophosphate), sodium pyrophosphate, sodium hexametaphosphate, sodium tripolyphosphate and the like. Component C may be used singly or in combination of two or more.
本開示の研磨液組成物中の成分Ｃの含有量は、研磨速度を維持しつつ表面粗さの悪化を抑制する観点から、０．３質量％以上が好ましく、０．５質量％以上がより好ましく、１質量％以上が更に好ましく、そして、同様の観点から、１０質量％以下が好ましく、７質量％以下がより好ましく、５質量％以下が更に好ましい。より具体的には、成分Ｃの含有量は、０．３質量％以上１０質量％以下が好ましく、０．５質量％以上７質量％以下がより好ましく、１質量％以上５質量％以下が更に好ましい。成分Ｃが２種以上の組合せである場合、成分Ｃの含有量は、それらの合計含有量をいう。 The content of component C in the polishing composition of the present disclosure is preferably 0.3% by mass or more, more preferably 0.5% by mass or more, from the viewpoint of suppressing deterioration of surface roughness while maintaining the polishing rate. It is preferably 1% by mass or more, more preferably 1% by mass or less, and from the same viewpoint, preferably 10% by mass or less, more preferably 7% by mass or less, and even more preferably 5% by mass or less. More specifically, the content of component C is preferably 0.3% by mass or more and 10% by mass or less, more preferably 0.5% by mass or more and 7% by mass or less, and further 1% by mass or more and 5% by mass or less. preferable. When component C is a combination of two or more, the content of component C refers to their total content.
本開示の研磨液組成物中の成分Ａと成分Ｃとの質量比Ａ／Ｃ（成分Ａの含有量／成分Ｃの含有量）は、研磨速度を維持しつつ表面粗さの悪化を抑制する観点から、０．５以上が好ましく、１以上がより好ましく、１．５以上が更に好ましく、そして、同様の観点から、２６以下が好ましく、２０以下がより好ましく、１６以下が更に好ましい。より具体的には質量比Ａ／Ｃは、０．５以上２６以下が好ましく、１以上２０以下がより好ましく、１．５以上１６以下が更に好ましい。 The mass ratio A/C (content of component A/content of component C) of component A and component C in the polishing composition of the present disclosure suppresses deterioration of surface roughness while maintaining the polishing rate. From a viewpoint, it is preferably 0.5 or more, more preferably 1 or more, further preferably 1.5 or more, and from the same viewpoint, it is preferably 26 or less, more preferably 20 or less, and still more preferably 16 or less. More specifically, the mass ratio A/C is preferably 0.5 or more and 26 or less, more preferably 1 or more and 20 or less, and even more preferably 1.5 or more and 16 or less.
本開示の研磨液組成物中の成分Ｂと成分Ｃとの質量比Ｂ／Ｃ（成分Ｂの含有量／成分Ｃの含有量）は、研磨速度を維持しつつ表面粗さの悪化を抑制する観点から、０．０１以上が好ましく、０．０３以上がより好ましく、０．０５以上が更に好ましく、そして、同様の観点から、５０以下が好ましく、３０以下がより好ましく、２０以下が更に好ましく、１０以下が更に好ましい。より具体的には質量比Ｂ／Ｃは、０．０１以上５０以下が好ましく、０．０１以上３０以下がより好ましく、０．０３以上２０以下が更に好ましく、０．０５以上１０以下が更に好ましい。 The mass ratio B/C (content of component B/content of component C) of component B and component C in the polishing composition of the present disclosure suppresses deterioration of surface roughness while maintaining the polishing rate. From the viewpoint, it is preferably 0.01 or more, more preferably 0.03 or more, and further preferably 0.05 or more, and from the same viewpoint, it is preferably 50 or less, more preferably 30 or less, and further preferably 20 or less, 10 or less is more preferable. More specifically, the mass ratio B/C is preferably 0.01 or more and 50 or less, more preferably 0.01 or more and 30 or less, still more preferably 0.03 or more and 20 or less, and even more preferably 0.05 or more and 10 or less. .
［水］
本開示の研磨液組成物は、媒体として水を含有する。水としては、例えば、蒸留水、イオン交換水、純水、超純水等が挙げられる。本開示の研磨液組成物中の水の含有量は、成分Ａ、成分Ｂ、成分Ｃ及び後述する任意成分を除いた残余とすることができる。具体的には、本開示の研磨液組成物中の水の含有量は、研磨液組成物の取扱いがさらに容易になるため、５５質量％以上が好ましく、７０質量％以上がより好ましく、８０質量％以上が更に好ましく、８５質量％以上が更に好ましく、そして、研磨速度向上の観点から、９９質量％以下が好ましく、９８質量％以下がより好ましく、９７質量％以下が更に好ましい。したがって、水の含有量は、５５質量％以上９９質量％以下が好ましく、７０質量％以上９８質量％以下がより好ましく、８０質量％以上９７質量％以下が更に好ましく、８５質量％以上９７質量％以下が更に好ましい。
[water]
The polishing composition of the present disclosure contains water as a medium. Examples of water include distilled water, ion-exchanged water, pure water, and ultrapure water. The content of water in the polishing composition of the present disclosure can be the balance after removing component A, component B, component C, and optional components described later. Specifically, the content of water in the polishing composition of the present disclosure is preferably 55% by mass or more, more preferably 70% by mass or more, and more preferably 80% by mass, in order to facilitate handling of the polishing composition. % or more, more preferably 85 mass % or more, and from the viewpoint of improving the polishing rate, it is preferably 99 mass % or less, more preferably 98 mass % or less, and even more preferably 97 mass % or less. Therefore, the water content is preferably 55% by mass or more and 99% by mass or less, more preferably 70% by mass or more and 98% by mass or less, still more preferably 80% by mass or more and 97% by mass or less, and 85% by mass or more and 97% by mass or less. More preferred are:
［その他の成分］
本開示の研磨液組成物は、一又は複数の実施形態において、必要に応じてさらにその他の成分を含有することができる。その他の成分としては、例えば、成分Ｂ及びＣ以外の酸又はその塩、酸化剤、複素環芳香族化合物、脂肪族アミン化合物、脂環式アミン化合物、水溶性高分子、増粘剤、分散剤、防錆剤、塩基性物質、界面活性剤、可溶化剤等が挙げられる。本開示の研磨液組成物中の前記その他の成分の含有量は、０質量％以上が好ましく、０質量％超がより好ましく、０．１質量％以上が更に好ましく、そして、１０質量％以下が好ましく、５質量％以下がより好ましい。より具体的には、その他の成分の含有量は、０質量％以上１０質量％以下が好ましく、０質量％超１０質量％以下がより好ましく、０．１質量％以上５質量％以下が更に好ましい。
[Other ingredients]
The polishing composition of the present disclosure can further contain other components as necessary in one or more embodiments. Other components include, for example, acids other than components B and C or salts thereof, oxidizing agents, heterocyclic aromatic compounds, aliphatic amine compounds, alicyclic amine compounds, water-soluble polymers, thickeners, dispersants. , rust inhibitors, basic substances, surfactants, solubilizers and the like. The content of the other components in the polishing composition of the present disclosure is preferably 0% by mass or more, more preferably more than 0% by mass, still more preferably 0.1% by mass or more, and 10% by mass or less. Preferably, 5% by mass or less is more preferable. More specifically, the content of other components is preferably 0% by mass or more and 10% by mass or less, more preferably 0% by mass or more and 10% by mass or less, and even more preferably 0.1% by mass or more and 5% by mass or less. .
本開示の研磨液組成物は、一又は複数の実施形態において、リン酸エステル化合物を含んでもよいし、含まなくてもよい。
また、本開示の研磨液組成物は、一又は複数の実施形態において、成分Ａ、成分Ｂ、成分Ｃ及び水からなる研磨液組成物であってもよい。
In one or more embodiments, the polishing composition of the present disclosure may or may not contain a phosphate ester compound.
Moreover, in one or more embodiments, the polishing composition of the present disclosure may be a polishing composition comprising component A, component B, component C, and water.
［研磨液組成物のｐＨ］
本開示の研磨液組成物のｐＨは、研磨速度を維持しつつ表面粗さの悪化を抑制する観点から、０．９以上が好ましく、１以上がより好ましく、１．５以上が更に好ましく、そして、同様の観点から、６以下が好ましく、５以下がより好ましく、４．５以下が更に好ましい。より具体的には、本開示の研磨液組成物のｐＨは、０．９以上６以下が好ましく、１以上５以下がより好ましく、１．５以上４．５以下が更に好ましい。ｐＨは、上述した成分Ｂ及び成分Ｃや公知のｐＨ調整剤等を用いて調整することができる。本開示において、上記ｐＨは、２５℃における研磨液組成物のｐＨであり、ｐＨメータを用いて測定でき、例えば、ｐＨメータの電極を研磨液組成物へ浸漬して２分後の数値とすることができる。
[pH of polishing composition]
The pH of the polishing composition of the present disclosure is preferably 0.9 or higher, more preferably 1 or higher, and even more preferably 1.5 or higher, from the viewpoint of suppressing deterioration of surface roughness while maintaining the polishing rate. , from the same viewpoint, it is preferably 6 or less, more preferably 5 or less, and even more preferably 4.5 or less. More specifically, the pH of the polishing composition of the present disclosure is preferably 0.9 or more and 6 or less, more preferably 1 or more and 5 or less, and even more preferably 1.5 or more and 4.5 or less. The pH can be adjusted using the components B and C described above, a known pH adjuster, and the like. In the present disclosure, the above pH is the pH of the polishing composition at 25° C., which can be measured using a pH meter. For example, the pH is the value after 2 minutes after the electrode of the pH meter is immersed in the polishing composition. be able to.
［研磨液組成物の製造方法］
本開示の研磨液組成物は、一又は複数の実施形態において、成分Ａ、成分Ｂ、成分Ｃ及び水を配合してなる、ガラスハードディスク基板用研磨液組成物とすることができる。例えば、本開示の研磨液組成物は、成分Ａ、成分Ｂ、成分Ｃ及び水と、さらに所望により、その他の成分とを公知の方法で配合することにより製造できる。すなわち、本開示は、その他の態様において、少なくとも成分Ａ、成分Ｂ、成分Ｃ及び水を配合する工程を含む、研磨液組成物の製造方法（以下、「本開示の研磨液組成物の製造方法」ともいう）に関する。本開示において「配合する」とは、成分Ａ、成分Ｂ、成分Ｃ及び水、並びに必要に応じてその他の成分を同時に又は任意の順に混合することを含む。成分Ａの砥粒は、濃縮されたスラリーの状態で混合されてもよいし、水等で希釈してから混合されてもよい。成分Ａが複数種類の砥粒からなる場合、複数種類の砥粒は、同時に又はそれぞれ別々に配合できる。成分Ｃが複数種類のリン酸塩からなる場合、複数種類のリン酸塩は、同時に又はそれぞれ別々に配合できる。前記配合は、例えば、ホモミキサー、ホモジナイザー、超音波分散機及び湿式ボールミル等の混合器を用いて行うことができる。本開示の研磨液組成物の製造方法における各成分の好ましい配合量は、上述した本開示の研磨液組成物中の各成分の好ましい含有量と同じとすることができる。
[Method for producing polishing composition]
In one or more embodiments, the polishing composition of the present disclosure can be a polishing composition for glass hard disk substrates, which is obtained by blending component A, component B, component C, and water. For example, the polishing composition of the present disclosure can be produced by blending Component A, Component B, Component C, water, and, if desired, other components by a known method. That is, the present disclosure provides, in another aspect, a method for producing a polishing composition (hereinafter referred to as "method for producing a polishing composition of the present disclosure"), which includes a step of blending at least component A, component B, component C, and water. ”). In the present disclosure, "blending" includes mixing component A, component B, component C and water, and optionally other components simultaneously or in any order. The abrasive grains of component A may be mixed in a concentrated slurry state, or may be diluted with water or the like before being mixed. When component A consists of multiple types of abrasive grains, the multiple types of abrasive grains can be blended together or separately. When component C consists of multiple types of phosphates, the multiple types of phosphates can be blended simultaneously or separately. The blending can be performed using a mixer such as a homomixer, a homogenizer, an ultrasonic disperser, and a wet ball mill. The preferable compounding amount of each component in the method for producing the polishing composition of the present disclosure can be the same as the preferable content of each component in the polishing composition of the present disclosure described above.
本開示において「研磨液組成物中の各成分の含有量」とは、使用時、すなわち、研磨液組成物の研磨への使用を開始する時点における前記各成分の含有量をいう。本開示の研磨液組成物は、その保存安定性が損なわれない範囲で濃縮された状態で保存及び供給されてもよい。この場合、製造及び輸送コストを更に低くできる点で好ましい。本開示の研磨液組成物の濃縮物は、使用時に、必要に応じて前述の水で適宜希釈して使用すればよい。希釈倍率は、希釈した後に上述した各成分の含有量（使用時）を確保できれば特に限定されるものではなく、例えば、１０～１００倍とすることができる。 In the present disclosure, "the content of each component in the polishing composition" refers to the content of each component at the time of use, that is, when the polishing composition is started to be used for polishing. The polishing composition of the present disclosure may be stored and supplied in a concentrated state as long as its storage stability is not impaired. In this case, it is preferable in that manufacturing and transportation costs can be further reduced. The concentrate of the polishing composition of the present disclosure may be used by diluting it with the above-mentioned water as necessary at the time of use. The dilution ratio is not particularly limited as long as the content of each component described above (at the time of use) can be ensured after dilution, and can be, for example, 10 to 100 times.
［研磨液キット］
本開示は、その他の態様において、本開示の研磨液組成物を製造するためのキット（以下、「本開示の研磨液キット」ともいう）に関する。本開示の研磨液キットの一実施形態としては、例えば、成分Ａ及び水を含む砥粒分散液と、成分Ｂ及び成分Ｃを含む添加剤水溶液と、を相互に混合されない状態で含む、研磨液キット（２液型研磨液組成物）が挙げられる。前記砥粒分散液と前記添加剤水溶液とは、使用時に混合され、必要に応じて水を用いて希釈される。前記砥粒分散液及び前記添加剤水溶液にはそれぞれ必要に応じて、上述したその他の成分をさらに含有させることができる。本開示の研磨液キットによれば、研磨速度を維持しつつ、洗浄後の表面粗さの悪化を抑制できる研磨液組成物が得られうる。
[Polishing liquid kit]
In another aspect, the present disclosure relates to a kit for producing the polishing composition of the present disclosure (hereinafter also referred to as "polishing liquid kit of the present disclosure"). As an embodiment of the polishing liquid kit of the present disclosure, for example, a polishing liquid containing an abrasive dispersion containing component A and water and an additive aqueous solution containing component B and component C in a state in which they are not mixed with each other. A kit (two-component polishing liquid composition) may be mentioned. The abrasive dispersion and the additive aqueous solution are mixed at the time of use and diluted with water as necessary. The abrasive dispersion and the additive aqueous solution may further contain the above-described other components, if necessary. According to the polishing liquid kit of the present disclosure, it is possible to obtain a polishing liquid composition that can suppress deterioration of surface roughness after cleaning while maintaining the polishing rate.
［被研磨ガラス基板］
本開示の研磨液組成物を用いて研磨される被研磨ガラス基板は、一又は複数の実施形態において、ガラスハードディスク基板の製造工程で使用されるガラス基板である。前記ガラス基板の材質としては、例えば、石英ガラス、ソーダライムガラス、アルミノシリケートガラス、ボロシリケートガラス、アルミノボロシリケートガラス、無アルカリガラス、結晶化ガラス等が挙げられる。本開示の研磨液組成物は、一又は複数の実施形態において、アルミノシリケートガラス基板やアルミノボロシリケートガラス基板の研磨に好適に用いられる。本開示の被研磨ガラス基板は、一又は複数の実施形態において、水平磁気記録用基板、垂直磁気記録用基板、熱アシスト記録（ＨＡＭＲ）用基板のいずれにも用いることができる。
[Glass substrate to be polished]
A glass substrate to be polished that is polished using the polishing composition of the present disclosure is, in one or more embodiments, a glass substrate used in a process for manufacturing a glass hard disk substrate. Examples of the material of the glass substrate include quartz glass, soda lime glass, aluminosilicate glass, borosilicate glass, aluminoborosilicate glass, alkali-free glass, and crystallized glass. In one or more embodiments, the polishing composition of the present disclosure is suitably used for polishing an aluminosilicate glass substrate or an aluminoborosilicate glass substrate. In one or more embodiments, the polished glass substrate of the present disclosure can be used as a substrate for longitudinal magnetic recording, a substrate for perpendicular magnetic recording, or a substrate for heat assisted recording (HAMR).
被研磨ガラス基板の形状としては、例えば、ディスク状、プレート状、スラブ状、プリズム状等の平面部を有する形状や、レンズ等の曲面部を有する形状が挙げられる。中でも、ディスク状の被研磨ガラス基板が適している。ディスク状の被研磨ガラス基板の場合、その外径は例えば２ｍｍ以上１００ｍｍ以下程度であり、その厚みは例えば０．４ｍｍ以上２ｍｍ以下程度である。 The shape of the glass substrate to be polished includes, for example, a shape having a flat portion such as a disk shape, a plate shape, a slab shape and a prism shape, and a shape having a curved surface portion such as a lens. Among them, a disk-shaped glass substrate to be polished is suitable. In the case of a disk-shaped glass substrate to be polished, its outer diameter is, for example, about 2 mm to 100 mm, and its thickness is, for example, about 0.4 mm to 2 mm.
［ガラスハードディスク基板の製造方法］
一般に、ガラスハードディスク基板は、溶融ガラスの型枠プレス又はシートガラスから切り出す方法によってガラス基材を得る工程から、形状加工工程、端面研磨工程、粗研削工程、精研削工程、粗研磨工程、仕上げ研磨工程、化学強化工程を経て製造される。化学強化工程は仕上げ研磨工程の前に施しても良い。また各工程の間には洗浄工程が含まれることがある。研磨工程後のガラスハードディスク基板は、磁性膜の形成を含む記録部形成工程を経ることで磁気ディスク化されたガラスハードディスク基板となる。本開示の研磨液組成物は、仕上げ研磨工程における研磨（仕上げ研磨）に使用されることが好ましい。
[Method for manufacturing glass hard disk substrate]
In general, a glass hard disk substrate is produced by a process of obtaining a glass base material by mold pressing of molten glass or a method of cutting from sheet glass, followed by a shape processing process, an edge polishing process, a rough grinding process, a fine grinding process, a rough polishing process, and a finish polishing process. Manufactured through a process and a chemical strengthening process. The chemical strengthening process may be performed before the final polishing process. Also, a washing step may be included between each step. After the polishing step, the glass hard disk substrate becomes a glass hard disk substrate made into a magnetic disk through a recording portion forming step including the formation of a magnetic film. The polishing composition of the present disclosure is preferably used for polishing (finish polishing) in the final polishing step.
したがって、本開示は、その他の態様において、本開示の研磨液組成物を用いて被研磨ガラス基板を研磨する工程（以下、「本開示の研磨液組成物を用いた研磨工程」ともいう）を含む、ガラスハードディスク基板の製造方法（以下、「本開示の基板製造方法」ともいう）に関する。本開示の基板製造方法によれば、本開示における研磨液組成物を用いることで、高品質の磁気ディスク基板を高収率で、生産性よく製造できるという効果が奏されうる。 Therefore, in another aspect, the present disclosure provides a step of polishing a glass substrate to be polished using the polishing composition of the present disclosure (hereinafter also referred to as “polishing step using the polishing composition of the present disclosure”). (hereinafter also referred to as "substrate manufacturing method of the present disclosure"). According to the substrate manufacturing method of the present disclosure, by using the polishing liquid composition of the present disclosure, it is possible to produce high-quality magnetic disk substrates with high yield and high productivity.
（研磨工程）
本開示の研磨液組成物を用いた研磨工程は、一又は複数の実施形態において、被研磨ガラス基板の研磨対象面に本開示の研磨液組成物を供給し、前記研磨対象面に研磨パッドを接触させ、所定の圧力（荷重）をかけながら、研磨パッド及び被研磨基板の少なくとも一方を動かして研磨する工程である。また、本開示の研磨液組成物を用いた研磨工程は、その他の一又は複数の実施形態において、不織布状の有機高分子系研磨布等の研磨パッドを貼り付けた定盤で被研磨基板を挟み込み、本開示の研磨液組成物を研磨機に供給しながら、定盤や被研磨基板を動かして被研磨基板を研磨する工程である。
(polishing process)
In one or more embodiments, the polishing step using the polishing composition of the present disclosure comprises supplying the polishing composition of the present disclosure to a surface to be polished of a glass substrate to be polished, and applying a polishing pad to the surface to be polished. This is a step of polishing by moving at least one of the polishing pad and the substrate to be polished while bringing them into contact and applying a predetermined pressure (load). In addition, in one or more embodiments, the polishing step using the polishing composition of the present disclosure includes polishing a substrate to be polished on a surface plate to which a polishing pad such as a non-woven organic polymer polishing cloth is attached. It is a step of polishing the substrate to be polished by moving the surface plate and the substrate to be polished while sandwiching and supplying the polishing liquid composition of the present disclosure to the polishing machine.
被研磨基板の研磨工程が多段階で行われる場合は、本開示の研磨液組成物を用いた研磨工程は２段階目以降に行われるのが好ましく、最終研磨工程又は仕上げ研磨工程で行われるのがより好ましい。その際、前工程の研磨材や研磨液組成物の混入を避けるために、それぞれ別の研磨機を使用してもよく、またそれぞれ別の研磨機を使用した場合では、研磨工程毎に被研磨基板を洗浄することが好ましい。さらに、使用した研磨液を再利用する循環研磨においても、本開示の研磨液組成物は使用できる。研磨機としては、特に限定されず、基板研磨用の公知の研磨機が使用できる。 When the polishing process of the substrate to be polished is performed in multiple stages, the polishing process using the polishing composition of the present disclosure is preferably performed in the second stage or later, and is performed in the final polishing process or the finish polishing process. is more preferred. In this case, separate polishing machines may be used to avoid contamination of the polishing material and the polishing liquid composition in the previous step. It is preferred to wash the substrate. Furthermore, the polishing liquid composition of the present disclosure can also be used in circulatory polishing in which the used polishing liquid is reused. The polishing machine is not particularly limited, and a known polishing machine for polishing substrates can be used.
本開示の研磨液組成物を用いた研磨工程で使用される研磨パッドとしては、特に制限はなく、例えば、スエードタイプ、不織布タイプ、ポリウレタン独立発泡タイプ、又はこれらを積層した二層タイプ等の研磨パッドを使用することができ、研磨速度の観点から、スエードタイプの研磨パッドが好ましい。 The polishing pad used in the polishing step using the polishing composition of the present disclosure is not particularly limited, and examples include suede type, nonwoven fabric type, polyurethane closed foam type, and two-layer type polishing in which these are laminated. A pad can be used, and from the viewpoint of polishing speed, a suede type polishing pad is preferred.
研磨パッドの表面部材の平均開孔径は、研磨速度向上及びパッド寿命の観点から、５０μｍ以下が好ましく、４５μｍ以下がより好ましく、４０μｍ以下が更に好ましく、３５μｍ以下が更に好ましく、そして、パッドの研磨液保持性の観点から、０．０１μｍ以上が好ましく、０．１μｍ以上がより好ましく、１μｍ以上が更に好ましく、１０μｍ以上が更に好ましい。より具体的には、研磨パッドの表面部材の平均開孔径は、０．０１μｍ以上５０μｍ以下が好ましく、０．１μｍ以上４５μｍ以下がより好ましく、１μｍ以上４０μｍ以下が更に好ましく、１０μｍ以上３５μｍ以下が更に好ましい。研磨パッドの開孔径の最大値は、研磨速度維持の観点から、１００μｍ以下が好ましく、７０μｍ以下がより好ましく、６０μｍ以下が更に好ましく、５０μｍ以下が更に好ましい。 The average pore diameter of the surface member of the polishing pad is preferably 50 μm or less, more preferably 45 μm or less, still more preferably 40 μm or less, and even more preferably 35 μm or less, from the viewpoint of improving the polishing speed and pad life. From the viewpoint of retention, it is preferably 0.01 µm or more, more preferably 0.1 µm or more, still more preferably 1 µm or more, and even more preferably 10 µm or more. More specifically, the average pore size of the surface member of the polishing pad is preferably 0.01 μm or more and 50 μm or less, more preferably 0.1 μm or more and 45 μm or less, still more preferably 1 μm or more and 40 μm or less, and further preferably 10 μm or more and 35 μm or less. preferable. From the viewpoint of maintaining the polishing rate, the maximum pore size of the polishing pad is preferably 100 μm or less, more preferably 70 μm or less, even more preferably 60 μm or less, and even more preferably 50 μm or less.
本開示の研磨液組成物を用いた研磨工程における研磨荷重は、研磨速度向上の観点から、３ｋＰａ以上が好ましく、４ｋＰａ以上がより好ましく、そして、研磨中に研磨機に振動が発生しないように安定に研磨できる観点から、４０ｋＰａ以下が好ましく、１５ｋＰａ以下が更により好ましい。より具体的には、研磨荷重は、３ｋＰａ以上４０ｋＰａ以下が好ましく、４ｋＰａ以上１５ｋＰａ以下がより好ましい。本開示において研磨荷重とは、研磨時に被研磨基板の研磨面に加えられる定盤の圧力をいう。また、研磨荷重の調整は、定盤及び被研磨基板のうち少なくとも一方に空気圧や重りを負荷することにより行うことができる。 The polishing load in the polishing step using the polishing composition of the present disclosure is preferably 3 kPa or more, more preferably 4 kPa or more, from the viewpoint of improving the polishing speed, and is stable so that the polishing machine does not vibrate during polishing. 40 kPa or less is preferable, and 15 kPa or less is even more preferable from the viewpoint of being able to polish to a high degree. More specifically, the polishing load is preferably 3 kPa or more and 40 kPa or less, more preferably 4 kPa or more and 15 kPa or less. In the present disclosure, the polishing load refers to the pressure of the platen applied to the polishing surface of the substrate to be polished during polishing. Also, the polishing load can be adjusted by applying air pressure or a weight to at least one of the surface plate and the substrate to be polished.
本開示の研磨液組成物を用いた研磨工程における、本開示の研磨液組成物の供給速度は、コスト低減及び研磨速度向上の観点から、被研磨基板１ｃｍ2あたり、０．０１ｍＬ／分以上１ｍＬ／分以下が好ましく、０．０２５ｍＬ／分以上０．６ｍＬ／分以下がより好ましく、０．０５ｍＬ／分以上０．４ｍＬ／分以下が更に好ましく、０．１ｍＬ／分以上０．４ｍＬ／分以下が更により好ましい。また循環研磨をする場合であれば研磨液組成物を再利用できるので供給流量は上記記載の流量よりも多くなってもよい。 In the polishing step using the polishing composition of the present disclosure, the supply rate of the polishing composition of the present disclosure is 0.01 mL/min or more and 1 mL per 1 cm 2 of the substrate to be polished from the viewpoint of cost reduction and polishing rate improvement. / min or less, more preferably 0.025 mL / min or more and 0.6 mL / min or less, still more preferably 0.05 mL / min or more and 0.4 mL / min or less, 0.1 mL / min or more and 0.4 mL / min or less is even more preferred. In the case of circulation polishing, the supply flow rate may be higher than the flow rate described above because the polishing liquid composition can be reused.
本開示の研磨液組成物を研磨機へ供給する方法としては、例えばポンプ等を用いて連続的に供給を行う方法が挙げられる。研磨液組成物を研磨機へ供給する際は、全ての成分を含んだ１液で供給する方法の他、研磨液組成物の安定性等を考慮して、複数の配合用成分液に分け、２液以上で供給することもできる。後者の場合、例えば供給配管中又は被研磨基板上で、上記複数の配合用成分液が混合され、本開示の研磨液組成物となる。 Examples of the method of supplying the polishing composition of the present disclosure to the polishing machine include a method of continuous supply using a pump or the like. When supplying the polishing composition to the polishing machine, in addition to the method of supplying a single solution containing all the components, in consideration of the stability of the polishing composition, etc. Two or more liquids can be supplied. In the latter case, for example, in the supply pipe or on the substrate to be polished, the plurality of compounding component liquids are mixed to form the polishing liquid composition of the present disclosure.
（洗浄工程）
本開示の基板製造方法は、一又は複数の実施形態において、本開示の研磨液組成物を用いた研磨が施されたガラス基板（被洗浄基板）を、上述の洗浄剤組成物を用いて洗浄する工程（以下、「洗浄工程」ともいう）を含む。洗浄工程における被洗浄基板には、本開示の研磨液組成物を使用した研磨工程の直後のガラス基板や、研磨工程後に乾燥を防ぐための水等への浸漬工程、予備洗浄として水洗浄工程や酸洗浄工程等を経たガラス基板が含まれる。この洗浄工程は、一又は複数の実施形態において、（ａ）被洗浄基板を洗浄剤組成物に浸漬すること、及び／又は、（ｂ）洗浄剤組成物を射出して被洗浄基板の表面上に洗浄剤組成物を供給することにより行われる。
(Washing process)
In one or more embodiments of the substrate manufacturing method of the present disclosure, a glass substrate (substrate to be cleaned) that has been polished using the polishing composition of the present disclosure is cleaned using the cleaning agent composition described above. (hereinafter also referred to as “washing step”). The substrate to be cleaned in the cleaning step includes a glass substrate immediately after the polishing step using the polishing composition of the present disclosure, a step of immersion in water or the like to prevent drying after the polishing step, a water washing step as a preliminary cleaning, and a A glass substrate that has undergone an acid cleaning process or the like is included. In one or more embodiments, the cleaning step includes (a) immersing the substrate to be cleaned in the cleaning composition and/or (b) injecting the cleaning composition onto the surface of the substrate to be cleaned. by supplying the cleaning composition to the
前記方法（ａ）において、被洗浄基板の洗浄剤組成物への浸漬条件としては、特に制限されなくてもよい。例えば、洗浄剤組成物の温度は、安全性及び操業性の観点から、２０℃以上１００℃以下が挙げられ、浸漬時間は、洗浄剤組成物による洗浄性と生産効率の観点から、１０秒以上６０分以内が挙げられる。残留物の除去性及び残留物の分散性を高める観点から、洗浄剤組成物には超音波振動が付与されていると好ましい。超音波の周波数としては、例えば、２０ｋＨｚ以上２０００ｋＨｚ以下が挙げられる。 In the method (a), conditions for immersing the substrate to be cleaned in the cleaning composition are not particularly limited. For example, the temperature of the cleaning composition is 20° C. or higher and 100° C. or lower from the viewpoint of safety and workability, and the immersion time is 10 seconds or more from the viewpoint of cleaning performance and production efficiency with the cleaning composition. within 60 minutes. From the viewpoint of enhancing the removability of the residue and the dispersibility of the residue, it is preferable that the cleaning composition is subjected to ultrasonic vibration. The frequency of ultrasonic waves is, for example, 20 kHz or more and 2000 kHz or less.
前記方法（ｂ）では、残留物の洗浄性や油分の溶解性を促進させる観点から、超音波振動が与えられている洗浄剤組成物を射出して、被洗浄基板の表面に洗浄剤組成物を接触させて当該表面を洗浄するか、又は、洗浄剤組成物を被洗浄基板の表面上に射出により供給し、洗浄剤組成物が供給された当該表面を洗浄用ブラシでこすることにより洗浄することが好ましい。さらには、超音波振動が与えられている洗浄剤組成物を射出により洗浄対象の表面に供給し、かつ、洗浄剤組成物が供給された当該表面を洗浄用ブラシでこすることにより洗浄することが好ましい。 In the method (b), from the viewpoint of promoting the detergency of the residue and the solubility of the oil, the cleaning composition to which ultrasonic vibration is applied is injected to the surface of the substrate to be cleaned. or by spraying the cleaning composition onto the surface of the substrate to be cleaned and rubbing the surface supplied with the cleaning composition with a cleaning brush. preferably. Furthermore, cleaning is performed by supplying a cleaning composition to which ultrasonic vibration is applied to the surface to be cleaned by injection, and rubbing the surface to which the cleaning composition has been supplied with a cleaning brush. is preferred.
洗浄剤組成物を被洗浄基板の表面上に供給する手段としては、スプレーノズル等の公知の手段を用いることができる。洗浄用ブラシとしては、例えば、ナイロンブラシやＰＶＡ（ポリビニルアルコール）スポンジブラシ等の公知のものが挙げられる。超音波の周波数としては、前記方法（ａ）で好ましく採用される値と同様であればよい。 As means for supplying the cleaning composition onto the surface of the substrate to be cleaned, known means such as a spray nozzle can be used. Examples of the cleaning brush include known brushes such as nylon brushes and PVA (polyvinyl alcohol) sponge brushes. The frequency of the ultrasonic wave may be the same as the value preferably employed in the method (a).
洗浄工程では、前記方法（ａ）及び／又は前記方法（ｂ）に加えて、揺動洗浄、スピンナー等の回転を利用した洗浄、パドル洗浄等の公知の洗浄を用いる工程を１つ以上含んでもよい。 In the cleaning step, in addition to the method (a) and/or the method (b), one or more steps using known cleaning such as rocking cleaning, cleaning using rotation of a spinner or the like, and paddle cleaning may be included. good.
洗浄工程で用いる洗浄剤組成物としては、例えば、アルカリ剤、水、及び必要に応じて各種添加剤を含有するものが使用できる。アルカリ剤は、無機アルカリ剤及び有機アルカリ剤の少なくとも一方を用いることができる。無機アルカリ剤としては、例えば、アンモニア、水酸化カリウム、及び水酸化ナトリウム等が挙げられる。有機アルカリ剤としては、例えば、ヒドロキシアルキルアミン、テトラメチルアンモニウムハイドロオキサイド、及びコリンから選ばれる少なくとも１種が挙げられる。各種添加剤としては、例えば、非イオン界面活性剤、キレート剤、エーテルカルボキシレート、脂肪酸、アニオン性界面活性剤、水溶性高分子、消泡剤、アルコール類、防腐剤、酸化防止剤等が挙げられる。 As the cleaning composition used in the cleaning step, for example, one containing an alkali agent, water, and various additives as necessary can be used. At least one of an inorganic alkaline agent and an organic alkaline agent can be used as the alkaline agent. Examples of inorganic alkaline agents include ammonia, potassium hydroxide, sodium hydroxide, and the like. Examples of organic alkaline agents include at least one selected from hydroxyalkylamine, tetramethylammonium hydroxide, and choline. Examples of various additives include nonionic surfactants, chelating agents, ether carboxylates, fatty acids, anionic surfactants, water-soluble polymers, antifoaming agents, alcohols, preservatives, antioxidants, and the like. be done.
洗浄工程で用いる洗浄剤組成物のｐＨは、基板上の残留物の分散性を向上させる観点から、例えば、８以上１３以下が好ましい。上記のｐＨは、２５℃における洗浄剤組成物のｐＨであり、ｐＨメータ（東亜電波工業株式会社、ＨＭ－３０Ｇ）を用いて測定でき、例えば、電極を洗浄剤組成物へ浸漬して３分後の数値を採用できる。 The pH of the cleaning composition used in the cleaning step is preferably, for example, 8 or more and 13 or less from the viewpoint of improving the dispersibility of the residue on the substrate. The above pH is the pH of the cleaning composition at 25° C., and can be measured using a pH meter (HM-30G, Toa Denpa Kogyo Co., Ltd.). The latter numerical value can be adopted.
（磁性膜の形成工程）
本開示の基板製造方法は、一又は複数の実施形態において、被研磨ガラス基板の研磨工程及び洗浄工程後のガラス基板上に磁性膜を形成する工程、或いは、磁性膜の形成を含む記録部形成工程を有してもよい。
(Magnetic film forming process)
In one or more embodiments, the substrate manufacturing method of the present disclosure includes a step of forming a magnetic film on the glass substrate after the polishing step and the cleaning step of the glass substrate to be polished, or a step of forming a recording portion including the formation of the magnetic film. You may have a process.
［ガラス基板の研磨方法］
本開示は、その他の態様として、本開示の研磨液組成物を用いて被研磨ガラス基板を研磨することを含む、ガラス基板の研磨方法（以下、「本開示の研磨方法」ともいう）に関する。本開示の研磨方法を使用することにより、高品質の磁気ディスク基板を高収率で、生産性よく製造できるという効果が奏されうる。本開示の研磨方法における被研磨ガラス基板としては、上述のとおり、ガラスハードディスク基板の製造に使用されるものが挙げられる。具体的な研磨の方法及び条件は、上述した本開示の基板製造方法と同じ方法及び条件とすることができる。
[Glass substrate polishing method]
The present disclosure, as another aspect, relates to a method for polishing a glass substrate (hereinafter also referred to as "polishing method of the present disclosure"), which includes polishing a glass substrate to be polished using the polishing composition of the present disclosure. By using the polishing method of the present disclosure, it is possible to produce high-quality magnetic disk substrates with high yield and high productivity. Examples of the glass substrate to be polished in the polishing method of the present disclosure include those used for manufacturing glass hard disk substrates, as described above. The specific polishing method and conditions can be the same method and conditions as the substrate manufacturing method of the present disclosure described above.
本開示の研磨液組成物を用いて被研磨ガラス基板を研磨することは、一又は複数の実施形態において、本開示の研磨液組成物を被研磨基板の研磨対象面に供給し、前記研磨対象面に研磨パッドを接触させ、前記研磨パッド及び前記被研磨基板の少なくとも一方を動かして研磨することであり、或いは、不織布状の有機高分子系研磨布等の研磨パッドを貼り付けた定盤で被研磨基板を挟み込み、本開示の研磨液組成物を研磨機に供給しながら、定盤や被研磨基板を動かして被研磨基板を研磨することである。 Polishing a glass substrate to be polished using the polishing liquid composition of the present disclosure, in one or more embodiments, comprises supplying the polishing liquid composition of the present disclosure to the surface to be polished of the substrate to be polished, polishing by bringing a polishing pad into contact with the surface and moving at least one of the polishing pad and the substrate to be polished; The substrate to be polished is sandwiched, and the polishing liquid composition of the present disclosure is supplied to the polishing machine, while the surface plate and the substrate to be polished are moved to polish the substrate to be polished.
以下、実施例により本開示をさらに詳細に説明するが、これらは例示的なものであって、本開示はこれら実施例に制限されるものではない。 EXAMPLES The present disclosure will be described in more detail below with reference to examples, but these are examples and the present disclosure is not limited to these examples.
１．研磨液組成物の調製（実施例１～１０及び比較例１～７）
成分Ａ（コロイダルシリカ、平均粒径２０ｎｍ）、成分Ｂ（スルファミン酸）又は非成分Ｂ（表１に示す酸）、成分Ｃ（表１に示すリン酸塩）及びイオン交換水を、表１に記載の割合（質量％）で配合して撹拌することにより、実施例１～１０及び比較例１～７の研磨液組成物を調製した。
1. Preparation of polishing composition (Examples 1 to 10 and Comparative Examples 1 to 7)
Component A (colloidal silica, average particle size 20 nm), component B (sulfamic acid) or non-component B (acid shown in Table 1), component C (phosphate shown in Table 1) and ion-exchanged water are shown in Table 1. The polishing liquid compositions of Examples 1 to 10 and Comparative Examples 1 to 7 were prepared by blending and stirring in the stated proportions (% by mass).
表１に示す研磨液組成物の調製において、成分Ｂ、非成分Ｂ、成分Ｃには以下のものを使用した。
スルファミン酸［サンケミカル社製］（成分Ｂ）
硫酸［和光純薬工業社製］（非成分Ｂ）
リン酸［和光純薬工業社製］（非成分Ｂ）
クエン酸［磐田化学工業社製］（非成分Ｂ）
酒石酸［和光純薬工業社製］（非成分Ｂ）
酸性ピロリン酸ソーダ［ピロリン酸二水素二ナトリウム、燐化学工業社製］（成分Ｃ）
リン酸二水素カリウム［和光純薬工業社製］（成分Ｃ）
硫酸ナトリウム［和光純薬工業社製］（非成分Ｃ）
In the preparation of the polishing composition shown in Table 1, the components B, non-component B, and component C were as follows.
Sulfamic acid [manufactured by Sun Chemical Co., Ltd.] (Component B)
Sulfuric acid [manufactured by Wako Pure Chemical Industries] (non-component B)
Phosphoric acid [manufactured by Wako Pure Chemical Industries] (non-component B)
Citric acid [manufactured by Iwata Chemical Industry Co., Ltd.] (non-component B)
Tartaric acid [manufactured by Wako Pure Chemical Industries] (non-component B)
Acidic sodium pyrophosphate [disodium dihydrogen pyrophosphate, manufactured by Rin Kagaku Kogyo Co., Ltd.] (Component C)
Potassium dihydrogen phosphate [manufactured by Wako Pure Chemical Industries, Ltd.] (Component C)
Sodium sulfate [manufactured by Wako Pure Chemical Industries] (non-component C)
２．各種パラメータの測定方法
［シリカ粒子（成分Ａ）の平均粒径の測定方法］
コロイダルシリカ粒子を含む試料を、透過型電子顕微鏡「ＪＥＭ－２０００ＦＸ」（８０ｋＶ、１～５万倍、日本電子社製）により当該製造業者が添付した説明書に従って試料を観察し、ＴＥＭ（Ｔｒａｎｓｍｉｓｓｉｏｎ Ｅｌｅｃｔｒｏｎ Ｍｉｃｒｏｓｃｏｐｅ）像を写真撮影した。この写真をスキャナで画像データとしてパソコンに取り込み、解析ソフト「ＷｉｎＲＯＯＦ ｖｅｒ．３．６」（販売元：三谷商事）を用いて、個々のシリカ粒
子の円相当径を計測し、粒子径を求めた。このようにして、１０００個のシリカ粒子の粒子径を求めた後、これらの平均値を算出し、この平均値を平均粒径とした。
2. Method for measuring various parameters [Method for measuring average particle size of silica particles (component A)]
A sample containing colloidal silica particles is observed with a transmission electron microscope "JEM-2000FX" (80 kV, 10,000 to 50,000 times, manufactured by JEOL Ltd.) according to the instructions attached by the manufacturer, and a TEM (Transmission Electron) is used. Microscopic images were photographed. This photograph was scanned into a personal computer as image data, and the equivalent circle diameter of each silica particle was measured using analysis software "WinROOF ver.3.6" (sold by Mitani Shoji) to determine the particle diameter. . After obtaining the particle diameters of 1000 silica particles in this way, the average value was calculated, and this average value was defined as the average particle diameter.
［研磨液組成物のｐＨの測定方法］
研磨液組成物のｐＨは、ｐＨメータ（東亜ディーケーケー社製）を用いて２５℃にて測定し、電極を研磨液組成物へ浸漬して２分後の数値を採用した。測定結果を表１に示した。
[Method for measuring pH of polishing composition]
The pH of the polishing composition was measured at 25° C. using a pH meter (manufactured by Toa DKK Co., Ltd.), and the value 2 minutes after the electrode was immersed in the polishing composition was adopted. Table 1 shows the measurement results.
３．被研磨基板の調製
セリア砥粒を含有する研磨液組成物であらかじめ粗研磨したアルミノホウ珪酸ガラス基板を被研磨基板として用意した。基板中に含まれる構成元素は、Ｓｉの含有量は２４質量％、Ａｌの含有量は８質量％、Ｂの含有量は１質量％であった。構成元素は、ＥＳＣＡ（Ｅｌｅｃｔｒｏｎ Ｓｐｅｃｔｒｏｓｃｏｐｙ ｆｏｒ Ｃｈｅｍｉｃａｌ Ａｎａｌｙｓｉｓ）法を用い以下の測定条件で測定した。
＜ＥＳＣＡ測定条件＞
（１）試料作製
アルミノホウ珪酸ガラス基板を１ｃｍ×１ｃｍに切断し、カーボン製両面テープ上に乗せ固定した。表面のゴミ等を除くためにＡｒスパッタを加速電圧２ｋＶで６分間かけ、ＥＳＣＡ測定を実施した。
（２）測定条件
機器：アルバックファイ製 ＰＨＩ Ｑｕａｎｔｅｒａ ＳＸＭ
Ｘ線源：単色化ＡｌＫα線、１４８６．６ｅＶ、２５Ｗ、１５ｋＶ
ビーム径：１００μｍ
Ｘ線入射角：４５°
測定範囲：１０００×１０００（μｍ2）
Ｐａｓｓ ｅｎｅｒｇｙ：２８０．０(ｓｕｒｖｅｙ）、１１２．０ｅＶ(ｎａｒｒｏｗ）
Ｓｔｅｐ ｓｉｚｅ：１．００(ｓｕｒｖｅｙ)、０．２００ｅＶ(ｎａｒｒｏｗ)
測定元素：Ｃ，Ｏ，Ｍｇ，Ａｌ，Ｓｉ，Ｃａ，Ｓｒ，Ｓｎ，Ｂａ
帯電補正：Ｎｅｕｔｒａｌｉｚｅｒ及びＡｒ+照射
3. Preparation of Substrate to be Polished An aluminoborosilicate glass substrate which had been rough-polished in advance with a polishing liquid composition containing ceria abrasive grains was prepared as a substrate to be polished. As for the constituent elements contained in the substrate, the content of Si was 24% by mass, the content of Al was 8% by mass, and the content of B was 1% by mass. The constituent elements were measured under the following measurement conditions using the ESCA (Electron Spectroscopy for Chemical Analysis) method.
<ESCA measurement conditions>
(1) Sample preparation An aluminoborosilicate glass substrate was cut into a size of 1 cm x 1 cm, placed on a carbon double-sided tape and fixed. Ar sputtering was applied at an acceleration voltage of 2 kV for 6 minutes to remove dust and the like on the surface, and ESCA measurement was performed.
(2) Measurement conditions Equipment: PHI Quantera SXM manufactured by ULVAC-PHI
X-ray source: monochromatic AlKα rays, 1486.6 eV, 25 W, 15 kV
Beam diameter: 100 μm
X-ray incident angle: 45°
Measurement range: 1000×1000 (μm 2 )
Pass energy: 280.0 (survey), 112.0 eV (narrow)
Step size: 1.00 (survey), 0.200 eV (narrow)
Measurement elements: C, O, Mg, Al, Si, Ca, Sr, Sn, Ba
Charge correction: Neutralizer and Ar + irradiation
４．研磨方法
実施例１～１０及び比較例１～７の研磨液組成物を用いて、以下に示す研磨条件にて上記被研磨基板を研磨した。
4. Polishing Method Using the polishing liquid compositions of Examples 1 to 10 and Comparative Examples 1 to 7, the substrates to be polished were polished under the polishing conditions shown below.
[研磨条件]
研磨試験機：スピードファム社製「両面９Ｂ研磨機」
研磨パッド：スエードタイプ（厚さ０．９ｍｍ、平均開孔径３０μｍ、材質：発泡ウレタン）
研磨液組成物供給量：１００ｍＬ／分（被研磨基板１ｃｍ2あたりの供給速度：約０．３ｍＬ／分）
下定盤回転数：２４ｒｐｍ
研磨荷重：４．９ｋＰａ
キャリア：アラミド製、厚さ０．５ｍｍ
研磨時間：３０分
被研磨基板：アルミノボロシリケートガラス基板（外径９５ｍｍ、内径２５ｍｍ、厚さ０．６５ｍｍ）
投入基板枚数：５枚
[Polishing condition]
Polishing test machine: "Double-sided 9B polishing machine" manufactured by Speedfam
Polishing pad: suede type (thickness 0.9 mm, average pore diameter 30 μm, material: urethane foam)
Polishing liquid composition supply rate: 100 mL/min (supply rate per 1 cm 2 of substrate to be polished: about 0.3 mL/min)
Lower surface plate rotation speed: 24 rpm
Polishing load: 4.9 kPa
Carrier: Aramid, 0.5mm thick
Polishing time: 30 minutes Substrate to be polished: Aluminoborosilicate glass substrate (outer diameter 95 mm, inner diameter 25 mm, thickness 0.65 mm)
Number of input boards: 5
５．評価
［研磨速度の評価］
研磨前後の各基板１枚当たりの重さを計り（Ｓａｒｔｏｒｉｕｓ社製、「ＢＰ－２１０Ｓ」）を用いて測定し、各基板の質量変化から質量減少量を求めた。全５枚の平均の質量減少量を研磨時間で割った値を研磨速度とし、下記式により算出した。実施例１～１０、比較例１、３～７の研磨速度の測定結果を、下記表１に、比較例２を１００とした相対値として示す。
質量減少量（ｇ）＝｛研磨前の質量（ｇ）－ 研磨後の質量（ｇ）｝
研磨速度（ｍｇ／ｍｉｎ）＝質量減少量（ｍｇ）／ 研磨時間（ｍｉｎ）
5. Evaluation [Evaluation of polishing speed]
The weight of each substrate before and after polishing was measured using a weight (“BP-210S” manufactured by Sartorius), and the amount of weight reduction was determined from the weight change of each substrate. The value obtained by dividing the average mass reduction amount of all five sheets by the polishing time was defined as the polishing rate, which was calculated by the following formula. The measurement results of the polishing rates of Examples 1 to 10 and Comparative Examples 1 and 3 to 7 are shown in Table 1 below as relative values with Comparative Example 2 set to 100.
Mass decrease amount (g) = {mass before polishing (g) - mass after polishing (g)}
Polishing rate (mg/min)=mass reduction (mg)/polishing time (min)
［表面粗さの評価］
研磨後の基板を、２０ｐｐｍのＫＯＨ水溶液からなるｐＨ１２のアルカリ洗浄剤組成物（温度：２５℃）の入った槽内に１時間浸漬する。浸漬後の基板を、イオン交換水で６０秒間すすぎを行った後、基板表面を完全に乾燥させる。そして、各々の基板の両面を、下記測定条件にて、ＡＦＭ（Bruker製 Dimension Icon）を用いて表面粗さを測定し、平均値を算出した。表面粗さ（ＡＦＭ－Ｒａ）の結果を、下記表１に、比較例２を１００とした相対値として示す。
＜ＡＦＭの測定条件＞
Ｍｏｄｅ： Ｔａｐｐｉｎｇ ｍｏｄｅ
Ａｒｅａ： １×１μｍ
Ｓｃａｎ ｒａｔｅ： １．０Ｈｚ
Ｃａｎｔｉｌｅｖｅｒ： ＯＴＥＳＰＡ－Ｒ３
Ｌｉｎｅ： ２５６×２５６
[Evaluation of surface roughness]
The substrate after polishing is immersed in a tank containing an alkaline detergent composition of pH 12 (temperature: 25° C.) consisting of a 20 ppm KOH aqueous solution for 1 hour. After rinsing the immersed substrate with deionized water for 60 seconds, the substrate surface is completely dried. Then, the surface roughness of both sides of each substrate was measured using an AFM (Dimension Icon manufactured by Bruker) under the following measurement conditions, and the average value was calculated. The results of surface roughness (AFM-Ra) are shown in Table 1 below as relative values with Comparative Example 2 set to 100.
<AFM measurement conditions>
Mode: Tapping mode
Area: 1×1 μm
Scan rate: 1.0Hz
Cantilever: OTESPA-R3
Line: 256×256
上記表１に示すとおり、実施例１～１０の研磨液組成物は、比較例１～７の研磨液組成物に比べて、研磨速度が維持されつつ、洗浄後の基板の表面粗さの悪化が抑制されていた。 As shown in Table 1 above, the polishing liquid compositions of Examples 1 to 10, while maintaining the polishing rate, worsened the surface roughness of the substrate after cleaning compared to the polishing liquid compositions of Comparative Examples 1 to 7. was suppressed.
本開示の研磨液組成物によれば、研磨速度を維持しつつ、洗浄後の基板表面の表面粗さの悪化を抑制できる。したがって、本開示の研磨液組成物は、様々なガラス基板の製造において有用であり、中でも、ハードディスク用ガラス基板の製造に有用である。 According to the polishing composition of the present disclosure, deterioration of surface roughness of the substrate surface after cleaning can be suppressed while maintaining the polishing rate. Therefore, the polishing composition of the present disclosure is useful in the production of various glass substrates, especially in the production of glass substrates for hard disks.
Claims (9)
前記リン酸塩は、アルカリ金属リン酸水素塩である、ガラスハードディスク基板用研磨液組成物。 Contains abrasive grains, sulfamic acid, phosphate, and water ,
The polishing composition for a glass hard disk substrate , wherein the phosphate is an alkali metal hydrogen phosphate .
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| JP2004027042A (en) | 2002-06-26 | 2004-01-29 | Yuka Sangyo Kk | Gelled product of fine particle dispersion and fine particle dispersion obtained from the same |
| JP2014141667A (en) | 2012-12-27 | 2014-08-07 | Sanyo Chem Ind Ltd | Polishing liquid for electronic material |
| JP2014203503A (en) | 2013-04-10 | 2014-10-27 | 株式会社オハラ | Method for manufacturing hard disk substrate |
| JP2014217904A (en) | 2013-05-07 | 2014-11-20 | コニカミノルタ株式会社 | Method of manufacturing glass article |
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| JP2004027042A (en) | 2002-06-26 | 2004-01-29 | Yuka Sangyo Kk | Gelled product of fine particle dispersion and fine particle dispersion obtained from the same |
| JP2014141667A (en) | 2012-12-27 | 2014-08-07 | Sanyo Chem Ind Ltd | Polishing liquid for electronic material |
| JP2014203503A (en) | 2013-04-10 | 2014-10-27 | 株式会社オハラ | Method for manufacturing hard disk substrate |
| JP2014217904A (en) | 2013-05-07 | 2014-11-20 | コニカミノルタ株式会社 | Method of manufacturing glass article |
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