JP6330628B2 - Manufacturing method of glass substrate - Google Patents

Manufacturing method of glass substrate Download PDF

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JP6330628B2
JP6330628B2 JP2014228177A JP2014228177A JP6330628B2 JP 6330628 B2 JP6330628 B2 JP 6330628B2 JP 2014228177 A JP2014228177 A JP 2014228177A JP 2014228177 A JP2014228177 A JP 2014228177A JP 6330628 B2 JP6330628 B2 JP 6330628B2
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polishing
glass substrate
pad
liquid
polishing pad
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JP2015111487A (en
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宮谷 克明
克明 宮谷
桂瑛 蕭
桂瑛 蕭
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AGC Inc
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Asahi Glass Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00Lapping machines or devices; Accessories
    • B24B37/04Lapping machines or devices; Accessories designed for working plane surfaces
    • B24B37/07Lapping machines or devices; Accessories designed for working plane surfaces characterised by the movement of the work or lapping tool
    • B24B37/10Lapping machines or devices; Accessories designed for working plane surfaces characterised by the movement of the work or lapping tool for single side lapping
    • B24B37/105Lapping machines or devices; Accessories designed for working plane surfaces characterised by the movement of the work or lapping tool for single side lapping the workpieces or work carriers being actively moved by a drive, e.g. in a combined rotary and translatory movement
    • B24B37/107Lapping machines or devices; Accessories designed for working plane surfaces characterised by the movement of the work or lapping tool for single side lapping the workpieces or work carriers being actively moved by a drive, e.g. in a combined rotary and translatory movement in a rotary movement only, about an axis being stationary during lapping
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00Lapping machines or devices; Accessories
    • B24B37/04Lapping machines or devices; Accessories designed for working plane surfaces
    • B24B37/042Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (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の製造方法に関する。   The present invention relates to a method for producing a glass substrate.

磁気記録装置等に用いられる磁気記録媒体用のガラス基板としては、従来、アルミニウム合金基板が使用されてきたが、高記録密度化の要求に伴い、アルミニウム合金基板に比べて硬く、平坦性および平滑性に優れるガラス基板が主流となってきている。   Conventionally, an aluminum alloy substrate has been used as a glass substrate for a magnetic recording medium used in a magnetic recording apparatus or the like, but it is harder, flatter and smoother than an aluminum alloy substrate due to the demand for higher recording density. Glass substrates having excellent properties are becoming mainstream.

磁気記録媒体用のガラス基板は、ガラス素基板を所定形状に切断後、端面、および、主平面について研磨等を行うことにより製造される。この磁気記録媒体用ガラス基板の製造方法における研磨工程では、ガラス基板を研磨用キャリアに保持させ、研磨パッドを用いて、砥粒を含む研磨液(スラリー)をガラス基板と研磨パッドとの間に供給しながら研磨する。   A glass substrate for a magnetic recording medium is manufactured by cutting a glass base substrate into a predetermined shape and then polishing the end face and the main plane. In the polishing step in the method of manufacturing the glass substrate for magnetic recording medium, the glass substrate is held by a polishing carrier, and a polishing liquid (slurry) containing abrasive grains is interposed between the glass substrate and the polishing pad using a polishing pad. Polish while feeding.

前記研磨工程において、ガラス基板の研磨中に研磨パッドの研磨面にキズ(研磨用キャリアが研磨パッドの研磨面を引っ掻く)が発生する。研磨パッドの研磨面にキズを有する状態でガラス基板を研磨すると、製品品質に問題が生じる、研磨中にガラス基板が破損して研磨面に傷が付いた場合は研磨パッドを交換する必要がある、などの問題が生じるおそれがある。また、研磨パッドの使用時間が短くなり、生産性に劣る、コストアップになるという問題もある。   In the polishing step, scratches (the polishing carrier scratches the polishing surface of the polishing pad) occur on the polishing surface of the polishing pad during polishing of the glass substrate. Polishing the glass substrate with scratches on the polishing surface of the polishing pad may cause product quality problems. If the glass substrate is damaged during polishing and the polishing surface is damaged, the polishing pad must be replaced. , Etc. may occur. In addition, the use time of the polishing pad is shortened, resulting in inferior productivity and increased cost.

研磨レートが低下した場合には研磨パッドの表面を削り研磨面を調整する(ドレス処理)必要が生じる。また、研磨パッドを使用して製造されたガラス基板が所望とする品質を満たさなくなったとき、耐用限界とみなされて新たな研磨パッドに交換する。   When the polishing rate is lowered, the surface of the polishing pad is scraped to adjust the polishing surface (dressing process). Further, when the glass substrate manufactured using the polishing pad does not satisfy the desired quality, it is regarded as a service life limit and is replaced with a new polishing pad.

ドレス処理または研磨パッドの交換により、研磨工程を一時停止しなければならず、ガラス基板の生産性が低下し、コストがかかるという問題がある。また、ドレス処理は研磨パッドの研磨面を削り調整する作業であるため、ドレス処理を行うにつれて研磨パッドの寿命は短くなる。   The polishing process must be temporarily stopped by dressing or changing the polishing pad, resulting in a problem that the productivity of the glass substrate is lowered and the cost is increased. Further, since the dressing process is an operation for trimming and adjusting the polishing surface of the polishing pad, the life of the polishing pad is shortened as the dressing process is performed.

また、特許文献1には、遊星歯車機構を用いた研磨工程を有する磁気ディスク用ガラス基板の製造方法において、上下定盤に貼付けされた研磨パッドに片削れ(偏磨耗)が生じることを抑制し、研磨パッドに起因する生産性の落ち込みを低減することを目的として、研磨工程は、前記上下定盤を所定の方向に回転させて前記ガラス基板の主表面を研磨する第1の研磨期間と、前記上下定盤を前記所定の方向と逆方向に回転させて前記ガラス基板の主表面を研磨する第2の研磨期間とを設けることが記載されている。   Further, in Patent Document 1, in the method for manufacturing a glass substrate for a magnetic disk having a polishing process using a planetary gear mechanism, it is possible to suppress the occurrence of one-side scraping (uneven wear) on the polishing pad attached to the upper and lower surface plates. In order to reduce the drop in productivity due to the polishing pad, the polishing step includes a first polishing period in which the upper and lower surface plates are rotated in a predetermined direction to polish the main surface of the glass substrate; It describes that a second polishing period for polishing the main surface of the glass substrate by rotating the upper and lower surface plates in a direction opposite to the predetermined direction is provided.

特開2011−67901号公報JP 2011-67901 A

しかしながら、特許文献1に開示されている技術では、ガラス基板の研磨中に研磨パッドの研磨面にキズが発生するのを十分に防ぎ、研磨パッドの寿命を延ばすという観点からは不十分であった。   However, the technique disclosed in Patent Document 1 is insufficient from the viewpoint of sufficiently preventing scratches on the polishing surface of the polishing pad during polishing of the glass substrate and extending the life of the polishing pad. .

したがって、本発明は、ガラス基板の研磨中に研磨パッドの研磨面にキズが発生するのを防ぎ、研磨パッドの寿命を延ばすことのできるガラス基板の製造方法を提供することを目的とする。   Therefore, an object of the present invention is to provide a method for producing a glass substrate that can prevent the polishing surface of the polishing pad from being scratched during polishing of the glass substrate and extend the life of the polishing pad.

本発明者らは、研磨液1μlを研磨パッドの研磨面に滴下してから50秒後の研磨液の接触角が50°以下となる研磨パッドと研磨液を用いて、研磨パッドに対する研磨液の浸透性を改善してガラス基板の主平面を研磨することにより、ガラス基板の研磨中に研磨パッドの研磨面にキズが発生するのを防ぎ、研磨パッドの寿命を延ばすことができることを見出し、本発明を完成させた。   The inventors of the present invention have used a polishing pad and a polishing liquid at which the contact angle of the polishing liquid after 50 seconds after dropping 1 μl of the polishing liquid on the polishing surface of the polishing pad is 50 ° or less, and It has been found that by polishing the main surface of the glass substrate with improved permeability, scratches on the polishing surface of the polishing pad can be prevented during polishing of the glass substrate, and the life of the polishing pad can be extended. Completed the invention.

すなわち、本発明は以下の通りである。
(1)ショアD硬度が40以下である発泡樹脂の研磨層を有する研磨パッドと、砥粒として一次粒子径が3〜50nmであるシリカを含有する研磨液とを用いて、研磨用キャリアの保持孔に保持されたガラス基板の主平面を研磨する研磨工程と、ガラス基板の表面を洗浄する洗浄工程とを有する、ガラス基板の製造方法であって、
前記研磨工程において、研磨液1μlを研磨パッドの研磨面に滴下してから50秒後の研磨液の接触角が50°以下となる研磨パッドと研磨液を用いてガラス基板の主平面を研磨することを特徴とするガラス基板の製造方法。
(2)前記研磨用キャリアにおいて、研磨液1μlを研磨用キャリアの表面に滴下してから0.1秒後の研磨液の接触角が75°以下である(1)に記載のガラス基板の製造方法。
(3)前記研磨液は、25℃における粘度が1.7mPa・s以下である(1)または(2)に記載のガラス基板の製造方法。
(4)前記研磨液は、pH1〜pH6であり、砥粒であるシリカの含有量が5〜25質量%である(1)〜(3)のいずれか1に記載のガラス基板の製造方法。
(5)前記ガラス基板は、中央部に円孔を有する磁気記録媒体用ガラス基板である(1)〜(4)のいずれか1に記載のガラス基板の製造方法。
That is, the present invention is as follows.
(1) Holding a polishing carrier using a polishing pad having a foamed resin polishing layer having a Shore D hardness of 40 or less and a polishing liquid containing silica having a primary particle diameter of 3 to 50 nm as abrasive grains A method for producing a glass substrate, comprising: a polishing step for polishing a main plane of a glass substrate held in a hole; and a cleaning step for cleaning the surface of the glass substrate,
In the polishing step, the main surface of the glass substrate is polished by using the polishing pad and the polishing liquid at which the contact angle of the polishing liquid is 50 ° or less after 50 seconds from dropping 1 μl of the polishing liquid onto the polishing surface of the polishing pad. A method for producing a glass substrate, comprising:
(2) In the polishing carrier, the glass substrate according to (1), wherein a contact angle of the polishing liquid 0.1 seconds after dropping 1 μl of the polishing liquid onto the surface of the polishing carrier is 75 ° or less. Method.
(3) The said polishing liquid is a manufacturing method of the glass substrate as described in (1) or (2) whose viscosity in 25 degreeC is 1.7 mPa * s or less.
(4) The method for producing a glass substrate according to any one of (1) to (3), wherein the polishing liquid has a pH of 1 to 6 and a silica content of 5 to 25 mass%.
(5) The method for producing a glass substrate according to any one of (1) to (4), wherein the glass substrate is a glass substrate for a magnetic recording medium having a circular hole in a central portion.

本発明のガラス基板の製造方法によれば、研磨パッドに対する研磨液の浸透性を改善し、仕上げ研磨工程において、研磨パッドにキズが生じることを抑制できる。このことにより、研磨パッドの寿命を長くすることができ、磁気記録媒体用ガラス基板の製造工程における生産性の向上、およびコストの低減を図ることができる。   According to the method for producing a glass substrate of the present invention, it is possible to improve the permeability of the polishing liquid with respect to the polishing pad and to prevent the polishing pad from being scratched in the final polishing step. As a result, the life of the polishing pad can be lengthened, and the productivity can be improved and the cost can be reduced in the manufacturing process of the glass substrate for magnetic recording medium.

図1は、研磨用キャリアを搭載可能なガラス基板の両面研磨装置について説明する図である。FIG. 1 is a diagram for explaining a double-side polishing apparatus for a glass substrate on which a polishing carrier can be mounted. 図2は、ガラス基板の斜視図である。FIG. 2 is a perspective view of the glass substrate.

[ガラス基板の製造方法の概略]
本実施形態のガラス基板の製造方法の概略について説明する。
[Outline of glass substrate production method]
The outline of the manufacturing method of the glass substrate of this embodiment is demonstrated.

本発明において、ガラス基板は、アモルファスガラスでもよく、結晶化ガラスでもよく、ガラス基板の表層に強化層を有する強化ガラス(例えば、化学強化ガラス)でもよい。   In the present invention, the glass substrate may be amorphous glass, crystallized glass, or tempered glass (for example, chemically tempered glass) having a tempered layer on the surface layer of the glass substrate.

具体的には、例えば、ガラス基板に高い機械的強度が求められる場合、ガラス基板の表層に強化層を形成する強化工程(例えば、化学強化工程)を実施することが好ましい。強化工程は、最初の研磨工程前、最後の研磨工程後、または各研磨工程間のいずれで実施してもよい。   Specifically, for example, when high mechanical strength is required for the glass substrate, it is preferable to perform a strengthening step (for example, a chemical strengthening step) for forming a reinforcing layer on the surface layer of the glass substrate. The strengthening step may be performed either before the first polishing step, after the last polishing step, or between each polishing step.

本発明のガラス基板のガラス素基板は、フロート法、フュージョン法、プレス成形法、ダウンドロー法またはリドロー法等の方法により成形されるが、本発明はこの点で限定されない。   The glass substrate of the glass substrate of the present invention is formed by a method such as a float method, a fusion method, a press molding method, a down draw method, or a redraw method, but the present invention is not limited in this respect.

ガラス基板は、上述の方法で成形されたガラス素基板に、
(工程1)ガラス素基板を、中央部に円形孔を有する円盤形状に加工した後、内周側面と外周側面を面取り加工する形状付与工程;
(工程2)ガラス基板の端面(内周端面および外周端面)を研磨する端面研磨工程;
(工程3)ガラス基板の上下両主平面を研磨する主表面研磨工程;
(工程4)ガラス基板を精密洗浄して乾燥する洗浄工程;
を含む工程を施すことによって製造される。
The glass substrate is a glass substrate formed by the above-described method,
(Step 1) A shape imparting step of chamfering the inner peripheral side surface and the outer peripheral side surface after processing the glass substrate into a disk shape having a circular hole in the center portion;
(Step 2) An end surface polishing step for polishing the end surfaces (the inner peripheral end surface and the outer peripheral end surface) of the glass substrate;
(Step 3) Main surface polishing step for polishing the upper and lower main surfaces of the glass substrate;
(Step 4) A cleaning step of precisely cleaning and drying the glass substrate;
It is manufactured by performing the process including.

そして、上述の工程を含む製造方法によって得られたガラス基板は、その後さらにその表面に下地層、磁性層、保護層または潤滑膜等を形成することによって磁気記録媒体(磁気ディスク)とすることができる。   And the glass substrate obtained by the manufacturing method including the above-mentioned process can be used as a magnetic recording medium (magnetic disk) by further forming an underlayer, a magnetic layer, a protective layer or a lubricating film on the surface thereof. it can.

主表面研磨工程の前において、主平面のラップ(例えば、遊離砥粒ラップ、固定砥粒ラップなど)を実施してもよく、また、各工程間にガラス基板の洗浄(工程間洗浄)またはガラス基板表面のエッチング(工程間エッチング)を実施してもよい。   Prior to the main surface polishing step, main surface lapping (for example, loose abrasive lapping, fixed abrasive lapping, etc.) may be performed, and glass substrate cleaning (inter-step cleaning) or glass between each step Etching of the substrate surface (inter-process etching) may be performed.

なお、ここで言う主平面のラップは、広義の主平面の研磨である。また、研磨工程は、1次研磨のみでもよく、1次研磨と2次研磨を行ってもよく、2次研磨の後に3次研磨を行ってもよい。   Note that the main plane lapping here is polishing of the main plane in a broad sense. Further, the polishing step may be only primary polishing, primary polishing and secondary polishing may be performed, or tertiary polishing may be performed after secondary polishing.

次に、各々の工程について、説明する。
(工程1)形状付与工程
形状付与工程では、ガラス素基板を、中央部に円形孔を有する円盤形状に加工した後、内周側面と外周側面を面取り加工する。形状付与工程における、内周および外周側面部の面取り加工は、一般にダイヤモンド砥粒を固定した砥石を用いて行う。
Next, each step will be described.
(Step 1) Shape imparting step In the shape imparting step, the glass base substrate is processed into a disk shape having a circular hole in the center, and then the inner peripheral side surface and the outer peripheral side surface are chamfered. The chamfering processing of the inner and outer peripheral side surfaces in the shape imparting step is generally performed using a grindstone to which diamond abrasive grains are fixed.

(工程2)端面研磨工程
端面研磨工程では、ガラス基板の内周端面および外周端面を端面研磨する。外周端面および内周端面の研磨は、どちらを先に実施してもよい。
(Step 2) End Surface Polishing Step In the end surface polishing step, the inner peripheral end surface and the outer peripheral end surface of the glass substrate are end polished. Either the outer peripheral end face or the inner peripheral end face may be polished first.

(工程3)主表面研磨工程
主表面研磨工程では、両面研磨装置を用いて、ガラス基板の主平面に研磨液を供給しながらガラス基板の上下主平面を研磨する。なお、両面研磨装置としては、特に限定されないが、例えば、キャリアの直径サイズが16インチ、20インチまたは22インチのものが使用できる両面研磨機(例えば、16B型両面研磨装置、20B型両面研磨装置および22B型両面研磨装置等)が挙げられる。
(Step 3) Main surface polishing step In the main surface polishing step, the upper and lower main planes of the glass substrate are polished using a double-side polishing apparatus while supplying a polishing liquid to the main plane of the glass substrate. The double-side polishing apparatus is not particularly limited. For example, a double-side polishing machine that can use a carrier having a diameter of 16 inches, 20 inches, or 22 inches (for example, a 16B type double-side polishing apparatus or a 20B type double-side polishing apparatus). And a 22B type double-side polishing apparatus).

研磨工程は、1次研磨(仕上げ研磨)のみの1段研磨でもよいし、1次研磨と2次研磨(仕上げ研磨)を行う2段研磨でもよいし、1次研磨、2次研磨を経て3次研磨(仕上げ研磨)を行う3段研磨でもよい。通常、各々の研磨工程の間には、洗浄工程(工程間洗浄)を設ける。   The polishing step may be one-step polishing with only primary polishing (finish polishing), two-step polishing in which primary polishing and secondary polishing (finish polishing) are performed, or three after first polishing and second polishing. Three-stage polishing in which next polishing (finish polishing) is performed may be used. Usually, a cleaning process (inter-process cleaning) is provided between each polishing process.

なお、主表面研磨工程の前において、主平面のラップ(例えば、遊離砥粒ラップおよび固定砥粒ラップなど)を実施してもよい。ここで言う主平面のラップは、広義の主平面の研磨である。   Prior to the main surface polishing step, main surface lapping (for example, loose abrasive lapping and fixed abrasive lapping) may be performed. The main plane lap mentioned here is polishing of the main plane in a broad sense.

本発明のガラス基板の製造方法は、前記仕上げ研磨において、後述する特定の方法を実施することによって、研磨パッドに対する研磨液のなじみやすさを向上してガラス基板の研磨中に研磨パッドの研磨面にキズが発生するのを防ぎ、研磨パッドの寿命を延ばすものである。主表面研磨工程の詳細については、後述する。   The method for producing a glass substrate of the present invention improves the ease of adapting the polishing liquid to the polishing pad by performing a specific method described later in the final polishing, so that the polishing surface of the polishing pad is polished during the polishing of the glass substrate. This prevents the generation of scratches and extends the life of the polishing pad. Details of the main surface polishing step will be described later.

主表面研磨工程では、ガラス基板を研磨用キャリアに保持させ、研磨パッドを用いて、砥粒を含む研磨液をガラス基板と研磨パッドとの間に供給しながら研磨する研磨装置が用いられている。   In the main surface polishing step, a polishing apparatus is used that holds a glass substrate on a polishing carrier and uses a polishing pad to polish while supplying a polishing liquid containing abrasive grains between the glass substrate and the polishing pad. .

前記研磨装置では、上下定盤に研磨パッドを貼り付けてガラス基板を挟み込み、遊星歯車機構を用いてガラス基板と研磨パッドとを相対的に移動させることにより、ガラス基板の主平面を研磨している。該研磨装置による研磨は、複数のガラス基板を同時に研磨できるため、生産効率の面で優れた方法である。   In the polishing apparatus, the main surface of the glass substrate is polished by attaching the polishing pad to the upper and lower surface plates, sandwiching the glass substrate, and moving the glass substrate and the polishing pad relatively by using the planetary gear mechanism. Yes. Polishing by the polishing apparatus is an excellent method in terms of production efficiency because a plurality of glass substrates can be simultaneously polished.

前記研磨装置について図1を参照しながら説明する。   The polishing apparatus will be described with reference to FIG.

研磨装置12は、図1に示すように、ガラス基板30を設置可能な研磨用キャリア10をステンレス製のサンギヤ13、リングギヤ14間にセットするように構成される。サンギヤ13、リングギヤ14および研磨用キャリア10の外周面に形成されたギヤ部10aは、遊星歯車機構を構成し、サンギヤ13、リングギヤ14を所定の回転比率で回転駆動することにより、研磨用キャリア10が自転しながらサンギヤ13の周りを公転する。   As shown in FIG. 1, the polishing apparatus 12 is configured to set a polishing carrier 10 on which a glass substrate 30 can be set between a stainless sun gear 13 and a ring gear 14. The gear portion 10a formed on the outer peripheral surface of the sun gear 13, the ring gear 14 and the polishing carrier 10 constitutes a planetary gear mechanism, and the sun gear 13 and the ring gear 14 are rotationally driven at a predetermined rotation ratio, whereby the polishing carrier 10 Revolves around the sun gear 13 while rotating.

このとき、研磨用キャリア10は、ギヤ部10aの内側のガラス基板保持部10bに形成されたガラス基板保持孔11にガラス基板30を保持した状態で、ガラス基板30と対向する面に研磨パッド16、18が装着された上定盤15と下定盤17との間に狭持、押圧されている。そして、研磨パッド16、18と研磨用キャリア10、ガラス基板30との間には砥粒を含有する研磨液が供給され、研磨用キャリア10に保持されたガラス基板の両主平面が同時に研磨される。   At this time, the polishing carrier 10 has a polishing pad 16 on the surface facing the glass substrate 30 in a state where the glass substrate 30 is held in the glass substrate holding hole 11 formed in the glass substrate holding portion 10b inside the gear portion 10a. , 18 are sandwiched and pressed between the upper surface plate 15 and the lower surface plate 17. A polishing liquid containing abrasive grains is supplied between the polishing pads 16 and 18 and the polishing carrier 10 and the glass substrate 30, and both main planes of the glass substrate held by the polishing carrier 10 are simultaneously polished. The

例えば、上定盤15側の動摩擦係数が上昇し、ガラス基板30の自転または公転がスムーズに行われなくなる、または下定盤17側の動摩擦係数が上がり、ガラス基板30の自転または公転がスムーズに行われなくなる場合に、ガラス基板30が研磨用キャリア10に乗り上げる、若しくは研磨用キャリア10の下にもぐることで、研磨パッド16、18に傷が発生していると考えられる。   For example, the dynamic friction coefficient on the upper surface plate 15 side increases and the glass substrate 30 does not rotate or revolve smoothly, or the dynamic friction coefficient on the lower surface plate 17 side increases, and the glass substrate 30 rotates or revolves smoothly. It is considered that the scratches are generated on the polishing pads 16 and 18 when the glass substrate 30 rides on the polishing carrier 10 or goes under the polishing carrier 10 when it does not break.

ガラス基板30は、図2に示すように、両主平面31の中央部に円形孔を有する円盤状に形成され、内周側面32と外周側面33とを有する。研磨されたガラス基板30の板厚は、0.5mm〜1.0mmであることが好ましい。   As shown in FIG. 2, the glass substrate 30 is formed in a disk shape having a circular hole at the center of both main planes 31, and has an inner peripheral side surface 32 and an outer peripheral side surface 33. The plate thickness of the polished glass substrate 30 is preferably 0.5 mm to 1.0 mm.

研磨パッド16、18は、ショアD硬度が40以下である発泡樹脂の研磨層を有する研磨パッド(以下、研磨パッドともいう)である。ショアD硬度で40以下である発泡樹脂の研磨層を有する研磨パッドは、硬質ウレタンパッドの厚さ(典型的には1.5mm〜2.0mm)に比べて薄く、典型的には0.3mm〜1.2mm程度の厚さを有する。   The polishing pads 16 and 18 are polishing pads (hereinafter also referred to as polishing pads) having a foamed resin polishing layer having a Shore D hardness of 40 or less. A polishing pad having a polishing layer of a foamed resin having a Shore D hardness of 40 or less is thinner than a hard urethane pad (typically 1.5 mm to 2.0 mm), typically 0.3 mm. It has a thickness of about 1.2 mm.

また、パッド表面に形成される溝深さについても、硬質ウレタンパッドの溝深さ(典型的には1.2mm〜1.7mm)に比べて浅く、典型的には0.2mm〜1.0mm程度の深さを有する。   Also, the groove depth formed on the pad surface is shallower than the groove depth of the hard urethane pad (typically 1.2 mm to 1.7 mm), typically 0.2 mm to 1.0 mm. Has a depth of about.

したがって、ショアD硬度が40以下である発泡樹脂の研磨層を有する研磨パッドは、硬質ウレタンパッドに比べて、溝の深さが浅い場合、研磨液の研磨面への供給が不均一になりやすい傾向がある。   Accordingly, a polishing pad having a foamed resin polishing layer having a Shore D hardness of 40 or less tends to have a non-uniform supply of polishing liquid to the polishing surface when the groove depth is shallower than a hard urethane pad. Tend.

同時に研磨できるガラス基板30の枚数は、研磨用キャリア10、両面研磨装置12の大きさによって異なる。具体的には、例えば、直径16インチの研磨用キャリアを使用する16B型両面研磨装置においては、1バッチ当たり80〜110枚のガラス基板30を同時に研磨でき、直径22インチの研磨用キャリアを使用する22B型両面研磨装置においては、1バッチ当たり115〜222枚のガラス基板30を同時に研磨できる。なお、研磨を行う際、研磨用キャリア10の全てのガラス基板保持孔11にガラス基板30をセットする必要はない。   The number of glass substrates 30 that can be polished simultaneously varies depending on the size of the polishing carrier 10 and the double-side polishing apparatus 12. Specifically, for example, in a 16B type double-side polishing apparatus using a polishing carrier having a diameter of 16 inches, 80 to 110 glass substrates 30 can be simultaneously polished per batch, and a polishing carrier having a diameter of 22 inches is used. In the 22B double-side polishing apparatus, 115 to 222 glass substrates 30 can be simultaneously polished per batch. When polishing, it is not necessary to set the glass substrate 30 in all the glass substrate holding holes 11 of the polishing carrier 10.

(工程4)洗浄工程
洗浄工程では、仕上げ研磨後のガラス基板を、例えば、洗剤を用いたスクラブ洗浄、洗剤溶液へ浸漬した状態での超音波洗浄および純水へ浸漬した状態での超音波洗浄等を順次行い、イソプロピルアルコール等の蒸気により乾燥する。
(Process 4) Cleaning process In the cleaning process, for example, scrub cleaning using a detergent, ultrasonic cleaning in a state of immersing in a detergent solution, and ultrasonic cleaning in a state of immersing in pure water. Etc. are sequentially performed and dried with steam such as isopropyl alcohol.

[本発明のガラス基板の製造方法]
本発明のガラス基板の製造方法においては、上述の(工程3)の主表面研磨工程において、ショアD硬度が40以下である発泡樹脂の研磨層を有する研磨パッドと、砥粒として一次粒子径が3〜50nmであるシリカを含有する研磨液とを用いて、研磨用キャリアの保持孔に保持されたガラス基板の主平面を研磨する。
[Method for Manufacturing Glass Substrate of the Present Invention]
In the method for producing a glass substrate of the present invention, in the main surface polishing step of (Step 3) described above, a polishing pad having a foamed resin polishing layer having a Shore D hardness of 40 or less and a primary particle size as abrasive grains The main plane of the glass substrate held in the holding hole of the polishing carrier is polished with a polishing liquid containing silica having a thickness of 3 to 50 nm.

研磨パッドは、0.3〜1.2mm厚に積層され、硬度がショアD硬度で40以下であり、好ましくは30以下である。ショアD硬度が40超であると砥粒の押し込みによりガラスに微小な傷をつける虞がある。また、ショアA硬度は、20以上であることが好ましく、より好ましくは30以上である。ショアA硬度を30以上とすることにより十分な研磨速度を得ることができる。   The polishing pad is laminated to a thickness of 0.3 to 1.2 mm, and the hardness is 40 or less, preferably 30 or less in Shore D hardness. If the Shore D hardness is more than 40, there is a possibility that fine scratches may be caused on the glass by pressing the abrasive grains. Moreover, it is preferable that Shore A hardness is 20 or more, More preferably, it is 30 or more. A sufficient polishing rate can be obtained by setting the Shore A hardness to 30 or more.

このような条件を満たす研磨パッドの素材は、典型的には、発泡樹脂を研磨面に有するスエードパッド、不職布パッド、織布パッド等が挙げられ、そのうちスエードパッドが最も好ましいものとして挙げられる。   The material of the polishing pad satisfying such conditions typically includes a suede pad having a foamed resin on the polishing surface, an unemployed fabric pad, a woven fabric pad, etc., of which the suede pad is most preferable. .

研磨パッドの構造としては、具体的には、例えば、ベース層と、プラスチックフォーム等で作られた表面層(一般的にNAP層と呼ばれる)と、を有する構造が挙げられる。研磨パッドは、ドレス処理によって、表面層の表皮を研削除去されていることが好ましい。これにより、プラスチックフォームに含まれる気泡が開口され、ガラス基板を研磨する研磨面が形成される。   Specific examples of the structure of the polishing pad include a structure having a base layer and a surface layer (generally called a NAP layer) made of plastic foam or the like. It is preferable that the polishing pad is ground and removed by a dressing process. Thereby, the bubble contained in a plastic foam is opened, and the grinding | polishing surface which grind | polishes a glass substrate is formed.

このように、表面層の表皮を研削除去してプラスチックフォームの気泡を開口した状態の研磨パッドは、スエードタイプの研磨パッドともいわれる。研磨パッドは、ガラス基板の仕上げ研磨によく使用される。   Thus, the polishing pad in which the skin of the surface layer is removed by grinding to open the bubbles of the plastic foam is also referred to as a suede type polishing pad. A polishing pad is often used for finish polishing of a glass substrate.

研磨パッドは、ガラス基板を研磨する前に、予めドレッサを用いてドレス処理を施し、研磨パッドの研磨面の形状および表面粗さを調整することが好ましい。   The polishing pad is preferably subjected to dressing using a dresser in advance before polishing the glass substrate to adjust the shape and surface roughness of the polishing surface of the polishing pad.

例えば、ウレタン製の研磨パッドは、内部に発泡層を有し、その中に研磨剤粒子を一時的に保持する構成を有する。そのため、研磨パッドの研磨面に、この発泡層を開口させるために、ドレッサを用いてドレス処理し、研磨パッドの表面層を研削除去し、研磨面を形成させる必要がある。ドレス処理とは、研磨装置の定盤に研磨パッドを装着した後、ドレッサを用いて研磨パッドの表面層を研削除去する処理である。   For example, a polishing pad made of urethane has a configuration in which a foam layer is formed inside and abrasive particles are temporarily held therein. Therefore, in order to open the foamed layer on the polishing surface of the polishing pad, it is necessary to perform dressing using a dresser and to grind and remove the surface layer of the polishing pad to form a polishing surface. The dressing process is a process of grinding and removing the surface layer of the polishing pad using a dresser after mounting the polishing pad on the surface plate of the polishing apparatus.

研磨液に砥粒として含有されるシリカの一次粒子径は3〜50nmであり、5〜40nmであることが好ましく、7〜30nmであることがより好ましい。シリカの一次粒子径を3nm未満であると、高い研磨レートを得ることが難しくなり生産性に劣るおそれがある。これは、シリカ表面の活性が強くなり、研磨されずに基板表面に付着しやすくなるからである。また、シリカの一次粒子径が50nm超であると、磁気記録媒体の高記録密度化に対応できる主平面の表面粗さに研磨することが困難となる。   The primary particle diameter of silica contained as abrasive grains in the polishing liquid is 3 to 50 nm, preferably 5 to 40 nm, and more preferably 7 to 30 nm. When the primary particle diameter of silica is less than 3 nm, it is difficult to obtain a high polishing rate, and productivity may be deteriorated. This is because the activity of the silica surface becomes strong and it is easy to adhere to the substrate surface without being polished. Further, when the primary particle diameter of silica is more than 50 nm, it becomes difficult to polish to a surface roughness of the main plane that can cope with a higher recording density of the magnetic recording medium.

研磨液は、pH1〜pH6であることが好ましく、より好ましくはpH2〜pH6であり、さらに好ましくはpH3〜pH5.5である。研磨液のpHを6以下とすることにより、研磨パッドとガラス基板との摩擦が生じにくくなり、研磨パッドに傷が生じるのを防ぎ、レートが落ちるのを防ぐことができる。研磨液のpHを1以上とすることにより、ガラス基板の表面が荒れにくくなり、研磨装置が錆びるのを防ぐことができる。   The polishing liquid is preferably pH 1 to pH 6, more preferably pH 2 to pH 6, and further preferably pH 3 to pH 5.5. By setting the pH of the polishing liquid to 6 or less, friction between the polishing pad and the glass substrate is less likely to occur, so that the polishing pad can be prevented from being scratched and the rate can be prevented from dropping. By setting the pH of the polishing liquid to 1 or more, the surface of the glass substrate is hardly roughened, and the polishing apparatus can be prevented from being rusted.

研磨液のpHは、pH標準液[フタル酸塩pH標準液(pH4.01)、中性リン酸塩pH標準液(pH6.86)、ホウ酸塩pH標準液(pH9.18)]を使用し、3点校正を行った後、純水でpH電極を洗浄後、pH測定機を用いて研磨液のpHを測定する。pH測定機としては、堀場製作所社製のpH測定器(型式:D−53S)を用いることができる。   The pH of the polishing solution is a pH standard solution [phthalate pH standard solution (pH 4.01), neutral phosphate pH standard solution (pH 6.86), borate pH standard solution (pH 9.18)]. Then, after three-point calibration, the pH electrode is washed with pure water, and then the pH of the polishing liquid is measured using a pH measuring machine. As the pH measuring device, a pH measuring device (model: D-53S) manufactured by HORIBA, Ltd. can be used.

研磨液は、砥粒であるシリカの含有量が5〜25質量%であることが好ましく、より好ましくは5〜20質量%、さらに好ましくは5〜15質量%である。シリカの含有量を25質量%以下とすることにより、研磨液の粘度が上がりすぎるのを防ぎ、研磨液の研磨用パッドに対する浸透性の減少を抑制することができる。また、シリカの含有量を5質量%以上とすることにより、十分な研磨レートが得られる。   It is preferable that content of the silica which is an abrasive grain is 5-25 mass%, More preferably, it is 5-20 mass%, More preferably, it is 5-15 mass%. By setting the content of silica to 25% by mass or less, it is possible to prevent the viscosity of the polishing liquid from increasing excessively and to suppress a decrease in the permeability of the polishing liquid to the polishing pad. A sufficient polishing rate can be obtained by setting the silica content to 5 mass% or more.

研磨パッドおよび研磨液は、研磨液1μlを研磨パッドの研磨面に滴下してから50秒後の研磨液の接触角が50°以下となる組み合わせとする。該接触角は、好ましくは45°以下、より好ましくは40°以下、さらに好ましくは38°以下である。   The polishing pad and the polishing liquid are combined such that the contact angle of the polishing liquid after 50 seconds after dropping 1 μl of the polishing liquid onto the polishing surface of the polishing pad is 50 ° or less. The contact angle is preferably 45 ° or less, more preferably 40 ° or less, and still more preferably 38 ° or less.

研磨液1μlを前記研磨パッドの研磨面に滴下してから50秒後の研磨液の接触角が50°以下となる関係を満たす、研磨液と研磨パッドの組み合わせでガラス基板の主平面を研磨することによって、ガラス基板研磨中に研磨パッドに傷が発生することが防止でき、研磨パッドの寿命が長くなり、生産性を向上し、コストを低減できる。   The main surface of the glass substrate is polished with a combination of the polishing liquid and the polishing pad that satisfies the relationship that the contact angle of the polishing liquid after 50 seconds after dropping 1 μl of the polishing liquid on the polishing surface of the polishing pad is 50 ° or less. As a result, it is possible to prevent the polishing pad from being damaged during the polishing of the glass substrate, to prolong the life of the polishing pad, to improve productivity, and to reduce costs.

研磨液1μlを研磨パッドの研磨面に滴下してから50秒後の研磨液の接触角が50°を超える研磨パッドと研磨液とを用いてガラス基板を研磨した場合、ガラス基板研磨中に研磨パッドの表面に傷が生じやすくなり、研磨パッドの寿命が短くなる問題が生じる。   When 1 μl of the polishing liquid is dropped on the polishing surface of the polishing pad and the glass substrate is polished using a polishing pad and a polishing liquid with a contact angle of the polishing liquid exceeding 50 ° after 50 seconds, polishing is performed during polishing of the glass substrate. There is a problem that the surface of the pad is easily damaged, and the life of the polishing pad is shortened.

研磨パッドに対する研磨液の浸透性は、次のように評価する。研磨パッドの研磨面をドレス処理し、純水を用いて洗浄したあと、研磨パッドを室温で1日乾燥させる。乾燥させた研磨パッドの研磨面に、研磨液1μlを滴下し、研磨液を滴下してから50秒後の接触角を、接触角測定装置を用いて測定する。接触角測定装置としては、接触角測定装置(メーカ:協和界面科学製、型式:PCA−1)を用いることができる。   The permeability of the polishing liquid to the polishing pad is evaluated as follows. The polishing surface of the polishing pad is dressed and washed with pure water, and then the polishing pad is dried at room temperature for 1 day. 1 μl of polishing liquid is dropped on the polishing surface of the dried polishing pad, and the contact angle 50 seconds after the polishing liquid is dropped is measured using a contact angle measuring device. As the contact angle measuring device, a contact angle measuring device (manufacturer: manufactured by Kyowa Interface Science, model: PCA-1) can be used.

研磨液1μlを研磨パッドの研磨面に滴下してから50秒後の研磨液の接触角が50°以下とするには、具体的には、例えば、砥粒の粒子径が小さく、砥粒の含有量が5〜25質量%であっても分散性に優れる研磨液、このような研磨液に対する親和性に優れる研磨パッドを選択することが挙げられる。   In order to make the contact angle of the polishing liquid 50 seconds or less after dropping 1 μl of the polishing liquid on the polishing surface of the polishing pad, specifically, for example, the particle diameter of the abrasive grains is small, Even if the content is 5 to 25% by mass, it is possible to select a polishing liquid having excellent dispersibility and a polishing pad having excellent affinity for such a polishing liquid.

研磨用キャリアと研磨液は、研磨液1μlを研磨用キャリアの表面に滴下してから0.1秒後の研磨液の接触角が好ましくは75°以下であり、より好ましくは70°以下であり、さらに好ましくは65°以下である組み合わせとすることが好ましい。   For the polishing carrier and the polishing liquid, the contact angle of the polishing liquid 0.1 seconds after dropping 1 μl of the polishing liquid onto the surface of the polishing carrier is preferably 75 ° or less, more preferably 70 ° or less. More preferably, the combination is 65 ° or less.

研磨液1μlを研磨用キャリアの表面に滴下してから0.1秒後の研磨液の接触角が75°以下である研磨液とキャリアの組み合わせでガラス基板の主平面を研磨することによって、ガラス基板の研磨中に研磨パッドに傷が発生することが防止でき、研磨パッドの寿命が長くなり、生産性を向上し、コストを低減できる。   By dripping 1 μl of the polishing liquid onto the surface of the polishing carrier, the main surface of the glass substrate is polished by a combination of a polishing liquid and a carrier whose polishing liquid contact angle is 75 ° or less after 0.1 seconds. The polishing pad can be prevented from being damaged during the polishing of the substrate, the life of the polishing pad can be extended, the productivity can be improved, and the cost can be reduced.

研磨用キャリアに対する研磨液の接触角は次のように評価する。乾燥させた研磨用キャリアの表面に、研磨液1μlを滴下し、研磨液を滴下してから0.1秒後の接触角を接触角測定装置を用いて測定する。接触角測定装置としては、接触角測定装置(メーカ:協和界面科学製、型式:PCA−1)を用いることができる。   The contact angle of the polishing liquid with respect to the polishing carrier is evaluated as follows. 1 μl of the polishing liquid is dropped on the surface of the dried polishing carrier, and the contact angle 0.1 seconds after the polishing liquid is dropped is measured using a contact angle measuring device. As the contact angle measuring device, a contact angle measuring device (manufacturer: manufactured by Kyowa Interface Science, model: PCA-1) can be used.

研磨液は、25℃における粘度が1.7mPa・s以下であることが好ましく、より好ましくは1.6mPa・s以下である。また、通常1.1mPa・s以上であることが好ましく、より好ましくは1.2mPa・s以上である。研磨液の粘度を1.7mPa・s以下とすることにより、ガラス基板研磨中に研磨パッドの表面に傷が生じにくくなり、研磨パッドの寿命を延ばすことができる。また、1.1mPa・s未満になると、ガラスと研磨パッドの間で出来る液膜が薄くなりすぎて、摩擦力が高くなり、研磨機の振動などが発生し、好ましくない。   The polishing liquid preferably has a viscosity at 25 ° C. of 1.7 mPa · s or less, more preferably 1.6 mPa · s or less. Moreover, it is preferable that it is 1.1 mPa * s or more normally, More preferably, it is 1.2 mPa * s or more. By setting the viscosity of the polishing liquid to 1.7 mPa · s or less, the surface of the polishing pad is hardly damaged during polishing of the glass substrate, and the life of the polishing pad can be extended. On the other hand, if it is less than 1.1 mPa · s, the liquid film formed between the glass and the polishing pad becomes too thin, the frictional force becomes high, and the vibration of the polishing machine is generated, which is not preferable.

研磨液1μlを研磨用キャリアの表面に滴下してから0.1秒後の研磨液の接触角が好ましくは75°以下とするには、具体的には、例えば、粒子サイズが小さく、砥粒濃度が5〜25質量%であっても高分散性である研磨液、疎水性の強すぎない研磨用キャリアを選択することが挙げられる。   In order that the contact angle of the polishing liquid after 0.1 second after dropping 1 μl of the polishing liquid on the surface of the polishing carrier is preferably 75 ° or less, specifically, for example, the particle size is small and the abrasive grains Even if the concentration is 5 to 25% by mass, it is possible to select a polishing liquid that is highly dispersible and a polishing carrier that is not too hydrophobic.

以下に本発明の実施例について具体的に説明するが、本発明はこれらに限定されない。   Examples of the present invention will be specifically described below, but the present invention is not limited to these.

[ガラス基板の製造]
(工程1)形状付与工程
フロート法で成形されたシリケートガラス板を、中央部に円孔を有する円盤形状ガラス基板に加工した。この円盤形状ガラス基板の内周側面と外周側面を面取り加工した。その後、ガラス基板の上下面のラッピングを、酸化アルミニウム砥粒を用いて行い、砥粒を洗浄除去した。
[Manufacture of glass substrates]
(Process 1) Shape imparting process The silicate glass plate shape | molded by the float process was processed into the disk shaped glass substrate which has a circular hole in the center part. The inner peripheral side surface and the outer peripheral side surface of this disk-shaped glass substrate were chamfered. Thereafter, lapping of the upper and lower surfaces of the glass substrate was performed using aluminum oxide abrasive grains, and the abrasive grains were washed and removed.

(工程2)端面研磨工程
内周側面と内周面取り部を研磨ブラシと酸化セリウム砥粒を用いて研磨し、内周側面と内周面取り部のキズを除去し、鏡面となるように加工した。次に、内周端面研磨を行ったガラス基板を、外周側面と外周面取り部を研磨ブラシと酸化セリウム砥粒を用いて研磨し、外周側面と外周面取り部のキズを除去し、鏡面となるように加工した。内周端面研磨と外周端面研磨を行ったガラス基板は、超音波洗浄により、砥粒を洗浄除去した。
(Step 2) End surface polishing step The inner peripheral side surface and the inner peripheral chamfered portion were polished with a polishing brush and cerium oxide abrasive grains, and scratches on the inner peripheral side surface and the inner peripheral chamfered portion were removed to make a mirror surface. . Next, the outer peripheral side surface and the outer peripheral chamfered portion are polished with a polishing brush and a cerium oxide abrasive grain, and the outer peripheral side surface and the outer peripheral chamfered portion are removed from scratches to become a mirror surface. It was processed into. The glass substrate that had been subjected to inner peripheral end surface polishing and outer peripheral end surface polishing was cleaned and removed by ultrasonic cleaning.

(工程3)主表面研磨工程
次に、図2の両面研磨装置を使用して、ガラス基板の主平面を1次研磨、次いで、洗浄、乾燥した。その後、ガラス基板の主平面を2次研磨し、次いで、洗浄、乾燥した。
(Step 3) Main Surface Polishing Step Next, using the double-side polishing apparatus of FIG. 2, the main surface of the glass substrate was subjected to primary polishing, then washed and dried. Thereafter, the main plane of the glass substrate was secondarily polished, then washed and dried.

洗浄後のガラス基板に対して、3次研磨(仕上げ研磨)を実施した。仕上げ研磨の研磨具としては、前述のドレス処理を施した後の軟質ウレタン製の研磨パッド(0.65mm厚に積層され、硬度がショアD硬度で24、ショアA硬度で72)と、平均一次粒子直径が20〜30nmのコロイダルシリカを含有する研磨液とを用いて、16B型両面研磨装置(スピードファム社製:DSM−16B−5PV)を使用して、上下主平面を研磨した。研磨時間は、総研磨量が上下両主平面の厚さ方向の合計で1μmになるように設定した。
例1〜7で使用した研磨パッドについて説明する。例1〜7では、3種類の研磨パッドを使用した。例1および例2では親水性が高い研磨パッドAを使用した。例3〜5では、研磨パッドAより親水性が低い研磨パッドBを使用した。例6および7では、研磨パッドBよりもさらに親水性が低い研磨パッドCを使用した。
また、例1〜7で使用した研磨液について説明する。例1〜7では、3種類の研磨液を使用した。例1、例3、および例6では、研磨液Aを使用した。例2、例4、および例7では、研磨液Bを使用した。例5では、研磨液Cを使用した。研磨用キャリアに対する研磨液の接触角は、研磨液Cを用いた場合に大きく、研磨液Bを用いた場合に小さくなっているが、これは研磨液の電解質の濃度の差異によると考える。つまり、研磨液Cは研磨液中の電解質の濃度が高く、研磨液Aの電解質の濃度は研磨液Cの次に高く、研磨液Bの電解質の濃度は研磨液Aよりも低い。
Tertiary polishing (final polishing) was performed on the cleaned glass substrate. As a polishing tool for final polishing, a polishing pad made of soft urethane after being subjected to the above-mentioned dressing treatment (laminated to a thickness of 0.65 mm, hardness is 24 for Shore D hardness, 72 for Shore A hardness), and average primary The upper and lower main planes were polished using a 16B double-side polishing apparatus (DSM-16B-5PV manufactured by Speedfam Co., Ltd.) using a polishing liquid containing colloidal silica having a particle diameter of 20 to 30 nm. The polishing time was set so that the total polishing amount was 1 μm in total in the thickness direction of the upper and lower main planes.
The polishing pad used in Examples 1 to 7 will be described. In Examples 1 to 7, three types of polishing pads were used. In Examples 1 and 2, polishing pad A having high hydrophilicity was used. In Examples 3 to 5, polishing pad B having lower hydrophilicity than polishing pad A was used. In Examples 6 and 7, polishing pad C, which is lower in hydrophilicity than polishing pad B, was used.
Moreover, the polishing liquid used in Examples 1 to 7 will be described. In Examples 1 to 7, three types of polishing liquids were used. In Examples 1, 3, and 6, polishing liquid A was used. In Example 2, Example 4, and Example 7, the polishing liquid B was used. In Example 5, the polishing liquid C was used. The contact angle of the polishing liquid with respect to the polishing carrier is large when the polishing liquid C is used and is small when the polishing liquid B is used. This is considered to be due to the difference in the electrolyte concentration of the polishing liquid. That is, the polishing liquid C has a high electrolyte concentration, the polishing liquid A has an electrolyte concentration next to the polishing liquid C, and the polishing liquid B has an electrolyte concentration lower than the polishing liquid A.

主表面研磨工程に用いた研磨液は、25℃における粘度を1.6mPa・s、研磨液における砥粒(シリカ)の含有量は7質量%とした。研磨液のpHは4となるようにクエン酸で調整した。   The polishing liquid used in the main surface polishing step had a viscosity at 25 ° C. of 1.6 mPa · s, and the content of abrasive grains (silica) in the polishing liquid was 7% by mass. The pH of the polishing liquid was adjusted with citric acid so as to be 4.

[評価方法]
(1)研磨パッドに対する研磨液の接触角
例1〜例7で使用した研磨パッドは、研磨面をドレス処理し、純水を用いて洗浄した後、室温で1日乾燥させた。乾燥させた研磨パッドの研磨面に、研磨液1μlを滴下し、研磨液を滴下してから50秒後の接触角を接触角測定装置(協和界面科学製、型式:PCA−1)により測定した。
[Evaluation method]
(1) Contact angle of polishing liquid with respect to polishing pad The polishing pad used in Examples 1 to 7 was dressed on the polishing surface, washed with pure water, and then dried at room temperature for 1 day. 1 μl of polishing liquid was dropped onto the polishing surface of the dried polishing pad, and the contact angle 50 seconds after the polishing liquid was dropped was measured with a contact angle measuring device (manufactured by Kyowa Interface Science, model: PCA-1). .

(2)研磨用キャリアに対する研磨液の接触角
乾燥させた研磨用キャリアの表面に、研磨液1μlを滴下し、研磨液を滴下してから0.1秒後の接触角を接触角測定装置(協和界面科学製、型式:PCA−1)により測定した。
(2) Contact angle of polishing liquid with respect to polishing carrier 1 μl of polishing liquid is dropped onto the surface of the dried polishing carrier, and the contact angle 0.1 seconds after dropping the polishing liquid is measured with a contact angle measuring device ( It was measured by Kyowa Interface Science, model: PCA-1.

(3)研磨パッドの寿命
研磨パッドの寿命は、前記工程3の3次研磨(仕上げ研磨)において、研磨開始から、研磨パッドの研磨面に傷が生じた時点または研磨時にガラスが破損し、パッドに傷が発生して使用を停止した時点までの研磨パッドでガラス基板の主平面を研磨した時間の積算を測定し、下記A〜Cに示す基準により評価した。
A:研磨パッドでガラス基板の主平面を研磨した時間の積算が1200分間以上
B:研磨パッドでガラス基板の主平面を研磨した時間の積算が800分間以上、1200分間未満
C:研磨パッドでガラス基板の主平面を研磨した時間の積算が800分間未満
(3) Life of the polishing pad The life of the polishing pad is the same as that in the third polishing (finish polishing) in the above-described step 3, since the polishing surface of the polishing pad is damaged or glass is damaged when polishing is started. The integration of the time for polishing the main surface of the glass substrate with the polishing pad up to the point of time when the scratch was generated and the use was stopped was measured and evaluated according to the criteria shown in the following AC.
A: Accumulation time of polishing main surface of glass substrate with polishing pad is 1200 minutes or more B: Accumulation time of polishing main surface of glass substrate with polishing pad is 800 minutes or more and less than 1200 minutes C: Glass with polishing pad The accumulated time for polishing the main surface of the substrate is less than 800 minutes.

(4)研磨液の粘度
研磨液の粘度は、25℃の研磨液について、回転速度100rpmで、粘度計(メーカ:東機産業製、型式:回転式粘度計RE80L)を用いて測定した。
(4) Viscosity of polishing liquid The viscosity of the polishing liquid was measured with a viscometer (manufacturer: manufactured by Toki Sangyo Co., Ltd., model: rotary viscometer RE80L) at a rotational speed of 100 rpm with respect to the polishing liquid at 25 ° C.

(5)研磨液のpH
研磨液のpHは、純正化学製pH標準液[フタル酸塩pH標準液(pH4.01)、中性リン酸塩pH標準液(pH6.86)、ホウ酸塩pH標準液(pH9.18)]を使用し、3点校正を行った後、純水でpH電極を洗浄後、pH測定機(堀場製作所社製、型式:D−53S)を用いて研磨液のpH測定を行った。
(5) pH of polishing liquid
The pH of the polishing solution is a pH standard solution manufactured by Pure Chemical [phthalate pH standard solution (pH 4.01), neutral phosphate pH standard solution (pH 6.86), borate pH standard solution (pH 9.18). ], The pH electrode was washed with pure water, and then the pH of the polishing liquid was measured using a pH measuring machine (Horiba, Ltd., model: D-53S).

結果を表1に示す。   The results are shown in Table 1.

Figure 0006330628
Figure 0006330628

表1に示すように、研磨液1μlを研磨パッドの研磨面に滴下してから50秒後の研磨液の研磨パッドに対する接触角が50°以下である例1〜5は、該接触角が50°超である例6および7と比較して、研磨パッドの寿命が長かった。   As shown in Table 1, Examples 1 to 5 in which the contact angle of the polishing liquid to the polishing pad 50 seconds after dropping 1 μl of the polishing liquid onto the polishing surface of the polishing pad is 50 ° or less have a contact angle of 50 The life of the polishing pad was longer compared to Examples 6 and 7, which were above °.

この結果から、研磨液1μlを研磨パッドの研磨面に滴下してから50秒後の研磨液の研磨パッドに対する接触角が50°以下である研磨液と研磨パッド、つまり、研磨パッドに対する研磨液の浸透性がよい研磨液と研磨パッドとの組み合わせを用いることにより、研磨パッドの寿命を延ばせることがわかった。   From this result, the polishing liquid and the polishing pad having a contact angle of 50 ° or less with respect to the polishing pad 50 seconds after dropping 1 μl of the polishing liquid onto the polishing surface of the polishing pad, that is, the polishing liquid to the polishing pad It has been found that the life of the polishing pad can be extended by using a combination of a polishing liquid and a polishing pad with good permeability.

また、研磨液1μlを研磨用キャリアの表面に滴下してから0.1秒後の研磨液の研磨用キャリアに対する接触角が75°以下である例1〜4は、該接触角が75°超である例5と比較して、研磨パッドの寿命がより長かった。   In addition, in Examples 1 to 4 in which the contact angle of the polishing liquid to the polishing carrier 0.1 seconds after dropping 1 μl of the polishing liquid on the surface of the polishing carrier is 75 ° or less, the contact angle exceeds 75 °. The life of the polishing pad was longer than that of Example 5 which is

この結果から、研磨液1μlを研磨用キャリアの表面に滴下してから0.1秒後の研磨液の研磨用キャリアに対する接触角が75°以下である研磨液と研磨用キャリアを用いることにより、研磨パッドの寿命をより延ばせることがわかった。   From this result, by using a polishing liquid and a polishing carrier in which the contact angle of the polishing liquid with respect to the polishing carrier 0.1 seconds after dropping 1 μl of the polishing liquid on the surface of the polishing carrier is 75 ° or less, It has been found that the life of the polishing pad can be further extended.

Claims (5)

ショアD硬度が40以下である発泡樹脂の研磨層を有する研磨パッドと、砥粒として一次粒子径が3〜50nmであるシリカを含有する研磨液とを用いて、研磨用キャリアの保持孔に保持されたガラス基板の主平面を研磨する研磨工程と、ガラス基板の表面を洗浄する洗浄工程とを有する、ガラス基板の製造方法であって、
前記研磨工程において、研磨液1μlを研磨パッドの研磨面に滴下してから50秒後の研磨液の接触角が50°以下となる研磨パッドと研磨液を用いてガラス基板の主平面を研磨することを特徴とするガラス基板の製造方法。
Using a polishing pad having a foamed resin polishing layer having a Shore D hardness of 40 or less, and a polishing liquid containing silica having a primary particle diameter of 3 to 50 nm as abrasive grains, held in the holding holes of the polishing carrier A method for producing a glass substrate, comprising: a polishing step for polishing a principal plane of the glass substrate, and a cleaning step for cleaning the surface of the glass substrate,
In the polishing step, the main surface of the glass substrate is polished by using the polishing pad and the polishing liquid at which the contact angle of the polishing liquid is 50 ° or less after 50 seconds from dropping 1 μl of the polishing liquid onto the polishing surface of the polishing pad. A method for producing a glass substrate, comprising:
前記研磨用キャリアにおいて、研磨液1μlを前記研磨用キャリアの表面に滴下してから0.1秒後の研磨液の接触角が75°以下である請求項1記載のガラス基板の製造方法。   2. The method for producing a glass substrate according to claim 1, wherein in the polishing carrier, the contact angle of the polishing solution after 0.1 seconds after dropping 1 μl of the polishing solution on the surface of the polishing carrier is 75 ° or less. 前記研磨液は、25℃における粘度が1.7mPa・s以下である請求項1または2に記載のガラス基板の製造方法。   The method for producing a glass substrate according to claim 1, wherein the polishing liquid has a viscosity at 25 ° C. of 1.7 mPa · s or less. 前記研磨液は、pH1〜pH6であり、砥粒であるシリカの含有量が5〜25質量%である請求項1〜3のいずれか1項に記載のガラス基板の製造方法。   The said polishing liquid is pH1-pH6, and content of the silica which is an abrasive grain is 5-25 mass%, The manufacturing method of the glass substrate of any one of Claims 1-3. 前記ガラス基板は、中央部に円孔を有する磁気記録媒体用ガラス基板である請求項1〜4のいずれか1項に記載のガラス基板の製造方法。   The said glass substrate is a glass substrate for magnetic recording media which has a circular hole in the center part, The manufacturing method of the glass substrate of any one of Claims 1-4.
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