JP2006351081A - Grinding method of magnetic disk substrate - Google Patents

Grinding method of magnetic disk substrate Download PDF

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JP2006351081A
JP2006351081A JP2005174056A JP2005174056A JP2006351081A JP 2006351081 A JP2006351081 A JP 2006351081A JP 2005174056 A JP2005174056 A JP 2005174056A JP 2005174056 A JP2005174056 A JP 2005174056A JP 2006351081 A JP2006351081 A JP 2006351081A
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polishing
rinsing
glass substrate
grinding
substrate
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JP4560789B2 (en
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Kengo Kainuma
研吾 貝沼
Mitsuyoshi Ichino
光由 市野
Naohiro Jinnai
直寛 神内
Takeshi Kobayashi
毅 小林
Kazuto Higuchi
和人 樋口
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Fuji Electric Co Ltd
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Fuji Electric Holdings Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a grinding-processing method in which quality of products is improved by preventing dirt of a grinding pad and clogging caused by grinding and preventing variation of quality of coarseness of a ground surface. <P>SOLUTION: The grinding method of a glass substrate for a magnetic disk includes at least a process in which the glass substrate for the magnetic disk is ground and a process in which the glass substrate is rinsed after grinding. The grinding process includes a finish-grinding-processing-process using colloidal silica as a main component of grinding grains. The method is characterized in that the rinse process is performed while rinse liquid is applied without stopping a surface plate directly after this grinding, the rinse liquid used in this rinse process is pure water including surfactant, further, pH is adjusted to 8-12 by adding alkali. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

本発明は、ハードディスク装置用の磁気記録媒体である磁気ディスクに用いるための情報記録媒体用ガラス基板の研磨方法に関する。   The present invention relates to a method for polishing a glass substrate for an information recording medium for use in a magnetic disk that is a magnetic recording medium for a hard disk device.

ハードディスクは、年々小型化、大容量化の一途をたどっている。そのため磁気記録媒体(以下磁気ディスクとも称する)の高密度化が進み、さらには磁気ヘッドの浮上量もますます小さくなってきている。このような現状から、磁気ディスク基板の表面精度の向上が求められている。磁気ディスク基板の表面精度を向上するには、磁気ディスク基板の研磨工程で、基板表面粗さの低減、基板の微少うねりの低減及びマイクロスクラッチ等の基板表面の欠陥の低減が求められる。また、砥粒や研磨カス等の残留のない基板が求められる。   Hard disks are becoming smaller and larger in capacity year after year. For this reason, the density of magnetic recording media (hereinafter also referred to as magnetic disks) is increasing, and the flying height of the magnetic head is also becoming smaller. Under such circumstances, improvement of the surface accuracy of the magnetic disk substrate is required. In order to improve the surface accuracy of the magnetic disk substrate, it is required to reduce the substrate surface roughness, reduce the slight waviness of the substrate, and reduce defects on the substrate surface such as micro scratches in the polishing process of the magnetic disk substrate. Further, a substrate having no residue of abrasive grains or polishing residue is required.

磁気ディスク基板の表面精度を向上するには、研磨布(パッド)に、孔径がより小さいものが使われてきている。また硬い研磨パッドが用いられてきている。このような状況下では、研磨粒子や研磨カスが研磨パッドの孔に滞留および/または付着しやすく、連続的に研磨を行うと、パッドの汚れや目詰まりを引き起こす。これは、加工表面の粗さの品質にバラツキを引き起こす原因となるため、定期的にパッドドレッシングを行う必要がある。   In order to improve the surface accuracy of the magnetic disk substrate, a polishing cloth (pad) having a smaller hole diameter has been used. Hard polishing pads have been used. Under such circumstances, the abrasive particles and debris are likely to stay and / or adhere to the pores of the polishing pad, and continuous polishing causes the pad to become dirty and clogged. Since this causes variations in the quality of the roughness of the processed surface, it is necessary to periodically perform pad dressing.

しかしながら、パッドに付着した研磨粒子や研磨カスをパッドドレッシングで完全に除去するのは難しく、研磨粒子や研磨カスが研磨回数と共にパッド表面に堆積してしまう。研磨中、これらが基板表面と擦れ合うことにより、基板表面の品質を不安定化させる要因となっている。   However, it is difficult to completely remove the abrasive particles and debris adhering to the pad by the pad dressing, and the abrasive particles and debris accumulate on the pad surface with the number of times of polishing. During polishing, these rub against the substrate surface, which causes the quality of the substrate surface to become unstable.

例えば、Ni−Pめっきアルミニウム合金基板の研磨加工は2段階加工が行われており、研磨剤として1段階目にアルミナ、2段階目の仕上げにコロイダルシリカが使われている。ここで1段目のアルミナと粒を2段目の加工工程に持ち込まないようリンス方法およびリンス液が検討されている。特許文献1、2および3はその1例であり、最近になってもさらに優れたリンス剤が求められており、開発が進められている。   For example, a polishing process of a Ni—P plated aluminum alloy substrate is performed in two stages, and alumina is used as the polishing agent in the first stage and colloidal silica is used in the finishing process in the second stage. Here, a rinsing method and a rinsing liquid have been studied so as not to bring the first-stage alumina and grains into the second-stage processing step. Patent Documents 1, 2 and 3 are examples thereof, and even recently, a more excellent rinse agent has been demanded, and development is in progress.

また、ガラス基板の仕上げ研磨に関しては、例えば特許文献4がある。この文献には、ガラス基板を研磨後に純水でリンスした後、ガラス基板表面上のコロイダルシリカを除去するためにpH12以下のアルカリ性水溶液で基板を洗浄すること、およびこの洗浄液に洗浄補助剤としてアニオン性またはノニオン性界面活性剤を添加することが開示されている。   Further, for example, there is Patent Document 4 regarding finish polishing of a glass substrate. In this document, a glass substrate is rinsed with pure water after polishing, and then the substrate is washed with an alkaline aqueous solution having a pH of 12 or less in order to remove colloidal silica on the surface of the glass substrate. Addition of a neutral or nonionic surfactant is disclosed.

さらに、特許文献5には、半導体ウェハの洗浄工程に使用しうる半導体ウェハの洗浄方法および洗浄装置が開示されている。特に、この文献には、半導体ウェハ上に頑強に付着している粒子を除去し、さらに洗浄後のセルフクリーニングを容易に行うことができる方法と装置が開示されている。さらにこの文献には、洗浄液として界面活性剤を使用することが開示されているが、この文献の洗浄工程は、研磨後のリンス工程またはブラシ洗浄によるスクラブ洗浄工程を経た後の洗浄工程に関する。   Further, Patent Document 5 discloses a semiconductor wafer cleaning method and a cleaning apparatus that can be used in a semiconductor wafer cleaning process. In particular, this document discloses a method and an apparatus that can remove particles firmly attached on a semiconductor wafer and can easily perform self-cleaning after cleaning. Further, although this document discloses the use of a surfactant as a cleaning liquid, the cleaning process of this document relates to a cleaning process after a rinsing process after polishing or a scrub cleaning process by brush cleaning.

特開2000−144193号公報JP 2000-144193 A 特開平10−152674号公報JP-A-10-152675 特開2004−182800号公報JP 2004-182800 A 特開2004−63062号公報JP 2004-63062 A 特開平8−71511号公報JP-A-8-71511

上述のように研磨後の洗浄については種々の検討がなされているが、ガラス基板の仕上げ研磨の直後におけるリンス工程で、パッドの汚染に係わるガラス基板表面の品質の不安定化を防止するためのリンス方法に関しては、未だ十分な検討が行われていないのが現状である。   As described above, various studies have been made on the cleaning after polishing. In the rinsing process immediately after the final polishing of the glass substrate, in order to prevent destabilization of the quality of the glass substrate surface due to pad contamination. The rinsing method has not yet been fully examined.

本発明は、リンス工程において、研磨で生じる研磨パッドの汚染および目詰まりを防止することにより、このような汚染および目詰まりの発生に起因する研磨された基板表面の粗さの品質のバラツキを防止し、製品の品質を向上できる研磨加工方法を提供することを目的とする。   In the rinsing process, the present invention prevents contamination of the polishing pad and clogging caused by polishing, thereby preventing variations in roughness quality of the polished substrate surface due to the occurrence of such contamination and clogging. And it aims at providing the grinding | polishing processing method which can improve the quality of a product.

本発明は、磁気ディスク用ガラス基板の研磨方法に関する。この方法は、磁気ディスク用ガラス基板を研磨する工程と、研磨後に該ガラス基板をリンスする工程とを少なくとも含み、前記研磨工程がコロイダルシリカを研磨砥粒の主成分として用いる仕上研磨加工工程を含み、前記リンス工程がこの研磨直後に、定盤を停止せずにリンス液を流しながら行われ、このリンス工程で用いられるリンス液が界面活性剤を含有した純水であり、さらにアルカリを添加してpHが8〜12に調整されたものである。   The present invention relates to a method for polishing a glass substrate for a magnetic disk. This method includes at least a step of polishing a glass substrate for magnetic disk and a step of rinsing the glass substrate after polishing, and the polishing step includes a finish polishing step using colloidal silica as a main component of abrasive grains. The rinsing step is performed immediately after this polishing while flowing the rinsing liquid without stopping the surface plate. The rinsing liquid used in this rinsing step is pure water containing a surfactant, and further added with alkali. The pH is adjusted to 8-12.

本発明の研磨方法は、リンス工程の後に、さらに純水にアルカリを添加してpH8から12に調整された第二のリンス液で追加リンスすることができる。   In the polishing method of the present invention, after the rinsing step, additional rinsing can be performed with a second rinsing liquid adjusted to pH 8 to 12 by adding alkali to pure water.

本発明の研磨方法を用いることにより、表面粗さ(Ra)の安定した基板を得ることができ、さらにはパッドの交換頻度も低減できる、という効果が得られる。   By using the polishing method of the present invention, it is possible to obtain a substrate having a stable surface roughness (Ra) and to reduce the frequency of pad replacement.

本発明を以下に詳細に説明する。
本発明で使用しうるガラス基板は、例えば中心に円孔を有した円盤状をなす、磁気ディスク等の磁気情報記録媒体の基板として用いられるものである。この磁気記録媒体用ガラス基板の材料としては、特に限定されないが、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、結晶化ガラス等が挙げられる。これらのガラス基板は、例えばフロート法、ダウンドロー法、リドロー法またはプレス法などの従来の手順で製造することができる。
The present invention is described in detail below.
The glass substrate that can be used in the present invention is used, for example, as a substrate for a magnetic information recording medium such as a magnetic disk having a disk shape with a circular hole in the center. The material for the magnetic recording medium glass substrate is not particularly limited, and examples thereof include soda lime glass, aluminosilicate glass, borosilicate glass, and crystallized glass. These glass substrates can be manufactured by a conventional procedure such as a float method, a downdraw method, a redraw method, or a press method.

上述したように磁気記録媒体は、その表面と、この磁気記録媒体に情報を読み書きするためのヘッドとの距離を狭めることにより、高密度記録化が図られている。磁気記録媒体の表面とヘッドとの距離を狭める場合、磁気記録媒体用ガラス基板の表面に凹凸が存在すると基板上に形成される磁性膜からなる磁気記録部にも凹凸が形成さる。データを読み取るためにヘッドが移動中にこの凹凸に接触または干渉し、記録された情報が正確に読み取れなかったり、ヘッドが破損したり、磁気記録部が傷ついたりする場合があり、不具合を起こすおそれがある。このような不具合を防止するため、磁気記録媒体用ガラス基板を、高精度な研磨処理で研磨することにより、凹凸の発生を抑える試みがなされている。しかし、さらに品質の安定性を保持できる研磨方法が求められている。   As described above, high-density recording is achieved by reducing the distance between the surface of the magnetic recording medium and the head for reading and writing information on the magnetic recording medium. When the distance between the surface of the magnetic recording medium and the head is narrowed, if irregularities exist on the surface of the glass substrate for magnetic recording medium, the irregularities are also formed on the magnetic recording portion formed of the magnetic film formed on the substrate. The head may come in contact with or interfere with this unevenness to read data, and the recorded information may not be read accurately, the head may be damaged, or the magnetic recording section may be damaged, causing problems. There is. In order to prevent such problems, attempts have been made to suppress the occurrence of unevenness by polishing the glass substrate for magnetic recording media with a highly accurate polishing process. However, there is a demand for a polishing method that can maintain the quality stability.

本発明者らは、このような凹凸が形成される原因を検討し、ガラス基板表面に凹凸が形成される要因の1つは、リンス工程において、研磨工程で使用される砥粒が研磨パッドの汚染または目詰まりを引き起こし、連続的な研磨により、このような汚染または目詰まりした研磨パッドが、ガラス基板を傷つけることを見出した。このような汚染または目詰まりした研磨パッドから汚染を除去したり、目詰まりした砥粒を完全に取り除くことは困難である。また、汚染や目詰まりした研磨パッドを汚染または目詰まりするごとに新しいものと交換することはコストの増加に繋がる。   The present inventors have examined the cause of the formation of such irregularities, and one of the causes for the formation of irregularities on the surface of the glass substrate is that the abrasive grains used in the polishing step in the rinsing step are those of the polishing pad. It has been found that such a contaminated or clogged polishing pad damages the glass substrate due to contamination or clogging, and continuous polishing. It is difficult to remove contamination from such a contaminated or clogged polishing pad or to completely remove clogged abrasive grains. In addition, replacing a contaminated or clogged polishing pad with a new one every time it is contaminated or clogged leads to an increase in cost.

本発明者らは、このような不都合を防止することにより、汚染および目詰まりの発生に起因する研磨表面粗さの品質のバラツキを防止し、製品の品質を向上させる、研磨方法を見出した。本発明の研磨方法は、ガラス基板表面の研磨工程がコロイダルシリカを研磨砥粒の主成分として用いる仕上げ研磨工程を含み、この研磨工程直後のリンス工程が、定盤を停止せずにリンス液を流しながら行われ、このリンス液が界面活性剤を含有した純水であり、さらにアルカリを添加してpHが8〜12に調整されたものであることを特徴とする。   The inventors of the present invention have found a polishing method that prevents such inconvenience, thereby preventing variations in the quality of the polished surface roughness due to the occurrence of contamination and clogging and improving the quality of the product. In the polishing method of the present invention, the polishing process on the surface of the glass substrate includes a finish polishing process using colloidal silica as a main component of the abrasive grains, and the rinsing process immediately after the polishing process is performed without rinsing the surface plate. The rinsing solution is pure water containing a surfactant, and the pH is adjusted to 8 to 12 by adding an alkali.

このような工程を含むことにより、本発明の方法は、仕上げ研磨工程で使用された砥粒(コロイダルシリカ)をガラス基板表面から除去すると同時に、研磨パッドへの砥粒の堆積を防止ができる。これにより、長時間連続的に仕上げ研磨を行った場合であっても研磨パッドの汚染または目詰まりを防止でき、研磨パッドの汚染または目詰まりに基づくガラス基板表面の品質のばらつきを防止することが可能となる。   By including such a step, the method of the present invention can remove the abrasive grains (colloidal silica) used in the finish polishing step from the glass substrate surface and at the same time prevent the abrasive grains from being deposited on the polishing pad. As a result, contamination or clogging of the polishing pad can be prevented even when finish polishing is performed continuously for a long time, and variations in the quality of the glass substrate surface due to contamination or clogging of the polishing pad can be prevented. It becomes possible.

本発明の研磨方法は、仕上げ研磨工程と、この直後のリンス工程を少なくとも含む。本発明では、ガラス基板は仕上げ研磨工程に先立って、ガラス基板の切り出し、切り出した基板の粗研磨加工等の従来の加工を施される。   The polishing method of the present invention includes at least a final polishing step and a rinsing step immediately after this. In the present invention, prior to the finish polishing step, the glass substrate is subjected to conventional processing such as cutting out the glass substrate and rough polishing processing of the cut out substrate.

本発明の研磨方法では、まず、シート状のガラス板から円盤状のガラス基板を切り出し、その外径寸法及び内径寸法を所定長さとした後、ガラス基板の表面に以下の研磨処理を施す。なお、研磨処理は、ガラス基板を一枚ずつ研磨する枚葉方式、複数枚のガラス基板を一度に研磨するバッチ方式のいずれの方式で行ってもよいが、生産性の観点から、一般にはバッチ方式が用いられている。   In the polishing method of the present invention, first, a disk-shaped glass substrate is cut out from a sheet-like glass plate, and the outer diameter dimension and inner diameter dimension thereof are set to predetermined lengths, and then the following polishing treatment is performed on the surface of the glass substrate. The polishing treatment may be performed by either a single wafer method in which glass substrates are polished one by one or a batch method in which a plurality of glass substrates are polished at one time. The method is used.

研磨処理では、まず、ガラス基板の表面にラップ加工が施される。このラップ加工は、ガラス基板の厚み、平面度、平行度を所定値にするとともに、大きなうねり、欠け(チッピング)、ひび(クラック)等の大きな欠陥等を取り除くために行われる。   In the polishing process, first, lapping is performed on the surface of the glass substrate. This lapping is performed to set the thickness, flatness, and parallelism of the glass substrate to predetermined values, and to remove large defects such as large waviness, chipping (chipping), and cracking (crack).

ラップ加工の後に、一般には2段階の粗研磨加工がガラス基板の表面に施される。この粗研磨加工は、ラップ跡(マイクロクラック)を除去すると共に、表面状態を良好にするために行われ、従来の条件・方法を適用することができる。例えば、ガラス基板の表面を粗研磨するために1段目の加工は、硬質ポリッシャ(例えば、JIS K6253−1997に規定される硬度(タイプA)が75〜95)等が使用され、2段目の加工に軟質ポリッシャ(例えば硬度60〜75)が使用される。   After lapping, generally, a two-step rough polishing process is performed on the surface of the glass substrate. This rough polishing process is performed in order to remove lap marks (microcracks) and improve the surface condition, and conventional conditions and methods can be applied. For example, a hard polisher (for example, a hardness (type A) defined in JIS K6253-1997 is 75 to 95) or the like is used for the first step for rough polishing the surface of the glass substrate. A soft polisher (for example, hardness 60-75) is used for the process of this.

粗研磨加工の研磨剤には、例えば1段目には、平均粒径1.2μm前後、2段目には、粒径数百nm以下の研磨材を溶媒としての水に分散させてスラリー状としたものが使用される。該研磨材としては、アルミナ砥粒、酸化セリウムや酸化ランタン等の希土類酸化物、酸化ジルコニウム、二酸化マンガン、酸化アルミニウム、コロイダルシリカ等が挙げられる。これらのうち、希土類酸化物は研磨効率が優れていることから好ましく、希土類酸化物のなかでも酸化セリウムがより好ましい。   As the abrasive for rough polishing, for example, the first stage has an average particle size of about 1.2 μm, and the second stage has an abrasive having a particle size of several hundred nm or less dispersed in water as a solvent to form a slurry. Is used. Examples of the abrasive include alumina abrasive grains, rare earth oxides such as cerium oxide and lanthanum oxide, zirconium oxide, manganese dioxide, aluminum oxide, and colloidal silica. Of these, rare earth oxides are preferred because of their excellent polishing efficiency, and cerium oxide is more preferred among the rare earth oxides.

この粗研磨加工でガラス基板は、その表面の表面粗さ(Ra)が0.5nm未満、好ましくはRaを0.3nm未満とすることが好ましい。   In this rough polishing, the glass substrate has a surface roughness (Ra) of less than 0.5 nm, preferably Ra of less than 0.3 nm.

本発明では、例えば上記の砥粒を含むスラリーを流しながら、定盤上に保持されたガラス基板を回転させ、研磨パッドを当接させて基板表面上を擦ることにより粗研磨工程を行うことができる。   In the present invention, for example, the rough polishing step is performed by rotating the glass substrate held on the surface plate while rubbing the slurry containing the above-mentioned abrasive grains, and abutting the polishing pad and rubbing the surface of the substrate. it can.

次に、ガラス基板の表面に仕上げ研磨加工が施される。この仕上げ研磨加工は、表面状態を平滑で高品質なものとするために行われる。   Next, finish polishing is performed on the surface of the glass substrate. This finish polishing is performed in order to make the surface state smooth and high quality.

この仕上げ研磨工程ではガラス基板の表面を研磨するために、発泡ウレタン、不織布などの研磨パッドを使用することができる。   In this final polishing step, a polishing pad such as foamed urethane or nonwoven fabric can be used to polish the surface of the glass substrate.

仕上げ研磨工程の研磨剤には、二酸化ケイ素(SiO)を主成分とし、平均粒径が150nm以下である粒子、好ましくはコロイダルシリカ、を溶媒に分散させて得られた懸濁液が使用される。研磨剤中における粒子の濃度は、3〜40質量%とすることが好ましい。 As the polishing agent in the final polishing step, a suspension obtained by dispersing particles having silicon dioxide (SiO 2 ) as a main component and having an average particle diameter of 150 nm or less, preferably colloidal silica, in a solvent is used. The The concentration of particles in the abrasive is preferably 3 to 40% by mass.

本発明では、例えば純水にコロイダルシリカを含むスラリーを流しながら、定盤上に保持されたガラス基板(粗研磨されたもの)を回転させ、研磨パッドを当接させて基板表面上を擦ることにより仕上げ研磨工程を行うことができる。   In the present invention, for example, while flowing a slurry containing colloidal silica in pure water, a glass substrate (roughly polished) held on a surface plate is rotated, and a polishing pad is contacted to rub on the substrate surface. Thus, the finish polishing step can be performed.

仕上げ研磨工程での研磨レート、研磨時間、加工圧力、定盤回転数、スラリ供給量などの諸条件は、従来のものを適用できるが、例えば、Speed FAM 9B両面研磨機(5キャリアタイプ)の場合、好ましくは以下の範囲である。
研磨レート:10〜100nm/min
研磨時間:1〜20分
加工圧力:40〜120g/cm
定盤回転数:上6〜15rpm、下20〜40rpm
スラリ供給量:50〜250cc/分
Conventional conditions can be applied to various conditions such as polishing rate, polishing time, processing pressure, surface plate rotation speed, and slurry supply amount in the final polishing process. For example, a Speed FAM 9B double-side polishing machine (5-carrier type) In the case, it is preferably in the following range.
Polishing rate: 10 to 100 nm / min
Polishing time: 1 to 20 minutes Processing pressure: 40 to 120 g / cm 2
Surface plate rotation speed: Upper 6-15 rpm, Lower 20-40 rpm
Slurry supply amount: 50-250cc / min

次に、仕上げ研磨工程の直後に、リンス工程を行う。このリンス工程は、ガラス基板の表面及び研磨パッドの中から残留する研磨剤を洗い流すこと、および、研磨パッド表面への研磨剤と研磨クズの堆積を防止するために行われる。   Next, a rinse process is performed immediately after the finish polishing process. This rinsing step is performed in order to wash away the abrasive remaining from the surface of the glass substrate and the polishing pad, and to prevent accumulation of abrasive and polishing debris on the surface of the polishing pad.

ガラス基板をリンスするためのリンス液としては、アルカリと界面活性剤を含む。特に本発明では、溶媒に水を用い、アルカリにより、pH8〜12の範囲内に調製されたリンス液を用いる。   The rinsing liquid for rinsing the glass substrate includes an alkali and a surfactant. In particular, in the present invention, water is used as a solvent, and a rinse solution prepared in the range of pH 8 to 12 with an alkali is used.

界面活性剤は、アニオン系界面活性剤及びノニオン系界面活性剤からなる群から選ばれた少なくとも1種である。アニオン系界面活性剤は、好ましくは、カルボン酸塩、スルホン酸塩、硫酸エステル塩、燐酸エステル塩の低分子の化合物及び高分子型化合物からなる群から選ばれた少なくとも1種である。ノニオン系界面活性剤は、好ましくは、多価アルコール、ポリオキシエチレンアルキルエーテル、脂肪酸酸化エチレン、ポリプロピレングリコール酸化エチレン、脂肪族アミンおよび脂肪族アミドの酸化エチレン化合物、ポリオキシエチレン脂肪酸エステルからなる群から選ばれた少なくとも1種である。   The surfactant is at least one selected from the group consisting of an anionic surfactant and a nonionic surfactant. The anionic surfactant is preferably at least one selected from the group consisting of a low molecular weight compound such as a carboxylate, a sulfonate, a sulfate ester salt, and a phosphate ester salt, and a polymer compound. The nonionic surfactant is preferably selected from the group consisting of polyhydric alcohols, polyoxyethylene alkyl ethers, fatty acid ethylene oxides, polypropylene glycol ethylene oxides, aliphatic amines and ethylene oxide compounds of aliphatic amides, and polyoxyethylene fatty acid esters. At least one selected.

アルカリは、好ましくは、NaOH、KOH、NaCO、NaSO、KCO、KSO、および有機アルカリ塩からなる群から選ばれた少なくとも1種である。このアルカリにより、本発明のリンス液のpHを調節する。 The alkali is preferably at least one selected from the group consisting of NaOH, KOH, Na 2 CO 3 , Na 2 SO 4 , K 2 CO 3 , K 2 SO 4 , and an organic alkali salt. The pH of the rinse solution of the present invention is adjusted by this alkali.

リンス液の界面活性剤の含有量は、界面活性剤の種類により異なるが、東邦化学工業のトーホークリンや花王のクリンスルーの場合には、0.05〜3重量%である。アルカリは、所望のpHとなる量を添加する。   The content of the surfactant in the rinsing liquid varies depending on the type of the surfactant, but it is 0.05 to 3% by weight in the case of Toho Chemical manufactured by Toho Chemical Industry or Kao Clean Through. The alkali is added in an amount that provides the desired pH.

本発明のリンス工程は、仕上げ研磨工程の直後に、このリンス工程は、研磨剤に代えて本発明のリンス液をを供給しながら研磨パッドにより表面を擦ることにより行われる。本発明では、上記リンス液を流しながら、定盤を停止せずに研磨パッドによりガラス表面を擦りながらリンス工程を行うことが好ましい。リンス時間、加工圧力、定盤回転数、スラリ供給量などの諸条件は、本発明の目的を達成する限り特に限定されないが、例えば、上述のSpeed FAM 9B両面研磨機(5キャリアタイプ)の場合、以下の範囲が好適である。
リンス時間:0.5〜5分
加工圧力:10〜50g/cm
定盤回転数:上3〜15rpm、下10〜40rpm
リンス液供給量:0.5〜2L/分
The rinsing step of the present invention is performed immediately after the finish polishing step by rubbing the surface with a polishing pad while supplying the rinsing liquid of the present invention instead of the abrasive. In the present invention, it is preferable to perform the rinsing step while rubbing the glass surface with a polishing pad without stopping the surface plate while flowing the rinsing liquid. Various conditions such as the rinsing time, processing pressure, surface plate rotation speed, and slurry supply amount are not particularly limited as long as the object of the present invention is achieved. The following ranges are preferred.
Rinse time: 0.5 to 5 minutes Processing pressure: 10 to 50 g / cm 2
Surface plate rotation speed: Upper 3-15 rpm, lower 10-40 rpm
Rinse solution supply amount: 0.5 to 2 L / min

本発明のリンス工程では、研磨パッドは、予め決められた枚数の仕上げ研磨とリンスを行った後、ブラシキャリアなどによりドレッシングを施すことが好ましい。   In the rinsing step of the present invention, the polishing pad is preferably dressed with a brush carrier or the like after a predetermined number of finish polishing and rinsing.

本発明では、上記のリンス工程に続いて、後リンス工程を行うことが好ましい。これは、リンス後に界面活性剤が残留している研磨パッドで、次の研磨を実施すると、スラリ本来の研磨特性が得られず、レートの低下や研磨表面の微小うねりなどの悪影響が現れることがあるためである。このような減少を防止するために、本発明では、界面活性剤でのリンス直後に、続けてアルカリ水溶液で後リンスを実施することが好ましい。このアルカリ水溶液は、純水にNaOH、KOH、NaCO、NaSO、KCO、KSO、および有機アルカリ塩からなる群から選ばれた少なくとも1種を含み、pH値8〜12を有するものである。後リンスは、上記のリンス工程と同様な手順で行うことができる。 In this invention, it is preferable to perform a post-rinsing process following said rinse process. This is a polishing pad in which the surfactant remains after rinsing, and when the next polishing is performed, the original polishing characteristics of the slurry cannot be obtained, and adverse effects such as a decrease in rate and micro waviness of the polishing surface may appear. Because there is. In order to prevent such a decrease, in the present invention, it is preferable to perform post-rinsing with an alkaline aqueous solution immediately after rinsing with a surfactant. This alkaline aqueous solution contains at least one selected from the group consisting of NaOH, KOH, Na 2 CO 3 , Na 2 SO 4 , K 2 CO 3 , K 2 SO 4 , and an organic alkali salt in pure water, and has a pH It has a value of 8-12. The post rinse can be performed in the same procedure as the above rinse step.

リンス工程後、基板は、必要に応じて、アルカリ洗剤を用いたスクラブ洗浄、純水中の超音波(例えば1000kHz)でのリンス、遠心乾燥などの通常の手順を施すことができる。   After the rinsing step, the substrate can be subjected to ordinary procedures such as scrub cleaning using an alkaline detergent, rinsing with ultrasonic waves (for example, 1000 kHz) in pure water, and centrifugal drying as necessary.

以上申し述べた通り、本発明の研磨方法は、1)研磨開始/基板設置、2)研磨(例えば粗研磨+仕上げ研磨)、3)界面活性剤含有アルカリリンス液でのリンス、4)研磨終了/基板取り出し、により示される一連の工程を少なくとも含む。さらに、本発明では、上記3)のリンスの後、3’)アルカリ水溶液でのリンスをさらに含むことができる。   As described above, the polishing method of the present invention includes 1) polishing start / substrate setting, 2) polishing (for example, rough polishing + finish polishing), 3) rinsing with a surfactant-containing alkaline rinse solution, 4) polishing end / It includes at least a series of steps indicated by removing the substrate. Further, the present invention may further include 3 ') rinsing with an aqueous alkaline solution after the rinsing of 3).

本発明の方法により得られる磁気ディスク用ガラス基板は、表面粗さ(Ra)=0.08〜0.25nmを持つことができる。   The glass substrate for magnetic disks obtained by the method of the present invention can have a surface roughness (Ra) = 0.08 to 0.25 nm.

以下、本発明の実施例を説明する。なお、以下の実施例は例示であり、本発明はこれらの実施例に限定されない。   Examples of the present invention will be described below. In addition, the following Examples are illustrations and this invention is not limited to these Examples.

(実施例1)
平均粒径0.1μmのコロイダルシリカを約10重量%含み、pHが9.5に調整されたスラリを用いて、ガラス基板を表1の研磨条件で仕上げ研磨した。ここで、仕上げ研磨加工前の基板は、その前工程の粗研磨工程により、Ra=0.25nm程度になっている。
Example 1
The glass substrate was finish-polished under the polishing conditions shown in Table 1 using a slurry containing about 10% by weight of colloidal silica having an average particle size of 0.1 μm and having a pH adjusted to 9.5. Here, the substrate before the finish polishing is about Ra = 0.25 nm due to the rough polishing step in the previous step.

Figure 2006351081
Figure 2006351081

仕上げ研磨が終了すると同時に、研磨剤(スラリー)の供給を停止してリンス液に切り替え、表2に示した条件でリンスを実施した。リンス液は、純水にリン酸系界面活性剤(花王社製洗浄剤)を約1重量%含むガラス基板用洗浄剤を2重量%の割合で添加し、さらにNaOHを使ってpHを10.5に調整した。研磨を4回連続で実施する毎に、ナイロン製のブラシキャリアでパッドドレッシングを実施した。   At the same time as the finish polishing was completed, the supply of the abrasive (slurry) was stopped and switched to the rinse liquid, and the rinse was performed under the conditions shown in Table 2. The rinsing liquid is prepared by adding a glass substrate cleaning agent containing about 1% by weight of a phosphoric acid type surfactant (cleaning agent manufactured by Kao Corporation) to pure water at a rate of 2% by weight, and further using NaOH to adjust the pH to 10. Adjusted to 5. Every time polishing was performed four times in succession, pad dressing was performed with a nylon brush carrier.

Figure 2006351081
Figure 2006351081

研磨後の基板は、アルカリ洗剤を用いてスクラブ洗浄後、超音波(1000kHz)の純水でリンス後、遠心乾燥を実施した。   The substrate after polishing was scrubbed using an alkaline detergent, rinsed with ultrasonic (1000 kHz) pure water, and then subjected to centrifugal drying.

(比較例)
実施例のリンス液の代わりに、純水にNaOHを加えてpHを10.5にした水溶液を使用した。研磨条件、洗浄条件は、実施例1と同じ条件とした。
(Comparative example)
Instead of the rinsing liquid of the example, an aqueous solution in which NaOH was added to pure water to make the pH 10.5 was used. The polishing conditions and cleaning conditions were the same as in Example 1.

(実施例と比較例の比較評価)
実施例および比較例で研磨して洗浄した基板の表面をAFMで評価した結果を図1に示す。AFMの測定条件を以下に示す。
測定エリア:10μm×10μm
解像度:512×512
走査速度:1Hz
評価項目:面平均粗さ(Ra)
(Comparative evaluation of examples and comparative examples)
FIG. 1 shows the result of evaluation of the surface of the substrate polished and cleaned in Examples and Comparative Examples by AFM. AFM measurement conditions are shown below.
Measurement area: 10μm × 10μm
Resolution: 512 × 512
Scanning speed: 1Hz
Evaluation item: Surface average roughness (Ra)

図1に示されるように、比較例は研磨バッチ数30回からRaが増加傾向を示している。このように表面粗さが大きくなるのは、パッド表面の顕微鏡およびSEM観察により、パッドの表面に堆積した研磨剤と研磨クズが原因であることが明らかとなっている。   As shown in FIG. 1, the comparative example shows an increasing trend of Ra from 30 polishing batches. It is clear from the microscope and SEM observation of the pad surface that the surface roughness is increased due to the abrasive and polishing debris deposited on the surface of the pad.

本発明の実施例は、リンス工程において、基板表面の研磨剤および研磨クズが除去されると同時に、所定pHを有し、且つ界面活性剤を含んだリンス液を用いることにより、パッド表面への研磨剤と研磨クズの堆積を防止できる。このため、研磨バッチ数40回までの間、品質(Ra)の安定した基板の研磨加工ができることがわかる。   In the embodiment of the present invention, in the rinsing step, the polishing agent and polishing debris on the substrate surface are removed, and at the same time, by using a rinsing liquid having a predetermined pH and containing a surfactant, Accumulation of abrasive and polishing debris can be prevented. For this reason, it turns out that the grinding | polishing process of the board | substrate with stable quality (Ra) can be performed for up to 40 polishing batches.

(リンス液の液性(pH))
リンス液のpHと、研磨/リンス能の関係を調査した。結果を表3に示した。界面活性剤を添加したリンス液は添加していない液に比べて、大きいパッドの洗浄効果が得られる。また、液性がpH8以下ではパッドの清浄性を保てず、基板自体にも残渣が残り易い傾向が有る。またpHが12を超えるとコロイダルシリカの分散状態が不安定になるため、研磨表面の粗さをコントロールできず、表面粗さのバラツキが大きくなる傾向がある。
(Rinse solution liquidity (pH))
The relationship between the pH of the rinse solution and the polishing / rinsing ability was investigated. The results are shown in Table 3. The rinsing liquid to which the surfactant is added provides a larger pad cleaning effect than the liquid to which the surfactant is not added. In addition, when the liquidity is pH 8 or less, the cleanliness of the pad cannot be maintained, and the residue tends to remain on the substrate itself. If the pH exceeds 12, the dispersion state of the colloidal silica becomes unstable, so that the roughness of the polished surface cannot be controlled and the variation in the surface roughness tends to increase.

Figure 2006351081
Figure 2006351081

このように、リンス工程で用いるリンス液を、単にリンス液に界面活性剤を添加すること、あるいはリンス液のpHを所定のアルカリ性にすることのみでは、基板上の表面粗さのばらつきを制御することができない。しがたって研磨後のリンス液としては、界面活性剤を添加し、且つその液性をpH8〜12にコントロールしたものが適当である。また、本発明のリンス液は、仕上げ研磨工程にコロイダルシリカを用いる場合に特に有意な効果を示す。   As described above, the surface roughness variation on the substrate is controlled only by adding a surfactant to the rinse liquid used in the rinse process or by making the pH of the rinse liquid predetermined alkaline. I can't. Therefore, as the rinsing liquid after polishing, a liquid in which a surfactant is added and the liquid property is controlled to pH 8 to 12 is suitable. Moreover, the rinse liquid of the present invention exhibits a particularly significant effect when colloidal silica is used in the final polishing process.

(追加リンス)
本発明の研磨工程では、リンス工程後に研磨パッドに界面活性剤が残留するが、このようなパッドで、次の研磨を実施すると、スラリ本来の研磨特性が得られず、レートの低下や研磨表面の微小なうねりなどの悪影響が現れることがある。その対策として、界面活性剤でのリンス直後に、続けてアルカリ水溶液でリンスを実施することにより、パッドの残存界面活性剤濃度を減らし、研磨特性を安定に維持することができる。
(Additional rinse)
In the polishing step of the present invention, the surfactant remains on the polishing pad after the rinsing step. However, when the next polishing is carried out with such a pad, the original polishing characteristics of the slurry cannot be obtained, and the rate is lowered or the polishing surface is reduced. Adverse effects such as small swells may appear. As a countermeasure, by rinsing with an alkaline aqueous solution immediately after rinsing with a surfactant, the remaining surfactant concentration of the pad can be reduced and the polishing characteristics can be maintained stably.

実施例および比較例において研磨加工した基板の洗浄後の表面をAFMで評価した結果を示す図である。It is a figure which shows the result of having evaluated the surface after washing | cleaning of the board | substrate which grind-processed in the Example and the comparative example by AFM.

Claims (2)

磁気ディスク用ガラス基板を研磨する工程と、研磨後に該ガラス基板をリンスする工程とを少なくとも含む磁気ディスク用ガラス基板の研磨方法であって、前記研磨工程がコロイダルシリカを研磨砥粒の主成分として用いる仕上げ研磨工程を含み、前記リンス工程がこの研磨直後に、定盤を停止せずにリンス液を流しながら行われ、このリンス工程で用いられるリンス液が界面活性剤を含有した純水であり、さらにアルカリを添加してpHが8〜12に調整されたものであることを特徴とする研磨方法。   A method of polishing a glass substrate for magnetic disk comprising at least a step of polishing a glass substrate for magnetic disk and a step of rinsing the glass substrate after polishing, wherein the polishing step comprises colloidal silica as a main component of abrasive grains. Including a final polishing process to be used, and the rinsing process is performed immediately after this polishing while flowing the rinsing liquid without stopping the surface plate, and the rinsing liquid used in this rinsing process is pure water containing a surfactant. Further, a polishing method wherein the pH is adjusted to 8 to 12 by further adding an alkali. リンス工程の後に、さらに純水にアルカリを添加してpH8から12に調整された第二のリンス液で追加リンスすることを特徴とする請求項1に記載の研磨方法。
2. The polishing method according to claim 1, wherein after the rinsing step, additional rinsing is performed with a second rinsing liquid adjusted to pH 8 to 12 by adding alkali to pure water.
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