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JP2014191851A - Manufacturing method of glass substrate for information recording medium - Google Patents

Manufacturing method of glass substrate for information recording medium Download PDF

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JP2014191851A
JP2014191851A JP2013068692A JP2013068692A JP2014191851A JP 2014191851 A JP2014191851 A JP 2014191851A JP 2013068692 A JP2013068692 A JP 2013068692A JP 2013068692 A JP2013068692 A JP 2013068692A JP 2014191851 A JP2014191851 A JP 2014191851A
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glass substrate
mass
information recording
recording medium
polishing
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Noriko Shimazu
典子 島津
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Hoya Corp
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  • Grinding Of Cylindrical And Plane Surfaces (AREA)
  • Grinding And Polishing Of Tertiary Curved Surfaces And Surfaces With Complex Shapes (AREA)
  • Surface Treatment Of Glass (AREA)
  • Glass Compositions (AREA)
  • Manufacturing Of Magnetic Record Carriers (AREA)

Abstract

PROBLEM TO BE SOLVED: To provide a manufacturing method of a glass substrate for an information recording medium capable of reducing a change in a signal-to-noise ratio (SNR) of the information recording medium even in the case where "acceptance cleaning" is performed.SOLUTION: A manufacturing method of a glass substrate for an information recording medium used for an information recording medium includes: a step of preparing a glass substrate; a first polishing step of polishing the glass substrate; a step of applying chemical strengthening treatment to the polished glass substrate; a second polishing step of polishing the glass substrate to which the chemical strengthening treatment has been applied; and a step of cleaning the polished glass substrate. In a composition of the glass substrate, a ratio of [LiO+NaO+KO] is 7 mass% to 30 mass%, and the total variation in the composition of [LiO+NaO+KO] on a top layer of the glass substrate to the end of the step of cleaning the glass substrate after the second polishing step is within 50ng/cm.

Description

本発明は、情報記録媒体用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 for an information recording medium.

近年、ハードディスクドライブ(HDD)装置においては、記録密度が増々高密度化されてきている。記録密度の高密度化により、情報記録媒体(メディア)と情報記録媒体上を浮上しながら記録の読み書きを行なうヘッドとのギャップは数nm程度にまで狭小化している。   In recent years, in a hard disk drive (HDD) device, the recording density has been increased. As the recording density is increased, the gap between the information recording medium (medium) and the head that reads and writes the recording while floating on the information recording medium is narrowed to about several nanometers.

情報記録媒体に用いられる情報記録媒体用ガラス基板(以下、単にガラス基板と称する場合もある)は、記録密度の高密度化に対応するためにガラス基板の表面欠陥を低減させて、ヘッドとの衝突を起こさないようにしている。   A glass substrate for an information recording medium used for an information recording medium (hereinafter sometimes simply referred to as a glass substrate) reduces surface defects of the glass substrate in order to cope with an increase in recording density, I try not to cause a collision.

記録密度が600Gbit/inch(面記録密度)以上のハードディスクドライブ装置に用いられるガラス基板の場合、ガラス基板の表面の清浄性を向上させるため、ガラス基板への磁気薄膜層の形成前に、従来の最終洗浄工程の後に、さらに、アルカリ性の溶液でガラス基板を洗浄し、ガラス基板上のわずかなパーティクルも除去するという工程が新たに導入されている(特許文献1参照)。 In the case of a glass substrate used in a hard disk drive device having a recording density of 600 Gbit / inch 2 (surface recording density) or more, in order to improve the cleanliness of the surface of the glass substrate, before the formation of the magnetic thin film layer on the glass substrate, After the final cleaning step, a step of cleaning the glass substrate with an alkaline solution and removing a small amount of particles on the glass substrate is newly introduced (see Patent Document 1).

しかし、次世代の630Gbit/inch(面記録密度)対応で、特に組成として、アルカリ金属、アルカリ土類金属成分の多いガラス基板、化学強化処理(面強化処理)を施したガラス基板を情報記録媒体用ガラス基板として用いた場合に、平滑性、清浄性に問題がないにもかかわらず、電磁変換特性(SNR)が低下してしまうという問題が発生した。 However, it is compatible with the next generation of 630 Gbit / inch 2 (surface recording density), and in particular records information on glass substrates with many alkali metals and alkaline earth metal components, and glass substrates that have been subjected to chemical strengthening (surface strengthening). When used as a glass substrate for a medium, there is a problem that the electromagnetic conversion characteristics (SNR) are lowered although there is no problem in smoothness and cleanliness.

このようなガラス基板を精査した結果、製造後のガラス基板に対して磁気薄膜層を形成した後に、磁気信号のシグナルノイズ比のバラつきが発生し、リード・ライトエラーの発生要因となっている可能性が見出された。このような磁気信号のシグナルノイズ比のバラつきの要因について更に検討を進めた結果、下記のことが判明した。   As a result of scrutinizing such a glass substrate, after forming a magnetic thin film layer on the manufactured glass substrate, the signal-to-noise ratio of the magnetic signal varies, which may cause read / write errors. Sex was found. As a result of further investigation on the cause of the variation in the signal-to-noise ratio of the magnetic signal, the following was found.

情報記録媒体に用いられるガラス基板は、製造後一旦密封状態にして搬送用BOXに梱包されて搬送される。次に、ガラス基板は、梱包が解かれ搬送用BOXから取り出される。その後、ガラス基板に磁性層を塗布する工程に供される。   A glass substrate used for an information recording medium is once sealed after being manufactured, and is packed in a transport BOX and transported. Next, the glass substrate is unpacked and taken out from the transfer BOX. Then, it is used for the process of apply | coating a magnetic layer to a glass substrate.

その際、梱包時、搬送時、取り出し時に、ガラス基板の表面状態が不均一化したり、微細なパーティクルが付着する場合がある。ガラス基板の表面状態を均一化する為に、アルカリ溶液のような比較的洗浄性が高く、場合によってはガラス基板の表面を若干溶解させるような特性を持つ洗剤を用いて、ガラス基板の表面の洗浄(以下、「受け入れ洗浄」と称する。)が行なわれている(特許文献2参照)。   At this time, the surface state of the glass substrate may become non-uniform or fine particles may adhere during packing, transporting, or taking out. In order to make the surface state of the glass substrate uniform, a detergent having a characteristic such as a relatively high detergency such as an alkaline solution and, in some cases, slightly dissolving the surface of the glass substrate is used. Cleaning (hereinafter referred to as “acceptance cleaning”) is performed (see Patent Document 2).

国際公開第2008/004470号International Publication No. 2008/004470 特開2006−127624号公報JP 2006-127624 A

上述の磁気信号のシグナルノイズ比のバラツキは、このような磁気薄膜層の形成直前に行なわれるアルカリ洗浄において、ガラス表面の安定状態が損なわれて発生しており、ガラス基板自体を製造後に検査しても要因が判明し得なかったことが明らかになった。さらに、ガラス基板のアルカリ洗浄耐性のバラツキも、磁気信号のシグナルノイズ比のバラツキの発生要因であることも判明した。   The above-mentioned variation in the signal-to-noise ratio of the magnetic signal is caused by the alkali cleaning performed immediately before the formation of such a magnetic thin film layer because the stable state of the glass surface is impaired, and the glass substrate itself is inspected after manufacturing. However, it became clear that the cause could not be determined. Furthermore, it was also found that the variation in resistance to alkali cleaning of the glass substrate is also a cause of variation in the signal-to-noise ratio of the magnetic signal.

通常、金属系の付着物を落とすために、ガラス基板を酸性洗剤で洗浄する工程、ガラス基板を次の工程へ搬送する工程で酸性洗剤を用いる。しかし、アルカリ金属および/またはアルカリ土類金属量の多いガラス基板、化学強化処理(面強化処理)を施したガラス基板は、酸を用いる工程中でアルカリ金属がガラス基板の表層から溶出し、この溶出量によって「受け入れ洗浄」でのアルカリ耐久性に差異が生じてしまうことが分かった。この結果、信号対雑音比(S/N比:SNR)のバッチ間バラツキが発生していた。   Usually, in order to drop metallic deposits, an acidic detergent is used in the step of washing the glass substrate with an acidic detergent and the step of transporting the glass substrate to the next step. However, a glass substrate with a large amount of alkali metal and / or alkaline earth metal, or a glass substrate subjected to chemical strengthening treatment (surface strengthening treatment), the alkali metal is eluted from the surface layer of the glass substrate during the process using acid. It was found that the alkali durability in “acceptance cleaning” varies depending on the elution amount. As a result, signal-to-noise ratio (S / N ratio: SNR) varies between batches.

本発明は、上記の実情に鑑みてなされたものであって、「受け入れ洗浄」を行なった場合であっても、ガラス基板の表層からのアルカリ金属の溶出量を所定の範囲に抑制することで、当該ガラス基板を用いて情報記録媒体を製造した場合であっても、情報記録媒体の信号対雑音比(SNR)の変化を小さく抑制することを可能とする情報記録媒体用ガラス基板の製造方法を提供することを目的とする。   The present invention has been made in view of the above situation, and even when “acceptance cleaning” is performed, by suppressing the elution amount of alkali metal from the surface layer of the glass substrate to a predetermined range. A method of manufacturing a glass substrate for an information recording medium that can suppress a change in signal-to-noise ratio (SNR) of the information recording medium even when the information recording medium is manufactured using the glass substrate The purpose is to provide.

本発明に基づいた情報記録媒体用ガラス基板の製造方法においては、情報記録媒体に用いられる情報記録媒体用ガラス基板の製造方法であって、ガラス基板を準備する工程と、上記ガラス基板を研磨する第1研磨工程と、研磨が施された上記ガラス基板に対して化学強化処理を施す工程と、上記化学強化処理が施された上記ガラス基板を研磨する第2研磨工程と、研磨された上記ガラス基板を洗浄する工程とを備え、上記ガラス基板の組成は、[LiO+NaO+KO]の割合が、7質量%〜30質量%であり、上記第2研磨工程の後上記ガラス基板を洗浄する工程が終了するまでの間における、上記ガラス基板の表層の[LiO+NaO+KO]の組成の変化量の合計が、50ng/cm以内である。 In the manufacturing method of the glass substrate for information recording media based on this invention, it is a manufacturing method of the glass substrate for information recording media used for an information recording medium, Comprising: The process of preparing a glass substrate, The said glass substrate is grind | polished. A first polishing step, a step of subjecting the glass substrate subjected to polishing to a chemical strengthening treatment, a second polishing step of polishing the glass substrate subjected to the chemical strengthening treatment, and the polished glass A step of cleaning the substrate, wherein the composition of the glass substrate is such that the ratio of [Li 2 O + Na 2 O + K 2 O] is 7% by mass to 30% by mass, and the glass substrate is disposed after the second polishing step. The total change amount of the composition of [Li 2 O + Na 2 O + K 2 O] on the surface layer of the glass substrate is 50 ng / cm 3 or less until the cleaning step is completed.

他の形態においては、[LiO+NaO+KO]の組成の変化量の合計が、40ng/cm以内である。 In another embodiment, the total change amount of the composition of [Li 2 O + Na 2 O + K 2 O] is within 40 ng / cm 3 .

他の形態においては、上記第2研磨工程の後上記ガラス基板を洗浄する工程が終了するまでの間における、上記ガラス基板の上記表層の組成の変化量が、Liが0.1質量%以上1質量%以下、Naが0.1質量%以上2.1質量%以下、Kが0.05質量%以上0.5質量%以下である。   In another embodiment, the amount of change in the composition of the surface layer of the glass substrate after the second polishing step until the step of washing the glass substrate is completed is such that Li is 0.1 mass% or more 1 Mass% or less, Na is 0.1 mass% or more and 2.1 mass% or less, and K is 0.05 mass% or more and 0.5 mass% or less.

他の形態においては、上記ガラス基板の上記表層の組成の変化量が、Naが0.1質量%以上1.0質量%以下、Kが0.05質量%以上0.1質量%以下である。   In another embodiment, the amount of change in the composition of the surface layer of the glass substrate is such that Na is 0.1% by mass or more and 1.0% by mass or less, and K is 0.05% by mass or more and 0.1% by mass or less. .

本発明によれば、「受け入れ洗浄」を行なった場合であっても、ガラス基板の表層からのアルカリ金属の溶出量を所定の範囲に抑制することで、当該ガラス基板を用いて情報記録媒体を製造した場合であっても、情報記録媒体の信号対雑音比(SNR)の変化を小さく抑制することを可能とする情報記録媒体用ガラス基板の製造方法を提供することを提供することを可能とする。   According to the present invention, even when “acceptance cleaning” is performed, the amount of alkali metal eluted from the surface layer of the glass substrate is suppressed to a predetermined range, so that the information recording medium can be used with the glass substrate. Even when manufactured, it is possible to provide a method for manufacturing a glass substrate for an information recording medium that can suppress a small change in the signal-to-noise ratio (SNR) of the information recording medium. To do.

実施の形態における情報記録媒体用ガラス基板の斜視図である。It is a perspective view of the glass substrate for information recording media in an embodiment. 実施の形態における情報記録媒体の斜視図である。It is a perspective view of the information recording medium in an embodiment. 実施の形態における情報記録媒体の製造方法を示すフロー図である。It is a flowchart which shows the manufacturing method of the information recording medium in embodiment. 「化学強化工程」を施したガラス基板と、「化学強化工程」を施していないガラス基板とに対して、(A)は酸に接触しない「工程」を採用した場合のアルカリ成分の溶出量、(B)は酸への接触が多い「工程」を採用した場合のアルカリ成分の溶出量を示す図である。For a glass substrate that has been subjected to a “chemical strengthening step” and a glass substrate that has not been subjected to a “chemical strengthening step”, (A) is an elution amount of an alkali component when a “step” that does not contact an acid is employed, (B) is a figure which shows the elution amount of an alkali component at the time of employ | adopting the "process" with many contacts to an acid. 実施例1〜3および比較例1〜2における情報記録媒体用ガラス基板の評価結果を示す図である。It is a figure which shows the evaluation result of the glass substrate for information recording media in Examples 1-3 and Comparative Examples 1-2. 実施例A〜Hにおける情報記録媒体用ガラス基板の評価結果を示す図である。It is a figure which shows the evaluation result of the glass substrate for information recording media in Examples AH.

以下に、本発明の実施の形態および実施例について説明する。同一または相当する部分に同一の参照符号を付し、その説明を繰返さない場合がある。以下に説明する実施の形態および実施例において、個数、量などに言及する場合、特に記載がある場合を除き、本発明の範囲は必ずしもその個数、量などに限定されない。以下の実施の形態において、各々の構成要素は、特に記載がある場合を除き、本発明にとって必ずしも必須のものではない。   Embodiments and examples of the present invention will be described below. The same or corresponding parts are denoted by the same reference symbols, and the description thereof may not be repeated. In the embodiments and examples described below, when referring to the number, amount, and the like, the scope of the present invention is not necessarily limited to the number, amount, and the like unless otherwise specified. In the following embodiments, each component is not necessarily essential to the present invention unless otherwise specified.

本実施の形態においては、ガラス組成を示す「%」表示は特に断らない限り「mol%」を示すものとする。「LiO+NaO+KO」等のような化学式の加算表記は、そのような化学式で示される成分の合計量を示すものとする。たとえば、「LiO+NaO+KO」とはLiOとNaOとKOとの合計量を示す。 In the present embodiment, “%” indicating a glass composition indicates “mol%” unless otherwise specified. An addition notation of a chemical formula such as “Li 2 O + Na 2 O + K 2 O” indicates the total amount of components represented by such chemical formula. For example, “Li 2 O + Na 2 O + K 2 O” indicates the total amount of Li 2 O, Na 2 O, and K 2 O.

(情報記録媒体1の構成)
図1および図2を参照して、情報記録媒体用ガラス基板1Gおよび情報記録媒体1の構成について説明する。図1は、情報記録媒体用ガラス基板1Gの斜視図、図2は、情報記録媒体の斜視図である。
(Configuration of information recording medium 1)
With reference to FIG. 1 and FIG. 2, the structure of the glass substrate 1G for information recording media and the information recording medium 1 is demonstrated. FIG. 1 is a perspective view of a glass substrate 1G for an information recording medium, and FIG. 2 is a perspective view of the information recording medium.

図1に示すように、情報記録媒体1に用いられる情報記録媒体用ガラス基板1G(以下、「ガラス基板1G」と称する。)は、中心に孔11が形成された環状の円板形状を呈している。ガラス基板1Gは、外周端面12、内周端面13、表主表面14、および裏主表面15を有している。ガラス基板1Gとしては、アモルファスガラス等を用い、たとえば、外径約65mm、内径約20mm、厚さ約0.8mm、表面粗さは、約2.0Å以下である。   As shown in FIG. 1, an information recording medium glass substrate 1G used for the information recording medium 1 (hereinafter referred to as “glass substrate 1G”) has an annular disk shape with a hole 11 formed in the center. ing. The glass substrate 1G has an outer peripheral end face 12, an inner peripheral end face 13, a front main surface 14, and a back main surface 15. As the glass substrate 1G, amorphous glass or the like is used. For example, the outer diameter is about 65 mm, the inner diameter is about 20 mm, the thickness is about 0.8 mm, and the surface roughness is about 2.0 mm or less.

ガラス基板1Gのインチサイズに特に限定はなく、0.8インチ、1.0インチ、1.8インチ、2.5インチ、3.5インチ各種ガラス基板1Gを、情報記録媒体用のディスクとして製造してもよい。   The inch size of the glass substrate 1G is not particularly limited, and various glass substrates 1G of 0.8 inch, 1.0 inch, 1.8 inch, 2.5 inch, and 3.5 inch are manufactured as disks for information recording media. May be.

落下衝撃によるガラス基板1Gの割れに対して有効であることから、ガラス基板1Gの厚みは0.30mm〜2.2mmが好ましい。ここでいうガラス基板1Gの厚みとは基板上の点対象となる任意の何点かで測定した値の平均値を意味する。   The thickness of the glass substrate 1G is preferably 0.30 mm to 2.2 mm because it is effective against cracking of the glass substrate 1G due to drop impact. The thickness of the glass substrate 1 </ b> G here means an average value of values measured at some arbitrary points to be pointed on the substrate.

ガラス基板1の大きさは、たとえば0.8インチ、1.0インチ、1.8インチ、2.5インチ、または3.5インチである。ガラス基板の厚さは、破損防止の観点から、たとえば0.30mm〜2.2mmである。本実施の形態におけるガラス基板の大きさは、外径が約64mm、内径が約20mm、厚さが約0.8mmである。ガラス基板の厚さとは、ガラス基板上の点対象となる任意の複数の点で測定した値の平均によって算出される値である。ガラス基板の高硬度化の観点から、ガラス基板1のビッカース硬度は、610kg/mm以上であるとよい。 The size of the glass substrate 1 is, for example, 0.8 inch, 1.0 inch, 1.8 inch, 2.5 inch, or 3.5 inch. The thickness of the glass substrate is, for example, 0.30 mm to 2.2 mm from the viewpoint of preventing breakage. In the present embodiment, the glass substrate has an outer diameter of about 64 mm, an inner diameter of about 20 mm, and a thickness of about 0.8 mm. The thickness of the glass substrate is a value calculated by averaging the values measured at a plurality of arbitrary points to be pointed on the glass substrate. From the viewpoint of increasing the hardness of the glass substrate, the Vickers hardness of the glass substrate 1 is preferably 610 kg / mm 2 or more.

ガラス基板には、ガラス転移温度(Tg)が、650℃以上のガラスであれば、どのような組成でも構わないが、LiO+NaO+KOの割合が、7質量%〜30質量%であるようなアルカリ成分が多く含まれる組成であると、よりアルカリ成分の溶出によるSNR変化が大きくなるため、本実施の形態における効果が顕著に得られるのでよい。 The glass substrate may have any composition as long as the glass transition temperature (Tg) is glass of 650 ° C. or higher, but the ratio of Li 2 O + Na 2 O + K 2 O is 7% by mass to 30% by mass. If the composition contains a lot of alkali components, the SNR change due to elution of the alkali components becomes larger, so that the effects in this embodiment may be remarkably obtained.

本実施の形態においては、SiO+Al+Bの割合が50質量(wt)%〜85質量(wt)%であり、MgO+CaO+KOの割合が2質量(wt)%〜20質量(wt)%であることが好ましい。 In the present embodiment, the ratio of SiO 2 + Al 2 O 3 + B 2 O 3 is 50 mass (wt)% to 85 mass (wt)%, and the ratio of MgO + CaO + K 2 O is 2 mass (wt)% to 20 The mass (wt)% is preferred.

さらに、後述の化学強化工程(S70)において、アルミノシリケートガラスが、イオン交換による応力層を形成しやすい観点から、以下の組成のガラスを用いることが、より好ましい。   Furthermore, in the chemical strengthening step (S70) described later, it is more preferable to use a glass having the following composition from the viewpoint that the aluminosilicate glass easily forms a stress layer by ion exchange.

好ましいガラス基板の組成は、例えば、SiOが、50質量(wt)%〜70質量(wt)%、Alが、0質量(wt)%〜20質量(wt)%、Bが、0質量(wt)%〜5質量(wt)%、Pが、0.1質量(wt)%〜3質量(wt)%、NaOが、2質量(wt)%〜6質量(wt)%、MgOが、6質量(wt)%〜12質量(wt)%、CaOが、0.1質量(wt)%〜3質量(wt)%、ZnOが、3質量(wt)%〜8質量(wt)%、TiOが、3質量(wt)%〜8質量(wt)%、LiOが、0質量(wt)%〜4質量(wt)%、NaOが、2質量(wt)%〜6質量(wt)%、KOが、0質量(wt)%〜3質量(wt)%である。 Preferred glass substrate compositions include, for example, SiO 2 of 50 mass (wt)% to 70 mass (wt)%, Al 2 O 3 of 0 mass (wt)% to 20 mass (wt)%, B 2 O. 3 is 0 mass (wt)% to 5 mass (wt)%, P 2 O 5 is 0.1 mass (wt)% to 3 mass (wt)%, Na 2 O is 2 mass (wt)% ~ 6 mass (wt)%, MgO is 6 mass (wt)% to 12 mass (wt)%, CaO is 0.1 mass (wt)% to 3 mass (wt)%, ZnO is 3 mass ( wt)% to 8 mass (wt)%, TiO 2 is 3 mass (wt)% to 8 mass (wt)%, Li 2 O is 0 mass (wt)% to 4 mass (wt)%, Na 2 O is 2 mass (wt)% to 6 mass (wt)%, and K 2 O is 0 mass (wt)% to 3 mass (wt)%.

図2に示すように、情報記録媒体1は、上記したガラス基板1Gの表主表面14上に磁気薄膜層23が形成されている。図示では、表主表面14上にのみ磁気薄膜層23が形成されているが、裏主表面15上に磁気薄膜層23を設けることも可能である。   As shown in FIG. 2, in the information recording medium 1, a magnetic thin film layer 23 is formed on the front main surface 14 of the glass substrate 1G. In the figure, the magnetic thin film layer 23 is formed only on the front main surface 14, but it is also possible to provide the magnetic thin film layer 23 on the back main surface 15.

磁気薄膜層23の形成方法としては従来公知の方法を用いることができ、たとえば、磁性粒子を分散させた熱硬化性樹脂をガラス基板1G上にスピンコートして形成する方法、スパッタリングにより形成する方法、無電解めっきにより形成する方法が挙げられる。   As a method of forming the magnetic thin film layer 23, a conventionally known method can be used. For example, a method of spin-coating a thermosetting resin in which magnetic particles are dispersed on the glass substrate 1G, a method of forming by sputtering. The method of forming by electroless plating is mentioned.

スピンコート法での膜厚は約0.3〜1.2μm程度、スパッタリング法での膜厚は0.04〜0.08μm程度、無電解めっき法での膜厚は0.05〜0.1μm程度であり、薄膜化および高密度化の観点からはスパッタリング法および無電解めっき法による膜形成がよい。   The film thickness by spin coating is about 0.3 to 1.2 μm, the film thickness by sputtering is about 0.04 to 0.08 μm, and the film thickness by electroless plating is 0.05 to 0.1 μm. From the viewpoint of thinning and high density, film formation by sputtering and electroless plating is preferable.

磁気薄膜層23に用いる磁性材料としては、特に限定はなく従来公知のものが使用できるが、高い保持力を得るために結晶異方性の高いCoを基本とし、残留磁束密度を調整する目的でNi、Crを加えたCo系合金などが好適である。近年では、熱アシスト記録用に好適な磁性層材料として、FePt系の材料が用いられるようになってきている。   The magnetic material used for the magnetic thin film layer 23 is not particularly limited, and a conventionally known material can be used. However, in order to obtain a high coercive force, Co having high crystal anisotropy is basically used for the purpose of adjusting the residual magnetic flux density. Co-based alloys to which Ni and Cr are added are suitable. In recent years, FePt-based materials have been used as magnetic layer materials suitable for heat-assisted recording.

磁気ヘッドの滑りをよくするために磁気薄膜層23の表面に潤滑剤を薄くコーティングしてもよい。潤滑剤としては、例えば液体潤滑剤であるパーフロロポリエーテル(PFPE)をフレオン系などの溶媒で希釈したものが挙げられる。   In order to improve the sliding of the magnetic head, the surface of the magnetic thin film layer 23 may be thinly coated with a lubricant. Examples of the lubricant include those obtained by diluting perfluoropolyether (PFPE), which is a liquid lubricant, with a freon-based solvent.

必要により下地層、保護層を設けてもよい。情報記録媒体1における下地層は磁性膜に応じて選択される。下地層の材料としては、例えば、Cr、Mo、Ta、Ti、W、V、B、Al、Niなどの非磁性金属から選ばれる少なくとも一種以上の材料が挙げられる。   If necessary, an underlayer and a protective layer may be provided. The underlayer in the information recording medium 1 is selected according to the magnetic film. Examples of the material for the underlayer include at least one material selected from nonmagnetic metals such as Cr, Mo, Ta, Ti, W, V, B, Al, and Ni.

下地層は単層とは限らず、同一又は異種の層を積層した複数層構造としても構わない。例えば、Cr/Cr、Cr/CrMo、Cr/CrV、NiAl/Cr、NiAl/CrMo、NiAl/CrV等の多層下地層としてもよい。   The underlayer is not limited to a single layer, and may have a multi-layer structure in which the same or different layers are stacked. For example, a multilayer underlayer such as Cr / Cr, Cr / CrMo, Cr / CrV, NiAl / Cr, NiAl / CrMo, or NiAl / CrV may be used.

磁気薄膜層23の摩耗、腐食を防止する保護層としては、例えば、Cr層、Cr合金層、カーボン層、水素化カーボン層、ジルコニア層、シリカ層などが挙げられる。保護層は、下地層、磁性膜など共にインライン型スパッタ装置で連続して形成できる。保護層は、単層としてもよく、あるいは、同一又は異種の層からなる多層構成としてもよい。   Examples of the protective layer for preventing wear and corrosion of the magnetic thin film layer 23 include a Cr layer, a Cr alloy layer, a carbon layer, a hydrogenated carbon layer, a zirconia layer, and a silica layer. The protective layer can be formed continuously with an in-line sputtering apparatus, such as an underlayer and a magnetic film. The protective layer may be a single layer, or may have a multilayer structure composed of the same or different layers.

上記保護層上に、あるいは上記保護層に替えて、他の保護層を形成してもよい。例えば、上記保護層に替えて、Cr層の上にテトラアルコキシランをアルコール系の溶媒で希釈した中に、コロイダルシリカ微粒子を分散して塗布し、さらに焼成して酸化ケイ素(SiO2)層を形成してもよい。   Another protective layer may be formed on the protective layer or instead of the protective layer. For example, in place of the protective layer, colloidal silica fine particles are dispersed and coated on a Cr layer diluted with an alcohol-based solvent, and then fired to form a silicon oxide (SiO2) layer. May be.

(ガラス基板1Gの製造工程)
次に、図3を参照して、本実施の形態に係るガラス基板1Gおよび情報記録媒体1の製造方法を説明する。図3は、ガラス基板1Gおよび情報記録媒体1の製造方法を示すフロー図である。
(Manufacturing process of glass substrate 1G)
Next, a method for manufacturing the glass substrate 1G and the information recording medium 1 according to the present embodiment will be described with reference to FIG. FIG. 3 is a flowchart showing a method for manufacturing the glass substrate 1G and the information recording medium 1.

まず、ステップ10(以下、「S10」と略す。ステップ11以降も同様。)の「ガラス溶融工程」において、ガラス基板を構成するガラス素材を溶融する。   First, in the “glass melting step” of step 10 (hereinafter abbreviated as “S10”, the same applies to step 11 and subsequent steps), the glass material constituting the glass substrate is melted.

S11の「プレス成形工程」において、溶融させたガラス素材を上型および下型を用いたプレスによりガラス基板を作製した。使用したガラス組成は、一般的なアルミノシリケートガラスを用いた。ガラス基板の作製方法としては成形に限らず、公知の手法である板ガラスからの切り出し等でも構わず、ガラス組成もこれに限らない。   In the “press molding step” of S11, a glass substrate was produced by pressing the molten glass material using an upper mold and a lower mold. The glass composition used was a general aluminosilicate glass. The method for producing the glass substrate is not limited to molding, and may be cut out from plate glass, which is a known technique, and the glass composition is not limited thereto.

S12の「第1ラップ工程」において、ガラス基板の両主表面をラッピング加工した。この第1ラップ工程は、遊星歯車機構を利用した両面ラッピング装置を用いて行なった。具体的には、ガラス基板の両面に上下からラップ定盤を押圧させ、研削液をガラス基板の主表面上に供給し、これらを相対的に移動させてラッピング加工を行なった。このラッピング加工により、おおよそ平坦な主表面を有するガラス基板を得た。   In the “first lapping step” of S12, both main surfaces of the glass substrate were lapped. This first lapping step was performed using a double-sided lapping device using a planetary gear mechanism. Specifically, the lapping platen was pressed on both surfaces of the glass substrate from above and below, the grinding liquid was supplied onto the main surface of the glass substrate, and these were moved relatively to perform lapping. By this lapping process, a glass substrate having a substantially flat main surface was obtained.

S13の「コアリング工程」において、円筒状のダイヤモンドドリルを用いて、ガラス基板の中心部に穴を形成し、円環状のガラス基板を作製した。ガラス基板の内周端面、および外周端面をダイヤモンド砥石によって研削し、所定の面取り加工を実施した。   In the “coring step” of S13, a cylindrical diamond drill was used to form a hole in the center of the glass substrate to produce an annular glass substrate. The inner peripheral end surface and the outer peripheral end surface of the glass substrate were ground with a diamond grindstone, and a predetermined chamfering process was performed.

S14の「第2ラップ工程」において、ガラス基板の両主表面について、上記第1ラップ工程(S12)と同様に、ラッピング加工を行なった。この第2ラップ工程を行なうことにより、前工程のコアリングおよび端面加工において主表面に形成された微細な凹凸形状を予め除去しておくことができる。その結果、後工程での主表面の研磨時間を短縮することができる。   In the “second lapping step” of S14, lapping was performed on both main surfaces of the glass substrate in the same manner as in the first lapping step (S12). By performing the second lapping step, the fine uneven shape formed on the main surface in the coring and end face processing in the previous step can be removed in advance. As a result, the polishing time of the main surface in the subsequent process can be shortened.

S15の「外周研磨工程」において、ガラス基板の外周端面について、ブラシ研磨による鏡面研磨を行なった。このとき研磨砥粒としては、一般的な酸化セリウム砥粒を含むスラリーを用いた。本実施の形態では、S10〜S15が、ガラス基板を準備する工程となる。   In the “peripheral polishing step” of S15, the outer peripheral end face of the glass substrate was subjected to mirror polishing by brush polishing. At this time, as the abrasive grains, a slurry containing general cerium oxide abrasive grains was used. In the present embodiment, S10 to S15 are steps for preparing a glass substrate.

S16の「第1ポリッシュ工程」において、主表面研磨を行なった。この第1ポリッシュ工程は、上述の第1および第2ラップ工程(S12,S14)において主表面に残留したキズおよび反りを矯正することを主目的とするものである。この第1ポリッシュ工程においては、遊星歯車機構を有する両面研磨装置により主表面の研磨を行なった。研磨剤としては、一般的な酸化セリウム砥粒を用いた。   In the “first polishing step” of S16, main surface polishing was performed. The first polishing step is mainly intended to correct scratches and warpage remaining on the main surface in the first and second lapping steps (S12, S14) described above. In the first polishing step, the main surface was polished by a double-side polishing apparatus having a planetary gear mechanism. As the abrasive, general cerium oxide abrasive grains were used.

S17の「化学強化工程」において、ガラス基板1Gの主表面に対して表面強化層を形成した。具体的には、300℃に加熱された硝酸カリウム(70%)と硝酸ナトリウム(30%)の混合溶液中に、ガラス基板1Gを約30分間浸漬することによって化学強化を行なった。その結果、ガラス基板の内周端面および外周端面のリチウムイオンおよびナトリウムイオンが、化学強化溶液中のナトリウムイオンおよびカリウムイオンにそれぞれ置換され、圧縮応力層が形成されることでガラス基板の主表面及び端面が強化された。   In the “chemical strengthening step” of S17, a surface reinforcing layer was formed on the main surface of the glass substrate 1G. Specifically, chemical strengthening was performed by immersing the glass substrate 1G in a mixed solution of potassium nitrate (70%) and sodium nitrate (30%) heated to 300 ° C. for about 30 minutes. As a result, the lithium ion and sodium ion on the inner peripheral end surface and outer peripheral end surface of the glass substrate are respectively replaced with sodium ions and potassium ions in the chemical strengthening solution, and a compressive stress layer is formed, thereby forming the main surface of the glass substrate and The end face was strengthened.

S18の「第2ポリッシュ工程」において、主表面研磨工程を施した。この第2ポリッシュ工程は上述までの工程で発生、残存している主表面上の微小欠陥等を解消して鏡面状に仕上げること、反りを解消し所望の平坦度に仕上げることを目的とする。この第2ポリッシュ工程は、遊星歯車機構を有する両面研磨装置により研磨を行なった。研磨剤としては、平滑面を得る為に平均粒径が約20nmのコロイダルシリカを用いた。   In the “second polishing step” of S18, a main surface polishing step was performed. This second polishing step aims to eliminate the fine defects on the main surface that have been generated and remain in the above-described steps and finish it in a mirror shape, to eliminate warpage and finish it to a desired flatness. In the second polishing step, polishing was performed by a double-side polishing apparatus having a planetary gear mechanism. As the abrasive, colloidal silica having an average particle diameter of about 20 nm was used to obtain a smooth surface.

S19の「洗浄工程」において、ガラス基板の主表面、端面の最終洗浄を実施する。これによりガラス基板上に残存する付着物を除去する。   In the “cleaning step” of S19, final cleaning of the main surface and end surface of the glass substrate is performed. Thereby, the deposits remaining on the glass substrate are removed.

S20の「検査工程」において、ガラス基板の表層の組成の変化量の検査を行なった。その後、S21の「磁気薄膜成膜工程」において、上述の検査の結果合格した、ガラス基板の両主表面に、Cr合金からなる密着層、CoFeZr合金からなる軟磁性層、Ruからなる配向制御下地層、CoCrPt合金からなる垂直磁気記録層、C系の保護層、F系からなる潤滑層を順次成膜することにより、垂直磁気記録方式の情報記録媒体を製造した。この構成は垂直磁気記録方式の構成の一例であり、面内情報記録媒体として磁性層等を構成してもよい。その後、「後熱処理工程」を実施することで、情報記録媒体が完成する。   In the “inspection step” of S20, the amount of change in the composition of the surface layer of the glass substrate was inspected. After that, in the “magnetic thin film deposition step” of S21, both main surfaces of the glass substrate that passed the above-described inspection were subjected to an adhesion layer composed of a Cr alloy, a soft magnetic layer composed of a CoFeZr alloy, and an orientation control composed of Ru. An information recording medium of a perpendicular magnetic recording system was manufactured by sequentially forming a base layer, a perpendicular magnetic recording layer made of a CoCrPt alloy, a C-based protective layer, and an F-based lubricating layer. This configuration is an example of a configuration of a perpendicular magnetic recording system, and a magnetic layer or the like may be configured as an in-plane information recording medium. Thereafter, by performing a “post heat treatment step”, the information recording medium is completed.

本実施の形態におけるガラス基板の製造方法は、以上のように構成される。このガラス基板の製造方法を用いることで、図1に示すガラス基板1Gが得られる。その後、このようにして得られたガラス基板1Gを用いて、図2に示す情報記録媒体1が得られる。   The manufacturing method of the glass substrate in this Embodiment is comprised as mentioned above. The glass substrate 1G shown in FIG. 1 is obtained by using this glass substrate manufacturing method. Thereafter, the information recording medium 1 shown in FIG. 2 is obtained using the glass substrate 1G thus obtained.

ここで、図4を参照して、上述のS17の「化学強化工程」を施したガラス基板と、「化学強化工程」を施していないガラス基板とに対して、(A)は酸に接触しない「工程」を採用した場合のアルカリ成分の溶出量を示し、(B)は酸への接触が多い「工程」を採用した場合のアルカリ成分の溶出量を示している。ここでの、「工程」とは、搬送間におけす水への浸漬工程、洗浄工程を意味する。   Here, with reference to FIG. 4, (A) does not contact an acid with respect to the glass substrate which performed the above-mentioned "chemical strengthening process" of S17, and the glass substrate which has not performed the "chemical strengthening process". The elution amount of the alkali component when the “process” is adopted is shown, and (B) shows the elution amount of the alkali component when the “process” where the contact with the acid is large is adopted. Here, the “process” means a dipping process in water and a cleaning process between transports.

酸に接触しない「工程」を採用した(A)の場合、「化学強化工程」を施したガラス基板のアルカリ成分の溶出量は、「化学強化工程」を施していないガラス基板の溶出量に比較して少ない。しかし、酸への接触が多い「工程」を採用した(B)の場合、化学強化工程」を施したガラス基板のアルカリ成分の溶出量は、「化学強化工程」を施していないガラス基板の溶出量に比較して多くなっている。   In the case of (A), which employs a “process” that does not come into contact with acid, the elution amount of the alkali component of the glass substrate subjected to the “chemical strengthening step” is compared with the elution amount of the glass substrate not subjected to the “chemical strengthening step”. And there are few. However, in the case of (B), which employs a “process” that has a lot of contact with acid, the elution amount of the alkali component of the glass substrate subjected to the “chemical strengthening process” is the elution amount of the glass substrate not subjected to the “chemical strengthening process”. It is larger than the amount.

ガラス基板の製造工程中において、アルカリ成分の溶出量が多いと、受け入れ洗浄でのアルカリ洗浄耐性が低くなり、SNRバラツキを発生する。したがって、ガラス基板の製造工程中において、アルカリ成分の溶出量を抑制する「工程」の採用が重要となる。   If the elution amount of the alkali component is large during the manufacturing process of the glass substrate, the alkali cleaning resistance in the receiving cleaning is lowered and SNR variation is generated. Therefore, it is important to adopt a “process” that suppresses the elution amount of the alkali component during the manufacturing process of the glass substrate.

(実施例)
第2研磨工程(S18)後の洗浄工程(S18)の条件を各種設定して、第2研磨工程(S18)の後ガラス基板を洗浄する工程が終了するまでの間における、ガラス基板の表層の組成の変化量を調整するようにした。
(Example)
Various conditions of the cleaning step (S18) after the second polishing step (S18) are set, and the surface layer of the glass substrate during the second polishing step (S18) until the step of cleaning the glass substrate is completed. The amount of change in composition was adjusted.

以下の実施例ではガラス基板の材料として、質量%で、LiO=4.0%、NaO=11.0%、KO=1.0%、MgO=1.0%、CaO=2.0%、SiO=65.5%、Al=15.5%の組成のガラス材料を用いた。 In the following examples, as a material of the glass substrate, by mass%, Li 2 O = 4.0%, Na 2 O = 11.0%, K 2 O = 1.0%, MgO = 1.0%, CaO = 2.0%, SiO 2 = 65.5%, Al 2 O 3 = 15.5% glass material was used.

ガラス基板は100枚を1バッチとして、第2研磨工程(S18)まで製造した。その後、以下の実施例1〜比較例2で示した条件の50mLの溶液で処理を行なった。その後、10枚を抜き取り、その溶液中へのLi、Na、Kの溶出量を、ICP−MS(誘導結合プラズマ質量分析装置、エスアイアイナノテクノロジー社製 SPQ9700)を用いて評価した。   The glass substrates were manufactured up to the second polishing step (S18), with 100 batches as one batch. Then, it processed with the 50 mL solution of the conditions shown in the following Examples 1-comparative example 2. Then, 10 sheets were extracted, and the elution amounts of Li, Na, and K in the solution were evaluated using ICP-MS (inductively coupled plasma mass spectrometer, SPQ9700 manufactured by SII Nano Technology).

更に、残りから10枚を抜き取り、40℃において、pH11 NaOHで30分処理した際のSi溶出量を、ICP−AES(誘導結合プラズマ発光分析分光装置、エスアイアイナノテクノロジー社製 SPS3520UV)で測定し、「平均値」および「3σ」で評価した。   Further, 10 pieces were extracted from the remaining, and the amount of Si elution when treated with pH 11 NaOH at 40 ° C. for 30 minutes was measured with ICP-AES (inductively coupled plasma emission spectrometer, SPS3520UV manufactured by SII Nano Technology). , “Average value” and “3σ”.

残りのガラス基板80枚に、磁気薄膜層を形成し、SNR評価を行った。(100枚加工したもののうち、10枚は枚葉で処理、残り90枚は通常の製造工程で製造した。)
以下に示す実施例1〜比較例2において、図5に、Li+Na+Kの溶出量(ng/cm)、Si溶出量(ppb)、SNR変化(db)を示す。図5中の、Si溶出量の()内の値は、3σの値を示す。値が小さいほど、バラツキが小さいことを示す。
A magnetic thin film layer was formed on the remaining 80 glass substrates, and SNR evaluation was performed. (Of the processed 100 sheets, 10 were processed with single wafers, and the remaining 90 were manufactured in a normal manufacturing process.)
In Examples 1 and 2 shown below, FIG. 5 shows the elution amount (ng / cm 3 ), Li elution amount (ppb), and SNR change (db) of Li + Na + K. In FIG. 5, the value in () of the Si elution amount indicates a value of 3σ. The smaller the value, the smaller the variation.

判定基準としては、+0.15dbの場合は「AAA」、0以上0.15db未満の場合は「AA」、0未満−0.1db以下の場合は「A」、0〜−0.1db以下は「B」、−0.11〜0.20dbは「C」、−0.21〜0.30dbは「D」、−0.31db〜は「E」と評価した。   The judgment criteria are “AAA” for +0.15 db, “AA” for 0 or more and less than 0.15 db, “A” for less than 0 and −0.1 db or less, and “A” for 0 to −0.1 db or less. “B” and −0.11 to 0.20 db were evaluated as “C”, −0.21 to 0.30 db as “D”, and −0.31 db and “E” as “E”.

(実施例1)
各工程間は、搬送工程(浸漬)では、pH8の溶液中に1分浸漬させた後、次の工程に進み、第2研磨工程(S18)後の洗浄工程(S19)をアルカリ洗剤を用いて行なった。実施例1では、Li+Na+Kの溶出量が、33ng/cm、Si溶出量が、80ppb(3σの値は「6」)、SNR変化が、0dbであった。判定は、「B」であった。
Example 1
Between each process, in a conveyance process (immersion), after being immersed in a solution of pH 8 for 1 minute, the process proceeds to the next process, and the cleaning process (S19) after the second polishing process (S18) is performed using an alkaline detergent. I did it. In Example 1, the elution amount of Li + Na + K was 33 ng / cm 3 , the Si elution amount was 80 ppb (the value of 3σ was “6”), and the SNR change was 0 db. The determination was “B”.

(実施例2)
各工程間は、搬送工程(浸漬)では、pH7の純水中に1分浸漬させた後、次の工程に進み、第2研磨工程(S18)後の洗浄工程(S19)をアルカリ洗剤を用いて行なった。実施例2では、Li+Na+Kの溶出量が、35ng/cm、Si溶出量が、100ppb(3σの値は「9」)、SNR変化が、−0.01dbであった。判定は、「B」であった。
(Example 2)
Between each process, in the conveyance process (immersion), after being immersed in pure water of pH 7 for 1 minute, the process proceeds to the next process, and the cleaning process (S19) after the second polishing process (S18) is performed using an alkaline detergent. It was done. In Example 2, the elution amount of Li + Na + K was 35 ng / cm 3 , the Si elution amount was 100 ppb (the value of 3σ was “9”), and the SNR change was −0.01 db. The determination was “B”.

(実施例3)
各工程間は、搬送工程(浸漬)では、pH7の純水中に5分間滞留させた後、次の工程に進み、第2研磨工程(S18)の洗浄工程(S19)をアルカリ洗剤を用いて行なった。実施例3では、Li+Na+Kの溶出量が、48ng/cm、Si溶出量が、105ppb(3σの値は「10」)、SNR変化が、−0.03dbであった。判定は、「C」であった。
(Example 3)
Between each process, in a conveyance process (immersion), after being kept in pure water of pH 7 for 5 minutes, the process proceeds to the next process, and the cleaning process (S19) of the second polishing process (S18) is performed using an alkaline detergent. I did it. In Example 3, the elution amount of Li + Na + K was 48 ng / cm 3 , the Si elution amount was 105 ppb (the value of 3σ was “10”), and the SNR change was −0.03 db. The determination was “C”.

(比較例1)
各工程間は、搬送工程(浸漬)では、pH3の溶液中に5分間滞留させた後、次の工程に進み、第2研磨工程(S18)の洗浄工程(S19)をアルカリ洗剤を用いて行なった。比較例1では、Li+Na+Kの溶出量が、55ng/cm、Si溶出量が、200ppb(3σの値は「55」)、SNR変化が、−0.4dbであった。判定は、「D」であった。
(Comparative Example 1)
Between each process, in a conveyance process (immersion), after being kept in a solution of pH 3 for 5 minutes, the process proceeds to the next process, and the cleaning process (S19) of the second polishing process (S18) is performed using an alkaline detergent. It was. In Comparative Example 1, the elution amount of Li + Na + K was 55 ng / cm 3 , the Si elution amount was 200 ppb (the value of 3σ was “55”), and the SNR change was −0.4 db. The determination was “D”.

(比較例2)
各工程間は、搬送工程(浸漬)では、pH5の溶液中に5分間滞留させた後、次の工程に進み、第2研磨工程(S18)の洗浄工程(S19)をアルカリ洗剤を用いて行なった。比較例1では、Li+Na+Kの溶出量が、60ng/cm、Si溶出量が、180ppb(3σの値は「40」)、SNR変化が、−0.32dbあった。判定は、「D」であった。
(Comparative Example 2)
Between each process, in a conveyance process (immersion), after being kept in a solution of pH 5 for 5 minutes, the process proceeds to the next process, and the cleaning process (S19) of the second polishing process (S18) is performed using an alkaline detergent. It was. In Comparative Example 1, the elution amount of Li + Na + K was 60 ng / cm 3 , the Si elution amount was 180 ppb (the value of 3σ was “40”), and the SNR change was −0.32 db. The determination was “D”.

(実施例A〜H)
第2研磨工程(S18)後の洗浄工程(S18)の条件を各種設定して、アルカリ金属の変化量を調整した。ガラス基板は100枚を1バッチとして、第2研磨工程(S18)まで製造した。実施例1〜比較例2で示した工程と同一条件になるように50mLの溶液で処理を行なった。
(Examples A to H)
Various conditions of the cleaning step (S18) after the second polishing step (S18) were set to adjust the amount of change in alkali metal. The glass substrates were manufactured up to the second polishing step (S18), with 100 batches as one batch. The treatment was carried out with 50 mL of the solution so as to be the same conditions as the steps shown in Example 1 and Comparative Example 2.

その後、10枚を抜き取り、その溶出液をICP−MS(誘導結合プラズマ質量分析装置、エスアイアイナノテクノロジー社製 SPQ9700)を用いてLi、Na、Kの溶出量を評価し、Li+Na+Kの溶出量が同一であることを確認した。   Thereafter, 10 samples were extracted, and the elution amount of Li, Na, K was evaluated using ICP-MS (inductively coupled plasma mass spectrometer, SPQ9700 manufactured by SII Nano Technology), and the elution amount of Li + Na + K was Confirmed to be the same.

残り90枚から10枚を抜き取り、XPS(走査型X線光電子分光分析装置、アルバック・ファイ社製 Quantera SXM)を使用し、極表面の元素分析を行ない元の調合組成に比べてのLi,Na,Kの変化量を評価した。   Ten sheets are extracted from the remaining 90 sheets, and XPS (Scanning X-ray Photoelectron Spectrometer, Quantera SXM manufactured by ULVAC-PHI) is used to perform elemental analysis of the extreme surface, compared to the original composition of Li, Na. , K change was evaluated.

更に、残り80枚から10枚を抜き取り、40℃において、pH11、NaOHで30分処理した際のSi溶出量をICP−AES(誘導結合プラズマ発光分析分光装置、エスアイアイナノテクノロジー社製 SPS3520UV)で測定し、平均値および3σで評価した。   Furthermore, 10 sheets were extracted from the remaining 80 sheets, and the elution amount of Si when treated with pH 11 and NaOH for 30 minutes at 40 ° C. was measured with ICP-AES (inductively coupled plasma emission spectrometer, SPS3520UV manufactured by SII Nano Technology). Measured and evaluated by average value and 3σ.

残りのガラス基板70枚に、磁気薄膜層を形成し、SNR評価を行った。(100枚加工したもののうち、10枚は枚葉で処理、残り90枚は通常の製造工程で製造した。)
以下に示す実施例A〜Hにおいて、図6に、Li+Na+Kの溶出量(ng/cm)、Liの変化量(質量%)、Naの変化量(質量%)、Kの変化量(質量%)、Si溶出量(ppb)、および、SNR変化(db)を示す。図5中の、Si溶出量の()内の値は、3σの値を示す。値が小さいほど、バラツキが小さいことを示す。判定基準としては、SNR変化が、+0.15dbの場合は「AAA」、0以上0.15db未満の場合は「AA」、0未満−0.1db以下の場合は「A」、0〜−0.1db以下は「B」、−0.11〜0.20dbは「C」、−0.21〜0.30dbは「D」、−0.31db〜は「E」と評価した。
Magnetic thin film layers were formed on the remaining 70 glass substrates, and SNR evaluation was performed. (Of the processed 100 sheets, 10 were processed with single wafers, and the remaining 90 were manufactured in a normal manufacturing process.)
In Examples A to H shown below, FIG. 6 shows the elution amount of Li + Na + K (ng / cm 3 ), the change amount of Li (mass%), the change amount of Na (mass%), and the change amount of K (mass%). ), Si elution amount (ppb), and SNR change (db). In FIG. 5, the value in () of the Si elution amount indicates a value of 3σ. The smaller the value, the smaller the variation. The judgment criteria are “AAA” when the SNR change is +0.15 db, “AA” when 0 or more and less than 0.15 db, “A” when less than 0 and less than −0.1 db, 0 to −0 .1 db or less was evaluated as “B”, −0.11 to 0.20 db as “C”, −0.21 to 0.30 db as “D”, and −0.31 db as “E”.

(実施例A)
各工程間は、搬送工程(浸漬)では、溶液中に浸漬させることなく、(ガラス基板の表面が乾かないように)1分以内に直接次の工程に進み、第2研磨工程(S18)後の洗浄工程(S19)をアルカリ洗剤を用いて行なった。実施例Aでは、Li+Na+Kの溶出量は、38ng/cm、Liの変化量は、0.15質量%、Naの変化量は、0.10質量%、Kの変化量は、0.06質量%、Si溶出量は、60ppb(3σの値は「5」)、および、SNR変化は、0.16dbあった。判定は、「AAA」であった。
(Example A)
Between each process, in the transport process (immersion), the process proceeds directly to the next process within 1 minute (so that the surface of the glass substrate does not dry) without being immersed in the solution, and after the second polishing process (S18). The washing step (S19) was performed using an alkaline detergent. In Example A, the elution amount of Li + Na + K was 38 ng / cm 3 , the change amount of Li was 0.15 mass%, the change amount of Na was 0.10 mass%, and the change amount of K was 0.06 mass %, Si elution amount was 60 ppb (3σ value was “5”), and SNR change was 0.16 db. The determination was “AAA”.

(実施例B)
各工程間は、搬送工程(浸漬)でpH8の溶液中に30秒浸漬させた後で、次の工程に進み、第2研磨工程(S18)後の洗浄工程(S19)をアルカリ洗剤を用いて行なった。実施例Bでは、Li+Na+Kの溶出量は、38ng/cm、Liの変化量は、0.30質量%、Naの変化量は、1.10質量%、Kの変化量は、0.08質量%、Si溶出量は、80ppb(3σの値は「10」)、および、SNR変化は、0.04dbあった。判定は、「AA」であった。
(Example B)
Between each process, after being immersed in a pH 8 solution for 30 seconds in the transport process (immersion), the process proceeds to the next process, and the cleaning process (S19) after the second polishing process (S18) is performed using an alkaline detergent. I did it. In Example B, the elution amount of Li + Na + K was 38 ng / cm 3 , the change amount of Li was 0.30% by mass, the change amount of Na was 1.10% by mass, and the change amount of K was 0.08% by mass. %, The elution amount of Si was 80 ppb (the value of 3σ was “10”), and the SNR change was 0.04 db. The determination was “AA”.

(実施例C)
各工程間は、搬送工程(浸漬)でpH7の純水中に30秒浸漬させた後で、次の工程に進み、第2研磨工程(S18)後の洗浄工程(S19)をアルカリ洗剤を用いて行なった。実施例Cでは、Li+Na+Kの溶出量は、38ng/cm、Liの変化量は、0.25質量%、Naの変化量は、0.90質量%、Kの変化量は、0.13質量%、Si溶出量は、85ppb(3σの値は「8」)、および、SNR変化は、0.05dbあった。判定は、「AA」であった。
(Example C)
Between each process, after being immersed in pH 7 pure water for 30 seconds in the transport process (immersion), the process proceeds to the next process, and the cleaning process (S19) after the second polishing process (S18) is performed using an alkaline detergent. It was done. In Example C, the elution amount of Li + Na + K is 38 ng / cm 3 , the change amount of Li is 0.25% by mass, the change amount of Na is 0.90% by mass, and the change amount of K is 0.13% by mass. %, Si elution amount was 85 ppb (the value of 3σ was “8”), and the SNR change was 0.05 db. The determination was “AA”.

(実施例D)
各工程間は、搬送工程(浸漬)でpH7の純水中に1分浸漬させた後で、次の工程に進み、第2研磨工程(S18)後の洗浄工程(S19)をアルカリ洗剤を用いて行なった。実施例Dでは、Li+Na+Kの溶出量は、38ng/cm、Liの変化量は、0.30質量%、Naの変化量は、2.13質量%、Kの変化量は、0.40質量%、Si溶出量は、100ppb(3σの値は「10」)、および、SNR変化は、−0.02dbあった。判定は、「A」であった。
(Example D)
Between each process, after being immersed in pure water of pH 7 for 1 minute in the transport process (immersion), the process proceeds to the next process, and the cleaning process (S19) after the second polishing process (S18) is performed using an alkaline detergent. It was done. In Example D, the elution amount of Li + Na + K was 38 ng / cm 3 , the change amount of Li was 0.30% by mass, the change amount of Na was 2.13% by mass, and the change amount of K was 0.40% by mass. %, The elution amount of Si was 100 ppb (the value of 3σ was “10”), and the SNR change was −0.02 db. The determination was “A”.

(実施例E)
各工程間は、搬送工程(浸漬)でpH8の溶液中に1分浸漬させた後で、次の工程に進み、第2研磨工程(S18)後の洗浄工程(S19)をアルカリ洗剤を用いて行なった。実施例Eでは、Li+Na+Kの溶出量は、38ng/cm、Liの変化量は、0.33質量%、Naの変化量は、0.33質量%、Kの変化量は、0.54質量%、Si溶出量は、90ppb(3σの値は「10」)、および、SNR変化は、−0.06dbあった。判定は、「A」であった。
(Example E)
Between each process, after being immersed in a pH 8 solution for 1 minute in the transport process (immersion), the process proceeds to the next process, and the cleaning process (S19) after the second polishing process (S18) is performed using an alkaline detergent. I did it. In Example E, the elution amount of Li + Na + K was 38 ng / cm 3 , the change amount of Li was 0.33 mass%, the change amount of Na was 0.33 mass%, and the change amount of K was 0.54 mass %, Si elution amount was 90 ppb (the value of 3σ was “10”), and the SNR change was −0.06 db. The determination was “A”.

(実施例F)
各工程間は、搬送工程(浸漬)でpH7.5の溶液中に1分浸漬させた後で、次の工程に進み、第2研磨工程(S18)後の洗浄工程(S19)をアルカリ洗剤を用いて行なった。実施例Fでは、Li+Na+Kの溶出量は、38ng/cm、Liの変化量は、1.03質量%、Naの変化量は、0.38質量%、Kの変化量は、0.17質量%、Si溶出量は、100ppb(3σの値は「7」)、および、SNR変化は、−0.07dbあった。判定は、「A」であった。
(Example F)
Between each process, after being immersed in a pH 7.5 solution for 1 minute in the transport process (immersion), the process proceeds to the next process, and the cleaning process (S19) after the second polishing process (S18) is performed with an alkaline detergent. Performed. In Example F, the elution amount of Li + Na + K is 38 ng / cm 3 , the change amount of Li is 1.03% by mass, the change amount of Na is 0.38% by mass, and the change amount of K is 0.17 mass%. %, The elution amount of Si was 100 ppb (the value of 3σ was “7”), and the SNR change was −0.07 db. The determination was “A”.

(実施例G)
各工程間は、搬送工程(浸漬)でpH8の溶液中に5分滞留させた後で、次の工程に進み、第2研磨工程(S18)後の洗浄工程(S19)をアルカリ洗剤を用いて行なった。実施例Gでは、Li+Na+Kの溶出量は、38ng/cm、Liの変化量は、0.90質量%、Naの変化量は、2.13質量%、Kの変化量は、0.52質量%、Si溶出量は、105ppb(3σの値は「10」)、および、SNR変化は、−0.15dbあった。判定は、「B」であった。
(Example G)
Between each process, after being allowed to stay in the pH 8 solution for 5 minutes in the transport process (immersion), the process proceeds to the next process, and the cleaning process (S19) after the second polishing process (S18) is performed using an alkaline detergent. I did it. In Example G, the elution amount of Li + Na + K is 38 ng / cm 3 , the change amount of Li is 0.90% by mass, the change amount of Na is 2.13% by mass, and the change amount of K is 0.52% by mass. %, The elution amount of Si was 105 ppb (the value of 3σ was “10”), and the SNR change was −0.15 db. The determination was “B”.

(実施例H)
各工程間は、搬送工程(浸漬)でpH7の純水中に5分滞留させた後で、次の工程に進み、第2研磨工程(S18)後の洗浄工程(S19)をアルカリ洗剤を用いて行なった。実施例Hでは、Li+Na+Kの溶出量は、38ng/cm、Liの変化量は、1.02質量%、Naの変化量は、2.22質量%、Kの変化量は、0.60質量%、Si溶出量は、110ppb(3σの値は「8」)、および、SNR変化は、−0.17dbあった。判定は、「B」であった。
(Example H)
Between each process, after being kept in pure water of pH 7 for 5 minutes in the transport process (immersion), the process proceeds to the next process, and the cleaning process (S19) after the second polishing process (S18) is performed using an alkaline detergent. It was done. In Example H, the elution amount of Li + Na + K was 38 ng / cm 3 , the change amount of Li was 1.02 mass%, the change amount of Na was 2.22 mass%, and the change amount of K was 0.60 mass %, The elution amount of Si was 110 ppb (the value of 3σ was “8”), and the SNR change was −0.17 db. The determination was “B”.

以上の実施例1〜3、実施例A〜H、および、比較例1,2によれば、ガラス基板の組成は、LiO+NaO+KOの割合が、比較的多いガラス素材を用いた場合であっても、第2研磨工程の後ガラス基板を洗浄する工程が終了するまでの間における、ガラス基板の表層の[LiO+NaO+KO]の組成の変化量の合計が、50ng/cm以内(実施例1〜3、実施例A〜H)となる条件で洗浄を行なうことで、当該ガラス基板を用いて情報記録媒体を製造した場合であっても、情報記録媒体のSNRの変化を小さくすることが可能となる。

[LiO+NaO+KO]の組成の変化量の合計が、40ng/cm以内(実施例1、2、実施例A〜H)であれば、より情報記録媒体のSNRの変化を小さくすることが可能となる。
According to the above Examples 1 to 3, Examples A to H, and Comparative Examples 1 and 2, the glass substrate was composed of a glass material having a relatively large proportion of Li 2 O + Na 2 O + K 2 O. Even in this case, the total change amount of the composition of [Li 2 O + Na 2 O + K 2 O] on the surface layer of the glass substrate until the step of cleaning the glass substrate after the second polishing step is completed is 50 ng. Even when the information recording medium is manufactured using the glass substrate by performing cleaning under the conditions within / cm 3 (Examples 1 to 3, Examples A to H), the SNR of the information recording medium It is possible to reduce the change of.
)
If the total change amount of the composition of [Li 2 O + Na 2 O + K 2 O] is within 40 ng / cm 3 (Examples 1, 2, and Examples A to H), the change in SNR of the information recording medium is further reduced. It becomes possible to do.

第2研磨工程の後ガラス基板を洗浄する工程が終了するまでの間における、ガラス基板の表層の組成の変化量が、Liが0.1質量%以上1質量%以下、Naが0.1質量%以上2.1質量%以下、Kが0.05質量%以上0.5質量%以下であれば(実施例A〜C)であれば、より情報記録媒体のSNRの変化(+0.04〜+0.16)を小さくすることが可能となる。   The amount of change in the composition of the surface layer of the glass substrate during the period after the second polishing step until the step of cleaning the glass substrate is completed, Li is 0.1 mass% or more and 1 mass% or less, and Na is 0.1 mass % To 2.1% by mass and K is 0.05% to 0.5% by mass (Examples A to C), the change in SNR of the information recording medium (+0.04 to +0.16) can be reduced.

より好ましくは、ガラス基板の表層の組成の変化量が、Naが0.1質量%以上1.0質量%以下、Kが0.05質量%以上0.1質量%以下であれば(実施例B)、より情報記録媒体のSNRの変化(+0.04)を小さくすることが可能となる。   More preferably, the amount of change in the composition of the surface layer of the glass substrate is such that Na is 0.1% by mass or more and 1.0% by mass or less, and K is 0.05% by mass or more and 0.1% by mass or less (Example) B) The SNR change (+0.04) of the information recording medium can be further reduced.

以上、本発明の実施の形態および実施例について説明したが、今回開示された実施の形態および実施例はすべての点で例示であって制限的なものではないと考えられるべきである。本発明の範囲は特許請求の範囲によって示され、特許請求の範囲と均等の意味および範囲内でのすべての変更が含まれることが意図される。   Although the embodiments and examples of the present invention have been described above, the embodiments and examples disclosed this time should be considered as illustrative in all points and not restrictive. The scope of the present invention is defined by the terms of the claims, and is intended to include any modifications within the scope and meaning equivalent to the terms of the claims.

1 情報記録媒体、1G 情報記録媒体用ガラス基板、11 孔、12 外周端面、13 内周端面、14 表主表面、15 裏主表面、23 磁気薄膜層。   DESCRIPTION OF SYMBOLS 1 Information recording medium, 1G Glass substrate for information recording media, 11 hole, 12 outer peripheral end surface, 13 inner peripheral end surface, 14 front main surface, 15 back main surface, 23 magnetic thin film layer.

Claims (4)

情報記録媒体に用いられる情報記録媒体用ガラス基板の製造方法であって、
ガラス基板を準備する工程と、
前記ガラス基板を研磨する第1研磨工程と、
研磨が施された前記ガラス基板に対して化学強化処理を施す工程と、
前記化学強化処理が施された前記ガラス基板を研磨する第2研磨工程と、
研磨された前記ガラス基板を洗浄する工程と、
を備え、
前記ガラス基板の組成は、[LiO+NaO+KO]の割合が、7質量%〜30質量%であり、
前記第2研磨工程の後前記ガラス基板を洗浄する工程が終了するまでの間における、前記ガラス基板の表層の[LiO+NaO+KO]の組成の変化量の合計が、50ng/cm以内である、情報記録媒体用ガラス基板の製造方法。
A method for producing a glass substrate for an information recording medium used for an information recording medium,
Preparing a glass substrate;
A first polishing step for polishing the glass substrate;
Applying chemical strengthening treatment to the polished glass substrate;
A second polishing step of polishing the glass substrate subjected to the chemical strengthening treatment;
Cleaning the polished glass substrate;
With
The composition of the glass substrate is such that the ratio of [Li 2 O + Na 2 O + K 2 O] is 7% by mass to 30% by mass,
The total change amount of the composition of [Li 2 O + Na 2 O + K 2 O] on the surface layer of the glass substrate after the second polishing step until the step of cleaning the glass substrate is completed is 50 ng / cm 3. The manufacturing method of the glass substrate for information recording media which is within.
[LiO+NaO+KO]の組成の変化量の合計が、40ng/cm以内である、請求項1に記載の情報記録媒体用ガラス基板の製造方法。 The total amount of change in composition of [Li 2 O + Na 2 O + K 2 O] is within 40 ng / cm 3, a method of manufacturing a glass substrate for information recording medium according to claim 1. 前記第2研磨工程の後前記ガラス基板を洗浄する工程が終了するまでの間における、前記ガラス基板の前記表層の組成の変化量が、Liが0.1質量%以上1質量%以下、Naが0.1質量%以上2.1質量%以下、Kが0.05質量%以上0.5質量%以下である、請求項1または2に記載の情報記録媒体用ガラス基板の製造方法。   The amount of change in the composition of the surface layer of the glass substrate during the period after the second polishing step until the step of cleaning the glass substrate is completed, Li is 0.1 mass% or more and 1 mass% or less, and Na is The manufacturing method of the glass substrate for information recording media of Claim 1 or 2 which is 0.1 mass% or more and 2.1 mass% or less and K is 0.05 mass% or more and 0.5 mass% or less. 前記ガラス基板の前記表層の組成の変化量が、Naが0.1質量%以上1.0質量%以下、Kが0.05質量%以上0.1質量%以下である、請求項3に記載の情報記録媒体用ガラス基板の製造方法。   The amount of change in the composition of the surface layer of the glass substrate is such that Na is 0.1 mass% or more and 1.0 mass% or less, and K is 0.05 mass% or more and 0.1 mass% or less. The manufacturing method of the glass substrate for information recording media of.
JP2013068692A 2013-03-28 2013-03-28 Manufacturing method of glass substrate for information recording medium Pending JP2014191851A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106337171A (en) * 2015-07-07 2017-01-18 株式会社神户制钢所 Bottom-deposited substrate for Ni-coating technology, laminate body having Ni-coated layer and magnetic recording medium
JP2017021884A (en) * 2015-07-07 2017-01-26 株式会社神戸製鋼所 GROUND LAYER COATING SUBSTRATE USED FOR Ni PLATING, LAMINATE INCLUDING Ni PLATING LAYER, AND MAGNETIC RECORDING MEDIUM

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106337171A (en) * 2015-07-07 2017-01-18 株式会社神户制钢所 Bottom-deposited substrate for Ni-coating technology, laminate body having Ni-coated layer and magnetic recording medium
JP2017021884A (en) * 2015-07-07 2017-01-26 株式会社神戸製鋼所 GROUND LAYER COATING SUBSTRATE USED FOR Ni PLATING, LAMINATE INCLUDING Ni PLATING LAYER, AND MAGNETIC RECORDING MEDIUM

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