WO2011121913A1 - 情報記録媒体用ガラス基板の製造方法 - Google Patents
情報記録媒体用ガラス基板の製造方法 Download PDFInfo
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- WO2011121913A1 WO2011121913A1 PCT/JP2011/001498 JP2011001498W WO2011121913A1 WO 2011121913 A1 WO2011121913 A1 WO 2011121913A1 JP 2011001498 W JP2011001498 W JP 2011001498W WO 2011121913 A1 WO2011121913 A1 WO 2011121913A1
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- WIPO (PCT)
- Prior art keywords
- glass substrate
- polishing
- information recording
- colloidal silica
- recording medium
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Classifications
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- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
- G11B5/8404—Processes or apparatus specially adapted for manufacturing record carriers manufacturing base layers
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C19/00—Surface treatment of glass, not in the form of fibres or filaments, by mechanical means
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24355—Continuous and nonuniform or irregular surface on layer or component [e.g., roofing, etc.]
Definitions
- the present invention relates to a method for producing a glass substrate for an information recording medium.
- a glass substrate as a substrate is polished a plurality of times with high accuracy, such as a rough polishing process and a precision polishing process.
- the glass material is required to have high smoothness and high cleanliness, and to improve productivity.
- Patent Document 1 As a method for achieving high smoothness, a method using silica-based abrasive grains for final polishing is known, but at the same time, as a means for improving productivity, it is known that the silica-based abrasive grains are circulated and used.
- Patent Document 2 In this final polishing, it is known that polishing is performed using a slurry to which a gelation inhibitor is added in order to prevent aggregation and gelation of the slurry (polishing liquid in which silica-based abrasive grains are dispersed).
- the purpose of the present invention is to prevent the colloidal silica from gelling by restricting the number of times it can be used in circulation when colloidal silica is used as an abrasive when precision polishing a glass material.
- An object of the present invention is to provide a method for producing a glass substrate for an information recording medium capable of improving productivity.
- the first subject of the present invention uses an abrasive containing colloidal silica in a glass material having an iron content of 0.5 ng / cm 2 or less and a surface roughness Ra of 1 nm or less. And a precision polishing step of precisely polishing under acidic conditions.
- the second subject of the present invention is a glass substrate for an information recording medium manufactured by the above manufacturing method.
- colloidal silica used for current precision polishing has a main particle size of 20 nm to 80 nm, and these are used for polishing while being dispersed by a dispersant or the like.
- iron (Fe) dissolved from a glass material, particularly trivalent iron ions (Fe 3+ ) is present in the polishing slurry, colloidal silica is gelled by this Fe or Fe 3+ .
- colloidal silica when colloidal silica is used and circulated as an abrasive, the colloidal silica aggregates in a gel form with the passage of time, resulting in a problem that the colloidal silica cannot be used as an abrasive.
- the present inventor has found that the colloidal silica is gelled when Fe is adhered to the glass material or when Fe 3+ is dissolved from Fe. Since Fe adhering to the glass material dissolves while in contact with colloidal silica, it is considered that Fe 3+ and colloidal silica come into contact with each other before being chelated and gelled. These tendencies appear more clearly as the particle size of colloidal silica is smaller. This is presumably because the smaller the particle size, the greater the number of point contacts with the glass material, and the greater the number of contact between colloidal silica and Fe 3+ , resulting in gelation.
- the present invention has been made in view of the above problems based on such knowledge.
- the glass substrate for an information recording medium is, for example, an annular base material (substrate) suitable for a magnetic hard disk as an information storage medium.
- the glass substrate manufacturing process involves forming a circular disk-shaped glass material by pressing or boring, and includes a lapping process, a polishing process, a post-polishing cleaning process, and a precision polishing process. Is.
- Li 2 O is 3.6% by mass
- Na 2 O is 11.2% by mass
- K 2 O is 0.4% by mass
- MgO is 0.6% by mass
- CaO is 1.6% by mass
- Al 2 O 3 is 14.9% by mass
- SiO 2 is 64.5% by mass
- ZrO 2 is 2.0% by mass
- CeO 2 is 0.5% by mass
- SnO 2 is 0.7% by mass. Is preferred.
- the annular glass material formed by the press method is ground with a relatively rough diamond grindstone.
- This lapping step may be performed once, preferably twice.
- the glass material after the lapping process is polished with cerium oxide by a double-side polishing machine.
- the double-side polishing machine preferably has a DLC coating process on the entire surface.
- DLC is an abbreviation for diamond-like carbon, which protects the surface of the processing machine and can prevent the adhesion of iron as completely as possible.
- the glass material after the polishing process is preferably washed.
- a cleaning tank made of polyvinyl chloride (PVC) is used in order to prevent infiltration of iron.
- the post-polishing washing step of the present invention it is preferable to wash with a pH 13 alkaline detergent and rinse. Subsequently, it is preferable to wash and rinse with a pH 0 acid detergent (nitric acid) and finally wash with HF (0.1% solution).
- cerium oxide it is most efficient to perform cleaning in the order of alkali cleaning, acid cleaning, and HF. This is because the abrasive is first dispersed and removed with an alkaline detergent, then the abrasive is dissolved and removed with an acid detergent, and finally, the glass is etched with HF to remove the abrasive that is deeply stuck.
- each detergent is degassed and washed while applying ultrasonic waves. By performing deaeration, it becomes possible to remove cerium oxide that is strongly attached. Moreover, the effect of cavitation is increased by using ultrasonic waves, and the dispersion effect by the alkaline detergent is increased.
- Application conditions are 40 kHz for an alkaline detergent, 80 kHz for an acid detergent, and 170 kHz for an HF detergent.
- 80 kHz for an acid detergent solubility for small adhesion is improved.
- HF it is preferable to apply an ultrasonic wave of 170 kHz. In that case, finer cerium oxide can be removed.
- the precision polishing step is performed by using the same polishing apparatus as that used in the rough polishing step, changing the polishing pad from a hard polishing pad to a soft polishing pad.
- the processing performed in this precision polishing step is, for example, a smooth surface having a maximum surface roughness (Rmax) of about 6 nm or less while maintaining the flat and smooth main surface obtained in the above-described rough polishing step.
- Rmax maximum surface roughness
- This is a mirror polishing process that gives a mirror finish.
- the abrasive it is preferable to use an abrasive containing colloidal silica having a particle diameter lower than that of the cerium-based abrasive in the rough polishing step and an average particle diameter of 20 nm.
- a polishing liquid (slurry) containing such an abrasive is supplied to the glass material, and the surface of the glass material is mirror-polished by relatively sliding the polishing pad and the glass material.
- Precision polishing is preferably performed at pH 0.8 to pH 2.0. By performing precise polishing in such a pH range, a ⁇ potential can be suitably applied.
- the ⁇ potential can be applied as the acidic condition increases (lower pH) or as the alkaline condition increases (higher pH).
- the pH is too low, rust from the machine increases or the substrate remains damaged, which is not preferable.
- the glass material that has undergone the precision polishing process is stored in water without being dried, and is transported to the next cleaning process in a wet state. This is because if the glass material is dried with the polishing residue remaining, it may be difficult to remove the polishing material (colloidal silica) by this final cleaning step.
- the cleaning liquid does not perform an etching action or a leaching action on the glass material, and is configured as a cleaning liquid having selective dissolution performance with respect to colloidal silica.
- a glass substrate is manufactured through a cleaning process.
- the surface roughness Ra is an arithmetic average roughness of a square region having a length of 5 ⁇ m and a width of 5 ⁇ m on the main surface of the glass substrate that has been subjected to the cleaning treatment, and is 10 with an atomic force microscope (AFM). This is an observation of a single glass substrate.
- Glass composition The following were prepared as the composition of the glass material.
- Example 1 After the lapping was completed, the glass base plate was washed with a 0.1% by mass hydrofluoric acid (HF) solution, and then a polishing process was performed with cerium oxide using a double-side polishing machine. At this time, the double-side polishing machine used in the polishing process was the one whose entire surface was DLC coated.
- HF hydrofluoric acid
- Washing was performed after the polishing step.
- a washing tank made of PVC was used, and washing was performed in the order of neutral detergent, pure water, pure water, and IPA.
- the surface roughness Ra after washing was 0.4 nm.
- the colloidal silica having an average particle diameter of 20 nm was processed with a double-side polishing machine using a slurry of colloidal silica and DLC coating on the entire surface.
- the pH at this time was 1.0.
- the pH after 20 cycles of use was 1.9.
- Example 2 The process of Example 1 was similarly completed until the polishing process, and the post-polishing cleaning process was performed in the order of 0.1% by mass of HF solution, neutral detergent, pure water, pure water, and IPA.
- the surface roughness Ra after cleaning was 0.6 nm.
- colloidal silica having an average particle diameter of 20 nm as a slurry was processed with a double-side polishing machine.
- the pH at this time was 0.8.
- the pH after 20 cycles of use was 1.8.
- Example 3 The process of Example 1 was similarly completed until the polishing process, and the post-polishing cleaning process was performed in the order of 0.1% by mass of HF solution, sulfuric acid, alkaline detergent, pure water, and IPA.
- the surface roughness Ra after washing was 0.9 nm.
- colloidal silica having an average particle diameter of 20 nm was made into a slurry and processed with a double-side polishing machine.
- the pH at this time was 1.0.
- the pH after 20 cycles of use was 1.9.
- Example 4 The process of Example 1 was similarly completed until the polishing process, and the post-polishing cleaning process was performed in the order of 0.1% by mass of HF solution, neutral detergent, pure water, pure water, and IPA.
- the surface roughness Ra after cleaning was 0.6 nm.
- colloidal silica having an average particle diameter of 20 nm was made into a slurry and processed with a double-side polishing machine.
- the pH at this time was 1.0.
- the pH after 20 cycles of use was 1.9.
- Example 5 The process of Example 1 was similarly completed until the polishing process, and post-polishing washing was performed in the order of 0.1 mass% HF solution, neutral detergent, pure water, pure water, and IPA.
- the surface roughness Ra after washing was 0.9 nm.
- colloidal silica having an average particle diameter of 20 nm as a slurry was processed with a double-side polishing machine.
- the pH at this time was 1.0.
- the pH after 20 cycles of use was 1.9.
- Example 2 The process of Example 1 was similarly completed until the polishing process, and the post-polishing washing process was performed in the order of 2.0 mass% HF solution, sulfuric acid (5N), alkaline detergent, pure water, and IPA.
- the surface roughness Ra was 1.2 nm.
- colloidal silica having an average particle diameter of 20 nm was made into a slurry and processed with a double-side polishing machine.
- the pH at this time was 1.0.
- the pH after 20 cycles of use was 1.9.
- the amount of Fe adhesion (Q) ng / cm 2 on the surface of the obtained glass substrate was determined using a general high frequency inductively coupled plasma mass spectrometer (ICP-MS) (7700 manufactured by Agilent Technologies, Inc.). Series) and the average value for 10 sheets was calculated.
- ICP-MS inductively coupled plasma mass spectrometer
- the slurry was repeatedly used 15 times in the precision polishing process, and the quality at the 5th, 7th, and 15th times was evaluated in four stages of ⁇ , ⁇ , ⁇ , and ⁇ . Evaluation is performed by the surface roughness Ra at each circulation number (5th, 7th, 15th).
- the surface roughness Ra was evaluated as follows by observing 10 glass substrates with an atomic force microscope (AFM) manufactured by Veecco.
- A The average surface roughness Ra is 0.03 nm or more and less than 0.1 nm.
- ⁇ The average surface roughness Ra is 0.1 nm or more and less than 0.15 nm.
- X The average of surface roughness Ra is 0.2 nm or more.
- the iron content attached to the surface is 0.5 ng / cm 2 or less and the surface roughness Ra is 1 nm or less, and the abrasive material containing colloidal silica is used under acidic conditions.
- Examples 1 to 5 which were precisely polished with the above, excellent evaluation results were obtained even when the slurry was recycled 20 times in the precision polishing step.
- Comparative Example 1 in which the iron content adhering to the surface was 1.3 ng / cm 2 resulted in inferior evaluation at any time of slurry use.
- the comparative example 2 in which the surface roughness of the glass substrate surface before the precision polishing step was 1.2 nm is the same as in Example 1 above. The result was slightly inferior to the evaluation compared to -5.
- the present invention is a method for producing a glass substrate for an information recording medium, using an abrasive containing colloidal silica in a glass material having an iron content of 0.5 ng / cm 2 or less attached to the surface, under acidic conditions.
- the glass material is provided with a precision polishing step for precision polishing, and the glass material has a surface roughness Ra of 1 nm or less before final polishing.
- the amount of Fe (iron, iron ions) on the surface of the glass material used in the precision polishing step is extremely small, so that the gelation of colloidal silica can be suppressed as much as possible. Therefore, by using colloidal silica having a small particle size, it is possible to increase the number of circulation uses and improve productivity. In addition, if a large amount of iron is attached to the glass material, the attached Fe is deeply pierced by the polishing machine (colloidal silica). Therefore, it cannot be removed by subsequent cleaning or the like.
- the amount of Fe on the surface of the glass material used in the precision polishing step is extremely small, the amount of Fe adhering to the glass material after polishing is also reduced, and the cleanliness of the glass substrate There is an advantage that smoothness can be enhanced.
- polishing process is very small, it can grind
- the amount of Fe on the surface of the glass material used in the precision polishing process is extremely small. From this fact, it is possible to maintain a large number of times of circulating use even if the abrasive containing colloidal silica is recycled under acidic conditions during precision polishing, and the productivity can be remarkably improved. Has a remarkable effect.
- the precision polishing step is performed at pH 0.8 to pH 2.0.
- the ⁇ potential can be suitably applied.
- the particle size of the colloidal silica used in the precision polishing step is 80 nm or less, and is substantially in the range of 10 nm to 80 nm.
- the manufacturing method uses at least two types of abrasives, and uses a separate double-side polishing machine.
- the glass substrate for information recording medium of the present invention is manufactured by the method for manufacturing a glass substrate for information recording medium.
Abstract
Description
プレス法で成形した環状のガラス素材は、比較的粗いダイヤモンド砥石で研削加工する。このラッピング工程は、1回でもよく、好ましくは、2回実行する。また、ラッピング工程を複数回実行する場合、間に粗研磨工程を施して、ラッピング工程で残留した傷や歪みを除去することが好ましい。
ラッピング工程を終えたガラス素材は、両面研磨機で酸化セリウムによって、研磨される。上記両面研磨機は、全面をDLCコーティング加工しているものが好ましい。DLCとは、ダイヤモンドライクカーボンの略称であり、加工機の表面を保護し、鉄分の付着を可及的に完全に防ぐことが可能となるものである。
ポリッシュ工程後のガラス素材は、洗浄されることが好ましい。このポリッシュ後洗浄工程では、鉄分の侵入を防止するために、ポリ塩化ビニール(PVC)製の洗浄槽を使用する。
次に、精密研磨工程は、上記粗研磨工程で使用したものと同様の研磨装置を用い、研磨パッドを硬質研磨パッドから軟質研磨パッドに替えて実施される。この精密研磨工程で行う処理は、上述した粗研磨工程で得られた平坦平滑な主表面を維持しつつ、例えば主表面の表面粗さの最大高さ(Rmax)が6nm程度以下である平滑な鏡面に仕上げるような鏡面研磨処理である。研磨材としては、粗研磨工程のセリウム系研磨材より粒子径が低い、平均粒子径は20nmの、コロイダルシリカを含む研磨材を用いることが好ましい。かかる研磨材を含む研磨液(スラリー)をガラス素材に供給し、研磨パッドとガラス素材とを相対的に摺動させて、ガラス素材の表面を鏡面研磨する。
上記精密研磨工程を終えたガラス素材の最終洗浄工程は下記の通りに行われる。
ガラス素材の組成として、以下のものを用意した。
ラッピング終了後のガラス素板を0.1質量%のフッ化水素酸(HF)溶液で洗浄した後、両面研磨機で酸化セリウムによってポリッシュ工程を行った。この時ポリッシュ工程で使用する両面研磨機は、全面をDLCコーティング加工しているものを使用した。
実施例1の工程をポリッシュ工程まで同じように終了し、ポリッシュ後洗浄工程を0.1質量%のHF溶液、中性洗剤、純水、純水、IPAの順で施した。洗浄後の表面粗さRaは0.6nmであった。その後、コロイダルシリカ平均粒径20nmのコロイダルシリカをスラリとし、両面研磨機で加工を行った。このときのpHは、0.8とした。この際使用したスラリが何回循環できるかを確認するため、循環使用し続けた際の表面粗さRaが変化しないかどうかを確認した。20回循環使用後のpHは1.8であった。
実施例1の工程をポリッシュ工程まで同じように終了し、ポリッシュ後洗浄工程を0.1質量%のHF溶液、硫酸、アルカリ洗剤、純水、IPAの順で施した。洗浄後の表面粗さRaは0.9nmであった。その後コロイダルシリカ平均粒径20nmのコロイダルシリカをスラリとし、両面研磨機で加工を行った。このときのpHは、1.0とした。この際使用したスラリが何回循環できるかを確認するため、循環使用し続けた際の表面粗さRaが変化しないかどうかを確認した。20回循環使用後のpHは1.9であった。
実施例1の工程をポリッシュ工程まで同じように終了し、ポリッシュ後洗浄工程を0.1質量%のHF溶液、中性洗剤、純水、純水、IPAの順で施した。洗浄後の表面粗さRaは0.6nmであった。その後コロイダルシリカ平均粒径20nmのコロイダルシリカをスラリとし、両面研磨機で加工を行った。このときのpHは、1.0とした。この際使用したスラリが何回循環できるかを確認するため、循環使用し続けた際の表面粗さRaが変化しないかどうかを確認した。20回循環使用後のpHは1.9であった。
実施例1の工程をポリッシュ工程まで同じように終了し、ポリッシュ後洗浄を0.1質量%のHF溶液、中性洗剤、純水、純水、IPAの順で施した。洗浄後の表面粗さRaは0.9nmであった。その後、コロイダルシリカ平均粒径20nmのコロイダルシリカをスラリとし、両面研磨機で加工を行った。このときのpHは、1.0とした。この際使用したスラリが何回循環できるかを確認するため、循環使用し続けた際の表面粗さRaが変化しないかどうかを確認した。20回循環使用後のpHは1.9であった。
ラッピング工程終了後、一般の酸洗剤で洗浄し、DLCコーティングをしていない両面研磨機で加工、中性洗剤、純水、純水、IPAで洗浄を行った。洗浄後の表面粗さRaは0.4nmであった。その後コロイダルシリカ平均粒径20nmのコロイダルシリカをスラリとし、両面研磨機で加工を行った。このときのpHは、1.0とした。この際使用したスラリが何回循環できるかを確認するため、循環使用し続けた際の表面粗さRaが変化しないかどうかを確認した。20回循環使用後のpHは1.9であった。
実施例1の工程をポリッシュ工程まで同じように終了し、ポリッシュ後洗浄工程を2.0質量%のHF溶液、硫酸(5N)、アルカリ系洗剤、純水、IPAの順で施した。表面粗さRaは1.2nmであった。その後コロイダルシリカ平均粒径20nmのコロイダルシリカをスラリとし、両面研磨機で加工を行った。このときのpHは、1.0とした。この際使用したスラリが何回循環できるかを確認するため、循環使用し続けた際の表面粗さRaが変化しないかどうかを確認した。20回循環使用後のpHは1.9であった。
各実施例1~5、比較例1、2において、精密研磨工程での循環使用回数の可否をFe量や表面粗さRaで評価した。
○:表面粗さRaの平均が0.1nm以上0.15nm未満である。
△:表面粗さRaの平均が0.15nm以上0.2nm未満である。
×:表面粗さRaの平均が0.2nm以上である。
Claims (5)
- 表面に付着している鉄分が0.5ng/cm2以下であって、表面粗さRaが1nm以下であるガラス素材にコロイダルシリカを含む研磨材を用いて、酸性条件下で精密研磨する精密研磨工程を備えることを特徴とする情報記録媒体用ガラス基板の製造方法。
- 請求項1記載の情報記録媒体用ガラス基板の製造方法において、
上記精密研磨工程は、pH0.8~pH2.0で行うことを特徴とする情報記録媒体用ガラス基板の製造方法。 - 請求項1または2記載の情報記録媒体用ガラス基板の製造方法において、
上記精密研磨工程に使用するコロイダルシリカの粒径が80nm以下であることを特徴とする情報記録媒体用ガラス基板の製造方法。 - 請求項1から3の何れか1項に記載の情報記録媒体用ガラス基板の製造方法において、
上記製造方法は、少なくとも2種類の研磨材を使用し、それぞれ別の両面研磨機を使用することを特徴とする情報記録媒体用ガラス基板の製造方法。 - 請求項1から4の何れか1項に記載の情報記録媒体用ガラス基板の製造方法によって製造された情報記録媒体用ガラス基板。
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US13/638,871 US9076480B2 (en) | 2010-03-29 | 2011-03-15 | Method of producing glass substrate for information recording medium |
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