JP2001207161A - Composition for polishing a magnetic disk substrate - Google Patents
Composition for polishing a magnetic disk substrateInfo
- Publication number
- JP2001207161A JP2001207161A JP2000013858A JP2000013858A JP2001207161A JP 2001207161 A JP2001207161 A JP 2001207161A JP 2000013858 A JP2000013858 A JP 2000013858A JP 2000013858 A JP2000013858 A JP 2000013858A JP 2001207161 A JP2001207161 A JP 2001207161A
- Authority
- JP
- Japan
- Prior art keywords
- polishing
- magnetic disk
- composition
- disk substrate
- silicon oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000005498 polishing Methods 0.000 title claims abstract description 97
- 239000000203 mixture Substances 0.000 title claims abstract description 51
- 239000000758 substrate Substances 0.000 title claims abstract description 37
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 39
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 21
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 20
- 239000003349 gelling agent Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims description 12
- -1 phosphonic acid compound Chemical class 0.000 claims description 8
- 239000008119 colloidal silica Substances 0.000 claims description 7
- 239000011163 secondary particle Substances 0.000 claims description 7
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims description 4
- 229910021485 fumed silica Inorganic materials 0.000 claims description 4
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 claims description 3
- XBIUWALDKXACEA-UHFFFAOYSA-N 3-[bis(2,4-dioxopentan-3-yl)alumanyl]pentane-2,4-dione Chemical compound CC(=O)C(C(C)=O)[Al](C(C(C)=O)C(C)=O)C(C(C)=O)C(C)=O XBIUWALDKXACEA-UHFFFAOYSA-N 0.000 claims 1
- 230000003746 surface roughness Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 description 12
- 229910052782 aluminium Inorganic materials 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 239000003112 inhibitor Substances 0.000 description 7
- 238000001879 gelation Methods 0.000 description 6
- 230000001737 promoting effect Effects 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 4
- 239000011362 coarse particle Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- 229910002012 Aerosil® Inorganic materials 0.000 description 2
- 229910000531 Co alloy Inorganic materials 0.000 description 2
- 229910000599 Cr alloy Inorganic materials 0.000 description 2
- 239000006061 abrasive grain Substances 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 150000003009 phosphonic acids Chemical class 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- PPQJCISYYXZCAE-UHFFFAOYSA-N 1,10-phenanthroline;hydrate Chemical compound O.C1=CN=C2C3=NC=CC=C3C=CC2=C1 PPQJCISYYXZCAE-UHFFFAOYSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Landscapes
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
Abstract
(57)【要約】
【課題】 磁気ディスクの表面粗さが小さく、かつ突起
や研磨傷を発生させず、高密度記録が達成可能であり、
しかも経済的な速度で研磨できる磁気ディスク基板の研
磨用組成物を提供すること。
【解決手段】 水、酸化ケイ素、ゲル化防止剤、硝酸ア
ルミニウム及び過酸化水素からなる磁気ディスク基板研
磨用組成物。(57) [Summary] [PROBLEMS] To achieve high-density recording with a small surface roughness of a magnetic disk and no projections or polishing scratches.
In addition, to provide a polishing composition for a magnetic disk substrate which can be polished at an economical rate. A composition for polishing a magnetic disk substrate comprising water, silicon oxide, an anti-gelling agent, aluminum nitrate and hydrogen peroxide.
Description
【0001】本発明は磁気ディスク基板研磨用組成物に
関し、さらに詳しくは、磁気ヘッドが低浮上量で飛行す
るのに適した精度の高い磁気ディスク表面が得られる磁
気ディスク基板研磨用組成物に関する。The present invention relates to a composition for polishing a magnetic disk substrate, and more particularly to a composition for polishing a magnetic disk substrate capable of obtaining a highly accurate magnetic disk surface suitable for flying a magnetic head with a low flying height.
【0002】[0002]
【従来の技術】コンピューターやワードプロセッサーの
外部記憶装置の中で高速でアクセス出来る手段として磁
気ディスク(メモリーハードディスク)が広く使われて
いる。この磁気ディスクの代表的な一例は、Al合金基
板の表面にNiPを無電解メッキしたものを基板とし、
この基板を表面研磨した後、Cr合金下地膜、Co合金
磁性膜そしてカーボン保護膜を順次スパッターで形成し
たものである。磁気ディスク表面に磁気ヘッド浮上量以
上の高さを有する突起が残っていると、所定高さにて浮
上しながら高速で飛行する磁気ヘッドがその突起に衝突
して損傷する原因になる。また、磁気ディスク基板に突
起や研磨傷などがあるとCr合金下地膜やCo合金磁性
膜などを形成したとき、それらの膜の表面に突起が現
れ、また研磨傷に基づく欠陥が生じ、磁気ディスク表面
が精度の高い平滑面にならないので、ディスク表面の精
度を上げるには基板を精密に研磨する必要がある。2. Description of the Related Art A magnetic disk (memory hard disk) is widely used as a means which can be accessed at high speed in an external storage device of a computer or a word processor. A typical example of this magnetic disk is a substrate obtained by electrolessly plating NiP on the surface of an Al alloy substrate,
After polishing the surface of this substrate, a Cr alloy base film, a Co alloy magnetic film, and a carbon protective film were sequentially formed by sputtering. If a protrusion having a height equal to or higher than the flying height of the magnetic head remains on the surface of the magnetic disk, the magnetic head flying at a high speed while flying at a predetermined height may collide with the protrusion and be damaged. In addition, if the magnetic disk substrate has projections or polishing scratches, when a Cr alloy base film or a Co alloy magnetic film is formed, projections appear on the surface of those films, and defects due to the polishing scratches occur. Since the surface does not become a high-precision smooth surface, it is necessary to precisely polish the substrate to increase the accuracy of the disk surface.
【0003】このため、磁気ディスク基板の研磨におい
て、突起物をなくし、またはその高さをできるだけ低く
し、かつ研磨傷が生じ難い研磨用組成物として多くのも
のが提案されてきた。なかでも特開平10−12103
5(チタニアに硝酸アルミニウムを添加してなる組成物
を使用)はサブミクロンの酸化チタニウム粒子を砥粒と
して使用しているので従来に比較して高い面精度、研磨
速度は達成しやすいが、最近求められる面精度のレベル
には砥粒物質の硬度の影響で達成が困難な状況である。
また、特開平11−167715(コロイダルシリカに
硝酸アルミニウムを添加してなる組成物を使用)は砥粒
に硬度の小さい酸化ケイ素微粒子を使用しているため面
精度は得られやすいが、実生産に使用できる研磨速度の
達成が困難であった。[0003] For this reason, in polishing a magnetic disk substrate, many polishing compositions have been proposed as polishing compositions which eliminate protrusions or reduce the height thereof as much as possible and which hardly cause polishing scratches. Above all, Japanese Patent Application Laid-Open No. 10-12103
5 (using a composition obtained by adding aluminum nitrate to titania) uses submicron titanium oxide particles as abrasive grains, so that higher surface accuracy and polishing speed can be easily achieved as compared with the conventional method. It is difficult to achieve the required level of surface accuracy due to the influence of the hardness of the abrasive material.
Japanese Patent Application Laid-Open No. 11-167715 (using a composition obtained by adding aluminum nitrate to colloidal silica) uses silicon oxide fine particles having low hardness as abrasive grains, so that surface accuracy can be easily obtained. It was difficult to achieve a usable polishing rate.
【0004】[0004]
【発明が解決しようとする課題】高密度磁気記録を可能
とするアルミニウム磁気ディスク基板研磨用組成物に要
求される品質は、ヘッドの低浮上を可能とする高精度デ
ィスク面の達成である。本発明の目的は、磁気ディスク
の表面粗さが小さく、かつ突起や研磨傷を発生させず、
高密度記録が達成可能であり、しかも経済的な速度で研
磨できる磁気ディスク基板の研磨用組成物を提供するこ
とにある。The quality required of a polishing composition for an aluminum magnetic disk substrate that enables high-density magnetic recording is to achieve a high-precision disk surface that enables low flying of the head. An object of the present invention is to reduce the surface roughness of a magnetic disk and to prevent protrusions and polishing scratches from occurring.
An object of the present invention is to provide a polishing composition for a magnetic disk substrate, which can achieve high-density recording and can be polished at an economical rate.
【0005】[0005]
【課題を解決するための手段】本発明者らは、低浮上量
型アルミニウム磁気ディスクに要求される高精度の研磨
面を達成するための研磨剤について鋭意研究した結果、
酸化ケイ素を研磨材とし、これに硝酸アルミニウム、ゲ
ル化防止剤及び過酸化水素を配合してなる研磨用組成物
が優れた性能を示すことを見いだし、本発明の完成に至
った。すなわち、本発明は以下の各発明からなる。 (1)水、酸化ケイ素、ゲル化防止剤、硝酸アルミニウ
ム及び過酸化水素からなる磁気ディスク基板研磨用組成
物。 (2)酸化ケイ素がコロイダルシリカ、ヒュームドシリ
カ及びホワイトカーボンから選ばれる1種又は2種以上
である上記(1)に記載の磁気ディスク基板研磨用組成
物。 (3)酸化ケイ素の二次粒子の平均粒子径が0.03〜
0.5μmである上記(1)または(2)に記載の磁気
ディスク基板研磨用組成物。 (4)酸化ケイ素の研磨用組成物中濃度が3〜30質量
%である上記(1)〜(3)のいずれかに記載の磁気デ
ィスク基板研磨用組成物。 (5)ゲル化防止剤がホスホン酸系化合物、フェナント
ロリン及びアセチルアセトンアルミニウム塩から選ばれ
る1種又は2種以上である上記(1)〜(4)のいずれ
かに記載の磁気ディスク基板研磨用組成物。 (6)ホスホン酸系化合物が1−ヒドロキシエタン−
1,1−ジホスホン酸である上記(5)に記載の磁気デ
ィスク基板研磨用組成物。Means for Solving the Problems The present inventors have conducted intensive studies on an abrasive for achieving a high-accuracy polished surface required for a low flying height type aluminum magnetic disk.
It has been found that a polishing composition comprising silicon oxide as an abrasive and aluminum nitrate, an anti-gelling agent and hydrogen peroxide exhibits excellent performance, and the present invention has been completed. That is, the present invention includes the following inventions. (1) A composition for polishing a magnetic disk substrate comprising water, silicon oxide, an anti-gelling agent, aluminum nitrate and hydrogen peroxide. (2) The composition for polishing a magnetic disk substrate according to the above (1), wherein the silicon oxide is at least one selected from colloidal silica, fumed silica and white carbon. (3) The average particle size of the secondary particles of silicon oxide is 0.03 to
The composition for polishing a magnetic disk substrate according to the above (1) or (2), which has a thickness of 0.5 μm. (4) The polishing composition for a magnetic disk substrate according to any one of the above (1) to (3), wherein the concentration of the silicon oxide in the polishing composition is 3 to 30% by mass. (5) The composition for polishing a magnetic disk substrate according to any one of the above (1) to (4), wherein the gelling inhibitor is one or more selected from phosphonic acid compounds, phenanthroline and aluminum acetylacetone. . (6) the phosphonic acid compound is 1-hydroxyethane-
The composition for polishing a magnetic disk substrate according to the above (5), which is 1,1-diphosphonic acid.
【0006】本発明によれば、水、酸化ケイ素、ゲル化
防止剤、硝酸アルミニウム及び過酸化水素を含んでなる
組成物であって、ゲル化防止剤、硝酸アルミニウム及び
過酸化水素の3成分が混在することにより、より高い研
磨速度が得られることを特徴とする磁気ディスク基板研
磨用組成物が提供される。本発明の研磨用組成物は、例
えば磁気抵抗(MR)効果を利用した磁気ヘッド用磁気
ディスクに代表される高記録密度用の基板(通常、1G
bit/inch 2 以上の記録密度を有する)に有利に
適用できるが、それ以下の記録密度を有する磁気ディス
クに対しても信頼性向上という見地から効果的に応用で
きる。According to the present invention, water, silicon oxide, gelled
Inhibitor, comprising aluminum nitrate and hydrogen peroxide
A composition comprising an anti-gelling agent, aluminum nitrate and
The higher the concentration of hydrogen peroxide, the higher
Magnetic disk substrate lab characterized by high polishing speed
A polishing composition is provided. Polishing composition of the present invention is an example
For example, magnetism for magnetic heads utilizing the magnetoresistance (MR) effect
A substrate for high recording density represented by a disk (usually 1G
bit / inch Two Above recording density)
Applicable, but a magnetic disk with a lower recording density
Can be applied effectively from the perspective of improving reliability.
Wear.
【0007】[0007]
【発明の実施の形態】本発明の研磨用組成物に研磨材と
して含まれる酸化ケイ素は、特に限定されるものではな
く、コロイダルシリカ、ヒュームドシリカ、ホワイトカ
ーボンでも良く、二次粒子の平均粒子径は0.03〜
0.5μmであることが好ましい。二次粒子の平均粒子
径はレーザードップラー周波数解析式粒度分布測定器、
マイクロトラックUPA150(Honeywell社
製)により測定した値である。酸化ケイ素の二次粒子径
が大きくなると細目のゲル化、凝集は抑制しやすくなる
が、粗い粒子の存在確率も高くなるため、研磨傷発生の
原因となる。また、二次粒子径が小さくなると、前述の
ゲル化、凝集が起きやすくなり、やはり研磨傷発生の原
因となる。従って、本発明の研磨用組成物に研磨材とし
て含まれる酸化ケイ素の二次粒子の平均粒子径は0.0
3〜0.5μmであることが好ましく、更には0.04
〜0.2μmがより好ましい。BEST MODE FOR CARRYING OUT THE INVENTION The silicon oxide contained as an abrasive in the polishing composition of the present invention is not particularly limited, and may be colloidal silica, fumed silica, or white carbon. The diameter is 0.03 ~
It is preferably 0.5 μm. The average particle size of the secondary particles is measured by a laser Doppler frequency analysis type particle size distribution analyzer,
This is a value measured by Microtrac UPA150 (manufactured by Honeywell). When the secondary particle diameter of silicon oxide is large, fine gelation and agglomeration are easily suppressed, but the probability of existence of coarse particles is also high, which causes polishing scratches. In addition, when the secondary particle diameter is small, the above-mentioned gelation and aggregation are likely to occur, which also causes polishing scratches. Therefore, the average particle diameter of the secondary particles of silicon oxide contained as an abrasive in the polishing composition of the present invention is 0.0
It is preferably 3 to 0.5 μm, more preferably 0.04 μm.
0.20.2 μm is more preferable.
【0008】研磨用組成物中の酸化ケイ素の濃度が3質
量%未満の場合は研磨速度が著しく低い。また、濃度が
高くなるにつれて研磨速度は高くなるが、30質量%を
越えると研磨速度の上昇が見られないだけでなく、特に
コロイダルシリカではゲル化しやすくなる。経済性を加
味すると実用的には30質量%が上限となる。従って、
酸化ケイ素の組成物中濃度としては3〜30質量%の範
囲であることが好ましく、更には5〜15質量%が好ま
しい。When the concentration of silicon oxide in the polishing composition is less than 3% by mass, the polishing rate is extremely low. The polishing rate increases as the concentration increases. However, if the concentration exceeds 30% by mass, not only does the polishing rate not increase, but also gelation tends to occur particularly with colloidal silica. In consideration of economy, the upper limit is practically 30% by mass. Therefore,
The concentration of silicon oxide in the composition is preferably in the range of 3 to 30% by mass, more preferably 5 to 15% by mass.
【0009】本発明の研磨用組成物に用いるゲル化防止
剤、硝酸アルミニウム及び過酸化水素はこれら3成分の
混在により、大きな研磨促進の効果を出すが、それぞれ
の添加量はゲル化防止剤が0.1〜2質量%、更に好ま
しくは0.3〜1質量%、硝酸アルミニウムが1〜20
質量%、更に好ましくは2〜15質量%、過酸化水素が
0.2〜5質量%、更に好ましくは0.5〜3質量%で
ある。ゲル化防止剤の添加量が0.1質量%未満では研
磨促進への効果が低く、なお且つ、ゲル化しやすくな
る。また、ゲル化防止剤の添加量が2質量%を越えても
研磨促進への効果は高くならない。The anti-gelling agent, aluminum nitrate and hydrogen peroxide used in the polishing composition of the present invention can greatly enhance the polishing effect due to the mixture of these three components. 0.1 to 2% by mass, more preferably 0.3 to 1% by mass, aluminum nitrate is 1 to 20%
%, More preferably 2 to 15% by mass, and hydrogen peroxide is 0.2 to 5% by mass, more preferably 0.5 to 3% by mass. If the amount of the gelling inhibitor is less than 0.1% by mass, the effect of promoting the polishing is low, and the gelation is easily caused. Further, even if the addition amount of the gelling inhibitor exceeds 2% by mass, the effect of promoting the polishing does not increase.
【0010】硝酸アルミニウムの添加量が1質量%未満
では研磨促進への効果が低い。また、硝酸アルミニウム
の添加量が20質量%を越えるとよりゲル化しやすくな
る傾向がある。過酸化水素の添加量が0.2質量%未満
では研磨促進への効果が低い。また、過酸化水素の添加
量が5質量%を越えても研磨促進への効果は高くならな
い。When the amount of aluminum nitrate is less than 1% by mass, the effect on accelerating polishing is low. If the amount of aluminum nitrate exceeds 20% by mass, gelation tends to occur more easily. If the amount of added hydrogen peroxide is less than 0.2% by mass, the effect of promoting polishing is low. Further, even if the added amount of hydrogen peroxide exceeds 5% by mass, the effect of promoting polishing is not increased.
【0011】本発明に用いられるゲル化防止剤は、好ま
しくはホスホン酸系化合物、フェナントロリン及びアセ
チルアセトンアルミニウム塩から選ばれた1種又は2種
以上の混合物である。具体的には、ホスホン酸系化合物
としては、1−ヒドロキシエタン−1,1−ジホスホン
酸(C2 H6 O7 P2 )若しくはアミノトリメチレンホ
スホン酸(C2 H12O9 P3 N)を、フェナントロリン
としては、1,10−フェナントロリン一水和物(C12
H8 N2 ・H2 O)を、アセチルアセトンアルミニウム
塩としては、アセチルアセトンのアルミニウム錯塩(A
l2 〔CH(COCH3 )3 〕)をそれぞれ例示するこ
とが出来る。この中でも特に、研磨促進としては1−ヒ
ドロキシエタン−1,1−ジホスホン酸の効果が一番高
い。The gelling inhibitor used in the present invention is preferably one or a mixture of two or more selected from phosphonic acid compounds, phenanthroline and aluminum acetylacetone. Specifically, as the phosphonic acid compound, 1-hydroxyethane-1,1-diphosphonic acid (C 2 H 6 O 7 P 2 ) or aminotrimethylene phosphonic acid (C 2 H 12 O 9 P 3 N) And phenanthroline as 1,10-phenanthroline monohydrate (C 12
H 8 N 2 .H 2 O) as an aluminum salt of acetylacetone, aluminum complex salt of acetylacetone (A
l 2 [CH (COCH 3 ) 3 ]). Among these, 1-hydroxyethane-1,1-diphosphonic acid has the highest effect on promoting polishing.
【0012】上記の各成分濃度は磁気ディスク基板を研
磨する際の濃度である。研磨用組成物を製造し、運搬等
する場合は上記濃度より濃厚な組成物とし、使用に際し
て上記の濃度に薄めて使用するのが効率的である。The above-mentioned respective component concentrations are those at the time of polishing a magnetic disk substrate. When a polishing composition is manufactured and transported, it is efficient to use a composition that is thicker than the above concentration and dilute it to the above concentration before use.
【0013】本発明の研磨用組成物は酸化ケイ素にゲル
化防止剤、硝酸アルミニウム及び過酸化水素の3成分を
混在させることにより、大きな研磨促進の効果を出す
が、そのメカニズムについては定かではないが、ゲル化
防止剤の分散効果によるマイルドな機械研磨作用、過酸
化水素の酸化効果が硝酸アルミニウムの研磨促進効果を
増幅させ化学研磨作用をより効果的にさせるように働い
ていることが推測される。これら3成分が混在すること
により、どの2成分の混在よりも研磨速度が高く、研磨
傷及びピットの発生を抑制することが確認されている。The polishing composition of the present invention has a large polishing-promoting effect by mixing silicon oxide with three components of a gelling inhibitor, aluminum nitrate and hydrogen peroxide, but the mechanism is not clear. However, it is speculated that the mild mechanical polishing effect due to the dispersing effect of the gelling agent and the oxidizing effect of hydrogen peroxide work to amplify the polishing promoting effect of aluminum nitrate and make the chemical polishing effect more effective. You. It has been confirmed that when these three components are mixed, the polishing rate is higher than when any two components are mixed, and the generation of polishing scratches and pits is suppressed.
【0014】本発明の磁気ディスク基板の研磨用組成物
は前記の各成分の他に、界面活性剤、防腐剤等を添加す
ることができる。しかし、その種類及び添加量はゲル化
を引き起こさないよう注意が必要である。本発明の研磨
用組成物は、従来の研磨用組成物と同様に、水に酸化ケ
イ素を懸濁し、これにゲル化防止剤、硝酸アルミニウム
及び過酸化水素等を添加することによって調製すること
ができる。The polishing composition for a magnetic disk substrate of the present invention may contain a surfactant, a preservative and the like in addition to the above-mentioned components. However, care must be taken so that the type and amount of addition do not cause gelation. The polishing composition of the present invention can be prepared by suspending silicon oxide in water and adding an anti-gelling agent, aluminum nitrate and hydrogen peroxide to the same as in the conventional polishing composition. it can.
【0015】本発明の研磨用組成物を適用する磁気ハー
ドディスク基板は格別限定されるものではないが、アル
ミニウム(合金を含む)基板、とくに、例えばNiPを
無電解メッキしたアルミニウム基板の研磨に本発明の組
成物を適用すると、酸化ケイ素によるマイルドな機械的
研磨作用とゲル化防止剤、硝酸アルミニウム及び過酸化
水素による化学的研磨作用とが相俟って、高品質の研磨
面が得られる。研磨方法は一般にスラリー状研磨材に用
いられる研磨パッドを磁気ディスク基板上に摺り合わ
せ、パッドと基板の間にスラリーを供給しながらパッド
または基板を回転させる方法である。本発明の研磨用組
成物を用いて研磨した基板からつくられた磁気ディスク
は、マイクロピット、マイクロスクラッチ等微細な欠陥
について発生頻度が非常に低く、また表面粗さ(Ra)
も0.2〜0.3nm位であり、非常に平滑性に優れて
いる。The magnetic hard disk substrate to which the polishing composition of the present invention is applied is not particularly limited, but the present invention is applicable to polishing of an aluminum (including alloy) substrate, particularly, for example, an aluminum substrate electrolessly plated with NiP. By applying the composition described above, a high-quality polished surface can be obtained by combining the mild mechanical polishing action of silicon oxide with the chemical polishing action of an anti-gelling agent, aluminum nitrate and hydrogen peroxide. The polishing method is a method in which a polishing pad generally used for a slurry-like abrasive is rubbed on a magnetic disk substrate, and the pad or the substrate is rotated while supplying slurry between the pad and the substrate. A magnetic disk made from a substrate polished using the polishing composition of the present invention has a very low frequency of micro defects such as micro pits and micro scratches, and has a low surface roughness (Ra).
Is about 0.2 to 0.3 nm, which is very excellent in smoothness.
【0016】[0016]
【実施例】以下、本発明の実施例について具体的に説明
するが、本発明はこれらの実施例に限定されるものでは
ない。 (実施例1〜13)コロイダルシリカ(デュポン(株)
製、サイトンHT−50F)に水、ゲル化防止剤、硝酸
アルミニウム及び過酸化水素を表2に示す割合で添加
し、種々の水性研磨用組成物を調製し、以下に示す研磨
装置および研磨条件で研磨を行った。その結果を表2に
示す。なお、粒子径はレーザードップラー周波数解析式
粒度分布測定器、マイクロトラックUPA150(Ho
neywell社製)により測定した。粒度測定値を表
1に示す。EXAMPLES Examples of the present invention will be specifically described below, but the present invention is not limited to these examples. (Examples 1 to 13) Colloidal silica (Dupont Co., Ltd.)
Water, a gelling inhibitor, aluminum nitrate and hydrogen peroxide were added to the composition shown in Table 2 to prepare various aqueous polishing compositions. The polishing apparatus and polishing conditions shown below were used. Was polished. Table 2 shows the results. The particle size was measured using a laser Doppler frequency analysis type particle size distribution analyzer, Microtrac UPA150 (Ho
newwell). Table 1 shows the measured particle size.
【0017】(実施例14、15)ホワイトカーボン
(日本シリカ工業(株)製、E−150J)及びヒュー
ムドシリカ(日本アエロジル(株)製、AEROSIL
50)を媒体攪拌ミルにより粉砕、整粒により粗粒子を
除去し、二次粒子の平均粒子径が0.1μmの酸化ケイ
素を調製した。次に、水、ゲル化防止剤、硝酸アルミニ
ウム及び過酸化水素を表2に示す割合で添加し、種々の
水性研磨用組成物を調製し、以下に示す研磨装置および
研磨条件で研磨を行った。その結果を表2に示す。な
お、粒度測定値は表1に示す。(Examples 14 and 15) White carbon (manufactured by Nippon Silica Industry Co., Ltd., E-150J) and fumed silica (manufactured by Nippon Aerosil Co., Ltd., AEROSIL)
50) was pulverized with a medium stirring mill and coarse particles were removed by sizing to prepare silicon oxide having an average secondary particle diameter of 0.1 μm. Next, water, an anti-gelling agent, aluminum nitrate and hydrogen peroxide were added in the proportions shown in Table 2 to prepare various aqueous polishing compositions, and polished with the following polishing apparatus and polishing conditions. . Table 2 shows the results. Table 1 shows the measured particle size.
【0018】研磨条件 使用した基板:NiPを無電解メッキした3.5インチ
サイズのアルミニウムディスク。 使用した研磨装置および研磨条件 研磨試験機‥‥‥‥‥4ウェイ式両面ポリシングマシン 研磨パッド‥‥‥‥‥スエードタイプ(ポリテックスD
G、ロデール社製) 下定盤回転速度‥‥‥60rpm スラリー供給速度‥‥50ml/min 研磨時間‥‥‥‥‥‥5min 加工圧力‥‥‥‥‥‥50g/cm2 Polishing conditions Substrate used: A 3.5-inch size aluminum disk electrolessly plated with NiP. Polishing equipment and polishing conditions used Polishing tester 4-sided double-side polishing machine Polishing pad Suede type (Polytex D
G, manufactured by Rodale) Lower platen rotation speed ‥‥‥ 60 rpm Slurry supply speed ‥‥ 50 ml / min Polishing time ‥‥‥‥‥‥ 5 min Working pressure ‥‥‥‥‥‥ 50 g / cm 2
【0019】研磨特性の評価 研磨レート‥‥アルミニウムディスクの研磨前後の重量
減より換算。 表面粗さ‥‥‥タリステップ、タリデータ2000(ラ
ンクテーラーホブソン社製)を使用。 研磨傷および研磨ピットの深さは触針式表面解析装置P
−12(TENCOR社製)の3次元モードにより形状
解析し深さをもとめた。研磨特性の評価結果を表2に示
す。表2中の研磨傷Aは研磨傷深さが5nm以下であ
り、研磨傷Bは研磨傷深さが5〜10nmである。また
ピットAはピット深さが5nm以下であり、ピットBは
ピット深さが5〜10nmである。研磨傷深さが10n
mより大なもの、またピット深さが10nmより大なも
のは、実施例、比較例共に発生しなかった。Evaluation of polishing characteristics Polishing rate ‥‥ Calculated from weight loss before and after polishing an aluminum disk. Uses Taristep 2000 Taridata 2000 (Rank Taylor Hobson). The depth of polishing scratches and polishing pits is measured using a stylus type surface analyzer P
The shape was analyzed using a three-dimensional mode of -12 (manufactured by TENCOR) to determine the depth. Table 2 shows the evaluation results of the polishing characteristics. The polishing flaw A in Table 2 has a polishing flaw depth of 5 nm or less, and the polishing flaw B has a polishing flaw depth of 5 to 10 nm. Pit A has a pit depth of 5 nm or less, and pit B has a pit depth of 5 to 10 nm. Polishing scratch depth is 10n
Those larger than m and those having a pit depth larger than 10 nm did not occur in both the examples and comparative examples.
【0020】(比較例1〜2)コロイダルシリカ(サイ
トンHT−50F、デュポン(株)製)に水、ゲル化防
止剤、硝酸アルミニウム及び過酸化水素を表2に示す割
合で添加し、水性研磨用組成物を調製し、実施例と同様
に研磨した。その結果を表2に示す。(Comparative Examples 1-2) Water, an anti-gelling agent, aluminum nitrate and hydrogen peroxide were added to colloidal silica (Cyton HT-50F, manufactured by DuPont) at the ratios shown in Table 2, and aqueous polishing was performed. A composition for use was prepared and polished in the same manner as in the examples. Table 2 shows the results.
【0021】(比較例3)酸化チタニウム(スーパータ
イタニアF−2、昭和タイタニウム(株)製)を媒体攪
拌ミルにより粉砕、整粒により粗粒子を除去し、平均粒
子径0.3μmの酸化チタニウムをまず得た。次に、
水、硝酸アルミニウムを表2に示す割合で添加し、水性
研磨用組成物を調製し、実施例と同様に研磨した。その
結果を表2に示す。なお、粒度測定値は表1に示す。Comparative Example 3 Titanium oxide (Super Titania F-2, manufactured by Showa Titanium Co., Ltd.) was pulverized by a medium stirring mill, coarse particles were removed by sizing, and titanium oxide having an average particle diameter of 0.3 μm was obtained. I got it first. next,
Water and aluminum nitrate were added at the ratios shown in Table 2 to prepare an aqueous polishing composition, which was polished in the same manner as in the examples. Table 2 shows the results. Table 1 shows the measured particle size.
【0022】[0022]
【表1】 [Table 1]
【0023】[0023]
【表2】 [Table 2]
【0024】[0024]
【発明の効果】本発明の研磨用組成物を用いてディスク
の研磨を行うと、表面粗さが非常に小さく、しかも高い
速度で研磨することが出来る。研磨したディスクを用い
た磁気ディスクは低浮上型ハードディスクとして有用で
あり、高密度記録が可能である。特に、研磨したディス
クを用いた磁気ディスクは、MRヘッド用メディアに代
表される高記録密度媒体(1Gbit/inch2 以上
の記録密度を有する)として有用度が高い。それ以下の
記録密度を有する磁気ディスクに対しても高信頼性媒体
と言う観点で有用である。When the disk is polished using the polishing composition of the present invention, the surface roughness is very small and the polishing can be performed at a high speed. A magnetic disk using a polished disk is useful as a low-flying hard disk, and enables high-density recording. In particular, a magnetic disk using a polished disk is highly useful as a high recording density medium (having a recording density of 1 Gbit / inch 2 or more) typified by an MR head medium. It is also useful for a magnetic disk having a recording density lower than that in terms of a highly reliable medium.
フロントページの続き (72)発明者 多田 清志 大阪府堺市海山町6丁224番地 昭和アル ミニウム株式会社内 (72)発明者 冨田 賢二 大阪府堺市海山町6丁224番地 昭和アル ミニウム株式会社内 Fターム(参考) 3C058 CB01 CB02 CB03 CB10 DA02 5D112 AA02 BA06 GA09 GA14 GA30Continued on the front page (72) Inventor Kiyoshi Tada 6,224, Kaiyamacho, Sakai-shi, Osaka, Japan Showa Aluminum Co., Ltd. F term (reference) 3C058 CB01 CB02 CB03 CB10 DA02 5D112 AA02 BA06 GA09 GA14 GA30
Claims (6)
ルミニウム及び過酸化水素からなる磁気ディスク基板研
磨用組成物。1. A composition for polishing a magnetic disk substrate comprising water, silicon oxide, an anti-gelling agent, aluminum nitrate and hydrogen peroxide.
ムドシリカ及びホワイトカーボンから選ばれる1種又は
2種以上である請求項1に記載の磁気ディスク基板研磨
用組成物。2. The magnetic disk substrate polishing composition according to claim 1, wherein the silicon oxide is at least one selected from colloidal silica, fumed silica, and white carbon.
0.03〜0.5μmである請求項1または2に記載の
磁気ディスク基板研磨用組成物。3. The magnetic disk substrate polishing composition according to claim 1, wherein the average particle diameter of the secondary particles of silicon oxide is 0.03 to 0.5 μm.
量%である請求項1〜3のいずれか1項に記載の磁気デ
ィスク基板研磨用組成物。4. The magnetic disk substrate polishing composition according to claim 1, wherein the concentration of the silicon oxide in the composition is 3 to 30% by mass.
ェナントロリン及びアセチルアセトンアルミニウム塩か
ら選ばれる1種又は2種以上である請求項1〜4のいず
れか1項に記載の磁気ディスク基板研磨用組成物。5. The composition for polishing a magnetic disk substrate according to claim 1, wherein the anti-gelling agent is one or more selected from a phosphonic acid compound, phenanthroline and aluminum acetylacetonate. object.
タン−1,1−ジホスホン酸である請求項5に記載の磁
気ディスク基板研磨用組成物。6. The composition for polishing a magnetic disk substrate according to claim 5, wherein the phosphonic acid compound is 1-hydroxyethane-1,1-diphosphonic acid.
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2000013858A JP3877924B2 (en) | 2000-01-24 | 2000-01-24 | Magnetic disk substrate polishing composition |
MYPI20010276 MY118633A (en) | 2000-01-24 | 2001-01-22 | Abrasive composition for polishing magnetic recording disk substrates |
US09/767,024 US6478835B2 (en) | 2000-01-24 | 2001-01-23 | Abrasive composition for polishing magnetic recording disk substrates |
CN 01104631 CN1243070C (en) | 2000-01-24 | 2001-01-23 | Abrasive composition for polishing magnetic recording disk matrix |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2000013858A JP3877924B2 (en) | 2000-01-24 | 2000-01-24 | Magnetic disk substrate polishing composition |
Publications (3)
Publication Number | Publication Date |
---|---|
JP2001207161A true JP2001207161A (en) | 2001-07-31 |
JP2001207161A5 JP2001207161A5 (en) | 2005-08-04 |
JP3877924B2 JP3877924B2 (en) | 2007-02-07 |
Family
ID=18541393
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2000013858A Expired - Lifetime JP3877924B2 (en) | 2000-01-24 | 2000-01-24 | Magnetic disk substrate polishing composition |
Country Status (3)
Country | Link |
---|---|
JP (1) | JP3877924B2 (en) |
CN (1) | CN1243070C (en) |
MY (1) | MY118633A (en) |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2002327170A (en) * | 2001-04-27 | 2002-11-15 | Kao Corp | Polishing liquid composition |
JP2003155471A (en) * | 2001-08-21 | 2003-05-30 | Kao Corp | Polishing liquid composition |
JP2004067897A (en) * | 2002-08-07 | 2004-03-04 | Kao Corp | Roll-off reducing agent |
JP2009057570A (en) * | 2008-10-23 | 2009-03-19 | Kao Corp | Rinse composition |
JP2009120850A (en) * | 2001-08-21 | 2009-06-04 | Kao Corp | Polishing liquid composition |
WO2015146942A1 (en) * | 2014-03-28 | 2015-10-01 | 山口精研工業株式会社 | Polishing agent composition and method for polishing magnetic disk substrate |
WO2015146941A1 (en) * | 2014-03-28 | 2015-10-01 | 山口精研工業株式会社 | Polishing agent composition and method for polishing magnetic disk substrate |
JP2016069553A (en) * | 2014-09-30 | 2016-05-09 | 株式会社フジミインコーポレーテッド | Polishing composition |
WO2017051770A1 (en) * | 2015-09-25 | 2017-03-30 | 山口精研工業株式会社 | Abrasive material composition and method for polishing magnetic disk substrate |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4202172B2 (en) * | 2003-03-31 | 2008-12-24 | 株式会社フジミインコーポレーテッド | Polishing composition |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH09204657A (en) * | 1996-01-30 | 1997-08-05 | Showa Denko Kk | Polishing composition and method for polishing magnetic disc substrate |
JPH09208934A (en) * | 1996-01-30 | 1997-08-12 | Showa Denko Kk | Composition for polishing and polishing of magnetic disk substrate |
JPH10121035A (en) * | 1996-08-30 | 1998-05-12 | Showa Denko Kk | Composition for polishing magnetic disk substrate |
JPH10121034A (en) * | 1996-03-18 | 1998-05-12 | Showa Denko Kk | Composition for polishing magnetic disk substrate |
JPH10321569A (en) * | 1997-05-21 | 1998-12-04 | Fujimi Inkooporeetetsudo:Kk | Polishing composition |
JPH11246849A (en) * | 1997-11-06 | 1999-09-14 | Komag Inc | Colloidal silica slurry for polishing disk plated with nickelphosphide |
-
2000
- 2000-01-24 JP JP2000013858A patent/JP3877924B2/en not_active Expired - Lifetime
-
2001
- 2001-01-22 MY MYPI20010276 patent/MY118633A/en unknown
- 2001-01-23 CN CN 01104631 patent/CN1243070C/en not_active Expired - Fee Related
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH09204657A (en) * | 1996-01-30 | 1997-08-05 | Showa Denko Kk | Polishing composition and method for polishing magnetic disc substrate |
JPH09208934A (en) * | 1996-01-30 | 1997-08-12 | Showa Denko Kk | Composition for polishing and polishing of magnetic disk substrate |
JPH10121034A (en) * | 1996-03-18 | 1998-05-12 | Showa Denko Kk | Composition for polishing magnetic disk substrate |
JPH10121035A (en) * | 1996-08-30 | 1998-05-12 | Showa Denko Kk | Composition for polishing magnetic disk substrate |
JPH10321569A (en) * | 1997-05-21 | 1998-12-04 | Fujimi Inkooporeetetsudo:Kk | Polishing composition |
JPH11246849A (en) * | 1997-11-06 | 1999-09-14 | Komag Inc | Colloidal silica slurry for polishing disk plated with nickelphosphide |
Cited By (15)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2002327170A (en) * | 2001-04-27 | 2002-11-15 | Kao Corp | Polishing liquid composition |
JP2003155471A (en) * | 2001-08-21 | 2003-05-30 | Kao Corp | Polishing liquid composition |
JP2009120850A (en) * | 2001-08-21 | 2009-06-04 | Kao Corp | Polishing liquid composition |
JP2004067897A (en) * | 2002-08-07 | 2004-03-04 | Kao Corp | Roll-off reducing agent |
JP2009057570A (en) * | 2008-10-23 | 2009-03-19 | Kao Corp | Rinse composition |
WO2015146941A1 (en) * | 2014-03-28 | 2015-10-01 | 山口精研工業株式会社 | Polishing agent composition and method for polishing magnetic disk substrate |
WO2015146942A1 (en) * | 2014-03-28 | 2015-10-01 | 山口精研工業株式会社 | Polishing agent composition and method for polishing magnetic disk substrate |
JPWO2015146941A1 (en) * | 2014-03-28 | 2017-04-13 | 山口精研工業株式会社 | Abrasive composition and method for polishing magnetic disk substrate |
JPWO2015146942A1 (en) * | 2014-03-28 | 2017-04-13 | 山口精研工業株式会社 | Abrasive composition and method for polishing magnetic disk substrate |
US9856401B2 (en) | 2014-03-28 | 2018-01-02 | Yamaguchi Seiken Kogyo Co., Ltd. | Polishing composition and method for polishing magnetic disk substrate |
US9862863B2 (en) | 2014-03-28 | 2018-01-09 | Yamaguchi Seiken Kogyo Co., Ltd. | Polishing composition and method for polishing magnetic disk substrate |
JP2016069553A (en) * | 2014-09-30 | 2016-05-09 | 株式会社フジミインコーポレーテッド | Polishing composition |
WO2017051770A1 (en) * | 2015-09-25 | 2017-03-30 | 山口精研工業株式会社 | Abrasive material composition and method for polishing magnetic disk substrate |
JPWO2017051770A1 (en) * | 2015-09-25 | 2018-08-09 | 山口精研工業株式会社 | Abrasive composition and method for polishing magnetic disk substrate |
US10822525B2 (en) | 2015-09-25 | 2020-11-03 | Yamaguchi Seiken Kogyo Co., Ltd. | Polishing composition and method for polishing magnetic disk substrate |
Also Published As
Publication number | Publication date |
---|---|
CN1309160A (en) | 2001-08-22 |
JP3877924B2 (en) | 2007-02-07 |
MY118633A (en) | 2004-12-31 |
CN1243070C (en) | 2006-02-22 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US6117220A (en) | Polishing composition and rinsing composition | |
US8241516B2 (en) | Substrate for magnetic disk | |
US6569215B2 (en) | Composition for polishing magnetic disk substrate | |
JP4273475B2 (en) | Polishing composition | |
US6190443B1 (en) | Polishing composition | |
JP4439755B2 (en) | Polishing composition and method for producing memory hard disk using the same | |
JP3998813B2 (en) | Polishing composition | |
JPH10204416A (en) | Polishing composition | |
US20040127147A1 (en) | Polishing composition | |
JP3106339B2 (en) | Polishing composition | |
JP3877924B2 (en) | Magnetic disk substrate polishing composition | |
US20050028449A1 (en) | Polishing composition | |
US6478835B2 (en) | Abrasive composition for polishing magnetic recording disk substrates | |
JPH10152674A (en) | Composition for rinse | |
JPH09204657A (en) | Polishing composition and method for polishing magnetic disc substrate | |
TW528645B (en) | Composition for polishing magnetic disk substrate | |
JP2004253058A (en) | Polishing liquid composition | |
JPH1121545A (en) | Polishing composition | |
JP4074126B2 (en) | Polishing composition | |
JP3997153B2 (en) | Polishing liquid composition | |
JP2005008875A (en) | Abrasive composition and abrasion method | |
JP2000063805A (en) | Composition for abrasive finishing of magnetic disc substrate | |
JPH09316430A (en) | Composition for polishing magnetic disk substrate | |
US20010029705A1 (en) | Composition and method for polishing magnetic disk substrate, and magnetic disk polished therewith | |
JP3680022B2 (en) | Magnetic disk substrate polishing liquid |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20041224 |
|
A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20041224 |
|
RD13 | Notification of appointment of power of sub attorney |
Free format text: JAPANESE INTERMEDIATE CODE: A7433 Effective date: 20050530 |
|
A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20060719 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20060801 |
|
A521 | Written amendment |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20060928 |
|
TRDD | Decision of grant or rejection written | ||
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20061031 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20061101 |
|
R150 | Certificate of patent or registration of utility model |
Free format text: JAPANESE INTERMEDIATE CODE: R150 Ref document number: 3877924 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20091110 Year of fee payment: 3 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20121110 Year of fee payment: 6 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20121110 Year of fee payment: 6 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20151110 Year of fee payment: 9 |
|
EXPY | Cancellation because of completion of term |