TW581803B - Composition for polishing substrate for magnetic disk and method for producing substrate for magnetic disk - Google Patents

Abstract

A composition for polishing a substrate for a magnetic disk, which comprises water, fine titanium oxide particles and a polishing promoter, characterized in that 90 to 100% of the titanium oxide constituting said particles has the same crystal structure; and a method for producing a substrate for a magnetic disk using the composition. The composition can be used for polishing a substrate for a magnetic disk, at an economical polishing rate, so as to have a reduced surface roughness and to become free from the occurrence of fine defects such as projections, scraches by abrasion and micropits.

Description

581803 A7 B7 五、發明說明（1 ) 本發明係有關硏磨磁碟基板用組成物者，更詳細者係 有關磁頭低浮上量進行飛行而可取得適當精密度之高磁碟 表面之硏磨磁碟基板用組成物者。. 先行技術中，於電腦、文書處理機外部記憶裝置中可 於高速下讀取之方法之磁碟（記憶硬碟片）被廣泛使用之 。代表此磁磁之一例者係於A 1合金基板之表面上以 N i P經無電解電鍍者做爲基板、此基板進行表面硏磨後-，使C r合金基底膜、C 〇合金磁性膜、碳保護膜依序以 濺耙形成者。 磁碟表面殘留具有磁頭浮上量以上高度之突起則所定 高度浮上之同時，高速下飛行之磁頭將於其突起衝突導致 損傷之原因。又，於磁碟用基板出現突起、硏磨損傷則形 成Cr合金基底膜、Co合金磁性膜等時，於其膜之表面 出現突起，且，基於硏磨損傷產生缺陷，磁碟表面無法呈 精度高之平面，因此，務必於提昇碟片表面之精度時，使 基板進行精密之硏磨。 因此，硏磨磁碟用基板中，被提出多樣無突起物，且 儘可能其高度爲低者，同時不易產生硏磨損傷之硏磨用組 成物者。例如：以粒徑約爲1 μ m之鋁氧粉或鋁化合物做 爲砥粒使用者雖可回避先行技術之磁頭浮上量中磁碟突起 之衝突之精度下進行硏磨，惟，最近更顯著要求記錄密度 之提昇下而無法達成高標準之表面精度。另外，雖以數十 n m之二氧化矽膠質粒子做爲砥粒使用時易於達成高面精 度，惟，硏磨速度遲緩，而無法充份取得所需之量產性， 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） (請先閱讀背面之注意事項再填寫本頁) --------訂---------^__w. · -4 - 581803 A7 B7 五、發明說明（2) 同時，長時間之硏磨後於外圍被過份硏磨之（即角部面垂 )問題產生。 針對此，載於特開平1 0 - 1 2 1 0 3 5號公報之硏 磨用組成物以亞微細粒氧化鈦（二氧化鈦）微粒子做爲砥 粒使用，因此易達成高面精度、硏磨速度。此專利之組成 物中，金紅石型之氧化鈦其結晶小、密緻、且硬度高者， 故，硏磨能率佳，惟，易產生硏磨損傷，因此，總氧化鈦一 所佔金紅石型氧化鈦（金紅石化率）以1 0〜8 0 %者宜 0 該專利中其金紅石化率以1 〇〜8 0 %之氧化鈦者雖 理想，惟共存不同結晶結構之氧化鈦則其欲做成微粒子時 之解碎、粉碎將不易均勻、粒度之精度完整分佈亦不易。 其結果雖然微細凹痕、微細刮傷等微細缺陷頻度雖低卻有 產生之疑慮，故有基板生產收率不良之問題出現。 可做爲高密度磁記錄之鋁硏磨磁碟基板用之組成物所 要求之品質以可達成磁頭低浮上之高精度磁碟面者。 本發明之目的係爲提供一種磁碟表面粗細度小，且不 出現突起、硏磨損傷、微凹痕、微細刮傷等微細缺陷者， 可達成高密度記錄，同時可經濟快速硏磨之硏磨磁碟基板 用之組成物者。 本發明者精密硏討之結果發現氧化鈦硏磨材料大半不 共存相異之結晶結構，儘可能做成單一結構後，進行破碎 、粉碎時，呈完整均勻分佈粒度，藉此可取得磁頭可低浮 上之磁碟基材用之高精度面，且，未出現一般硏磨損傷， 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） -----------裝--------訂---------Aw. (請先閱讀背面之注意事項再填寫本頁) -5- 581803 經濟郎智慧財4¾員X.消費合阼fi卬Μ A7 B7 五、發明說明（3 ) 特別可防止硏磨損傷之微細缺陷之產生。本發明基於此發 現進而達成者。氧化鈦其任一此等結晶結構（單一結晶結 構）者只要爲9 0 %以上者任一結晶結構均可。 亦即，本發明係由氧化鈦微粒子、硏磨促進劑所組成 、該氧化鈦其單一結晶結構之氧化鈦爲9 0〜1 0 0 %者 爲特徵之硏磨磁碟基材用組成物者。 本發明硏磨用組成物可有效適用於利用磁性掊抗（ M R )效果之磁頭用磁碟所代表之高記錄密度用基板（一 般具有1Gb i t/i nch2以上之記錄密度），惟，針 對具有其以下之記錄密度之磁碟由其信賴性之提昇上亦可 有效應用。 先行技術之磁碟用基板中，成爲其問題點之硏磨損傷 深度爲1 0 nm以上者，而，本發明目的之低浮上型硬碟 基板中雖無先行技術之問題，深度若爲5 n m之微小硏磨 損傷仍呈磁性特性上之失誤，被判定爲實用上可容許範圍 以外者。 於本發明之硏磨用組成物做爲硏磨材料所含有之氧化 鈦微粒子係其結晶結構爲單一之9 0〜1 0 0 %者。亦即 ，銳鈦礦型、金紅石型或板鈦礦（B r 〇 q k 11 e )之任一氧化 鈦均爲9 0〜1 〇 〇%者。殘存之1 0%以下亦可共存另 外之結晶結構者。例如：銳鈦礦型之氧化鈦爲9 0 %以上 者，殘存爲金紅石型及/或板鈦礦之氧化鈦爲1 〇 %以下 者。單一結晶結構之氧化鈦爲9 0 %以下，亦即，若另外 之結晶結構爲大於1 0 %共存者則粒度分佈將呈不勻者。 本紙張尺度適用中國國家標準（CNS)A4規格（210 χ 297公釐） A__w— --------^------I--AWI (請先閱讀背面之注意事項再填寫本頁) -6- 581803 A7 B7 五、發明說明（4) 氧化鈦之結晶結構爲X線反射法（C u Κ α線使用） 如以下可進行固定。金紅石型氧化鈦之比率係由金紅石（ (請先閱讀背面之注意事項再填寫本頁) 1 1 〇 )面與銳鈦礦（1 0 1 )面之X線反射之頂點強度 比計算求取之。銳鈦礦（1 〇 1 )面與板鈦礦（1 2 0 ) 面重疊，而板鈦礦（1 2 1 )面（相對強度9 0%)與銳 鈦礦之所有面均未重疊，因此由此頂點強度求取板鈦礦（ 120)面之強度（100/90倍），由此與銳鈦礦（-1 〇 1 )面之頂點強度可求取兩者所含有比率者。 氧化鈦之製法於本發明中並無特別限定，通常藉由鈦 鐵礦或鈦渣與硫酸反應、溶解、水解、燒成之各工程所成 之硫酸法、或使金紅石礦進行紅熱脫水後於8 0 0 °C下進 行加熱之氯化爐中，通常氯氣以鈦做爲氯化物後進行氣化 ，將此精餾取得之四氯化鈦藉由直接熱分解後所製造之氯 氣法等者。 針對氧化鈦之結晶結構如：以四氯化鈦與氧等之混合 燃燒方法所製造之氣相法時，於最低溫下產生後呈安定者 爲銳鈦礦型者。於此進行熱處理後，燃燒後於8 1 6〜 經濟部智慧財產局員工消費合作社印制衣 1〇4 0 °C下取得板鈦礦型、其更高溫度域則取得金紅石 型結構之氧化鈦（理化學辭典第3版、p . 5 1 4〜 5 15)° 又，單一結晶結構爲9 0 %以上之氧化鈦爲市販者， 因此必要時將此粉碎、去除粗粒子後調整粒度後亦可用於 本發明者。 本發明所使用之氧化鈦之粒度分佈之二次粒子粒度分 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） 581803 _______B7 ______ 五、發明說明（5 ) 佈中，其累積90重量％之粒徑D90 (D90以下之粒 徑爲9 0重量％)與累積1 0重量％之粒徑D 1 0 ( (請先閱讀背面之注意事項再填寫本頁) D 1 0以下之粒徑爲1 0重量％)之比D9 0/D 1 〇爲 3以下者宜，更佳者爲2 . 7以下者。此比愈小代表分佈 粒度均勻度愈佳者。 本發明中氧化鈦之粒徑其做爲二次粒子之平均粒徑以 0 . 1〜1 · 0/zm者宜。二次粒子之平均粒徑係藉由激— 光多普勒周波數解析式粒度分佈測定器、微導向裝置 U P A 1 5 0 ( Honeywell公司製）後之所測定値者。 氧化鈦微粒子之硏磨速度依二次粒徑而定，當二次粒 徑變大時，則硏磨速度變高，易產生硏磨損傷，因而造成 磁氣特性之缺失之產生，做爲低浮上型硬碟基板者控制實 用上可容許程度之硏磨損傷極爲困難。因此，氧化鈦二次 粒子之平均粒徑以1 · 0 以下者宜。另外，由提高硏 磨速度，降低角部面垂其二次粒子之平均粒徑以〇 · 1 // m以上者宜。 經濟部智慧財產局員工消費合作社印製 更且，一次粒徑之大小即使變大易產生硏磨損傷，又 ，二次粒子之平均粒徑爲上述範圍之大小者，爲使一次粒 子變小硏磨速度變大，且可防止硏磨損傷之產生，由 S E Μ相片求出一次粒徑（長短徑之平均）之平均値以 〇· 01〜0 . 6//m之範圍者爲更佳。 針對本發明硏磨用組成物之氧化鈦之濃度，爲低濃度 時其硏磨速度降低。濃度變高硏磨速度亦變高，惟若超出 1 5重量％則硏磨速度上昇率呈鈍化。因經濟面進行加味 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） -8- 581803 A7 ______ B7 五、發明說明（6 ) 時其實用者以2 0重量％爲其上限。因此，硏磨用組成物 中之氧化鈦濃度爲2〜2 0重量％之範圍者宜。 本發明之硏磨用組成物中，氧化鈦具有機械性硏磨作 用，惟’爲更提高其硏磨能率，爲針對基板進行化學作用 而添加硏磨促進劑。做爲硏磨促進劑者如：硝酸鋁（ A 1 (1^〇3)3)、硫酸鋁（厶12(3〇4)3)、草酸 鋁（Al2(C2〇4)3)、硝酸鐵（Fe(N〇3)3)-、乳酸-錦（八1((：3：«5〇3)3)、葡糖酸（ 經濟部智慧財產笱員工消費合阼fi印製 :---.--------0 ^--------訂 i (請先閱讀背面之注意事項再填寫本頁) C 6 Η 1 2 0 7 ).蘋果酸（C4H6〇5)等可使用之。其中 又以鋁鹽及硝酸鹽者佳、更理想者爲硝酸鋁者。此等硏磨 促進劑可一種單獨使用或2種以上倂用者均可。硏磨促進 劑針對基板進行腐蝕作用等之化學作用後，於此藉由氧化 鈦加入機械性硏磨作用後，可大幅提昇硏磨能率。更且硏 磨促進劑之外，添加水溶性氧化劑亦可有效提高硏磨性能 。做爲水溶性氧化劑者可使用過氧化氫（Η 2〇2 )、硝酸 、過錳酸鉀（ΚΜη〇4)、過氯酸（HC 1〇4)、過氯 酸鈉（N a C 1〇4 )、次亞氯酸鈉（N a C 1〇）之1種 或2種以上者。其濃度若太高並無增加效果之優點，故以 1〇重量％以下爲適當者。 硏磨促進劑之添加量以1〜2 0重量％者宜，較佳者 爲1〜1 5重量％者。當硏磨促進劑之添加量小於〇 . 1 重量％則硏磨速度降低’所定量硏磨所需硏磨時間變長， 更增大角部面垂。添加量增加至1 5重量％時可提昇硏磨 速度，而大於1 5重量％則硏磨速度不再隨之增高。因此 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） -9 - 581803 A7 ____B7______ 五、發明說明（7 ) ，添加量大於1 5重量％雖不影響硏磨面，惟經濟上之考 量下，以2 0重量％爲其上限値。 又，該各成份濃度係硏磨磁碟用基板時之濃度者。製 造硏磨用組成物後，搬運等時由上記濃度作成濃厚之組成 物，使用時該濃度稀釋後使用者爲效率性者。 本發明之硏磨磁碟基板用組成物係由該銳鈦礦型氧化 鈦之9 0〜1 0〇％或金紅石型氧化鈦之9〇〜1 0 0% 或板鈦礦氧化鈦之9 0〜1 0 0 %之氧化鈦、硏磨促進劑 及水所成之生科狀者，必要時可添加水溶性氧化劑，此外’ ，亦可添加界面活性劑、防腐劑、及P Η調整劑之酸或鹼 等者。做爲硏磨促進劑者若使用硝酸鋁等之鋁酸性鹽時其 理想ρ Η爲2〜5者。當ρ Η小於2時，則硏磨機等之腐 蝕、作業上之問題將出現，大於5則硏磨效率產生障礙均 不理想。 本發明之硏磨用組成物與先行之硏磨用組成物相同， 於水上懸浮該結晶結構之氧化鈦可於此添加硏磨促進劑等 之後，進行調製之。 1 聲 ψ 4° ί :才 i L· (請先閱讀背面之注意事項再填寫本頁) 適於本發明硏磨用組成物之磁碟基板並未特別限定， 一般，鋁基板，特別是N i Ρ之無電解電鍍之鋁基板適用 於本發明之組成物後，藉由氧化鈦之機械性硏磨作用與藉 由硏磨促進劑進行化學性硏磨作用相乘效果之高品質之硏 磨面對於工業上有利者。 硏磨方法通常將生料狀硏磨材所使用之硏磨底座於磁 碟用基板上相疊後，將生料供於底座與基板中，同時使底 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） -10- 經濟卽智慧財產笱員工消費合阼Fi印裂 581803 A7 B7 五、發明說明（8 ) 座或基板進行旋轉之方法者。 藉由本發明硏磨用組成物由硏磨之基板製成之磁碟其 微凹痕、微細刮傷等微細之缺陷發生頻率極低，又，表面 粗細度（R a )爲3〜5 A左右者，平滑性良好者。 〔發明實施之最佳形態〕 以下，以實施例具體說明本發明，惟，本發明並非僅 限於此實施例者。 (實施例1〜1 6 ) 將昭和Taitanium (股份）製之高純度氧化鈦之super taUania F-10 (金紅石型氧化鈦9 8重量％，銳鈦礦型氧化 欽2重量％)及super taitania F-4 (銳鈦礦型氧化欽9 5 重量％、金紅石型氧化鈦5重量％)以媒體攪拌硏磨器進 行粉碎，去除微量粗大粒子後，先取得平均粒徑0 . 3 // m之氧化鈦。氧化鈦之結晶結構及其含有率係利用理學 電機（股份）製R A D - 2 B進行測定之。此等如表1顯 示分別之二氧化鈦①、二氧化鈦②者。 又，粒徑係藉由激光多普勒周波數解析式粒度分佈測 定器、微導向裝置UPA 1 5 0 ( Honeywell公司製）所測 定之。粒度測定値示於表1。 以下，做爲硏磨材料之該氧化鈦及硏磨促進劑，依不 同情況更可依表2所示之比例添加氧化劑，調整各種水性 硏磨用組成物後，依以下所示之硏磨裝置及硏磨條件下進 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） •I n ϋ ϋ I ϋ ϋ I ϋ · «ϋ ϋ H ·ϋ ϋ n ϋ·-、· ·ϋ ·ϋ ϋ ϋ ·ϋ ϋ I I (請先閱讀背面之注意事項再填寫本頁) -11 - 581803 A7 B7 五、發明說明（9 ) 行硏磨。做爲硏磨促進劑者使用硝酸銀時，其p Η値爲 2 . 3 〜4 · 1 者。 硏磨： 所使用之基板係使用N i Ρ無電解電鍍之3 . 5 i n c h之鋁碟片之硏磨裝置及硏磨條件 硏磨試驗器......4 wei式雙面拋光機 硏磨凹痕.......絨面型（polytex DG、Rodell製） 下定盤旋轉速度···· 60rpm 生料供給速度.....5 0 m 1 / m i η 硏磨時間.......5分鐘 加工壓力.......50g/cm2 硏磨特性之評定 硏磨率...... 由鋁碟片之硏磨前後之重量差換算 之 表面粗細度· · · · 使用 Turristep、Turrideta 2000 (Lanktaylerhobson 公司製） 硏磨損傷及硏磨凹痕之深度係藉由觸針式表面解析裝 置P — 1 2 ( Tencor公司製）之3次元模型後進行形狀解 析後求取深度。581803 A7 B7 V. Description of the invention (1) The present invention relates to a honing magnetic disk substrate composition, and in more detail, it relates to a honing magnetic surface of a high magnetic disk surface that can obtain appropriate precision by flying a magnetic head with a low flying volume. Composition for dish substrate. In the prior art, magnetic disks (memory hard disks) that can be read at high speed in external memory devices of computers and word processors are widely used. An example of this magnetism is that the surface of the A 1 alloy substrate is electrolessly plated with Ni P as the substrate, and the substrate is surface-honed to make the C r alloy base film and the C o alloy magnetic film. 2. The carbon protective film is sequentially formed by splashing rakes. The protrusions on the surface of the magnetic disk that have a height above the head's floating height remain at the same height, and the head flying at high speed will collide with the protrusions and cause damage. In addition, when protrusions and honing damage occur on the substrate for magnetic disks, a Cr alloy base film and a Co alloy magnetic film are formed, and protrusions appear on the surface of the film, and the defects on the surface of the magnetic disk cannot be accurate due to honing damage. High plane, so it is necessary to make the substrate precision honing when improving the accuracy of the surface of the disc. For this reason, various substrates for honing magnetic disks have been proposed, which have no protrusions and whose height is as low as possible, and at the same time, the components for honing are unlikely to cause honing damage. For example: using aluminum oxide powder or aluminum compound with a particle size of about 1 μm as the particles, although users can avoid honing with the accuracy of the disk head protrusion in the prior art, the honing is performed, but it has become more significant recently. It is required to improve the recording density without achieving a high standard of surface accuracy. In addition, although it is easy to achieve high surface accuracy when using tens of nanometer silicon dioxide particles as grains, the honing speed is slow, and the required mass productivity cannot be fully achieved. This paper is applicable to China Standard (CNS) A4 specification (210 X 297 mm) (Please read the precautions on the back before filling this page) -------- Order --------- ^ __ w. · -4 -581803 A7 B7 V. Description of the invention (2) At the same time, after long time honing, the problem of excessive honing (that is, the corner surface is hanging down) on the periphery occurs. In view of this, the honing composition described in JP-A No. 10-1 2 1 0 3 5 uses submicron titanium oxide (titanium dioxide) fine particles as honing particles, so it is easy to achieve high surface accuracy and honing speed. . In the composition of this patent, rutile-type titanium oxide has small crystals, dense and high hardness. Therefore, the honing energy rate is good, but honing damage is easy to occur. Therefore, the total titanium oxide accounts for rutile. Titanium oxide (rutile conversion rate) is preferably 10 ~ 80%. Titanium oxide with rutile conversion rate of 10 ~ 80% in this patent is ideal, but titanium oxide with different crystal structure coexists. It is not easy to disintegrate and pulverize when it is to be made into fine particles, and it is not easy to complete the distribution of particle size accuracy. As a result, although the frequency of fine defects such as fine dents and fine scratches is low, there is a concern that a problem may arise in that the substrate production yield is poor. It can be used as a composition for aluminum honing disk substrates for high-density magnetic recording. The required quality is to achieve a high-precision disk surface with low head floating. The object of the present invention is to provide a magnetic disk with a small thickness without the occurrence of fine defects such as protrusions, honing damage, micro-dents, micro-scratches, etc., which can achieve high-density recording and economical and rapid honing. Compositions for polishing disc substrates. As a result of intensive investigations by the present inventors, it was found that most of the titanium oxide honing materials do not coexist with different crystalline structures. After being made into a single structure as much as possible, the particles are completely and uniformly distributed when crushing and pulverizing, thereby achieving a low magnetic head The high-precision surface of the floating disk substrate, and there is no general honing damage. The paper size applies to China National Standard (CNS) A4 (210 X 297 mm) ---------- -Install -------- Order --------- Aw. (Please read the precautions on the back before filling in this page) -5- 581803 Economy Lang Smart Money 4¾ member X. Consumption fi 卬 Μ A7 B7 V. Description of the invention (3) Particularly, it can prevent the generation of fine defects of honing damage. The present invention has been made based on this finding. Any one of these crystalline structures (single crystalline structure) of titanium oxide may be any crystalline structure of 90% or more. That is, the present invention is a composition for honing a magnetic disk substrate, which is composed of titanium oxide fine particles and a honing accelerator, and the titanium oxide has a single crystal structure of 90% to 100% titanium oxide. . The honing composition of the present invention can be effectively applied to a substrate for high recording density represented by a magnetic head magnetic disk using a magnetic resistance (MR) effect (generally having a recording density of 1 Gb it / inch 2 or more). The following recording density disks can also be effectively applied from the improvement of their reliability. In the prior art magnetic disk substrate, the depth of the honing damage that is the problem point is 10 nm or more. However, although the low floating type hard disk substrate of the present invention has no prior art problem, the depth is 5 nm. The slight honing damage was still a mistake in magnetic properties and was judged to be outside the practically acceptable range. The titanium oxide fine particles contained in the honing composition of the present invention as a honing material have a single crystal structure of 90% to 100%. That is, any titanium oxide of anatase type, rutile type or brookite type (B r 〇 q k 11 e) is 90% to 100%. The remaining 10% or less can also coexist with other crystal structures. For example: anatase titanium oxide is 90% or more, and rutile type and / or brookite titanium oxide is 10% or less. The single crystal structure of titanium oxide is 90% or less, that is, if the other crystal structure is more than 10% coexistence, the particle size distribution will be uneven. This paper size applies to Chinese National Standard (CNS) A4 specification (210 χ 297 mm) A__w— -------- ^ ------ I--AWI (Please read the notes on the back before filling (This page) -6- 581803 A7 B7 V. Description of the invention (4) The crystal structure of titanium oxide is X-ray reflection method (used by Cu κ α line). It can be fixed as follows. The ratio of rutile titanium oxide is calculated by calculating the vertex intensity ratio of the X-ray reflection of the rutile ((Please read the precautions on the back before filling in this page) 1 1) surface and the anatase (1 0 1) surface. Take it. The anatase (101) plane overlaps with the brookite (120) plane, while the brookite (121) plane (relative strength 90%) does not overlap with all of the anatase planes, so Based on the vertex strength, the intensity (100/90 times) of the brookite (120) plane can be obtained, and the ratio between the two can be obtained from the vertex intensity of the anatase (-1 〇1) plane. The method for producing titanium oxide is not particularly limited in the present invention. Usually, the method is a sulfuric acid method produced by various processes of reacting, dissolving, hydrolyzing, and firing ilmenite or titanium slag with sulfuric acid, or red hot dehydration of rutile ore. In a chlorination furnace heated at 800 ° C, the chlorine gas is usually gasified by using titanium as a chloride, and the titanium tetrachloride obtained by this rectification is produced by direct thermal decomposition of the chlorine gas method, etc. By. For the crystalline structure of titanium oxide, such as the gas phase method produced by the mixed combustion method of titanium tetrachloride and oxygen, the one that shows stability after being produced at the lowest temperature is the anatase type. After heat treatment, the brookite type was obtained at 1016 ° C after printing, and the rutile type structure was obtained at a temperature of 1,080 ° C in the consumer cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs. Titanium (3rd edition of the Dictionary of Physics and Chemistry, p. 5 1 4 to 5 15) ° In addition, titanium oxide with a single crystal structure of 90% or more is a marketer. Therefore, if necessary, pulverize and remove coarse particles to adjust the particle size. It can also be used by the inventors. The secondary particle size of the particle size distribution of titanium oxide used in the present invention is in accordance with the Chinese national standard (CNS) A4 specification (210 X 297 mm) 581803 _______B7 ______ 5. Description of the invention (5) 90% by weight particle diameter D90 (particle size below D90 is 90% by weight) and 10% by weight cumulative particle diameter D 1 0 ((Please read the precautions on the back before filling out this page) D 1 0 or less The particle diameter is 10% by weight) and the ratio D9 0 / D 1 0 is preferably 3 or less, and more preferably 2.7 or less. The smaller the ratio, the better the uniformity of the distribution particle size. The particle diameter of the titanium oxide in the present invention is preferably 0.1 to 1 · 0 / zm as the average particle diameter of the secondary particles. The average particle diameter of the secondary particles is measured by a laser-Doppler frequency analysis type particle size distribution measuring device and a micro-guide device U P A 1 50 (manufactured by Honeywell). The honing speed of titanium oxide particles is determined by the secondary particle size. When the secondary particle size becomes larger, the honing speed becomes higher, and it is easy to cause honing damage, which results in the loss of magnetic characteristics and is low. It is extremely difficult for a floating hard disk substrate to control abrasion damage that is practically tolerable. Therefore, it is preferable that the average particle diameter of the titanium oxide secondary particles is 1 · 0 or less. In addition, by increasing the honing speed, the average particle size of the secondary particles in the corner surface should be reduced by more than 0 · 1 // m. Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs, even if the size of the primary particle size is large, it is easy to cause honing damage, and the average particle size of the secondary particles is within the above range, in order to make the primary particles smaller. The grinding speed is increased and the occurrence of honing damage can be prevented. It is more preferable to obtain the average of the primary particle size (average of the long and short diameters) from the SEM photograph in the range of 0.01 to 0.6 / m. With regard to the concentration of titanium oxide in the honing composition of the present invention, the honing speed decreases when the concentration is low. The higher the concentration, the higher the honing speed, but if it exceeds 15% by weight, the honing speed increase rate becomes passivated. Due to the economic side, the paper size applies the Chinese National Standard (CNS) A4 specification (210 X 297 mm) -8- 581803 A7 ______ B7 5. In the description of the invention (6), its practical limit is 20% by weight. . Therefore, the titanium oxide concentration in the honing composition is preferably in the range of 2 to 20% by weight. In the honing composition of the present invention, titanium oxide has a mechanical honing function, but a honing accelerator is added to increase the honing energy rate and to perform a chemical action on the substrate. As honing accelerators, such as: aluminum nitrate (A 1 (1 ^ 〇3) 3), aluminum sulfate (厶 12 (3〇4) 3), aluminum oxalate (Al2 (C2〇4) 3), iron nitrate (Fe (N〇3) 3)-, lactic acid-brocade (eight 1 ((: 3: «5〇3) 3), gluconic acid (intelligent property of the Ministry of Economic Affairs, employee consumption, and fi printing: --- .-------- 0 ^ -------- Order i (Please read the precautions on the back before filling this page) C 6 Η 1 2 0 7). Malic acid (C4H6〇5) It can be used. Among them, aluminum salt and nitrate are preferred, and aluminum nitrate is more desirable. These honing accelerators can be used alone or in combination of two or more. Honing accelerators are targeted at substrates. After the chemical action such as corrosion effect, the mechanical honing effect can be greatly increased by adding titanium oxide here. Besides the honing accelerator, the addition of a water-soluble oxidant can also effectively improve the honing performance. As a water-soluble oxidant, hydrogen peroxide (H2O2), nitric acid, potassium permanganate (KMη〇4), perchloric acid (HC 104), sodium perchlorate (N a C 1 〇4), one or more of sodium hypochlorite (N a C 1〇), and its concentration Too high does not have the advantage of increasing the effect, so 10% by weight or less is appropriate. The addition amount of honing accelerator is preferably 1 to 20% by weight, and more preferably 1 to 15% by weight. When If the honing accelerator is added in an amount of less than 0.1% by weight, the honing speed will decrease. The honing time required for the specified amount of honing will be longer, and the corner surface will increase. When the amount is increased to 15% by weight, 硏Grinding speed, and honing speed is no longer increased with greater than 15% by weight. Therefore, this paper size applies the Chinese National Standard (CNS) A4 specification (210 X 297 mm) -9-581803 A7 ____B7______ 5. Description of the invention ( 7) Although the added amount is more than 15% by weight, it does not affect the honing surface, but for economic consideration, the upper limit is 20% by weight. Also, the concentration of each component is the concentration when honing the substrate for a magnetic disk. After manufacturing the honing composition, it is made a thick composition from the above concentration during transportation and the like, and the user is efficient after diluting the concentration during use. The composition for the honing disk substrate of the present invention is made of the sharp 90 ~ 100% of Titanite Titanium Oxide or Rutile Oxidation 90 to 100% of titanium or 90 to 100% of brookite titanium oxide, titanium oxide, honing accelerator, and water-derived bioforms, if necessary, water-soluble oxidizing agents can be added. ', Can also add surfactants, preservatives, and acid or base of P Η adjuster, etc. As a honing accelerator, if the use of aluminum acid salts such as aluminum nitrate, the ideal ρ Η is 2 to 5 When ρ Η is less than 2, the corrosion and operation problems of the honing machine will appear. If it is greater than 5, the honing efficiency will be an obstacle. The honing composition of the present invention is the same as the previous honing composition. The titanium oxide in which the crystal structure is suspended on water can be prepared by adding a honing accelerator and the like. 1 sound ψ 4 ° ί: Cai i L · (Please read the precautions on the back before filling in this page) The magnetic disk substrate suitable for the honing composition of the present invention is not particularly limited. Generally, the aluminum substrate, especially N High-quality honing that multiplies the mechanical honing effect of titanium oxide and the chemical honing effect by a honing accelerator after the aluminum substrate of IP is applied to the composition of the present invention The face is industrially advantageous. Honing method Generally, the honing base used for the raw material honing material is stacked on the magnetic disk substrate, and the raw material is supplied into the base and the substrate. At the same time, the paper size of the base is applicable to the Chinese National Standard (CNS) A4. Specifications (210 X 297 mm) -10- Economic, intellectual property, employee consumption, Fi print 581803 A7 B7 V. Description of the invention (8) The method of rotating the seat or substrate. A magnetic disk made of a honing substrate by using the honing composition of the present invention has extremely low occurrence frequency of micro-dents, micro-scratches and the like, and the surface roughness (R a) is about 3 to 5 A. Those with good smoothness. [Best Mode for Carrying Out the Invention] Hereinafter, the present invention will be specifically described by way of examples. However, the present invention is not limited to those examples. (Examples 1 to 16) Super taUania F-10 (rutile titanium oxide 98% by weight, anatase oxide 2% by weight) and super taitania made of high-purity titanium oxide manufactured by Showa Taitanium F-4 (anatase-type oxin 95% by weight, rutile-type titanium oxide 5% by weight) was pulverized with a media stirring honing machine, and after removing a few coarse particles, an average particle diameter of 0.3 / m was first obtained. Titanium oxide. The crystal structure and content of titanium oxide were measured using R A D-2 B manufactured by Rigaku Denki Co., Ltd. These are shown in Table 1 respectively as titanium dioxide ① and titanium dioxide ②. The particle size was measured by a laser Doppler frequency analysis type particle size distribution measuring device and a micro-guide device UPA 150 (manufactured by Honeywell). The particle size measurement is shown in Table 1. In the following, as the honing material, the titanium oxide and the honing accelerator may be added with an oxidizing agent according to the ratio shown in Table 2 according to different situations. After adjusting various water-based honing compositions, the honing device shown below Paper size under honing conditions applies to China National Standard (CNS) A4 (210 X 297 mm) • I n ϋ ϋ I ϋ ϋ I ϋ · «ϋ ϋ H · ϋ ϋ n ϋ ·-, ·· ϋ · ϋ ϋ ϋ · ϋ ϋ II (Please read the precautions on the back before filling out this page) -11-581803 A7 B7 V. Description of Invention (9) Honing. When silver nitrate is used as a honing accelerator, its p Η 値 is 2.3 to 4 · 1. Honing: The substrate used is a honing device and honing tester for 3.5 inch aluminum discs using Ni IP electroless plating ... 4 wei double-sided polishing machine 硏Grinding dents .... Suede type (polytex DG, Rodell) Lower platen rotation speed ... 60rpm Raw material feed speed ... 5 0 m 1 / mi η Honing time .. ..... 5 minute processing pressure ......... 50g / cm2 Evaluation of honing characteristics Honing rate ... Surface thickness converted from the weight difference before and after honing of aluminum discs · · · · Turing step and Turrideta 2000 (made by Lanktaylerhobson). The depth of the honing damage and honing dents was analyzed using a 3-dimensional model of a stylus surface analysis device P-12 (manufactured by Tencor). Find the depth.

硏磨特性之評定結果如表2所示。表2中硏磨損傷A (請先閱讀背面之注意事項再填寫本頁) 裝--------訂---------. 度 深 痕 凹 其 A 痕 凹 且 者 下 以 m η 5 爲 度 深 傷 損 磨 硏 其 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） -12- 581803 B7 _____ 五、發明說明（10 ) (請先閱讀背面之注意事項再填寫本頁) 爲5 n m以下者。硏磨損傷B其硏磨損傷深度爲5〜1〇 nm者，又，凹痕B之凹痕深度爲5〜1 〇 nm者。硏磨 損傷深度大於1 0 n m、凹痕深度大於1 0 n m者均未發 生於實施例、比較例中。 又，板鈦礦型氧化鈦爲9 0〜1 0 0 %.者亦有相同效 果。The evaluation results of the honing characteristics are shown in Table 2. Honing damage A in Table 2 (please read the precautions on the back before filling this page). -------- Order ---------. The following paper uses m η 5 as the degree of deep damage. The paper size is applicable to China National Standard (CNS) A4 (210 X 297 mm) -12- 581803 B7 _____ V. Description of the invention (10) (Please read the back first (Notes on this page, please fill out this page) is below 5 nm. Honing damage B is one where the honing damage depth is 5 to 10 nm, and dent B has a dent depth of 5 to 10 nm. Honing Damage depths greater than 10 nm and dent depths greater than 10 nm did not occur in the Examples and Comparative Examples. In addition, those having a brookite-type titanium oxide of 90 to 100% have the same effect.

使用昭和Taitanium (股份）製之氧化鈦之super taitania F-1 (金紅石型氧化鈦5 0重量％、銳鈦礦型氧化 欽5 0重量％)及同F - 2 (金紅石型氧化鈦1 6重量％ 、銳鈦礦型氧化鈦8 4重量％ )後，調製如表2所示之水 性硏磨用組成物，與實施例同法進行硏磨。其結果如表2 所示。又，粒度測定値如表1所示。表中二氧化鈦③如上 述F _ 2所示、二氧化鈦④如F - 1所示。 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公爱） -13- 581803 A7B7 五、發明說明（11) 〔表1〕 氧化鈦 之種別 氧化鈦之結晶 結構與含有率 (重量％ ) 一次粒徑 (平均） (β m ) 二次粒徑 (平均） (// m ) D 9〇/ D 1 0 二氧化鈦① 金紅石型 9 8 銳鈦礦型 2 0 . 2 0 . 3 2 . 4 二氧化鈦② 銳鈦礦型 9 5 金紅石型 5 0.05 0 . 3 2 . 6 二氧化鈦③ 金紅石型 16 銳鈦礦型 8 4 0.06 0 . 3 3 . 4 二氧化鈦④ 金紅石型 5 0 銳鈦礦型 5〇 0 . 1 0 . 5 3 . 4 (請先閱讀背面之注意事項再填寫本頁) 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） -14- 581803 A7 B7 五、發明說明（12) 〔S漱〕 iII t 1 擊»^ (γ) (3)制粜陌嗽 (u t日 \UI7y) 條»£ s__) _后滕 00 <<<<<<<<< < < < < < < <Super taitania F-1 (rutile-type titanium oxide 50% by weight, anatase-type oxide 50% by weight) using titanium oxide made by Showa Taitanium (shares), and F-2 (rutile-type titanium oxide 1) After 6% by weight and anatase titanium oxide (84% by weight), the aqueous honing composition shown in Table 2 was prepared, and honing was performed in the same manner as in the example. The results are shown in Table 2. The particle size measurement is shown in Table 1. Titanium dioxide ③ in the table is shown as F _ 2 above, and titanium dioxide ④ is shown in F-1. This paper size applies the Chinese National Standard (CNS) A4 specification (210 X 297 public love) -13- 581803 A7B7 V. Description of the invention (11) [Table 1] Crystal structure and content ratio of titanium oxide (% by weight) ) Primary particle size (average) (β m) Secondary particle size (average) (// m) D 9〇 / D 1 0 Titanium dioxide ① Rutile 9 8 Anatase 2 0. 2 0. 3 2. 4 titanium dioxide ② anatase type 9 5 rutile type 5 0.05 0. 3 2. 6 titanium dioxide ③ rutile type 16 anatase type 8 4 0.06 0. 3 3. 4 titanium dioxide ④ rutile type 5 0 anatase type 5〇 0. 1 0. 5 3 4 (Please read the notes on the back before filling in this page) This paper size is applicable to China National Standard (CNS) A4 (210 X 297 mm) -14- 581803 A7 B7 5 、 Explanation of the invention (12) 〔S〕 iII t 1 hit »^ (γ) (3) system 粜 Mo Su (ut day \ UI7y) Article» £ s__) _Hou Teng 00 < < < < < < < < < < < < < < < <

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Ln©si^ Lo 1—I围鎰 qJ-Λ tr---------AW-. -15- 581803 A7 ___B7_____ 五、發明說明（13) 〔產業上可利用性〕 使用本發明硏磨用組成物進行碟片硏磨後，可取表面 粗細度小，且極不易產生微細凹痕、微細刮傷等微細缺陷 之硏磨面，且，可於高速度下進行硏磨者。使用硏磨之碟 片之磁碟者可有效做爲低浮上型硬碟之用者及可高密度記 錄者。 特別是，做爲硏磨碟片所使用之磁碟磁氣拮抗效果所― 利用之M R磁頭用之媒體所代表之高記錄密度媒體（具1 Gbi t/inch2以上之記錄密度）其有效率極高，而 其以下之媒體中由高信賴性媒體之觀點上亦爲有用者。 (請先閱讀背面之注意事項再填寫本頁) 經濟部智慧財產笱員!.消费合阼Fi印製 -16- 本紙張尺度適用中國國家標準（CNS)A4規格（210 X 297公釐） 案 號 類 別 89年 6月27日 89112650 以上各櫚由本局填註） 新型 •1換年月曰 -正Ln © si ^ Lo 1—I encircled qJ-Λ tr --------- AW-. -15- 581803 A7 ___B7_____ V. Description of the invention (13) [Industrial applicability] Use the invention 硏After the disc is honed by the polishing composition, a honing surface having a small surface thickness and extremely difficult to generate micro defects such as micro dents, micro scratches, and the like can be used at a high speed. Those who use honing discs can effectively use them as low-floating hard disks and recorders with high density. In particular, as a magnetic disk antagonistic effect for honing discs-high recording density media (with a recording density of 1 Gbi t / inch2 or more) represented by the media used by MR heads, it is extremely effective High, and the following media are also useful from the viewpoint of high-reliability media. (Please read the precautions on the reverse side before filling out this page) Intellectual Property Staff of the Ministry of Economic Affairs !. Printed by Consumers Fi- 16- This paper size applies to China National Standard (CNS) A4 (210 X 297 mm) Category: June 27, 89, 8912,650 and above All palms are to be filled by this bureau) New type • 1 Year of the month

581803 Μ專利説明書 發明 新型 名稱 中文 研磨磁碟基板用組成物及磁碟用基板之製造方法 英文 姓 名 國籍581803 Μ Patent specification Invention New name Chinese Composition for polishing magnetic disk substrate and manufacturing method of magnetic disk substrate English Name First Name Nationality

Composition for polishing substrate for magnetic disk and method for producing substrate for magnetic disk (1)宮田憲彦 (1)曰本國長野縣塩尻市大字宗賀一昭和電工株式会社塩尻生 産技術統括部内 裝 ^^發明 創作 人 住、居所 訂 經濟部智^叫洗^7^工％介合作社印製 三、申請人 姓 名 (名稱） 國 籍 住、居所 (事務所） 代表人 姓 名 (1)昭和電工股份有限公司 昭和電工株式会社 ⑴日本 (1)曰本國東京都港區芝大門一丁目一三番九號 (1)大橋光夫 <紙張尺度適用中國國家標準.（CNS)A4規格（ 210X 297公釐） 線Composition for polishing substrate for magnetic disk and method for producing substrate for magnetic disk (1) Miyata Kenhiko (1) said that the country's production technology integration department inside the big character Zonghe-I Showa Denko Corporation, Nagano, Nagano prefecture ^^ Inventor's residence, residence Ordered by the Ministry of Economic Affairs ^ Called wash ^ 7 ^ 工 ％ 介 介 社 社 printed 3. Name of applicant (name) Nationality residence, residence (office) Name of representative (1) Showa Denko Corporation Showa Denko Corporation ⑴ Japan ( 1) It is said that the number of Shiba Daiichi, Sanctuary No. 1 and No. 3 and No. 9 in Minato-ku, Tokyo, Japan (1) Hikari Ohashi & paper size is applicable to Chinese national standard. (CNS) A4 size (210X 297 mm) line

Claims (1)

581803 ABCD 申請專利範圍 第891 12650號專利申請案 中文申請專利範圍修 (請先閲讀背面之注意事項再填寫本頁) 民國 1 . 一種硏磨磁碟基板用組成物，其係至少含有水’ 氧化鈦微粒子，0 . 1重量％以上硏磨促進劑之磁碟基板 之硏磨用組成物，氧化鈦微粒子之二次粒子之平均粒徑爲 0 . 1〜1 . 0 // m，氧化鈦微粒子之二次粒子之粒度分佈 中，累積9 0重量％之粒徑與1 0重量％之粒徑比D 9 0 / D 1 〇爲3 . 0以內，且該氧化鈦之單一結晶結構之氧 化鈦爲90〜100%者。 2 ·如申請專利範圍第1項之硏磨用組成物，其中該 硏磨促進劑爲鋁鹽或硝酸鹽者。 3 .如申請專利範圍第2項之硏磨用組成物，其中該 鋁鹽爲硝酸鋁者。 4 ·如申請專利範圍第1項之硏磨用組成物，其中該 組成物爲含有水溶性氧化劑者。 經濟部智慧財產局員工消費合作社印製 5 · —種磁碟用基板之製造方法，其特徵係於磁碟用 基板（原板）與硏磨底座中供與如申請專利範圍第1項之 硏磨用組成物之同時，含使該磁碟用基板或該硏磨底座之 至少一方進行旋轉之工程者。 本紙張尺度適用中國國家橾準（CNS ) A4規格（210 X 297公釐）581803 ABCD Patent Application No. 891 12650 Patent Application Chinese Patent Application Revision (Please read the precautions on the back before filling this page) Republic of China 1. A composition for honing disk substrates, which contains at least water 'oxidation Titanium fine particles, a composition for honing a magnetic disk substrate having a honing accelerator of 0.1% by weight or more. The average particle diameter of the secondary particles of the titanium oxide fine particles is 0.1 to 1. 0 // m. In the particle size distribution of the secondary particles, the ratio of the cumulative particle diameter of 90% by weight to the particle size of 10% by weight D 9 0 / D 1 0 is within 3.0, and the titanium oxide has a single crystal structure. 90 to 100%. 2. The honing composition according to item 1 of the patent application, wherein the honing accelerator is an aluminum salt or a nitrate. 3. The honing composition according to item 2 of the patent application, wherein the aluminum salt is aluminum nitrate. 4. The honing composition according to item 1 of the scope of patent application, wherein the composition is one containing a water-soluble oxidizing agent. Printed by the Intellectual Property Bureau of the Ministry of Economic Affairs' Consumer Cooperatives 5 — A manufacturing method of magnetic disk substrates, which is characterized by being provided in the magnetic disk substrate (original plate) and the honing base for honing such as in the first patent application scope At the same time as using the composition, an engineer who rotates at least one of the magnetic disk substrate or the honing base is included. This paper size applies to China National Standard (CNS) A4 (210 X 297 mm)