200525016 (1) 玖、發明說明 【發明所屬之技術領域】 本發明係關於將金屬、塑膠、玻璃等精密硏磨加工所 用之硏磨用組成物與硏磨方法，詳言之係關於安裝於電腦 硬碟驅動之磁碟之硏磨用組成物及硏磨方法。 【先前技術】 隨著近年急增之高磁記憶密度化與小口徑化，硬碟驅 動之磁頭與磁碟之間隙，即爲能藉由縮小磁頭飛行高度更 加提高記憶密度，不斷要求能與此因應具有較高品質之加 工面之碟片，進行能與此因應的各種開發。 此高密度化最近發展，自目前的4 0GB發展至60 GB 、8 0GB中，對硏磨劑的要求更逐步上升，其要求項目以 硏磨率爲首，遍及低面粗度化，無表面缺陷（微細凹痕、 微細突起、微細刮傷），降低廣域性並局部性表面波紋， 防止端面緣垂，防止對碟片之硏磨砥粒粒子之黏附或表面 髒污，高洗淨性等多方面。 該硏磨用組成物係爲較之以往提高硏磨速度且爲得到 高品質之表面之各種建議之硏磨用組成物。 如硏磨時最重要特性之一之維持提高硏磨速度，且得 到很難產生刮傷、凹痕、突起等缺陷或硏磨損傷之高品質 硏磨面之組成物，特開昭6 2 — 2 5 1 8 7號公報建議以硝酸鋁 爲首之各種無機酸或其類鹽爲硏磨促進劑，或爲有效縮小 應提高面精度要求之硏磨面之粗度之加工，特開平2 — 8 4 4 8 5號公報建議葡糖酸、乳酸、其後之公報所載之有機 200525016 (2) 酸系腐蝕劑。再之爲有效製得以該高能率且無表面缺陷之 高品質的硏磨面之硏磨用組成物，特開平1 — 1 8 8 2 64號公 報建議添加勃姆石氧化鋁凝膠或膠態氧化鋁所成之硏磨用 組成物或特開平1 1 一 9 2 7 4 9號公報之螯化物亦作爲硏磨促 進劑。又勃姆石凝膠或膠態氧化鋁同時具有表面改質劑之 效果’以另外意義爲目的之緣垂防止劑於特開2002 — 1 6 7 5 7 5號公報建議聚環氧乙烷聚環氧丙烯烷基醚等羥基 局分子聚合物。 另方面硏磨砥粒，建議具有各種結晶形態之氧化鋁、 二氧化鈦、二氧化鈽、氧化鉻、二氧化矽等，其中主要使 用α氧化鋁，特開2002 - 3 02 7 3號公報建議將α氧化鋁與 中間氧化鋁與緣垂防止劑組合。 但於急速發展之電腦硬體領域，對於不斷強烈要求供 給具有提高較佳記錄密度、較高品質之加工面之基板之事 ’必須得滿足今後嚴格品質要求項目（硏磨率、面質、緣 垂等）。 爲提高該記錄密度，要求須碟片之平面度或平坦度優 良，面粗度變小，無凹痕、突起、刮傷、表面波紋，再者 無產生於碟片外周端部之緣垂之事，得於如此高品質加工 之較優良之硏磨用組成物。 本發明爲因應此類要求，達成高的硏磨速度，同時提 供能產生無表面缺陷高品質之硏磨用組成物。 【發明內容】 〔發明之揭示〕 -6- 200525016 (3) 得以解決該課題之本發明之硏磨用組成物’主旨係具 有水、硏磨砥粒、微細結晶粉末及含有1種以上之硏磨促 進劑。本發明如下所記。 (1 ) 一種硏磨用組成物，其特徵爲含有水、硏磨砥 粒、硏磨促進劑、及對硏磨砥粒之1次粒子之直徑比爲1 / 2〜1 / 1 0 0 0之微細結晶粉末之硏磨輔助砥粒。 (2 )如（1 )項之硏磨用組成物，其中硏磨輔助砥粒 之1次結晶粒徑爲〇.〇〇5Vm〜0.07Mm之範圍。 (3 )如（1 )或（2 )項之硏磨用組成物’其中硏磨 輔助砥粒之2次粒子之平均徑爲〇 · 〇 5 // m〜8 // m之範圍 〇 (4 )如（1 )至（3 )項中任一項之硏磨用組成物， 其中硏磨輔助砥粒之比表面積爲20〜250 m2/g。 (5 )如（1 )至（4 )項中任一項之硏磨用組成物， 其中硏磨輔助砥粒之含量爲〇 . 1〜2 0質量％之範圍。 (6 )如（1 )至（5 )項中任一項之硏磨用組成物， 其中硏磨輔助砥粒係自銨明礬法、NH4A1 ( OH ) 2C03法 ，以金屬鋁爲啓始原料之鋁烷氧基鋁金屬法，及以火花電 壓法生成之氧化鋁，霧化氧化鋁及/或勃姆石·擬勃姆石 •三羥鋁石生成之微細結晶氧化鋁。 (7 )如（】）至（6 )項中任一項之硏磨用組成物， 其中硏磨砥粒之1次結晶徑之平均粒徑爲〇. 1 m〜5 // m 之範圍。 (8 )如（1 )至（7 )項中任一項之硏磨用組成物， 其中硏磨砥粒之2次粒子之平均粒徑爲0.3 // m〜5 // m之 -7 - 200525016 (4) 範圍。 (9 )如（I )至（8 )項中任一項之硏磨用組成物， 其中硏磨砥粒係含至少】種選自氧化鋁、二氧化矽、二氧 化鈦、氧化鉻、二氧化鈽、氧化鈣、氧化鎂、氧化錳、氧 化鐵。 (1 0 )如（1 )至（9 )項中任一項之硏磨用組成物， 其中硏磨砥粒係含α氧化鋁。 (1】）如（1 )至（1 〇 )項中任一項之硏磨用組成物 ，其中硏磨砥粒係含1次結晶爲〇 · 5 // m以下，比表面積 (BET値）6〜15 m2 / g之三水鋁礦系α氧化鋁。 (1 2 )如（1 )至（Π )項中任一項之硏磨用組成物 ，其中硏磨砥粒與硏磨輔助砥粒係相同材質之砥粒。 (1 3 )如（1 )至（1 2 )項中任一項之硏磨用組成物 ，其中硏磨砥粒之含量爲1〜3 5質量。/〇之範圍。 (1 4 )如（1 )至（1 3 )項中任一項之硏磨用組成物 ，其中硏磨促進劑係含有至少一種以上之有機酸、無機酸 鹽、有機酸與有機酸鹽之組合、有機酸與無機酸鹽之組合 、鋁鹽凝膠化生成物、及有機膦酸螯合性化合物。 (I 5 )如（！ 4 )項之硏磨用組成物，其中至少一種爲 有機酸、無機酸鹽、有機酸與有機酸鹽之組合、及有機酸 與無機酸鹽之組合之硏磨促進劑之含量爲0 · 〇〗〜1 〇質量。 之範圍。 (1 6 )如（1 4 )項之硏磨用組成物，其中鋁鹽凝膠化 生成物或有機膦酸螯合性化合物之含量爲0.0】〜5質量％ 之範圍。 200525016 (5) (】7 )如（1 )至（1 6 )項中任一項之硏磨用組成物 ，其中pH値爲2〜6之範圍。 (1 8 )如（1 )至（1 7 )項中任一項之硏磨用組成物 ’其中表面改質劑係含有週期表第5族或第6族之非金屬 無機酸、或含有羥烷基烷基纖維素。 (1 9 )如（1 8 )項之硏磨用組成物，其中表面改質劑 係至少含有氨基磺酸、磷酸、硝酸、羥丙基纖維素、羥丙 基甲基纖維素、羥乙基甲基纖維素 '及乙基羥乙基甲基纖 維素中之一種。 (2 0 ) —種組成物，其特徵爲稀釋後成爲（1 )〜（ 1 9 )項中任一項之硏磨用組成物所成者。 (2 1 ) —種方法，其特徵爲使用（2 〇 )項之組成物做 爲輸送或保管用組成物。 (22 ) —種硏磨方法，其特徵爲使用（！）至（2〇 ) 項中任一項之組成物硏磨基板。 (2 3 ) —種硏磨方法，其特徵爲使用以高於硏磨時濃 度之高成分濃度調製組成物，稀釋濃度做成（〗）至（！ 9 )項中任一項之硏磨用組成物加以，用於硏磨。 (24) —種基板之製造方法，其特徵爲使用（22)或 (2 3 )之方法。 〔用以實施發明之形態〕 根據本發明之硏磨用組成物，係含有水、硏磨砥粒、 硏磨促進劑、及對硏磨砥粒之1次粒子之間之直徑比1 / 2〜1/]〇〇〇，以2/5〜1/100爲宜，較佳爲]/3〜]/ 200525016 (6) 3 0爲微細結晶粉末之硏磨輔助砥粒。硏磨輔助砥粒係明 顯輔助淤漿狀之硏磨用組成物中之硏磨砥粒之硏磨機能。 藉由該硏磨輔助砥粒之硏磨輔助之機構，認爲係爲硏 磨輔助砥粒之微細結晶砥粒介於硏磨面與硏磨砥粒之間， 承受硏磨砥粒之衝擊，或按壓於硏磨砥粒，該硏磨砥粒之 作動能量之傳達等，承受硏磨砥粒之影響。其結果推測爲 使輔助砥粒對硏磨面之直接機械能量集中，機構運作敏銳 的作用。 根據本發明之硏磨用組成物之硏磨輔助磁粒，該1次 結晶粒徑以〇 . 〇 〇 5 // m〜0.0 7 // m之範圍爲宜。 根據本發明之硏磨用組成物之硏磨輔助砥粒之2次粒 子之平均徑以〇 . 〇 5 μ m〜8 μ m之範圍爲宜。 硏磨輔助砥粒因對硏磨面之凹凸非常微細，集中對硏 磨面之直接機械能量，敏銳的硏磨作用。 根據本發明之硏磨用組成物之硏磨輔助砥粒，對硏磨 用組成物之含量以 0.1〜20質量％之範圍爲宜。若在此範 圍，硏磨輔助砥粒因須充分分布於硏磨面，集中對硏磨面 之直接機械能量，敏銳的硏磨作用。 本發明硏磨組成物所用之硏磨砥粒，係使用氧化鋁、 二氧化矽、二氧化鈦、氧化鉻、二氧化鈽、氧化鈣、氧化 鎂、氧化錳、氧化鐵等，尤以推薦使用氧化鋁。 在此使用之氧化鋁不限於α、0、7等結晶形，基質 之硏磨砥粒以硏磨速度高之α氧化鋁爲宜。又因由氣孔少 之緊密之結晶構造組成且α 1次結晶徑除保有硏磨能力外 愈小爲宜。〗次結晶徑以平均徑爲〇. 1〜5 // m之範圍，以 -10- 200525016 (7) 兼具強度與緊密之0.1〜0.5// m之範圍最佳。 藉由】次結晶集合形成之2次粒子之平均徑爲〇 · 3〜 5.0/zm之範圍，以0.5〜3//m之範圍爲宜。該含量爲1〜 3 5質量％之範圍，以5〜3 0質量％爲宜。 又作爲硏磨砥粒之用之氧化鋁亦得將平均粒子徑細的 微粒氫氧化鋁（三水鋁礦或三羥鋁）或勃姆石、擬勃姆石 等燒焙後以適當之燒焙溫度燒焙成氣孔少之緊密之結晶結 構加工之氫氧化鋁所製成。 具體言之，勃姆石系氫氧化鋁之燒焙品係達成較之結 晶水少量之三水鋁礦系氫氧化鋁之燒焙品之緊密的結晶結 構，提高硏磨率。另方面經濟性以1次結晶〇 · 5 // m以下 ，比表面積（BET値）6m2/g以上15 m2/g程度之三水 鋁礦系α氧化鋁尤佳。 1次結晶徑得自掃描型電子顯微鏡（S Ε Μ )照片之數 値解析平均徑，或2次粒子之平均徑用雷射繞射散射式粒 度分布機（如島津SALD200(U)或雷射多普樂繞射式粒度 分布測定機（如MT UPA )等計測求出。 作爲硏磨輔助砥粒之微細結晶粉末，得用與該硏磨砥 粒同一材質者，亦得使用異種材質者，但以使用同一材質 者較佳，以氧化鋁尤佳。 在此被作爲硏磨輔助砥粒若爲氧化鋁時，不限於於α 、0、r等結晶形，但自整備有助於與基質硏磨材之面粗 度與面質之目的可爲以1次結晶等級易於分離者。]次結 晶徑於0 · 0 0 5〜0 · 0 7 # η ]之車它圍’以〇 . 〇 1〜〇 . 0 5 // m之範 圍尤佳。結晶形以α 、0 、& 、（5 、r爲宜，以0 、5 、 -11 - 200525016 (8) r尤佳。該比表面積（BET値）以20〜2 5 0 m2/ g爲宜， 以60〜1〇〇 n]2 / g尤佳。2次粒子之平均徑爲0.05〜8 // m 之範圍，以0.5〜5//m之範圍爲宜。再者含量爲0.1〜20 質量％之範圍，以〇 . 5〜1 0質量％爲宜。 又，1次結晶徑D係自用BET比表面積計（如島津 FUROSOP Π )測定之比表面積S與粒小密度P利用下式 所算出（D〔//m〕= 6/ (p 〔g/cm3〕xS〔m2/g〕） )。2次粒子之平均徑用該雷射繞射散射式粒度分布機（ 如島津SALD2 00(H)或雷射多普樂繞射式粒度分布測定機 (如MT UPA)等計測求出。 硏磨輔助砥粒係於淤漿狀之硏磨用組成物中輔助硏磨 砥粒之硏磨機能。即經確認微小徑之微細結晶砥粒含硏磨 砥粒時，該微細結晶砥粒對硏磨面直接作用之硏磨作用明 顯提高，且無損於硏磨面之品質。 推測對此微細結砥粒之作用時，對硏磨砥粒首先憶起 以下之事實。即硏磨基板時，硏磨砥粒藉由攪拌運動產生 機械能量作用於硏磨面。爲此將硏磨砥粒之直徑變小有限 制。硏磨砥粒本身對硏磨面之凹凸不得不相對性地變粗大 〇 對該硏磨砥粒之硏磨輔助砥粒，因該直徑明顯微小， 其本身硏磨砥粒之運動能量微小且硏磨作用力小。反其， 認爲硏磨輔助砥粒爲微小半徑對硏磨面敏銳地作用。 且推定爲硏磨輔助砥粒之微細結晶砥粒介於硏磨面與 硏磨砥粒之間時，承受硏磨砥粒之衝擊，或按壓於硏磨砥 粒，傳達該硏磨砥粒之運動能量等，受硏磨砥粒之影響。 -12 - 200525016 Ο) 其結果係硏磨輔助砥粒將對硏磨面之直 銳地作用。此硏磨輔助砥粒介於硏磨面 輔助硏磨砥粒之作用。 又，硏磨面之凹凸之中，對於凸（ 輔助砥粒之砥粒作用力，凹（谷）部硏 覆硏磨面。爲此，防止凹（谷）部過多 根據本發明之硏磨用組成物，Ni -碟基板面之硏磨時明顯增加該硏磨速度 精度局減少局的緣垂或表面波紋可得局 本發明所用之微細結晶氧化鋁尤佳 法之氧化鋁（如昭和電工製UA系列、 歹IJ ) ，NH4A1(0H)2C03法之氧化鋁（如 列），以金屬鋁爲啓始原料之鋁烷氧基 如住友化學製 AKP系列），火花電壓 如岩谷化學製R、RA、RG、RK等級等 霧化氧化鋁（如昭和電工製UFA系列、 等之氧化鋁），及將勃姆石、擬勃姆石 鋁燒焙生成之衍生物氧化鋁（如S ORU 製、UOP 製 VARSALALUMINA 之氧化 # 有機酸以至少1種選自丙二酸、丁 酸、蘋果酸、檸檬酸、甘氨酸、天冬氨 酸、庚葡糖酸、亞氨乙酸、富馬酸所成 以至少]種選自硫酸鈉、硫酸鎂、硫酸 銨、硝酸鎳、硝酸鋁、硝酸銨、硝酸亞 磺酸鎳所成群。有機酸或無機酸鹽之含 接機械能量集中敏 與硏磨砥粒之間， 山）部集中該硏磨 磨輔助砥粒埋没被 地被硏磨。 P等被電鍍，鋁磁 ，並無表面缺陷面 品質之硏磨面。 者，例舉銨礬明礬 BAICOROX CR 系 大明化學製TM系 金屬法之氧化銘（ 法生成之氧化鋁（ ®純度氧化銘）， 日本AEROGY製 或三羥鋁石氫氧化 製、ALCOA化成 二酸、己二酸、乳 酸、酒石酸、葡糖 群爲宜，無機酸鹽 鎳、硫酸鋁、硫酸 鐵、氯化鋁、氨基 量以 0.0 ]〜]0質 -13- 200525016 (10) 量％之範圍爲宜。若太少則作爲硏磨促進劑之效果小，過 多會產生凹痕、突起使硏磨面之品質降低。或產生氧化鋁 粒子凝集等對液性不宜之影響。 該硏磨促進劑得使用有機酸與有機酸鹽，或有機酸與 無機酸鹽之組合。 有機酸同前述得至少1種選自丙二酸、丁二酸、己二 酸、乳酸、蘋果酸、檸檬酸、甘氨酸、天冬氨酸、酒石酸 、葡糖酸、庚葡糖酸、亞氨乙酸、富馬酸所成群，有機酸 鹽得至少1種選自該有機酸之鉀鹽、鈉鹽、銨鹽所成群。 又，無機酸鹽同前述得至少1種選自硫酸鈉、硫酸鎂、硫 酸鎳、硫酸鋁、硫酸銨、硝酸鎳、硝酸鋁、硝酸銨、硝酸 亞鐵、氯化鋁、氨基磺酸鎳所成群。有機酸與有機酸鹽， 或有機酸與無機酸鹽之組合，總含量皆爲對硏磨用組成物 全體之0.01〜10質量％之範圍爲宜。其中有機酸之含量至 少含 0.003質量％尤佳。該混合系之硏磨促進劑若少於 〇 . 〇 I質量時作爲硏磨促進劑之效果小，若超過I 0質量％ 時，硏磨用組成物之.黏性變太高，或產生氧化鋁粒子之凝 集等發生對液性不宜之影響。硏磨面產生凹痕、突起導致 品質降低。又，有機酸與有機酸鹽之組合時，同種之酸組 合較易得到對硏磨特性佳之結果。 該硏磨促進劑得使用鋁鹽之凝膠化生成物（如特開 2 002 — 2 073 2號公報）。具體言之係於將鋁鹽（如硫酸鋁 、氯化鋁、硝酸鋁、磷酸鋁、及硼酸鋁等無機酸鋁鹽，或 乙酸鋁、乳酸鋁、及硬脂酸鋁等有機酸鋁鹽等）含水物或 無水物中之一種溶解之水溶解，將氫氧化鈉、氫氧化鉀、 -14- 200525016 (11) 銨、以一甲基胺等烷基胺或三乙醇胺爲代表之烷醇胺等有 機胺化合物’甘氨酸等氨基酸，亞氨乙酸等螯化物、乙撐 二胺四乙酸醯胺酸系螯化物、二乙撐三胺五甲酸磷醯胺或 氨基三甲撐憐醯胺等氨基磷酸系螯化物所成群之一種，高 裁斷攪泮所得之凝膠化生成物，與於銘鹽錢與胺等與水反 應易產生自由經基之物質或於端基含氫基之化合物或氫氧 化鈉、氫氧化鉀等含氫基之混合鏈生成。 鋁鹽之凝膠化生成物佔硏磨用組成物全體之含量以 0.01〜5質量％之範圍爲宜，較佳爲0.05〜2質量°/〇。若太 少則效果小，過多會產生凝膠化、或凹痕、突起等表面缺 該硏磨促進劑，得使用有機膦酸螯化物（如特開 2 00 1 — 1 3 1 5 3 5號公報）。具體言之爲至少一種選自二乙 撐三胺五乙酸甲撐膦酸 '磷酸丁烷四羧酸、磷酸羥乙酸、 乙群 ， 成 酸 所 膦鹽 二類 烷此 乙及 羥酸 ， 膦 酸撐 膦甲 烷四 丙胺 環二 基撐 氨甲 、 六 酸、 膦酸 基膦 甲撐 二甲 基四 乙胺 羥二 有機膦酸螯化物佔硏磨用組成物全體之含量以〇 . 〇 1〜 5質量％之範圍爲宜，較佳爲〇 . 〇 5〜2質量％。若太少則硏 磨速度提高效果小，過多會產生凹痕、突起等表面缺陷。 本發明之硏磨用組成物，再者表面改質劑可含有含週 期表第5族、第6族之非金屬元素之無機酸。在此含週期 表第5族、第6族之非金屬元素之無機酸之例有氨基磺酸 、磷酸、硝酸等。藉由適當添加此類無機酸得抑制凹痕、 突起之產生以提高面質。本無機酸佔硏磨用組成物全體之 -15- 200525016 (12) 含量以〇·〇】〜5質量。/〇之範圍爲宜，較佳爲〇·〇5〜2質量°/〇 。若太少或過多效果變小，過多會降低硏磨速度。 表面改質劑（防緣垂劑），得使用羥烷基烷基纖維素 (以下稱爲HRRC，如WOO 1 /2 3 4 8 5號手冊）。例舉如羥 丙基纖維素（HPC )、羥丙基甲基纖維素（HPMC )、羥 乙基甲基纖維素（HEMC )、及乙基羥乙基纖維素（EHEC )。本HRRC佔硏磨用組成物全體之含量以0.001〜2質 量％之範圍爲宜，較佳爲0.0 1〜〇. 1質量％。若太少致緣垂 改善效果小，若過多會降低硏磨速度。 本發明之硏磨用組成物中，因應需求除上述以外之添 加劑，得添加氧化鋁凝膠、表面活性劑、洗淨劑、防鏽劑 、防腐劑、pH調整劑、增黏劑、再之其他之纖維類或表 面改質劑等。 又，構成如上述本發明之硏磨用組成之各種成分濃度 係硏磨基板時之適宜濃度。因此，調製本發明硏磨用組成 物時’調製較之該濃度濃厚之組成物，亦得於使用時薄化 該濃度之範圍內。 此濃厚之組成物，適宜作爲輸送保管用組成物之用。 本發明之硏磨用組成物之pH以2〜6之範圍爲宜。 再者，使用該硏磨用組成物之基板之硏磨方法並使用 該硏磨用組成物被硏磨之基板亦包含於本發明之範圍內。 【實施方式】 實施例 以下具體說明本發明之實施，但本發明非限定於此 -16- 200525016 (13) 以不脫離前、後述之主旨之變更實施全部包含於本發明之 技術範圍。 依以下要領調製硏磨用組成物後，評估硏磨特性。 (硏磨用組成物之調製） 將於燒焙爐之氫氧化鋁於大氣中約〗200艺加熱處理 製得α氧化鋁。又以市售之氧化鋁爲啓始將此粉碎、濕式 分級製作2次粒小平均粒度〇 . 7 # m之基質材氧化鋁試料 。另外準備將高純度氧化鋁或氫氧化鋁於適當溫度預燒所 生成之微細結晶氧化鋁。另方面，硏磨用組成物試料係將 銘鹽與胺水組合摻合，高裁斷攪拌製作鋁鹽之凝膠化生成 物。再將分別於第1表〜第3表之成分組成般，以水、氧 化鋁 '微細結晶氧化鋁、有機酸及有機酸鹽等硏磨促進劑 、鋁鹽之凝膠化生成物、螯合劑、週期表第5族及第6族 元表之無機酸、溶解於水之纖維素系之表面改質劑之順序 、秤量、摻合、混合供作硏磨試料。 硏磨條件及硏磨特性之評估方法示於下。 (硏磨條件） 被硏磨工件，係使用將Ni — P無電解電鍍之3、5吋 鋁碟，以下列條件進行硏磨試驗並碟片評估。 硏磨試驗條件 硏磨試驗機 9B雙面硏磨機（SYSTEM精工（股）製）200525016 (1) Description of the invention [Technical field to which the invention belongs] The present invention relates to a honing composition and a honing method for precision honing processing of metals, plastics, glass, etc., in detail, it is about installing on a computer Composition and method for honing hard disk-driven magnetic disks. [Previous technology] With the rapid increase in magnetic memory density and small diameter in recent years, the gap between the magnetic head and the magnetic disk driven by the hard disk is to further increase the memory density by reducing the flying height of the magnetic head. In response to discs with a high-quality machined surface, various developments can be made in response to this. This high-density development has recently developed. From the current 40GB to 60GB and 80GB, the requirements for honing agents have gradually increased. The requirements of the project are to take the honing rate as the lead, throughout the low surface roughness, no surface Defects (micro-dents, micro-protrusions, micro-scratches), reduce the wide area and local surface ripple, prevent the edge of the end surface from falling, prevent the adhesion of the abrasive particles of the disc or the surface dirt, high cleaning performance And so on. This honing composition is a honing composition which is variously proposed to increase the honing speed and to obtain a high-quality surface as compared with the past. Such as maintaining one of the most important characteristics during honing to improve the honing speed, and to obtain a high-quality honing surface composition that is difficult to produce defects such as scratches, dents, protrusions or honing damage, JP 6-2 — JP 2 5 1 8 7 proposes various inorganic acids or salts thereof such as aluminum nitrate as honing accelerators, or in order to effectively reduce the roughness of the honing surface which should improve the accuracy of the surface, JP 2- Bulletin 8 4 4 8 5 recommends gluconic acid, lactic acid, and organic 200525016 contained in subsequent bulletins (2) Acid-based corrosives. Furthermore, in order to effectively produce a honing composition having a high-quality honing surface with high energy efficiency and no surface defects, Japanese Patent Application Laid-Open No. 1-1 8 8 2 64 suggests adding boehmite alumina gel or colloidal state. The honing composition made of alumina or the chelate of JP-A No. 1 1-9 2 7 4 9 also serves as a honing accelerator. The boehmite gel or colloidal alumina also has the effect of a surface modifier at the same time. An anti-sagging agent with another purpose is proposed in JP 2002 — 1 6 7 5 7 5 Hydroxyl local molecular polymers such as epoxypropylene alkyl ether. On the other hand, honing grains, it is recommended to have various crystal forms of alumina, titania, hafnium dioxide, chromium oxide, silicon dioxide, etc. Among them, alpha alumina is mainly used. Alumina and intermediate alumina are combined with a sag prevention agent. However, in the rapidly developing field of computer hardware, for the continuous strong demand for the supply of substrates with a higher recording density and a higher quality processing surface, it must meet the strict quality requirements in the future (honing rate, surface quality, margin And so on). In order to increase the recording density, the flatness or flatness of the disc must be excellent, the surface roughness must be small, no dents, protrusions, scratches, surface ripples, and no edges generated at the outer peripheral end of the disc. The result is a better honing composition for such high-quality processing. In order to respond to such requirements, the present invention achieves a high honing speed while providing a high-quality honing composition without surface defects. [Summary of the Invention] [Disclosure of the Invention] -6- 200525016 (3) The honing composition of the present invention that solves the problem is mainly composed of water, honing honing grains, fine crystalline powder, and containing one or more kinds of honing Grinding accelerator. The present invention is described below. (1) A honing composition, characterized in that it contains water, honing honing grains, a honing accelerator, and a primary particle diameter ratio to the honing honing grains is 1/2 to 1/1 1 0 0 0 Honing of fine crystalline powder aids honing. (2) The honing composition according to item (1), wherein the primary crystal grain size of the honing auxiliary honing grains is in the range of 0.0005 Vm to 0.07 Mm. (3) If the composition for honing according to item (1) or (2), wherein the average diameter of the secondary particles of the honing auxiliary honing particles is in the range of 0. 〇 5 // m to 8 // m 0 (4 ) The honing composition according to any one of (1) to (3), wherein the specific surface area of the honing auxiliary honing particles is 20 to 250 m2 / g. (5) The honing composition according to any one of (1) to (4), wherein the content of the honing auxiliary honing particles is in a range of 0.1 to 20% by mass. (6) The honing composition according to any one of (1) to (5), wherein the honing auxiliary honing particles are from the ammonium alum method, the NH4A1 (OH) 2C03 method, and metal aluminum is used as the starting material. Aluminoxy aluminum metal method, and alumina generated by spark voltage method, atomized alumina and / or boehmite, pseudo-boehmite, trialumite, fine crystalline alumina. (7) The honing composition according to any one of ()) to (6), wherein the average grain diameter of the primary crystal diameter of the honing honing grains is in a range of 0.1 m to 5 // m. (8) The honing composition according to any one of (1) to (7), wherein the average particle size of the secondary particles of the honing honing grains is 0.3 // m to 5 // m of -7- 200525016 (4) Scope. (9) The honing composition according to any one of (I) to (8), wherein the honing honing grain contains at least one kind selected from alumina, silicon dioxide, titanium dioxide, chromium oxide, hafnium dioxide , Calcium oxide, magnesium oxide, manganese oxide, iron oxide. (1 0) The honing composition according to any one of the items (1) to (9), wherein the honing honing particles contain alpha alumina. (1)) The honing composition according to any one of the items (1) to (10), wherein the honing honing grain system contains primary crystals of 0.5 or less // m, and a specific surface area (BET 値) 6 ~ 15 m2 / g gibbsite based alumina. (1 2) The honing composition according to any one of items (1) to (Π), wherein the honing honing grain and the honing auxiliary honing grain are honing grains of the same material. (1 3) The honing composition according to any one of (1) to (1 2), wherein the content of the honing honing grains is 1 to 35 mass. / 〇 range. (1 4) The honing composition according to any one of (1) to (1 3), wherein the honing accelerator contains at least one kind of organic acid, inorganic acid salt, organic acid and organic acid salt. Combination, a combination of an organic acid and an inorganic acid salt, an aluminum salt gelation product, and an organic phosphonic acid chelating compound. (I 5) The honing composition according to item (! 4), at least one of which is an organic acid, an inorganic acid salt, a combination of an organic acid and an organic acid salt, and a honing promotion of a combination of an organic acid and an inorganic acid salt The content of the agent is 0 · 〇〗 ~ 1 〇 mass. Range. (16) The honing composition according to item (1), wherein the content of the aluminum salt gelation product or the organic phosphonic acid chelating compound is in the range of 0.0] to 5% by mass. 200525016 (5) () 7) The honing composition according to any one of (1) to (16), wherein the pH is in the range of 2 to 6. (1 8) The honing composition according to any one of (1) to (17), wherein the surface modifier contains a non-metallic inorganic acid of Group 5 or Group 6 of the periodic table, or contains a hydroxyl group Alkyl alkyl cellulose. (1 9) The honing composition according to item (1 8), wherein the surface modifier contains at least sulfamic acid, phosphoric acid, nitric acid, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, and hydroxyethyl One of methyl cellulose 'and ethyl hydroxyethyl methyl cellulose. (20) A composition characterized by being diluted to become a composition for honing according to any one of (1) to (19). (21) A method characterized by using the composition of (20) as a composition for transportation or storage. (22) A honing method characterized by honing a substrate using the composition of any one of (!) To (20). (2 3) —A kind of honing method, characterized in that the composition is prepared by using a high component concentration higher than the concentration at the time of honing, and the dilution concentration is used for honing at any one of the items () to (! 9) The composition is applied for honing. (24) A method for manufacturing a substrate, which is characterized by using the method of (22) or (2 3). [Form for Implementing the Invention] The honing composition according to the present invention contains water, a honing honing grain, a honing accelerator, and a diameter ratio of 1/2 between the primary particles of the honing honing grain. ~ 1 /] 〇〇〇, preferably 2/5 ~ 1/100, more preferably] / 3 ~] / 200525016 (6) 30 is a honing auxiliary grain of fine crystal powder. Honing auxiliary honing grains clearly assist the honing function of honing honing grains in a slurry-like honing composition. The honing auxiliary mechanism of the honing auxiliary honing grain is considered to be a fine crystalline honing grain of the honing auxiliary honing grain between the honing surface and the honing honing grain, and bears the impact of the honing honing grain. Or press on the karma grain, the transmission of the kinetic energy of the karma grain, etc., to withstand the influence of the karma grain. As a result, it is presumed that the direct mechanical energy of the auxiliary particles on the honing surface is concentrated, and the mechanism operation is sensitive. According to the honing auxiliary magnetic particles of the honing composition of the present invention, the primary crystal grain size is preferably in a range of 0.005 to 0.07 // m. The average diameter of the secondary particles of the honing auxiliary honing particles of the honing composition according to the present invention is preferably in the range of 0.05 μm to 8 μm. The honing auxiliary honing grains have very fine unevenness on the honing surface, which concentrates the direct mechanical energy on the honing surface and has a sharp honing effect. The honing auxiliary honing particles of the honing composition according to the present invention preferably have a content of the honing composition in the range of 0.1 to 20% by mass. If it is within this range, the honing auxiliary honing particles must be fully distributed on the honing surface, focusing on the direct mechanical energy of the honing surface, and the sharp honing effect. The honing honing grains used in the honing composition of the present invention use alumina, silicon dioxide, titanium dioxide, chromium oxide, hafnium dioxide, calcium oxide, magnesium oxide, manganese oxide, iron oxide, etc., and alumina is particularly recommended. . The alumina used here is not limited to crystalline forms such as α, 0, and 7, and it is preferable that the alumina particles of the substrate are α alumina having a high honing speed. It is also composed of a tight crystalline structure with few pores, and the smaller the α primary crystal diameter is, the smaller the size of the primary crystallization is. The average crystal diameter is in the range of 0.1 to 5 // m, and the range of -10- 200525016 (7) which has both strength and compactness is the best. The average diameter of the secondary particles formed by the secondary crystal assembly is in a range of 0.3 to 5.0 / zm, and preferably in a range of 0.5 to 3 // m. The content is in the range of 1 to 35 mass%, and preferably 5 to 30 mass%. The alumina used for honing honing grains can also be finely pulverized aluminum hydroxide (gibbsite or trihydroxyaluminum) or boehmite, pseudo-boehmite, etc. with a small average particle diameter. It is made by calcining aluminum hydroxide with close crystalline structure with few pores. Specifically, the calcined product of boehmite-based aluminum hydroxide achieves a tighter crystalline structure than the calcined product of gibbsite-based aluminum hydroxide with a smaller amount of crystal water, thereby improving the honing rate. On the other hand, economic efficiency is based on primary crystallization of 0.5 · m / m, and a specific surface area (BET 値) of 6 m2 / g to 15 m2 / g. The primary crystal diameter is obtained from the number-analytical average diameter of a scanning electron microscope (S EM) photograph, or the average diameter of secondary particles is measured by a laser diffraction scattering type particle size distribution machine (such as Shimadzu SALD200 (U) or laser Doppler diffraction type particle size distribution measuring machine (such as MT UPA) and other measurement. As the fine crystalline powder of honing auxiliary particles, the same material as the honing particles can also be used, However, it is better to use the same material, especially alumina. If it is used as a honing aid, the alumina is not limited to crystalline forms such as α, 0, and r, but self-assembly can help with the matrix. The purpose of the surface roughness and surface quality of the honing material can be easy to separate with a primary crystal grade.] The secondary crystal diameter is 0. 0 0 5 ~ 0 · 0 7 # η] It is surrounded by '. 〇. 〇 The range of 1 ~ 〇. 0 5 // m is particularly preferable. The crystal form is preferably α, 0, &, (5, r, preferably 0, 5, -11-200525016 (8) r. The specific surface area (BET 値) It is preferably 20 ~ 2 50 m2 / g, and more preferably 60 ~ 100n] 2 / g. The average diameter of the secondary particles is in the range of 0.05 ~ 8 // m, and 0.5 ~ 5 // m The range is preferably. In addition, the content is in a range of 0.1 to 20% by mass, and preferably 0.5 to 10% by mass. The primary crystal diameter D is a ratio measured by a BET specific surface area meter (such as Shimadzu FUROSOP Π). The surface area S and the small particle density P are calculated using the following formula (D [// m] = 6 / (p [g / cm3] xS [m2 / g]). The average diameter of the secondary particles is diffracted by the laser. Scattering type particle size distribution machine (such as Shimadzu SALD2 00 (H) or Laser Doppler diffraction type particle size distribution measuring machine (such as MT UPA), etc.). The honing auxiliary honing grain is used for slurry honing. The composition assists the honing function of honing honing grains. That is, when the fine crystalline honing grains with a small diameter are confirmed to contain honing honing grains, the honing effect of the fine crystalline honing grains on the honing surface is significantly improved without damage. The quality of the honing surface. When inferring the effect of this fine-grained honing grain, first remember the following facts about the honing honing grain. That is, when honing the substrate, the honing honing grain generates mechanical energy to act on the honing grain by stirring. Grinding surface. To this end, there is a limit to reducing the diameter of the honing grain. The honing grain itself has to face the unevenness of the honing surface. The ground becomes coarser. Because the diameter of the honing auxiliary grain is significantly smaller, the kinetic energy of the honing grain is small and the honing force is small. On the contrary, the honing auxiliary grain is considered to be It is a small radius that acts sharply on the honing surface. And it is estimated that the fine crystal grains of the honing auxiliary grains are between the honing surface and the honing grain. Grinding grains, which convey the movement energy of the honing grains, are affected by the honing grains. -12-200525016 〇) The result is that the honing auxiliary grains will act directly and sharply on the honing surface. This honing auxiliary honing grains is in the role of the honing honing grains. In addition, among the unevenness of the honing surface, the concave (valley) portion covers the honing surface with respect to the convex (auxiliary grain pressure). To prevent this, the concave (valley) portion is excessively used for honing according to the present invention. The composition, the surface of the Ni-disc substrate is significantly increased during honing. The precision of the honing speed is reduced, and local sags or surface ripples can be obtained. The fine crystalline alumina used in the present invention is particularly alumina (such as manufactured by Showa Denko). UA series, 歹 IJ), NH4A1 (0H) 2C03 alumina (such as listed), aluminum alkoxy with metal aluminum as the starting material (such as Sumitomo Chemical's AKP series), spark voltage such as Iwatani Chemical R, RA , Alumina, RG, RK grade and other atomized alumina (such as Showa Denko UFA series, and other alumina), and the boehmite, pseudo-boehmite aluminum firing derivative alumina (such as S ORU, UOP The oxidation of making VARSALALUMINA # Organic acid is made of at least one kind selected from malonic acid, butyric acid, malic acid, citric acid, glycine, aspartic acid, heptogluconic acid, iminoacetic acid, and fumaric acid] Species selected from sodium sulfate, magnesium sulfate, ammonium sulfate, nickel nitrate, aluminum nitrate, nitrate Groups of ammonium acid and nickel nitrite sulfinate. The organic energy or inorganic acid salt contains mechanical energy between the sensitive and honing grains, and the honing grains assist the honing grains to be ground honing . P, etc. are electroplated, aluminum magnetic, and have no surface defects. For example, ammonium alum alum BAICOROX CR is the oxidized inscription of TM metal produced by Daming Chemical (alumina produced by the method (® purity oxidized inscription), made by AEROGY in Japan or made by mayolite hydroxide, ALCOA is converted into diacid, Adipic acid, lactic acid, tartaric acid, and dextrose are suitable. The amount of inorganic acid nickel, aluminum sulfate, iron sulfate, aluminum chloride, and amino group is 0.0] ~] 0 quality-13- 200525016 (10) The amount% range is If it is too small, the effect as a honing accelerator is small. Too much will cause dents and protrusions to reduce the quality of the honing surface. Or agglomeration of alumina particles will have an unfavorable effect on liquidity. Use an organic acid and an organic acid salt, or a combination of an organic acid and an inorganic acid salt. The organic acid is at least one selected from the group consisting of malonic acid, succinic acid, adipic acid, lactic acid, malic acid, citric acid, glycine, Groups of aspartic acid, tartaric acid, gluconic acid, heptonic acid, iminoacetic acid, and fumaric acid. The organic acid salt is at least one selected from the potassium, sodium, and ammonium salts of the organic acid. In addition, the inorganic acid salt is at least one selected from the group consisting of sodium sulfate , Magnesium sulfate, nickel sulfate, aluminum sulfate, ammonium sulfate, nickel nitrate, aluminum nitrate, ammonium nitrate, ferrous nitrate, aluminum chloride, nickel sulfamate. Organic acids and organic acid salts, or organic acids and inorganic The total content of the acid salt is preferably in the range of 0.01 to 10% by mass based on the entire honing composition. The content of the organic acid is preferably at least 0.003% by mass. If there is less honing accelerator in the mixed system The effect as a honing accelerator is small at 〇I mass. If it exceeds 100% by mass, the viscosity of the honing composition becomes too high, or agglomeration of alumina particles occurs, which is not suitable for liquidity. The honing surface produces dents and protrusions that lead to a reduction in quality. In addition, when a combination of an organic acid and an organic acid salt, the same acid combination is easier to obtain good honing characteristics. The honing accelerator may use an aluminum salt. The gelled product (such as JP 2 002-2 073 2). Specifically, it is the aluminum salt (such as aluminum sulfate, aluminum chloride, aluminum nitrate, aluminum phosphate, and aluminum borate, and other inorganic acid aluminum) Salt, or aluminum acetate, aluminum lactate, and aluminum stearate And other organic acid aluminum salts, etc.) dissolve in water or one of the dissolved water, dissolve sodium hydroxide, potassium hydroxide, -14-200525016 (11) ammonium, alkylamine such as monomethylamine or triethanolamine Organic amine compounds such as alkanolamines, amino acids such as glycine, chelate compounds such as iminoacetic acid, ethylenediaminetetraacetic acid ammonium chelates, diethylenetriaminepentacarboxylate, phosphoramidine, or aminotrimethine A group of aminophosphoric acid chelate compounds such as ammonium. The gelation product obtained by high cutting and stirring, reacts with water such as Yu Mingshangan and amines and easily generates free radicals or contains hydrogen at the end groups. Compounds based on hydrogen or hydrogen-containing mixed chains such as sodium hydroxide and potassium hydroxide. The content of the gelled product of the aluminum salt in the entire honing composition is preferably in the range of 0.01 to 5% by mass, preferably It is 0.05 to 2 mass ° / 〇. If it is too small, the effect will be small. Too much will cause gelation, or dents, protrusions and other surfaces lack the honing accelerator. Organic phosphonic acid chelate (such as JP 2000-1 1 3 1 5 3 5 Bulletin). Specifically, it is at least one selected from the group consisting of diethylene triamine pentaacetic acid methylphosphonic acid 'butane tetracarboxylic acid phosphate, glycolic acid phosphoric acid, and ethyl group, acid salts of phosphonic acid salts of the second class, ethyl and hydroxy acids, phosphonic acid 〇1〜 5 The content of phosphinated methane tetrapropylamine cyclodiylcarbamate, hexaacid, phosphonophosphinomethylenedimethyltetraethylamine hydroxydiorganophosphonic acid chelate accounts for the entire composition of honing. The range of mass% is preferable, and it is preferably 0.05 to 2 mass%. If it is too small, the honing speed increase effect will be small, and too much will cause surface defects such as dents and protrusions. The honing composition of the present invention, and further, the surface modifier may contain an inorganic acid containing a non-metal element of Groups 5 and 6 of the periodic table. Examples of the inorganic acid containing non-metal elements of Groups 5 and 6 of the periodic table include sulfamic acid, phosphoric acid, nitric acid, and the like. By appropriately adding such an inorganic acid, the occurrence of dents and protrusions can be suppressed to improve the surface quality. The content of the present inorganic acid in the honing composition is -15-200525016 (12). The content is from 0.005 to 5 mass. The range of / 0 is suitable, and it is preferably from 0.05 to 2 mass ° / 〇. If it is too small or too much, the effect will be small, too much will reduce the honing speed. As a surface modifier (anti-sagging agent), hydroxyalkyl alkyl cellulose (hereinafter referred to as HRRC, such as WOO 1/2 3 4 8 5 manual) can be used. Examples include hydroxypropyl cellulose (HPC), hydroxypropyl methyl cellulose (HPMC), hydroxyethyl methyl cellulose (HEMC), and ethyl hydroxyethyl cellulose (EHEC). The content of the HRRC in the entire honing composition is preferably in the range of 0.001 to 2 mass%, and more preferably in the range of 0.01 to 0.1 mass%. If it is too little, the marginal improvement is small, if too much, the honing speed will be reduced. In the honing composition of the present invention, alumina gels, surfactants, detergents, rust inhibitors, preservatives, pH adjusters, tackifiers, and the like may be added according to the needs of additives other than the above. Other fibers or surface modifiers. The concentration of various components constituting the honing composition of the present invention as described above is a suitable concentration when honing the substrate. Therefore, when the composition for honing of the present invention is prepared, the composition which is thicker than the concentration can also be thinned within the range of the concentration during use. This thick composition is suitable for transporting and storing the composition. The pH of the honing composition of the present invention is preferably in the range of 2 to 6. Further, a method of honing a substrate using the honing composition and a substrate to be honed using the honing composition are also included in the scope of the present invention. [Embodiments] Examples The following specifically describes the implementation of the present invention, but the present invention is not limited to this. -16- 200525016 (13) All implementations without departing from the gist of the present invention are included in the technical scope of the present invention. After preparing the honing composition in the following manner, the honing characteristics were evaluated. (Preparation of the composition for honing) The aluminum hydroxide to be calcined in the atmosphere is heat-treated in the atmosphere for about 200 times to obtain α alumina. Starting with commercially available alumina, this crushing and wet classification was used to make a secondary alumina sample with a small average particle size of 0.7 # m. In addition, fine crystalline alumina produced by pre-calcining high-purity alumina or aluminum hydroxide at an appropriate temperature is prepared. On the other hand, the honing composition sample is a mixture of Ming salt and amine water, which is agitated with high cutting to produce a gelled product of aluminum salt. Then, the composition of the ingredients in Tables 1 to 3 is as follows. Water, alumina, fine-crystalline alumina, organic acids, and organic acid salts are used as honing accelerators, aluminum salt gelation products, and chelating agents. 5. The order, weighing, blending and mixing of inorganic acids in the periodic table of Group 5 and Group 6 inorganic table, cellulose-based surface modifiers dissolved in water, are used as honing samples. The evaluation methods of the honing conditions and honing characteristics are shown below. (Honing conditions) The workpiece to be honed was a 3 or 5 inch aluminum plate electrolessly plated with Ni—P. The honing test was performed under the following conditions and the plate was evaluated. Honing test conditions Honing test machine 9B double-sided honing machine (made by SYSTEM Seiko Co., Ltd.)
硏磨墊 H9900S 定盤旋轉數 上定盤28 rpni、下定盤45 rpm -17- 200525016 (14) 淑漿供給量 1 0 0 m 1 / m i η 硏磨時間 5分鐘 加工壓力 80g/cm2 (碟片之評估方法） 硏磨速度：自硏磨前後之碟片減少質量算出 硏磨面品質：表面缺陷（凹痕、突起、刮傷）用顯微 鏡觀察（NIKON微分干渉型 X 1〇〇)以十字型觀察5張 碟片之硏磨面表裏，無缺陷者爲良好（缺陷個數〇爲A、 1〜5爲B) 、6以上爲C (不良）。 表面粗度：Tencor P— 1 2 緣垂量：利用評估設備（S U F C 0 D E S E - 3 0 D )(小阪 製作所製）測定。若參照第1圖，沿著將已硏磨之硬碟表 面之外周部用評估設備描繪之描線S之外周端設垂直線h ，以h爲基準朝向碟片之中心之描線上3 0 0 0 # m之點爲A ，2 0 0 0 // m之點爲B時於通過A — B直線之延長線上自垂 直線h 5 00 " m之點爲C，將與設於C點之垂直線k與描 線S之交叉點爲D，將C 一 D間之長度t爲緣垂量加以測 定。 硏磨試驗之評估結果之第1表及第2表分別表示本發 明之實施例，第3表表示比較例。 200525016 (15) mV t〇K MU 嫌 S m 緣下垂 nm g ο § 〇 g g 表面 粗度 0< r- ON 寸 Os Os <N ON α； (N cK 表面 缺陷 等級 < < < < < < < 硏磨 速度 β m/ min 0.97 1.08 0.94 0.96 1.08 J 1.05 T—H 表面改質 HRRC 質量％ HPMC 0.05 HPMC 0.05 HPMC 0.05 HPMC 0.05 1 HPMC 0.05 HPMC 0.05 HPMC 0.05 無機酸 i質量％ 磷酸 0.1 磷酸 0.1 磷酸 0.1 磷酸 0.1 磷酸 0.1 麵 0, 磷酸 0.1 硏磨促進劑 螯合 質量％ NTMP 0.5 1_ NTMP 0.5 NTMP 0.5 NTMP 0.5 ! _1 NTMP 0.5 NTMP 0.5 NTMP 0.5 硫金呂 溶膠 質量％ to in 〇 o to d 有機酸鹽/ 無機酸鹽 質量％ 1_ ο o o to 種類 檸檬酸 銨礬 檸檬酸 銨礬 檸檬酸 銨礬 檸檬酸 銨礬 檸檬酸 銨礬 — 丨 1 檸檬酸 銨礬 檸檬酸 銨礬 有機酸 質量％ o to o d> VO 種類 檸檬酸 檸檬酸 檸檬酸 檸檬酸 檸檬酸 檸檬酸 檸檬酸 氧化鋁/大結晶氧化鋁 質量％ 6.0/ 1.0 6.0/ 1.0 6.0/ 1.0 6.0/ 1,0 6.0/ 1.0 6.0/ 1.0 6.0/ 1.0 1次 結晶徑 β\Λ\ 0.2/ 0.01 0.2/ 0.03 0.2/ 0.07 0.2/ 0.03 0.2/ 0.03 0.2/ 0.03 丨 0.2/ 0.05 種類 Α·1/ UAr A-2/ UAr A-l/ UAa A-l/ CRr Α·1/ UFAr A-l/ AKPr A-l/ rg γ 飄變匡 — (N 寸 Ό 卜 -19- 200525016 (16)Honing pad H9900S Rotation number of the upper platen 28 rpni, lower platen 45 rpm -17- 200525016 (14) Supply of sizing pulp 1 0 0 m 1 / mi η Honing time 5 minutes Processing pressure 80g / cm2 (disc Evaluation method) Honing speed: Calculate the quality of the honing surface from the reduced mass of the disc before and after honing: Surface defects (dents, protrusions, scratches) are observed with a microscope (NIKON differential dry type X 100), and cross type Observing the surface of the honing surface of 5 discs, no defect is good (the number of defects 0 is A, 1 to 5 is B), and 6 or more is C (defective). Surface roughness: Tencor P— 1 2 Edge sag: Measured with an evaluation device (SU F C 0 D E S E-3 0 D) (manufactured by Kosaka Manufacturing Co., Ltd.). If referring to FIG. 1, a vertical line h is set along the outer peripheral end of the tracing line S drawn by the evaluation device on the outer periphery of the hardened disk surface, and the drawing line toward the center of the disc with h as a reference 3 0 0 0 The point of # m is A, 2 0 0 0 // When the point of m is B, the vertical line passing through A — B from the vertical line h 5 00 " The point of m is C, which will be perpendicular to the point set at C The intersection of the line k and the tracing line S is D, and the length t between C and D is measured as the edge sag. Tables 1 and 2 of the evaluation results of the honing test show examples of the present invention, and Table 3 shows comparative examples. 200525016 (15) mV t〇K MU Suspend S m edge nm g ο § gg Surface roughness 0 < r- ON inch Os Os < N ON α; (N cK surface defect grade < < < < < < < Honing speed β m / min 0.97 1.08 0.94 0.96 1.08 J 1.05 T—H Surface modification HRRC mass% HPMC 0.05 HPMC 0.05 HPMC 0.05 HPMC 0.05 1 HPMC 0.05 HPMC 0.05 HPMC 0.05 inorganic acid i mass% Phosphoric acid 0.1 Phosphoric acid 0.1 Phosphoric acid 0.1 Phosphoric acid 0.1 Phosphoric acid 0.1 Surface 0, Phosphoric acid 0.1 Honing accelerator chelating mass% NTMP 0.5 1_ NTMP 0.5 NTMP 0.5 NTMP 0.5! _1 NTMP 0.5 NTMP 0.5 NTMP 0.5 Mass of sulfur gold sol to d organic acid salt / inorganic acid salt mass% 1_ ο oo to type ammonium citrate alum ammonium citrate alum ammonium citrate alum ammonium citrate alum ammonium citrate alum citrate — 丨 1 ammonium citrate alum ammonium citrate alum citrate % O to o d > VO Type Citric Acid Citric Acid Citric Acid Citric Acid Citric Acid Citric Acid Aluminate / Large Crystal Alumina Mass% 6.0 / 1.0 6.0 / 1.0 6.0 / 1.0 6.0 / 1,0 6.0 / 1.0 6.0 / 1.0 6.0 / 1.0 Primary crystal diameter β \ Λ \ 0.2 / 0.01 0.2 / 0.03 0.2 / 0.07 0.2 / 0.03 0.2 / 0.03 0.2 / 0.03 丨 0.2 / 0.05 Type A · 1 / UAr A-2 / UAr Al / UAa Al / CRr Α · 1 / UFAr Al / AKPr Al / rg γ Wandering Kuang — (N inch Ό -19-19 200525016 (16)
眯 m m 緣下垂 ηηι § o f_· o to r-_H 0 1 ( 表面 粗度 寸 C\ (N 〇\ m 〇< in 〇> 寸 (N 表面 缺陷 等級 < < PQ PQ 硏磨 速度 β m/min 1.06 1.03 1.08 1.07 f 1 '< r—K t a'i g 表面改質 HRRC 質量％ HPMC 0.05 HPC 0.05 1 1 1 1 無機酸 質量％ 1_ 磷酸 0.1 氨基磺 0.2 1 1 1 1 硏磨促進劑 螯合 質量％ | NTMP 0.5 NTMP 0.5 PBTC 1.0 1 1 PBTC 0.5 硫·銘 溶膠 質量％ d 1 1 有機酸鹽/ 無機酸鹽 質量％ o 1 o o 種類 蘋果酸 銨礬 檸檬酸 銨礬 1 檸檬酸 銨礬 檸檬酸 銨礬 檸檬酸 銨礬 有機酸 質量％ o 1 O 種類 蘋果酸 檸檬酸 1 檸檬酸 檸檬酸 檸檬酸 氧化鋁/大結晶氧化鋁 質量％ 1 6.0/ 1.0 6.0/ 1.0 6.0/ 1.0 1 6.0/ 6.0/ 1.0 6.0/ 1.0 1次 結晶徑 β 111 02/ 0.05 0.2/ 0.07 0.2/ 0.01 0.2/ 0.01 0.2/ 0.01 0.2/ 0.01 種類 A-1/ A-2r A-l/ A-l Θ A-l/ UAr A-l/ UAr A-l/ | UAr A-l/ UAr 〇〇 Cs o rs) m -20- 200525016 (17) 此本表中A 一1係三水鋁礦系之α氧化鋁，A — 2爲勃 姆石系之α氧化$g。^ a 7、u A α分別爲昭和電工製銨礬 月攀法之氧化銘，^了係viCORSKI製同法之r ’ UFA係昭和電工製霧化氧化相之7 ，AKP r係住友化學 _銘丨完氧基金屬法之7 ，RG r係岩谷化學之火花電壓法 之r ’ A — 2 7係勃姆石之燒焙r ，A — 1 0係三水鋁礦之 燒焙Θ氧化鋁。 -21 - 200525016 (18)眯 mm sag ηη § o f_ o to r-_H 0 1 (Surface roughness inch C \ (N 〇 \ m 〇 < in 〇 >) (N Surface defect grade < < PQ PQ Honing speed β m / min 1.06 1.03 1.08 1.07 f 1 '< r—K t a'i g Surface modification HRRC mass% HPMC 0.05 HPC 0.05 1 1 1 1 inorganic acid mass% 1_ phosphoric acid 0.1 sulfamate 0.2 1 1 1 1 硏Mill Accelerator Chelating Mass% | NTMP 0.5 NTMP 0.5 PBTC 1.0 1 1 PBTC 0.5 Sulfur · Ming Sol Mass% d 1 1 Organic Acid Salt / Inorganic Acid Salt% o 1 oo Type Ammonium Malate Alum Citric Ammonium Alum 1 Lemon Ammonium citrate, ammonium citrate, ammonium citrate, ammonium citrate, organic acid mass% o 1 O type malate citric acid 1 citric acid citrate aluminate citric acid / large crystalline alumina mass% 1 6.0 / 1.0 6.0 / 1.0 6.0 / 1.0 1 6.0 / 6.0 / 1.0 6.0 / 1.0 Primary crystal diameter β 111 02 / 0.05 0.2 / 0.07 0.2 / 0.01 0.2 / 0.01 0.2 / 0.01 0.2 / 0.01 Type A-1 / A-2r Al / Al Θ Al / UAr Al / UAr Al / | UAr Al / UAr 〇〇Cs o rs) m -20- 200525016 (17) A-1 series gibbsite in this table Α alumina, A-2 is the αg $ g of boehmite. ^ A 7, u A α is the oxidation inscription of the ammonium alum produced by Showa Denko, ^ is the same as the viCORSKI system. UFA is 7 of the atomized oxidation phase manufactured by Showa Denko, AKP r is Sumitomo Chemical_Ming 丨 Complete 7 of oxymetal method, RG r is r 'A — 2 7 of boehmite burning by Iwatani Chemical's spark voltage method Roasting r, A — 0 0 series gibbsite alumina Θ alumina. -21-200525016 (18)
陳 5； 劃 緣下垂 1 〇 \ Ο r-H r—Η Ο ^Η r_H O r—H t 11 o 〇〇 T'-'H r—H ο 00 r Ή b m 〇\ οο Ον m CN t—H (N 〇 r-H o o r-H Ο Η Ο ο 赘 Η 表面 缺陷 等級 m PQ CQ CQ U U Ο U & _侧 // m/min ο οο ο Ο m v〇 o oo VO o rn o ο Ον Ο 表面改質 HRRC 質量％ HPMC 0.05 HPMC 0.05 HPMC 0.05 HPMC 0.05 1 1 1 1 無機酸 質量％ 磷酸 0.1 磷酸 0.1 磷酸 0.1 磷酸 0.1 1 1 1 1 硏磨促進劑 <〇 鉚 質量％ NTMP 0.5 HEDP 0.5 NTMP 0.5 NTMP 0.5 PBTC 1.0 1 1 PBTC 0.5 質量％ ο d 1 1 Ο Ο 有機酸鹽/ 無機酸鹽 質量％ o 1 ΙΟ ΙΟ ο 種類 i檸檬酸 !銨礬 檸檬酸 銨礬 檸檬酸 銨礬 檸檬酸 銨礬 1 檸檬酸 銨礬 檸檬酸 銨礬 檸檬酸 錢攀 有機酸 質量％ ο o 1 <η ο 種類 檸檬酸 檸檬酸 檸檬酸 檸檬酸 1 檸檬酸 檸檬酸 檸檬酸 氧化鋁/大結晶氧化鋁 _丨 質量％ ο K ο 卜： ο 卜· 6.0/ 1.0 p ο 卜· ρ 卜· ο 卜· 1次 結晶徑 £ 3 (Ν Ο (Ν Ο ο rn 0.2/ 3.0 (N 〇 (Ν Ο (N Ο (Ν ο 種類 ι ! < (Ν < m < A-l/ A-3 1—I 1 < i < ψ ^ < r-H 1 < 一 (Ν m 寸 VsO 卜 00 -22- 200525016 (19) 本表中 A— 1、A— 3係同於第1表及第2表之三水 鋁礦系之α氧化鋁，同樣地A— 2爲勃姆石系之α氧化鋁 〇 該第1表及第2表係表示滿足本發明要件之實施例1 〜1 3之結果，得知皆可得表面缺陷、面粗度、緣垂等表 面性狀優異之硏磨面，並硏磨速度加快。對此如第3表所 示，不含微細結晶之比較例1〜8，均爲硏磨速度緩慢， 表面性狀亦不佳者。 又含有具有大結晶徑粉末之比較例4，較之不含此者 反而降低硏磨速度。 〔產業上之可利用性〕 本發明之硏磨用組成，因如上述所構成，硏磨速度快 且可製得無表面缺陷之高晶質鏡面加工面之點非常有用。 【圖式簡單說明】 第1圖係規定緣垂量之說明圖。 〔圖號說明〕 s :利用評估設備碟片外周端附近之描線 h :連於碟片外周端部之垂直線 A :位於自垂直線h之描線上3 0 0 0 # m之點 B :位於自垂直線h之描線上2 0 0 0 μ m之點 C :位於以通過A點、B點之直線上自垂直線h 500 # m之點 -23- 200525016 (20) k :通過C點之垂直線 D :垂直線k與描線S之交叉點 t : C點與D點間之長度（緣垂量） -24-Chen 5; Drooping sag 1 〇 \ Ο rH r—Η Ο ^ Η r_H O r—H t 11 o 〇〇T '-' H r—H ο 00 r Ή bm 〇 \ οο Ον m CN t—H ( N 〇rH oo rH 〇 Η Ο ο superficial surface defect level m PQ CQ CQ UU 〇 U & _ side // m / min ο οο ο ο mv〇o oo VO o rn o ο Ον 〇 Surface modification HRRC quality % HPMC 0.05 HPMC 0.05 HPMC 0.05 HPMC 0.05 1 1 1 1 Mass of inorganic acid% phosphoric acid 0.1 phosphoric acid 0.1 phosphoric acid 0.1 phosphoric acid 0.1 1 1 1 1 1 1 PBTC 0.5% by mass ο d 1 1 Ο 〇 Organic acid salt / inorganic acid salt by mass% o 1 ΙΟ ΙΟ ο kind i citric acid! Ammonium citrate ammonium citrate alum citrate ammonium citrate ammonium citrate alum citrate 1 ammonium citrate alum lemon Ammonium citrate, citric acid, organic acid,% by mass ο o 1 < η ο Kind of citric acid, citric acid, citric acid, citric acid, 1 citric acid, citric acid, citric acid, alumina / large crystalline alumina_ 丨% by mass ο K ο Bu: ο BU 6.0 / 1.0 p ο BU ρ BU ο BU 1 crystallization diameter £ 3 (N Ο (Ν Ο ο rn 0.2 / 3.0 (N 〇 (Ν Ο (N Ο (Ν ο kind ι! ≪ (Ν < m < Al / A-3 1-I 1 < i < ψ ^ & lt rH 1 < 1 (N m inch VsO bu 00 -22- 200525016 (19) In this table, A-1, A-3 are the same as those in Table 1 and Table 2 for the gibbsite alumina Similarly, A-2 is the alumina of the boehmite series. The first and second tables show the results of Examples 1 to 13 that meet the requirements of the present invention. It is known that surface defects and rough surfaces can be obtained. Honed surface with excellent surface properties such as degree and edge droop, and the honing speed is increased. As shown in Table 3, Comparative Examples 1 to 8 that do not contain fine crystals all have a slow honing speed and have no surface properties Comparative Example 4 which also contains powder having a large crystal diameter reduces the honing speed as compared with the case without containing it. [Industrial Applicability] The composition for honing according to the present invention is constituted as described above. The point that the grinding speed is fast and a highly crystalline mirror-finished surface without surface defects is very useful. [Brief description of the drawing] Fig. 1 is an explanatory drawing of the prescribed edge droop. [Illustration of drawing number] s: Trace line h near the outer peripheral end of the disc using the evaluation device: Vertical line A connected to the outer peripheral end of the disc A: Point 3 on the drawing line from the vertical line h 3 0 0 0 # m B: Located on Point C of 2 0 0 0 μm from the drawing line of the vertical line h: Located on a line passing through point A and point B From the point of the vertical line h 500 # m -23- 200525016 (20) k: passing through point C Vertical line D: Intersection point t of vertical line k and trace line S: Length between point C and point D (edge sag) -24-