TWI351334B - Submicron alpha alumina high temperature bonded ab - Google Patents

Submicron alpha alumina high temperature bonded ab Download PDF

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Publication number
TWI351334B
TWI351334B TW096148770A TW96148770A TWI351334B TW I351334 B TWI351334 B TW I351334B TW 096148770 A TW096148770 A TW 096148770A TW 96148770 A TW96148770 A TW 96148770A TW I351334 B TWI351334 B TW I351334B
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Taiwan
Prior art keywords
alumina
abrasive
high temperature
adhesive
vitreous
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Application number
TW096148770A
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English (en)
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TW200836883A (en
Inventor
Ralph Bauer
Margaret L Skowron
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Saint Gobain Ceramics
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Publication of TW200836883A publication Critical patent/TW200836883A/zh
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Publication of TWI351334B publication Critical patent/TWI351334B/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • B24D3/02—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
    • B24D3/04—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic
    • B24D3/14—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic ceramic, i.e. vitrified bondings
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D18/00—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • B24D3/02—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
    • B24D3/04—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic
    • B24D3/14—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic ceramic, i.e. vitrified bondings
    • B24D3/16—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic ceramic, i.e. vitrified bondings for close-grained structure, i.e. of high density
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • B24D3/34—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents characterised by additives enhancing special physical properties, e.g. wear resistance, electric conductivity, self-cleaning properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • B24D3/34—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents characterised by additives enhancing special physical properties, e.g. wear resistance, electric conductivity, self-cleaning properties
    • B24D3/342—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents characterised by additives enhancing special physical properties, e.g. wear resistance, electric conductivity, self-cleaning properties incorporated in the bonding agent
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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  • Compositions Of Oxide Ceramics (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

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1351334 九、發明說明： 【發明所屬之技術領域】 本發明之態樣大體係針對高溫經黏著研磨玉具及組份， 特疋。t係關於併有精細微結構氧化铭研磨砂粒之高溫 經黏著研磨劑。 【先前技術】 高效能研磨材料及組份已長㈣於各種X業加工應用， 包括精研/磨光，其中執行大塊材料移除，至精細拋光， 其中解決精細微米及次微米表面不規則性。接受該等加工 插作之典型材料包括各種陶究、玻璃、玻璃-陶究、金屬 及金屬纟金。研磨劑可呈現各種形式中之任一I，諸如如 研磨衆中之游離研磨劑，其中懸浮液中之疏鬆研磨顆粒用 於加工。或者，研磨劑可採取固定研磨劑之形式，諸如經 塗佈之研磨劑或經黏著之研磨劑。經塗佈之研磨劑大體上 分：為具有下伏基板之研磨組份，在下伏基板上研磨砂粒 或曰曰粒經由—系列頭膠（make c〇at)及底膠（size c〇at)黏附 至其。經黏著之研磨劑通常不具有下伏基板，且由經由基 質黏著材料黏著在一起之研磨砂粒之完整結構形成。 目則技術狀態之經黏著研磨劑利用玻璃質黏著材料，諸 如基於矽石之玻璃黏著基質。或者，用於某些應用之專業 經黏著研磨劑併有超級研磨砂粒（諸如立方碳化硼及金剛 石）’且可經由使用金屬合金黏著基質而整體地黏著。 雖然近年來經黏著研磨劑已持續經歷發展，但特定注意 力已賦予利用由破璃質材料形成之黏著基質的高溫經黏著 127841.doc 1351334 研磨劑。在美國專利5,282,875中描述高溫經黏著研磨組份 之實例。雖然目前技術狀態之高溫經黏著研磨組份已改 良效能及耐久性，但該技術中仍持續存在對進一步改良之 組份的需求。 【發明内容】 根據一態樣，提供一種高溫經黏著研磨劑，其包括氧化 鋁研磨砂粒及玻璃質黏著基質，該等研磨砂粒分布於該玻 璃質黏著基質中。該玻璃質黏著基質具有高溫度性質，包 括不小於約1 〇〇〇°c之固化溫度。氧化鋁研磨砂粒包含多 晶α-氧化鋁，該多晶α_氧化鋁具有一精細結晶微結構，其 特徵在於一不大於5〇〇 nm2a_氧化鋁平均域大小。該等氧 化鋁研磨砂粒進一步包含銷定劑（pinning叫㊁加），該銷定 劑包含一在多晶α-氧化銘相中之分散相。 根據另一態樣，提供一種高溫經黏著研磨劑，其包括氧 化鋁研磨砂粒及玻璃質黏著基質，該等砂粒分布於該玻璃 質黏者基負中。玻璃質黏著基質具有一不小於。匸之固 化溫度。氧化鋁研磨砂粒包含多晶α_氧化鋁，該多晶〜氧 化鋁具有一精細結晶微結構，其特徵在於一不大於打爪 之平均域大小。此外，氧化鋁研磨砂粒包含銷定劑，該銷 定劑包括分散於多晶α-氧化鋁相中之至少一氧化錯相。 另外，提供一種形成高溫經黏著研磨劑之方法。該方法 要求藉由在一不小於1350t之溫度下熱處理含有銷定劑之 α-氧化鋁前驅物而形成精細結晶微結構α_氧化鋁研磨砂 粒。接著形成一含有α-氧化鋁砂粒及玻璃質黏著基質材料 127841.doc 1351334 之成形體。此外，在一不小於iooo°c且高於玻璃質黏著基 質材料之熔點之固化溫度下進行該成形體之熱處理。氧化 铭研磨砂粒在熱處理之後具有一不大於約30〇 nm之平均結 晶域大小。 【實施方式】 * 根據一實施例，高溫經黏著研磨劑包括具有尤其精細微 結構及玻璃質黏著基質之氧化鋁研磨砂粒，氧化鋁研磨砂 粒係分布於玻璃質黏著基質中。 首先轉向對氧化紹研磨砂粒之描述，通常氧化铭研磨砂 粒主要由多晶α-氧化鋁形成。多晶α_氧化鋁大體形成砂粒 之主要相，亦即，至少50重量％。然而，大體而言氧化鋁 研磨砂粒為至少60重量。/。、經常至少8〇重量％，且在某些 實施例中至少90重量％之多晶α_氧化鋁。多晶心氧化鋁具 有精細結晶微結構，其特徵可在於α_氧化鋁平均域大小不 大於500 nm。結晶域為微結構之離散、可識別結晶區域， φ 其係由單^曰體積聚所形成，或可由單一晶體所形成。然 而，根據某些實施例，結晶域為單晶的，且經由掃描電子 顯微鏡分析可容易地觀察到。結晶域大小可為更精細的， ' 諸如不大於400 nm，或不大於3〇〇 nm。在更精細之晶體域 • A小之情況下’通常該等域如上文指出為單晶。該等精細 域可為尤其小的，諸如不大於2〇〇 nm，不大於19〇咖，或 甚至不大於180 nm。值得注意的是，精細結晶域大小在處 理之後係存在於高溫經黏著研磨組份中。尤其值得注意的 是，如經常地，用於形成高溫經黏著研磨劑之方法涉:固 127841.doc 1351334 化玻璃質黏著基質的高溫處理。該高溫處理具有使域成長 之趨勢，其係尤其不理想的《提供進一步細節於下文中。 如上文指出，氧化鋁研磨砂粒進一步包括銷定劑。銷定 劑為與砂粒之CX-氧化鋁微結構無關之材料，且可由分散於 多晶（X-氧儲基質相中之第二相識別。销定劑對於“销定、” 域大體為有效的，藉此防止在用以形成經黏著研磨組份之 燒結及/或高溫處理砂粒期間域過度成長。銷定劑之實例 包括氧化物、碳化物、氮化物及硼化物，以及其與多晶α 氧化鋁基質之反應產物。根據特定實施例，銷定劑包含 矽、硼、鈦、錯及稀土元素中之至少一者之氧化物，及其 與多晶ex-氧化鋁基質之反應產物。一特定銷定劑為氧^匕 錯，其形式大體為Zr02(二氧化錯〜）。氧化錯為尤其適合之 材料，且在多晶α-氧化鋁基質内大體為惰性的，以便與氧 化鋁進行非常有限之反應，藉此保持氧化锆晶體相，通常 為二氧化锆。銷定劑大體以不小於約〇.丨重量％之量（諸 如，不小於約0.5重量％，或不小於！ 〇重量％之量）存在於 氧化鋁研磨砂粒中。將銷定劑之下限選擇為對於防止域過 度成長有效的量。 根據一實施例，銷定劑以不大於4〇重量％之量（諸如，不 大於30重量％，不大於20重量％或甚至不大於1〇重量％之 量）存在於研磨砂粒中。在高溫經黏著研磨劑中，銷定劑 大體被識別為具有不大於5微米，諸如不大於丨微米之微粒 大小。已發現與銷定劑相關聯之精細微粒大小為有用的， 諸如不大於500 nm，或不大於3〇〇 nm，或不大於2〇〇 nm。 127841.doc 1351334 如下文更詳細地描述，在用於形成高溫經黏著研磨組份之 方法的内容中，銷定劑可以固體形式（諸如以次微米彤 式，尤其包括膠狀形式）引入於氧化鋁研磨砂粒中/。'或 者，銷定劑可引入於氧化鋁研磨砂粒或其前驅物中，使得 在高溫熱處理後，銷定劑前驅物即轉化成諸如所要氧化 物、碳化物、氮化物或硼化物之所要結晶相。 用以形成根據本發明之實施例之高溫經黏著研磨劑的處 理大體係以形成氧化鋁研磨砂粒開始。根據一特定實施 例，氧化鋁研磨砂粒係經由一接種方法所形成，其中適當 接種材料係與α-氧化鋁前驅物組合，繼之以熱處理將心氧 化銘前驅物轉化成所氧化㈣。該等晶種可根據仍 4’623,364形成’其中緞燒經接種凝膠氧化銘乾燥前驅物以 形成α-氧化鋁。可（諸如）藉由碾磨進一步處理經煅燒之心 氧化鋁以提供適當高表面積晶種材料。通常，表面積係由 不小於10 m2/g ’通常不小於2〇 m2/g，諸如不小於％ m2/g，或不小於4〇 m2/g之比表面積（SSA)量化。特定實施 例具有不小於50 m2/g之表面積。大體而言，限制表面 積，諸如不大於300 m2/g，諸如不大於250 m2/g 〇 接著將晶種材料與α_氧化鋁前驅物組合，α_氧化鋁前驅 物可呈現為用於轉化成α-氧化鋁之適當形式的鋁質材料之 右干形式中之任一者。該等前驅物材料包括（例如）水合氧 化鋁’包括氧化鋁三水合物（ΑΤΗ)及水鋁礦。如本文所 用，水鋁礦表示氧化鋁水合物，包括通常為Α1203 .Η20且 具有約15%之水含量之礦質水鋁礦，以及具有大於15%(諸 127841.doc •10· 1351334 如㈣至夠之水含量之偽水銘礦。因而，術語“水链礦， 將用於表示具有J5%至38%水含量（諸如15重量％錢重量 %水含量）之氧化紹水合物。應注意，包括偽水銘礦之水紹 鑛具有-特定及可識別之晶體結構，及因此獨特χ射線繞 射圖案，且因而與其他紹質材料（包括其他水合氧化 別開。 通常，（X·氧化銘前驅物（諸如水铭鑛）與接種材料组八， 使得晶種相對於晶種及^氧化紹前驅物之總固體含量以小 於0.2重里/〇之里存在。通常，晶種以小於兀重量％之量， 或通常以不大於20重量％之量存在。 晶種及α-氧化鋁前驅物大體以聚形式組合，其接著（諸 如）藉由添加適當酸或鹼（諸如硝酸）而膠凝。在膠凝之後， ，常乾燥、壓碎凝膠，且使經乾燥材料經過分類篩。可接 著使經分類之固體部分接受具有有限均熱時間之燒結處 理通；ϋ，進饤燒結達一不超過3〇分鐘之時間，諸如不大 於2〇分鐘’不大於15分鐘。根據特定實施例，燒結時間係 特別短的，諸如不大於丨〇分鐘。 根據-特定發展，將銷定劑或銷定劑前驅物添加至含有 晶種及&氧化銘前驅物之懸浮液中。通常，銷定劑或銷定 劑前驅物以基於(X-惫卜奴贵Sfff 軋化鋁刖驅物、晶種及銷定劑或銷定劑 前驅物之經組合固體含量之不大於40重量％的量存在（基於 最終α-氧化㈣'粒中之銷定劑之固體含量所算得大體 而言’銷定劑以基於如上文指出之總固體含量之不小於 0.1重量。/。之量(諸如’不小於約0 5重量。/。，或甚至不小於 127841.doc • 11 · 1351334 約1重量％之量）存在。 此外，根據一特定發展，在高於實現心氧化鋁前驅物轉 化至α-氧化銘所需之溫度的溫度下進行燒結。在某種意義 上，某些實施例要求“過度燒結，，α-氧化鋁前驅物材料。尤 其適合之溫度大體不小於135CTC，諸如不小於1375°c，不 小於1385 C，不小於1395°C或不小於1400°C。在此方面， 應注意，雖然精細微結構化接種α_氧化鋁材料已在此項技 術中开> 成，但通常該等材料係在較低溫度下，經常低於 I35(TC，諸如約130(rc下進行處理。在本文下文提供對利 用銷定劑及過度燒結之組合效應之進一步觀察。 在燒結之後，視情況接著使經分類之研磨砂粒與玻璃質 黏著材料組合，成形成適合之幾何輪廓（例如，磨光輪卜 其輪廓及形狀在經黏著研磨劑技術之内容中係非常值得重 視的。用以完成經黏著研磨組份之處理通常涉及固化溫度 下Us &本文所用’固化溫度表示與玻璃質黏著基 質材料相關聯之材料參數，且大體超過熔融溫度，且特定 言之，黏著材料之玻璃轉度為黏著基質 材料不僅變軟及變得可流動，而且變得可流動至確保完全 濕化及黏著至研磨砂粒之程度的最低溫度。通常，根據本 :之實施例之固化溫度不小於1〇〇〇。。，從而大體指示形成 向溫經黏著研磨劑。 根據以下描述製造特定實例。 實例 實例1 (比較） 127841.doc 1351334 在400 ml耐熱玻璃燒杯中，將自Hamburg以⑽⑽^之
Sasol InC獲得之商標名DISPERAL下的3〇克氧化鋁氫氧化 物（偽水鋁礦）粉末攪拌於61毫升之去離子水（電阻率為2 ΜΩ cm)中。 作為晶種原料，在旋轉窯中於11〇〇 c下煅燒*us 4,623,364中所製備之經接種凝膠氧化紹乾燥前驅物歷時$ 分鐘，以將氧化鋁轉化成具有如由BET方法量測之為15 m2/g至28 m2/g之表面積的α形式。將？2 kg的此α氧化鋁原 料與150 kg的去離子水混合，且將其饋入由 C〇mpany(headqUarters Seib，Germany)製造之水平式珠磨機 (horizontal bead mi丨 1)中。該設備的模 s*LMZ_25。進行 碾磨歷時24小時，其中使漿持續循環經過碾磨機。將如由 Saint-Gobain製造之以大小46之砂粒之大致4〇 “的氧化鋁 研磨劑用作碾磨介質。在碾磨之後，表面積為約75 m2/g » 使用攪拌將以上製備之丨.43克的晶種漿添加至Disperal 之漿中。 在授拌繼續時，接著使用攪拌將7.5克2〇重量％之HN03 /谷液添加至此混合物，所得混合物形成凝膠。 在95 C下乾燥凝膠一整夜，且接著使用木質面杖將其壓 碎。保留穿過30網篩及在45網篩上剩下之砂粒部分。 接著將5克所保留之砂粒置放於氧化鋁舟皿中，且置放 至預熱管式爐（Lindberg Blue M series STF 55433)中以用 於燒結。進行燒結歷時總共5分鐘。 127841.doc 1351334 在3個不同溫度，UOOt、1350 °c及1400t：下燒結試 樣。量測硬度及晶體大小性質。 藉由將1_22克經燒結之砂粒與〇 72克粉末玻璃混合且添 =2滴7.5重量％之聚乙烯醇（pVA)減而製造含有玻璃質黏 著基質之，，·二&結砂粒的經黏著研磨組份。玻璃粉末之組合 物大體為基於二氧化矽的，具有多數二氧化矽組份。典型 二氧化矽含量不小於50重量％，通常不小於6〇重量％，諸 如不小於65重里％。玻璃粉末之額外組份包括氧化物，諸 如氧化鋁、氧化鈉、氧化鎂、氧化鉀、氧化鋰、氧化硼' 氧化鈦、氧化鐵、氧化鈣、其他氧化物及其組合。選擇形 成黏著基質之玻璃粉末的特定組合物以具有如上文詳細論 述之理想高固化溫度及以。接著將混合物置放於125⑽ 不鏽鋼模中，且在1〇,〇〇〇 psi下加壓。接著將所得盤置放 於冷卻馬弗爐（Lindberg type川24)中，且在8小時内加熱 至高達125〇亡，且保持在此溫度歷時4小時，且接著冷卻8 1、時。所得盤經製備為拋光部分，且量測硬度及晶體大 小 0 實例2 此實例說明用以防止不理想晶體成長且提供耐蝕性之 fr02鎖定劑的效應。 如實例1製備研磨砂粒陶瓷體’除了以相對於最終氧化 紹值之0.5重量％ ’相對於最終氧化铭值之1〇重量％，及相 對於最終氧化鋁值之2 〇重量％之位準添加膠狀之外。 Zr02之來源為自Nyac〇i獲得之nyac〇l 2〇 之膠狀以〇2 127841.doc -14- 乙酸穩定化形式。如實合"製備試樣且量測試樣。 實例3 此實例說明用以防止不理想晶體成長且提供耐敍性之 Si02銷定劑的效應。 如實例1製備研磨砂粒陶究體，除了以相對於最終氧化 紹值之0.5重量％，相對於最終氧化結值之ι〇重量％，及相 對於最終氧化减之2.G重量％之位準添加膠狀逆之外。 之來源為自Nyacol Inc，AshIand，ma獲得之财 :狀Si〇2氨穩定化形式。如實⑷製備試樣且量測試樣。 實例4 實例》兒月用以防止不理想晶體成長且 Y203鎖定劑的效應。 注之 如實例1製備研磨砂粒陶咨 竞體’除了以相對於最終氧化 對二=’相對於最終氧化紹值之"重量％，及相 =終氧化紹值之2.0重量%之等效氧化紀位準 乙^^外石肖酸紀之來源來自Alrdich化學藥品。如實 丄I備试樣且量測試樣。 實例5 此實例說明以複合@ — 體之銷疋/抗蝕劑的效應，其包括氧 化鎂》如實例2中添加2 軋 石肖酸鎂溶液來製造㈣二及1重量％之叫〇作為 色標記作為實㈣㈣氧化㈣綱有 物為硝酸始之視覺指示器。所使用之氧化銘前驅 由對4等實例之抛光部分之掃描電子顯微法 127841.doc -15· 1351334 (SEM)里測上文描述之實例的晶體域大小。通常使用 5〇’_X之放大倍率’且在低於燒結溫度⑽π下熱钱刻試 樣歷時5分鐘，且在無統計校正之情況下藉由截距法報告 或獲=晶體域大小。根據本文之實施例’晶體域在高溫下 "¥穩疋的，其可依據晶體穩定性而量化。晶體穩定性 在本文中界定為如下所處的溫度：在該溫度下暴露5分鐘 之後，氧化鋁研磨砂粒經歷由平均域大小量化之不大於 5〇0 nm的有限域成長。本文之實施例具有至少14〇〇t之晶 體穩疋性，諸如至少約1 5 〇 〇 。 除晶體域大小之量化之外，使用若干技術量化腐钱程 度。在形成高溫經黏著研磨劑期間，玻璃質黏著材料基質 具有滲透及與氧化銘砂粒反應之趨勢。該攻擊為非常不理 想的，且可依據硬度而量測。本文中，藉由採取在中心處 及外邊緣附近（自外邊緣大致15至30微米）之較小經燒結體 (:〇·5 mm)的硬度資料來量測硬度。熟知維氏(vickers)微 入方法與5〇〇 g負載一起使用。觀察到，由於陶竟體經 2腐钱，因此隨著較軟相藉由與熔融料鹽玻璃反應而形 Ϊ位邊緣附近之硬度減小。亦藉由以幾百個PP-之位準併有形成經燒結體中之藍色銘酸銘的諸如氧化銘之 有色（標記）來量測腐钱。藉由觀察歸因於與㈣蹿相之反 應的_藍色之衰退’可視覺地監控腐钱之深；。另外 且特別值得注意地，可依據腐敍指標而量化腐姓 標由在1250t下氧仙研磨砂粒暴露 曰 中歷時4小時之㈣渗透之平均深度來表示：本 例展示不大於15微米之腐㈣標，諸如不大於微米= 127841.doc 1351334 表2說明添加劑氧化錯或氧化紀清楚地減小如由硬度之 較佳保持力表明之晶粒與玻璃之反應性。另外，諸如Zr〇2 之添加劑的使用清楚地最小化si〇2至晶粒中之入侵之渗 透’且鑒於熔融玻璃提供更穩定的晶粒。另外，清楚地觀 - 察到，當將氧化鈷添加劑用作顏色指示器時，如由藍色之 保持力所證明，當使用諸如Zr02之添加劑時反應之程度顯 著較低。 φ 根據本文之實施例，已提供尤其理想之精細微結構化高 溫經黏著研磨組份。該等精細微結構化組份顯著優於目前 技術狀態，目前技術狀態大體限於如在118 5,282,875中例 不之中間微結構化高溫經黏著研磨劑，us 5,282,875充其 量不過教示具有600 nm晶體域之微結構及具有35〇 nm或更 大之大小的α-氧化鋁單晶體（參見us 4,744,8〇2，以引用的 方式併入US 5,282,875中）。雖然精細微結構化氧化銘研磨 砂粒已在過去被利用用於游離研磨劑應用，但該等精細微 • 結構化氧化鋁研磨砂粒通常未在高溫經黏著研磨應用之内 合中被利用。已發現該等精細微結構化材料在處理期間溶 解於玻璃質黏著基質材料中，及/或在與該等高溫經黏著 • 力磨劑相Μ之熱處理射β1經歷晶體域過度成長。此清楚 地展示於上文描述之實例1中，其中最初精細微結構化材 料經展示為經歷域過度成長及過度腐蝕。 雖然不希詩任何特定理論㈣，但咸信敎劑之使用 ”研磨办粒之過燒結的組合在諸如高溫使用應用之高温處 理期間得到耐微結構改變的高穩定砂粒。咸信銷定劑:於 127841.d〇i -IS- 在升高溫度下常規觀察到之晶粒成長為有效的，同時咸信 過燒結處理條件賦予顯著改良之抗腐蝕性特徵且進一步增 強銷定劑之銷定效應。如本文描述之較高燒結溫度可導致 藉由晶粒邊界之經改質之結晶的方式更耐腐蝕之晶粒邊界 相，或晶粒邊界體積之均勻分布及/或某些晶粒邊界元素 至基質中之選擇性溶解。過燒結條件亦可以將額外耐蝕性 賦予黏著砂粒中之方式協同地影響銷定劑。無論何種機 制，觀察效應為«的，以根據本文之實施例之高溫經 黏著研磨組份展現穩定腐蝕特徵。 應進一步注意，先前技術接種技術已提及晶粒成長穩定 劑之利用，包括各種氧化穩定劑，以及與經接種溶膠-凝 膠氧化鋁研磨砂粒之燒結常規相關聯之高於130(rc的燒結 溫度。然而，已結合α-氧化鋁材料之大體製造而教示該等 晶粒成長抑制劑及燒結溫度，且已咸信該等精細微結構化 材料在高溫經黏著研磨組份之情形中將亦遭受晶粒過度成 長及/或過度腐蝕。然而，令人驚訝地發現，銷定劑材料 與過燒結條件之組合解決不僅處理期間之晶體域成長及高 溫經黏著研磨劑之使用條件，而且耐蝕性的所標記之不 足。 雖然已以特殊性說明且描述了本發明之實施例，但本發 明不欲限於所展示之細節，此係由於可在以任何方式不脫 離本發明之範疇的情況下進行各種修改及取代。舉例而 言，可提供額外或等效取代物，且可使用額外或等效製造 步驟。因而，對於熟習此項技術者而言，只不過使用常規 127841.doc -19· 1351334 實驗即可使本文揭示之本發明之進一步修改及等效物出 現，且咸信所有該等修改及等效物在由以下申請專利範圍 界定之本發明之範疇内。
127841.doc 20·

Claims (1)

1351334 ,.第㈨6148770號專利申請案(轉） ~一二 . 中文申請專利範圍替換本(10’0年4月）[cc年Z月二·::更)王：.·赛· .十、申請專利範圍： -------- 1 · 一種南溫經黏著研磨劍，其包含： 氧化鋁研磨砂粒；及 玻璃質黏著基質，其中該等氧化鋁研磨砂粒係分布於 該玻璃質黏著基質中，該玻璃質黏著基質具有一不小於 lootrc之固化溫度，其中 該等氧化鋁研磨砂粒包含具有一精細結晶微結構之多 晶α-氧化鋁，其特徵在於一不大於5〇〇 nni之α-氧化鋁平 均域大小，且其中該等氧化鋁研磨砂粒進一步包含銷定 劑’該銷定劑包含一在該多晶α·氧化紹中之分散相。 2. 如凊求項1之高溫經黏著研磨劑，其中該銷定劑為來自 由以下各者組成之群之至少一元素的氧化物：矽、硼、 欽、锆、稀土元素、其與該多晶…氧化鋁之反應產物及 其組合。 3. 如請求項2之高溫經黏著研磨劑，其中該銷定劑包含氧 化锆。 4. 如請求項1之高溫經黏著研磨劑，其中該銷定劑以—不 小於約0.1重量％之量存在於該等氧化鋁研磨砂粒中。 5. 如請求項4之高溫經黏著研磨劑，其中該銷定劑以約〇工 重量％至約20重量。/。之範圍存在於該等氧化鋁研磨砂教 中。 6·如請求項1之高溫經黏著研磨劑，其中該銷定劑具有一 不大於約1微米之平均微粒大小。 7·如請求項1之高溫經黏著研磨劑，其中該等氧化鋁研磨 127841-1000422.doc ⑴ 1334 砂粒具有一不大於400 nm之平均晶體域大小。 8 * ^ δ月求項7之高溫經黏著研磨劑’其中該多晶α-氧化鋁之 域為單晶’且具有一不大於200 nm之平均晶體域大小。 如π求項1之高溫經黏著研磨劑，其中該等氧化鋁研磨 砂粒具有一不大於300 nm之平均晶體域大小及至少14〇〇 C之晶體穩定性，其中晶體穩定性為如下所處之溫度： 在該溫度下暴露5分鐘之後，該等氧化鋁研磨砂粒經歷 由一不大於500 nm之平均域大小所量化之域成長。 1 〇.如凊求項1之高溫經黏著研磨劑，其中該等氧化鋁研磨 砂粒具有一不大於15 μιη之腐蝕指標，其中腐蝕指標為 在U5(TC下該等氧化鋁研磨砂粒暴露於熔融二氧化矽玻 璃中歷時4小時之後Si滲透之平均深度。 11.如凊求項1之高溫經黏著研磨劑，其中該玻璃質黏著基 質具有一不小於11 〇〇°C之固化溫度。 12·如請求項1之高溫經黏著研磨劑，其中該玻璃質黏著基 質具有一不小於約1000°C之玻璃轉移溫度Tg。 13.如請求項i之高溫經黏著研磨劑，其中該平均晶體域大 小不大於300 nm，且該銷定劑包含分散在該多晶〇氧化 鋁中之氧化锆相。 —種形成高溫經黏著研磨劑之方法，其包含： 藉由在一不小於135〇。(：之溫度下熱處理含有銷定劑之 α-氧化鋁前驅物，形成精細結晶微結構〜氧化鋁研磨砂 粒； 使用-玻璃質黏著基質材料形成一含有該等&氧化紹 127841-1000422.doc *2- 1351334 砂粒之成形體；及 在一固化溫度下熱處理該成形體，該固化溫度不小於 1000°C且高於該玻璃質黏著基質材料之熔點，該等氧化 鋁研磨砂粒在熱處理之後具有一不大於300 nm之平均結 晶域大小。 15.如請求項14之方法，其中該α-氧化鋁前驅物在晶種的存 在下進行熱處理。 •-r 12784M000422.doc
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