TW590987B - Alumina particles, method for producing the same, composition comprising the same, and alumina slurry for chemical mechanical polishing - Google Patents

Alumina particles, method for producing the same, composition comprising the same, and alumina slurry for chemical mechanical polishing Download PDF

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TW590987B
TW590987B TW89128193A TW89128193A TW590987B TW 590987 B TW590987 B TW 590987B TW 89128193 A TW89128193 A TW 89128193A TW 89128193 A TW89128193 A TW 89128193A TW 590987 B TW590987 B TW 590987B
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Taiwan
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gas
particles
alumina
alumina particles
patent application
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TW89128193A
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Chinese (zh)
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Hisao Kogoi
Jun Tanaka
Hayato Yamaya
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Showa Denko Kk
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Abstract

Alumina particles prepared from aluminum chloride by a vapor phase process, wherein said alumina is amorphous or a transition alumina having a crystal form of any of gamma, delta and theta or a mixture thereof and has an average primary particle diameter of 5 to 100 nm and an average diameter of secondary particles, which are formed by the agglomeration pf primary particles, of 50 to 800 nm.

Description

590987 經濟部智慧財產局員工消費合作社印製 A7 ____ B7_五、發明説明(2 ) 之方法(特開平1 1 — 2 6 8 9 1 1號公報)等亦可同樣 經由液相而合成原料,並且假燒取得過渡氧化鋁之方法。 此外亦有經由氣相法取得過渡氧化鋁之方法。例如於 真空容器內令金屬熔融、氣化,並導入氧化性氛圍氣且取 得超微粒子狀氧化物之方法,和令金屬鋁粉體於含有氧氣 之火焰中蒸發、氧化之方法(特公平5 — 5 3 7 2 2號公 報),將無水氯化鋁等所代表之金屬鹵予以汽化,並於本 生燈火焰中噴出、氧化之方法(特開平8 — 1 9 7 4 1 4 號公報)等月爲熟知。經由此類氣相法所製造之過渡氧化 鋁,比經由液相所生成之過渡氧化鋁,於凝集度更低,或 者接近正球狀形狀之極接近單分散。 近年,半導體基板上之電路的集成度爲有日益變高之 傾向,提高此集成度之方法乃注目於被稱爲C Μ P ( Chemical Mechanical Polishing )之技術。其爲對於基板上 形成電路及經由硏磨令平滑化交互進行使得電路複層化, 提高集成度之技術。供於C Μ P之硏磨流漿爲由氧化性金 屬鹽與界面活性劑等調整液性之水系溶劑,與在其中均勻 懸浮的無機粒子所構成。水系溶劑爲與被硏磨面予以化學 性反應,且無機粒子爲經由機械性的硏磨力而將被硏磨面 之該化合物削取。因此,對於無機粒子所要求者爲有效率 削取適度硬度之化合物,且其不包含令被硏磨面發生刮傷 等原因之粗大粒子和硬度顯著高之粒子。 經由煅燒工程所得之過渡氧化鋁爲包含許多粗大粒子 ,故即使實施強力的粉碎,亦難以令粗大粒子適於C Μ Ρ 本紙張尺度適用中國國家標準(CNS ) Α4規格(210Χ297公釐) (請先閱讀背面之注意事項再填寫本頁) 590987 A7 _B7___ 五、發明説明(3 ) (請先閲讀背面之注意事項再填寫本頁) 硏磨。又,無法迴避粉體煅燒之偏差,且混入硬度高粒子 之可能性高。另一方面,經由氣相法所得之粒子若爲球狀 ,或接近球狀,則與被硏磨面之摩擦力小,使得硏磨力變 小。爲了令硏磨力提高,若令初級粒子或二級粒子變大即 可,但並非爲粉體之特性上,粒度分佈擴大裂開,爲不存 在完全均勻粒徑之粒子。因此,隨著初級粒子或二級粒子 變大而使得含有粗大粒子的或然率飛躍地增大,結果亦令 刮傷的發生頻率增大。於前述特開平8 - 1 9 7 4 1 4號 公報中,雖|3載根據氣相法之煙霧狀氧化鋁,但未並考慮 此些點,且製造方法亦未揭示。 發明之揭示 本發明之目的爲在於提供即使適於C Μ P硏磨用粗粒 之程度亦爲粗大粒子少,且硏磨力亦優良之氧化鋁粒子, 其製造方法,令有該粒子之組成物及硏磨用氧化鋁流漿。 經濟部智慧財產局員工消費合作社印製 本發明者等人致力硏究,結果於氯化鋁做爲原料,並 將其汽化後,以氧化性氣體反應取得氧化鋁之方法中,控 制氣體混合,反應溫度等之製造條件,成功解決上述目的 並且取得氧化鋁粒子。 即,本發明基本上爲由以下之各發明所構成。 (1 ) 一種氧化鋁粒子,其爲由氯化鋁以氣相法所得之氧 化鋁粒子,該氧化鋁之結晶型爲無定型或過渡氧化鋁,且 平均初級粒徑爲5〜1 0 0 n m,初級粒子凝集而成之平 均二級粒徑爲5 0〜8 0 0 n m。 本紙張尺度適用中國國家標準(CNS ) A術Μ 210 X297^ ) 一 590987 A7 ___B7 五、發明説明(4 ) (請先閱讀背面之注意事項再填寫本頁) (2 ) —種氧化鋁粒子,其爲由氯化鋁以氣相法所得之氧 化鋁粒子,該粒子之結晶型爲無定型,r、δ、β之任一 種或其混合型’平均初級粒徑爲5〜1 0 0 n m,初級粒 子Μ集而成之平均一'級松徑爲5 0〜8 0 0 π m。 (3 )如上述(1 )或(2 )記載之氧化鋁粒子,其中大 於45#m之粒子爲0 · 05質量%以下。 (4 ) 一種氧化銘粒子之製造方法,其爲令氯化銘汽化, 並以氧化性氣體予以高溫氧化,製造上述(1 )〜(3 ) 任一項記載之氧化鋁粒子。 (5 )如上述(4 )記載之氧化鋁粒子之製造方法,其爲 於高溫氧化前,將氯化鋁汽化之氣體及氧化性氣體於 5〇0 t:以上預熱。 (6 ) —種氧化鋁粒子之製造方法,其中對反應器導入含 氯化銘之氣體(原料氣體)及氧化性氣體之噴出流速値分 別爲1 0 m /秒以上,且氧化性氣體流速/原料氣體流速 之値爲0 · 2以上且未滿1 〇,且氧化性氣體量爲令氯化 鋁化學計量性地氧化上所必要之氧化性氣體量之1倍以上 經濟部智慧財產局員工消贽合作社印製 〇 (7 )如上述(4 )〜(6 )任一項記載之氧化鋁粒子之 製造方法,其爲於汽化之氯化鋁氣體中含有5〜9 〇體積 %之氯化鋁。 · (8 )如上述(4 )〜(7 )任一項記載之氧化鋁粒子之 製造方法,其中氧化性氣體中之氧氣與水蒸氣之比例爲氧 热0 — 9 0體積% ’水蒸氣1 〇 - 1 〇 〇體積% ,氧氣與 ^紙張尺度適用中國國家標準(〇刚八4規格(21()\297公釐) 一 590987 A7 ___B7 五、發明説明(5 ) 水蒸氣之和爲1 〇〜1 〇 〇體積%。 (請先閱讀背面之注意事項再填寫本頁) (9 )如上述(4 )〜(8 )任一項記載之氧化鋁粒子之 製造方法,其中高溫氧化爲於反應器內之滯留時間1秒鐘 以下進行。 (1 0 ) —種氧化鋁粒子,其爲根據上述(4 )〜(9 ) 任一項記載之氧化鋁粒子之製造方法所取得。 (1 1 ) 一種組成物,其爲含有上述(1 )〜(3 )及( 1〇)任一項記載之氧化鋁粒子。 (1 2 ) —属硏磨用氧化鋁流漿,其爲包含上述(1 )〜 (3 )及(1 〇 )任一項記載之氧化鋁粒子。 本發明之上述及其他目的、效果、特徴及優點可由參 照所附圖面之以下說明所闡明。 圖面之簡單說明 圖1爲不出本發明氧化銘粒子製造中合適使用之裝置 流程之一例的方塊圖。 經濟部智慧財產局員工消費合作社印製 用以實施發明之最佳型態 以下,一邊參照所附圖面一邊詳細說明本發明之一實 施形態。本發明不被此實施形態所限定。 圖1爲示出本發明氧化鋁粒子製造中合適使用之裝置 流程之一例,裝置構成爲由原料供給機1、原料昇華器2 、惰性氣體預熱器3、原料氣體加熱器4、氧化性氣體加 熱器5、反應器6、冷卻器7及製品捕集器8所構成。 本紙張尺度適用中國國家棣準(CNS ) A4規格(210X297公釐) -8- 590987 A7 B7 五、發明説明(6 ) (請先閱讀背面之注意事項再填寫本頁) 首先,說明本發明之氧化鋁粒子之製造槪略。經由原 料供給機1將氯化鋁A供給至原料昇華器2。同時,將惰 性氣體B亦以惰性氣體預熱器3予以預熱後,供給至原料 昇華器2。由原料昇華器2所排出之原料氣體C爲繼續導 入原料氣體加熱器4中。原料昇華器2與原料氣體加熱器 4整體化亦無妨。含有如此加熱之氯化鋁氣體之原料氣體 C爲被導入反應器5。另一方面,氧化性氣體D爲經由氧 化性氣體加熱器6而被加熱,並且導入反應器5。以反應 器5完全將第化鋁氧化後,將冷卻用氣體E大量導入冷卻 器7,令反應被強制性地終了。以袋濾器等之捕集器8予 以捕集,取得製品P。排氣爲被送至排氣處理裝置(未圖 示)。 本發明之氧化鋁粒子爲令原料之氯化鋁汽化,並以氣 相經由氧化性氣體予以氧化所得之氧化鋁,結晶型爲無定 型,r、5、β等之所謂的過渡氧化鋁。 經濟部智慧財產局員工消費合作社印製 此些粒子爲由各種粒徑所構成,其平均初級粒徑爲5 〜1 0 0 n m,初級粒子爲弱凝集,並且形成具有5 〇〜 8 0 0 n m平均粒徑之二級粒子。此處所謂之平均初級粒 徑’爲經由B E T法所測定之比表面積所求出之換算粒徑 ,即,以B E T —點法所測定之比表面積(j I S r 1 6 2 6 )所換算之平均粒徑,所謂平均二級粒徑爲經由 激光部卜勒式粒度測定裝置所得之平均粒徑。以下說明粒 度分布之測定手續。即,於氧化鈦〇 · 〇 5克加入純水 5 0毫升及1 〇 %六偏磷酸蘇打水溶液1 〇 〇微升之流漿 本紙張尺度適用中國國家標準(CNS ) A4規格(210X297公釐)" ' -9- 590987 A7 __B7 __ 五、發明説明(7 ) (請先閱讀背面之注意事項再填寫本頁) 中,照射3分鐘超音波(4 6 K H z、6 5 W )。將此流 漿以激光繞射式粒度分佈測定裝置(株)島津製作所 S A L D — 2 0 0 0 J )測定粒度分佈。由如此測定之粒 度分佈即可計算平均二級粒徑。平均初級粒徑未滿5 n m 、平均二級粒徑未滿5 0 n m則硏磨力不夠充分,而平均 初級粒徑超過1 0 0 n m、平均二級粒徑超過8 0 0 n m ,則令硏磨中的刮傷頻率變高。 經濟部智慧財產局員工消費合作社印製 本發明之氧化鋁粒子爲適於C Μ P硏磨的理由雖未確 定,但推測、初級粒徑或二級粒徑爲適度變大,且形狀爲因 凝集粒而爲複雜形狀,對於提高硏磨速度爲非常有效果。 關於成爲刮傷原因的粒子,則因本發明之氧化鋁爲初級粒 子呈弱凝集形成二級粒子,故平均粒徑若在前述範圍內, 則即使存在粗大粒子,亦可藉由硏磨時的壓力而被輕易崩 散。以儘可能令粗大粒子崩散少者爲佳。例如,於純水 0 · 3公升中加入粉體5 0克,並且令攪拌後以超音波分 散2分鐘之流漿以水中過篩分級時之孔開4 5 // m以上( 大於45//m之粒子)者爲〇 · 〇5質量%以下爲佳。初 級粒子的弱凝集爲根據本發明記載之氣相法所製造之粒子 中所特有的性質。又,因爲本發明之氧化鋁爲無定型,T 、5、0等’故粒子本身之硬度亦比α -氧化鋁粒子低, 難發生刮傷。 如上述,本發明之氧化鋁粒子爲將氯化鋁氣體,以氧 化性氣體予以尚溫氧化而取得。氣化銘氣體之原料氯化銘 (通常爲無水氯化鋁)於常溫下爲粉末,故導入原料昇華 本紙張尺度適用中關家標準(〔剛八4胁(21(^297公釐) ' — -10 - 590987 A7 B7 — — ——— - ------- — 五、發明説明(8 ) 器2中予以氣體化。 (請先閱讀背面之注意事項再填寫本頁) 此時,氯化鋁氣體可經稀釋氣體予以稀釋。稀釋氣體 可選擇不與氯化鋁反應,且不被氧化者。惰性氣體B較佳 使用做爲載體氣體。此惰性氣體B亦可作用爲原料導入時 之密封氣體。惰性氣體B可列舉氮、氨、氬等,但並非限 定於此。惰性氣體B可有效將氯化鋁A氣體化,故在導入 原料昇華器2之前可預先加熱。惰性氣體B的預熱溫度爲 3〇°C以上,較佳爲5 0 °C以上,更佳爲2 0 〇 °C以上。 期望儘可能冷預熱溫度差小者爲佳,但可根據目的粒子之 大小,選擇令預熱溫度差不會超過3 0 0 t之範圍。 於原料昇華器2中導入之惰性氣體量爲A 1 C 1 3 / C A 1 C 1 3 +惰性)爲5〜9 0體積%,較.佳爲5〜8 0體 積% ’更佳爲7〜8 0體積%之範圍。此濃度爲與生產性 具有密切關係,且亦爲氧化鋁初級粒徑粒子爲控制因子。 即’氯化鋁(A 1 C 1 3 )之濃度若爲5〜9 0體積%以上 ,則發生許多均勻核,又,因爲反應性變高,故難形成經 由C V D支配所成長之粒子,取得粒度分佈窄之粒子。 經濟部智慧財產局員工消費合作社印製 其次,將亦可含有惰性氣體之氯化鋁氣體,即,原料 氣體C爲被導入與原料昇華器2連接之原料氣體加熱器4 並且加熱。加熱爲使用玻璃和陶瓷製加熱器等。更且,若 於此原料氣體加熱器4內充塡傳熱媒體,則可更有效對於 胃# m體C推進傳熱。傳熱媒體以陶瓷和玻璃等之耐熱材 料:,特別以石英玻璃和氧化鋁陶瓷等爲合適。形狀爲考慮 傳熱效率且以圓丨哀、篩環、蜂巢型、拉西環等爲佳。充塡 本紙張尺度適用中國國家棣準(CNS ) A4規格(210X297公釐) -11 - 590987 A7 B7 五、發明説明(1〇) 〇· 2 ,則反應器5內之氣體流量顯著偏低,並於反應器 5之壁面和捕集器8等中發生,附著氯化鋁,並且引起反 應器5和捕集器8之阻塞,製品污染。又,爲1 〇以上則 原料氣體之流速和氧化性氣體之流速平衡差,故於噴出流 速小之原料氣體之管嘴側,流速大之氧化性氣體回流,並 於此管嘴附近反應發生鍋垢,且引起管嘴堵塞。 同時,令各氣體的噴出流速爲1 〇 m /秒以上,較佳 爲2 0〜2〇〇m/秒、更佳3 0〜1 5 0m/秒,且氧 化性氣體爲,令氯化鋁氧化所必要之化學計量性份量之1倍 以上,較佳爲1〜1 0倍,更佳爲1〜4倍。尙,氣體流 速爲由流量和.溫度,管嘴噴出面積計算。 原料氣體C與氧化性氣體D爲被導入反應器5中,各 氣體組成及兩者份量比例若爲在上述範圍內,則氣體導入 方式即使爲並流、同流、直交流、斜交流等任何型態均可 迅速進行氧化,而較佳爲導入用之噴出口爲中心部使用原 料氣體、外側爲使用氧化性氣體之同軸雙套管管嘴之同軸 並流方式。 又,於防止氯化鋁對於製品之污染目的下,任何情況 均令氧化性氣體D之份量不低於將氯化鋁氧化所必要之化 學計量份量。 關於反應器5爲由反應器5中導入之氣體流量,將氧 化反應後之生成氣體量換算成標準狀態而算出’並將其除 以反應器5之容積之反應器滯留時間較佳爲1秒鐘以下, 更佳爲0 · 1秒鐘以下,特佳爲以〇 · 0 7秒鐘以下決定 本紙張尺度適用中國國家標準(CNS ) A4規格(21〇><297公嫠) (請先閱讀背面之注意事項再填寫本頁) 、tr 線 經濟部智慧財產局員工消費合作社印製 -13- 590987 A7 B7 五、發明説明(μ ) 反應器的大小。滯留時間爲與氧化鋁粒子,即二級粒徑具 有密切關係,故改變滯留時間則令適當之粒度變化,若超 過1秒鐘則二級粒徑變大,令粗大粒子增加故爲不佳'。 本發明所使用之反應器5的形狀爲任意,但由抑制鍋 垢附著等之方面而言,以圓柱狀爲有利。其材質可由進行 氯化鋁氣體之氧化反應時的耐熱、氧化性氣體氛圍之耐蝕 性等而決定。較佳之材質爲金屬鈦、黑鉛(水冷)、石英 玻璃等。氯化鋁氣體之氧化反應爲於高溫之反應器5內進 行。 先: 於本發明中,反應管內所導入之氣體於反應管內的流 速,爲了令氣體之混合爲完全進行,乃以流速大者爲佳, 特別以平均流速5 m /秒以上爲佳。反應管內之氣體流速 若爲5 m /秒以上,則可充分進行反應管內之混合,且 C V D支配所成長之粒子之發生少,不會生成粒度分佈廣 的粒子。 氧化反應後爲了控制二級粒徑,必須予以急冷。具體 而言,於反應器5連接冷卻器7,並將反應後之氣體導入 冷卻器7,且於此導入冷卻用氣體E,並且將水予以噴霧 等之方法。冷卻用氣體E可採用空氣、氮氣等,且冷卻器 7之平均氣體溫度爲1 0 0 °C以上且4 5 0 t以下,較佳 爲1 0 0 °C以上且4 0 0 °C以上,更佳爲1 0 0 t:以上且 3 5 0 °C以下吹入冷卻氣體。此溫度若愈低則愈佳,但需 要大量之冷卻用氣體’且在防止氣體中之水分結露之目的 下,可爲上述之溫度區域。如此停止粒子成長之氧化鋁, 本紙張尺度適用中國國家標準(CNS ) A4規格(210X297公釐) (請先閱讀背面之注意事項再填寫本頁) 、11 線 經濟部智慧財產局員工消費合作社印製 -14 - 590987 A7 B7 五、發明説明(12) (請先閲讀背面之注意事項再填寫本頁) 爲以袋濾器等之捕集器8予以捕集。同時排氣爲由捕集器 8中排出並且被送至排氣處理裝置.(未圖示)。尙,氧化 鋁之初級粒徑、二級粒徑可由改變噴出時之原料氣體C、 氧化性氣體D之溫度、原料氣體濃度、反應器滯留時間、 噴出流速等而加以控制。 以袋濾器等捕集器8所捕集之氧化鋁亦可經由加熱而 減低氯(C 1 )。其可使用電爐、外熱式旋轉審等。此時 ,加熱溫度爲1 5 0 °C〜8 5 0 °C,較佳爲1 5 0 °C〜 5 5〇°C,更隹爲2〇0 °C〜5 0 〇 °C。加熱溫度若未滿 1 5 0 °C,則無法充分除去氯,若爲8 5 0 °C以上,則因 製品氧化鋁之品質降低,故爲不佳。 經由採用以上的製造條件及裝置構造.,則可連續取得 初級粒徑爲5 n m以上且1 〇 〇 n m以下,二級粒徑爲 5 0 n m以上且8 0 0 n m以下,過渡氧化鋁,特別爲無 定型、r、(5、或Θ之氧化鋁粒子。 經濟部智慧財產局員工消費合作社印製 將此氧化銘粒子分散於水中,並依據公知方法加入 P Η調整劑、硏磨促進劑等,則可作成半導體基板等之硏 磨中合適的硏磨用流漿。又,可將氧化鋁粒子與有機溶劑 (例如,醇類、酮類等)等混合作成組成物,並將其利用 做爲紙等之塗佈劑亦可。 實施例 ’使用實施例,及比較例說明本發明,但本發明並非僅 限定於此些實施例。 本紙張尺度適用中關家標準(CNS ) Α4規格(21GX297公釐)"— -15- 590987 經濟部智慧財產局員工消費合作社印製 A7 B7_五、發明説明(13) 硏磨之評價 1 )硏磨方法 硏磨流漿爲使用將硝酸鐵9水合物(關東化學公司製 、試藥特級)3 · 5質量%溶解於水後’令氧化鋁2質量 %於該水溶液中均勻分散。硏磨性能爲以硏磨速率和選擇 比,損傷予以評價。所謂選擇比爲指欲硏磨之鎢等金屬的 硏磨速率、與未硏磨者爲佳之絕緣膜的硏磨速率之比。此 比大者則金,爲被硏磨且絕緣膜爲未被硏磨,故做爲硏磨 流漿之性能優良。 2)硏磨速率之評價 硏磨速率之評價爲以下列要領實施。將直徑2 0 m m 、厚度5 m m之鎢板(純度9 9 · 9質量% ) 5枚貼附於 直徑1 1 0mm、厚度5mm之玻璃製基板,作成被硏磨 材料。所使用之硏磨熱爲二層類型的半導體裝置硏磨用熱 (Rodel Nita(株)製I C 1〇〇〇/ Suba 4 0〇)。硏磨 機爲使用九本工業(株)製7941 — 338型、定盤徑 3 2 0 m m之單面拋光機。硏磨條件爲6 0 r p m、加工 壓力3 9 · 2 k P a、硏磨流漿供給速度1 〇 m 1 / m i η。於此條件硏磨1 5分鐘後,由被硏磨材料 之重量變化將硏磨速率換算成厚度而算出。 3 )選擇比之評價 本紙張尺度適用中關家標準(CNS ) Α4規格(210X297公釐) " -16- (请先閱讀背面之注意事項再填寫本頁) 訂 590987 A7 B7 五、發明説明(彳4) (請先閲讀背面之注意事項再填寫本頁) 選擇比之評價爲將矽基板上所形成之熱氧化膜硏磨’ 並由此硏磨速率與前述鎢板之硏磨速率而算出。以直徑6 吋,厚度6 2 5 // m矽晶圓上形成之熱氧化膜做爲被硏磨 材料,且硏磨墊爲二層類型之半導體裝置硏磨用墊(Rodel Nita(株)製I C 10〇〇/Suba 4 0 0 )。硏磨機爲使用 Speedfam (株)製SH— 24型、定盤徑320mm之半 導體裝置硏磨用單面拋光機。硏磨條件爲3 0 r p m、加 工壓力力3 9 · 2 k P a、硏磨流漿供給速度1 0 m 1 / m i η。於此條件硏磨1分鐘後,以光干涉式膜厚 測定裝置算出硏磨速率。 4)損傷之評價 損傷之評價爲以微分干涉顯微鏡觀察(5 0倍)下’ 測定每1 0視野之損傷個數’並以5階段評價。評價基準 爲如下: 1 :損傷0〜1個 2 :損傷2〜1 0個 經濟部智慧財產局員工消費合作社印製 3 :損傷1 〇〜5 0個 4:損傷5〇〜1〇〇個 5 :損傷1 0 0個以上 〔實施例1〕 以5 0 0°C加熱之氮氣9 · 4Nm3/hr (Ν爲意指 標準狀態)做爲載體氣體,並將無水氯化鋁5 1 本紙張尺度逋用中國國家標準(CNS ) A4規格(210X297公釐) ._ 一 590987 A7 B7 五、發明説明(15 ) (請先閲讀背面之注意事項再填寫本頁) k g/h r供給至原料昇華器。昇華器中所排出之含氯化 鋁氣體之氣體爲被導入加熱器中。此加熱器爲充塡外熱式 之矽石塊。此處所得之原料氣體溫度爲對於反應器之噴出 口爲850 °C ’原料濃度爲48體積%、噴出速度爲83 m /秒。 經濟部智慧財產局員工消費合作社印製 另一方面’將水蒸氣9 5體積%、氧氣5體積%之氧 化性氣體計6 8 N m 3 / h r以外熱式加熱器予以加熱。加 熱器爲充塡以矽石塊。藉其所加熱之氧化性氣體溫度爲對 於反應器之、噴出口爲85〇t:,噴出速度爲34m /秒。 兩氣體之噴出型態爲雙套管同軸並行流,氧化性氣體流速 /原料氣體流速之値爲0·41。反應器中之平均滞留時 間爲0 · 3秒,於反應器出口之正後方吹入室溫空氣,則 可令氣體溫度爲3 0 0 °C以下。其後,於袋濾器中所捕集 之氧化鋁爲平均初級粒徑爲4 5 n m、平均二級粒徑爲3 0〇n m之r氧化鋁。此氧化鋁以開孔4 5 // m予以水中 過篩時,篩上爲0 · 0 0 5質量%。使用該氧化鋁,實施 硏磨評價時,鎢之硏磨速率爲7 1 0 0 A / m i η,選擇 比爲5 1 0,損傷之評價爲2。 〔實施例2〕 以5 00 °C加熱之氮氣1 1 · 4Nm3/hr做爲載體 氣體,並將無水氯化鋁4 7 k g / h r供給至原料昇華器 。昇華器中所排出之含氯化鋁氣體之氣體爲被導入加熱器 中。此加熱器爲充塡外熱式之矽石塊。此處所得之原料氣 本紙張尺度適用中國國家標準(CNS〉A4規格(210X297公釐) 590987 A7 B7 經濟部智慧財產局員工消費合作社印製 五、發明説明(16) 體溫度爲對於反應器之噴出口爲8 3 0 °C,原料濃度爲4 1體積%、噴出速度爲7 2m/秒。. 另一方面,將水蒸氣1 0 0體積%之氧化性氣體’計 1 1 8Nm3/h r以外熱式加熱器予以加熱。加熱器爲充 塡以矽石塊。藉其所加熱之氧化性氣體溫度爲對於反應器 之噴出口爲8 3 5 C ’噴出速度爲1 7 9πί /秒。兩氣體 之噴出型態爲雙套管同軸並行流,氧化性氣體流速/原料 氣體流速之値爲2 · 5。反應器中之平均滯留時間爲 〇· 0 4秒j於反應器出口之正後方吹入室溫空氣,則可 令氣體溫度爲3 0 0 °C以下。其後,於袋濾器中所捕集之 氧化鋁爲平均初級粒徑爲3 0 n m、平均二級粒徑爲 1 5 0 n m之r氧化鋁。此氧化銘以開孔.4 5 v m予以水 中過篩時,篩上爲0·002質量%。使用該氧化鋁,實 施硏磨評價時,鎢之硏磨速率爲5 3 0 0 A / m i η,選 擇比爲4 2 0,損傷之評價爲1。 〔實施例3〕 以5 00°C加熱之氮氣1 1 · 4Nm3/h r做爲載體 氣體,並將無水氯化鋁4 7 k g / h r供給至原料昇華器 。昇華器中所排出之含氯化鋁氣體之氣體爲被導入加熱器 中。此加熱器爲充塡外熱式之矽石塊。此處所得之原料氣 體溫度爲對於反應器之噴出口爲8 3 0 °C,原料濃度爲 4 1體積%、噴出速度爲7 2m/秒。 另一方面,將水蒸氣8 0體積%、氧氣2 0體積%之 (請先閲讀背面之注意事項再填寫本頁) 本紙張尺度適用中國國家揉準(CNS ) A4規格(210X297公釐) 590987 A7 B7 五、發明説明(17) 氧化性氣體計1 4 8 N m 3 / h r以外熱式加熱器予以加熱 。加熱器爲充塡以矽石塊。藉其所加熱之氧化性氣體溫度 爲對於反應器之噴出口爲8 3 0 °C,噴出速度爲2 ◦〇 m /秒。兩氣體之噴出型態爲雙套管同軸並行流,氧化性 氣體流速/原料氣體流速之値爲2 · 8。反應器中之平均 滯留時間爲0 · 0 3秒,於反應器出口之正後方吹入室溫 空氣,則可令氣體溫度爲3 0 0 °C以下。其後,於袋濾器 中所捕集之氧化鋁爲平均初級粒徑爲2 0 n m、平均二級 粒徑爲8 0 n m之r氧化鋁。此氧化鋁以開孔4 5 # m予 以水中過篩時,篩上爲0 · 0 0 6質量%。使用該氧化鋁 ,實施硏磨評.價時,鎢之硏磨速率爲5 2 0 0 A/mi η,選擇比爲460,損傷之評價爲2。 〔實施例4〕 以5 0 0 °C加熱之氮氣3 1 Nm3 / hr做爲載體氣體 ,並將無水氯化鋁4 3 k g / h r供給至原料昇華器。昇 華器中所排出之含氯化鋁氣體之氣體爲被導入加熱器中。 此加熱器爲充塡外熱式之矽石塊。此處所得之原料氣體溫 度爲對於反應器之噴出口爲8 0 0°C,原料濃度爲1 9體 積%、噴出速度爲15 0m/秒。 另一方面,將水蒸氣6 0體積%、氧氣4 0體積%之 氧化性氣體計1 1 8 N m 3 / h r以外熱式加熱器予以加熱 。加熱器爲充塡以矽石塊。藉其所加熱之氧化性氣體溫度 爲對於反應器之噴出口爲8 0 〇°C,噴出速度爲9〇 本紙張尺度適用中國國家標準(CNS ) A4規格(210X297公釐) (請先閱讀背面之注意事項再填寫本頁) 訂 經濟部智慧財產局員工消費合作社印製 -20- 590987 A 7 B7 五、發明説明( 18 m /秒。兩氣體之噴出型態爲雙套管同軸並行流,氧化性 氣體流速/原料氣體流速之値爲0 · 6 0。反應器中之平 均滯留時間爲〇 · 〇 2秒,於反應器出口之正後方吹入室 溫空氣,則可令氣體溫度爲3 0 0 °C以下。其後,於袋濾 器中所捕集之氧化鋁爲平均初級粒徑1 5 n m、平均二級 粒徑爲7 0 π m之y氧化錦。此氧化錦以開孔4 5 // m予 以水中過篩時,篩上爲0 · 0 0 3質量%。使用該氧化鋁 ,實施硏磨評價時、,鎢之硏磨速率爲4 0 0 0 A / m i n ,選擇比爲<5 6 0,損傷之評價爲1。 (請先閱讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 〔實施例5〕 以5 0 0 °C加熱之氮氣3 0Nm3/h.r做爲載體氣體 ,並將無水氯化鋁4 5 k g / h r供給至原料昇華器。昇 華器中所排出之含氯化鋁氣體之氣體爲被導入加熱器中。 此加熱器爲充塡外熱式之矽石塊。此處所得之原料氣體溫 度爲對於反應器之噴出口爲8 0 0°C,原料濃度爲2 〇|| 積%、噴出速度爲14 3m/秒。 另一方面,將水蒸氣1 0 0體積%之氧化性氣體 4 5 0 N m 3 / h r以外熱式之氧化性氣體加熱器予以加熱 。氧化性氣體加熱器爲充塡以氧化鋁燒結體之塊。藉其戶斤 加熱之氧化性氣體溫度爲對於反應器之噴出口爲8 8 〇 t ,噴出速度爲1 2 7m/秒。兩氣體之噴出型態爲雙 同軸並行流,氧化性氣體流速/原料氣體流速之値爲 1 · 1。反應器中之平均滯留時間爲0 · 0 1秒,於反應 本紙張尺度適用中國國家標準(CNS ) A4規格(210X297公釐:) -m Γ Μ -21 - 590987 A 7 B7 五、發明説明(19 ) (請先閲讀背面之注意事項再填寫本頁) 器出口之正後方吹入室溫空氣,則可令氣體溫度爲3 0〇 °C以下。其後,於袋濾器中所捕集之氧化鋁爲平均初級粒 徑1 2 n m、平均二級粒徑爲3 0 0 n m之r氧化鋁。此 氧化鋁以開孔4 5 // m予以水中過篩時,篩上爲〇 . 〇〇5質 夏%。於此氧化鋁1 0 〇克中加入聚乙烯醇(1 2H : CULARE股份有限公司製)之4〇質量水溶液9 〇〇克。將 此流漿物以均質混合器(T.K.Robomix:特殊機化工業股份 有限公司製)於1 1 〇 〇 〇 r p m,實施3 0分鐘解碎., 調製塗佈液,將此塗佈液以棒塗器於樹脂塗層紙上塗佈, 乾燥成乾燥後之膜厚爲2 0 // m。乾燥後於塗膜上亦未發 生裂縫等。使用彩色印表機(BJC-645J: Canon股份有限公 司製)於其記錄紙上實施印字試驗時,油墨之吸收性、發 色性均爲非常優良。基材爲以聚對苯二甲酸乙二酯薄膜( 1 0 0 // m :東雷股份有限公司製),並進行同樣之試驗 時,塗膜之透明性亦爲良好。 〔實施例6〕 經濟部智慧財產局員工消资合作社印製 以5 00°C加熱之氮氣1 1 · 4Nm3/hr (N爲意 指標準狀態)做爲載體氣體,並將無水氯化銘4 7 k g / h r供給至原料昇華器。昇華器中所排出之含氯化 鋁氣體之氣體爲被導入加熱器中。此加熱器爲充塡外熱式 之矽石塊。此處所得之原料氣體溫度爲對於反應器之噴出 口爲8 3 0 °C,原料濃度爲4 1體積%、噴出速度爲7 2 m /秒。 本紙張尺度適用中國國家標準(CNS ) A4規格(210/297公釐) -22 - 590987 A7 B7 五、發明説明(21 ) 試驗。鎢之硏磨速率爲4 2 0 0 A / m i η,選擇比爲1 2 0,損傷之評價爲4。 〔比較例2〕 將三羥鋁石之結晶型平均二級粒徑4 0 // m之氫氧化 鋁予以煅燒,取得0氧化鋁。將其以氧化鋁球做爲粉碎媒 體之球磨實施濕式粉碎。將其靜置分級所得之氧化鋁爲平 均初級粒徑3 5 n m、平均二級粒徑1 5 0 0 n m之0氧 化鋁。此氧牝鋁以開孔4 5 # m予以水中過篩時,篩上爲 〇· 8質量%。使用該氧化鋁實施硏磨試驗。鎢之硏磨速 率爲5 1 0 0A/mi η,選擇比爲3 1 0,損傷之評價 爲5 〇 實施例1〜4及比較例1及2之調製條件及所得製品 之性質示於表1 ,且實施例5及6之調製條件及所得製品 之性質示於表2。 (請先閲讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 本紙張尺度適用中關家標準⑽)娜⑺οχ歸们 590987 A7 B7五、發明説明(22 ) 經濟部智慧財產局員工消費合作社印製 比較例2 趙W祕親安^ 3驅。 ^ 6 « ^ « 5¾ | ^ 11 一 μ? 喻龄®茗 蜜_⑴^ ^祕蟀β 比較例1 Iff ^ , Ν龄核幽1 。 動fflf鵾S竭鑛 郜豳与3班Φ 蜜_祕.® _實施例4 -§ ^ 2 § S 〇、〇 22 § 〇 1 〇〇 ^ 0.60 0.02 實施例3 11.4 500 47 41 830 72 g 〇 ^ ^ 〇 OO CN ^ QQ ^ 〇〇 0.03 實施例2 11.4 500 47 ,41 830 ί 72 〇 〇〇 ν〇 σ> i—H ι—Η OO τ—Η un CN 0.04 實施例1 os ^ ^ S ^ ^ 1 0.41 cn ^N □ 33 | 与 fg ή 5 义®赵I 滕& i涵涵g IS滔8艇觸輯g 嫉嫉鲥龚龚聽g 龚_靡蚝晒嫉雙 □ 33 m a$ ^ S is « 勞冢 I ^ h g | _聲f $涵铤 嫉^ w δ輯· 铝链 腾顧Β ^ sg 堠嫉» 祕 氧化性氣體流速)/(原料氣體流速)之比 平均滯留時間(秒) (請先閱讀背面之注意事項再填寫本頁)590987 Printed by A7 ____ B7_ of the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs 5. The method of invention description (2) (Japanese Patent Application Laid-Open No. 1 1-2 6 8 9 1 1) can also be used to synthesize raw materials through liquid phase. And the method of obtaining transitional alumina by sintering. There is also a method for obtaining transition alumina by a gas phase method. For example, a method of melting and gasifying a metal in a vacuum container, introducing an oxidizing atmosphere, and obtaining ultrafine particles of oxide, and a method of evaporating and oxidizing metal aluminum powder in a flame containing oxygen (special fair 5 — 5 3 7 2), a method of vaporizing metal halide represented by anhydrous aluminum chloride, etc., and spraying and oxidizing in the flame of a Bunsen burner (Japanese Patent Application Laid-Open No. 8-1 9 7 4 1 4), etc. Month is well known. The transition alumina produced by such a gas phase method has a lower degree of agglomeration than the transition alumina produced through a liquid phase, or is close to a monodisperse with a nearly spherical shape. In recent years, the degree of integration of circuits on semiconductor substrates has tended to become higher and higher. The method of improving this integration has focused on a technology called CMP (Chemical Mechanical Polishing). It is a technology for forming a circuit on a substrate and smoothing interaction through honing to make the circuit layered and improve the integration. The honing slurry for CMP is composed of an aqueous solvent that adjusts liquidity, such as an oxidizing metal salt and a surfactant, and inorganic particles uniformly suspended therein. The water-based solvent reacts chemically with the surface to be honed, and the inorganic particles are removed from the compound to be honed by a mechanical honing force. Therefore, what is required for inorganic particles is to efficiently remove compounds of moderate hardness, and it does not include coarse particles and particles with significantly high hardness that cause scratches on the honing surface. The transition alumina obtained through the calcination process contains many coarse particles, so even if strong crushing is performed, it is difficult to make the coarse particles suitable for C Μ P. This paper applies the Chinese National Standard (CNS) A4 specification (210 × 297 mm) (please Read the precautions on the back before filling this page) 590987 A7 _B7___ V. Description of the invention (3) (Please read the precautions on the back before filling out this page) Honing. In addition, it is impossible to avoid variations in powder calcination, and there is a high possibility of mixing particles with high hardness. On the other hand, if the particles obtained by the gas phase method are spherical or close to spherical, the frictional force with the surface to be honed is small, making the honing force small. In order to increase the honing force, it is sufficient to make the primary particles or secondary particles larger, but it is not a characteristic of the powder. The particle size distribution is enlarged and cracked, and there are no particles with a completely uniform particle size. Therefore, as the primary particles or secondary particles become larger, the probability of containing coarse particles increases dramatically, and as a result, the frequency of scratches also increases. In the aforementioned Japanese Patent Application Laid-Open No. 8-1 9 7 4 1 4, although | 3 contains aerosol-like alumina according to the gas phase method, these points have not been taken into consideration, and the manufacturing method has not been disclosed. DISCLOSURE OF THE INVENTION An object of the present invention is to provide alumina particles having a small number of coarse particles and excellent honing power even if they are suitable for CMP honing coarse particles, and a method for producing the alumina particles. Material and honing alumina slurry. The Consumers' Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs printed the inventors and others committed to research. As a result, aluminum chloride was used as a raw material, and after it was vaporized, the alumina was obtained by oxidizing gas reaction to control the gas mixing. Production conditions such as reaction temperature have successfully solved the above-mentioned object and obtained alumina particles. That is, the present invention is basically composed of the following inventions. (1) An alumina particle, which is an alumina particle obtained from aluminum chloride by a gas phase method, the crystalline form of the alumina is amorphous or transition alumina, and the average primary particle diameter is 5 to 100 nm The average secondary particle size of the primary particles is 50 ~ 800 nm. This paper size applies to the Chinese National Standard (CNS) A 210 × 297 ^) 590987 A7 ___B7 V. Description of the invention (4) (Please read the precautions on the back before filling this page) (2) — a kind of alumina particles, It is alumina particles obtained from aluminum chloride in a gas phase method, the crystal form of the particles is amorphous, and any of r, δ, β or a mixed type thereof has an average primary particle diameter of 5 to 100 nm, The average first-order loose diameter formed by the collection of primary particles M is 50 to 800 π m. (3) The alumina particles according to the above (1) or (2), wherein the particles larger than 45 # m are 0.05 mass% or less. (4) A method for producing oxidized particles, comprising vaporizing chlorinated particles and oxidizing them with an oxidizing gas at a high temperature to produce the alumina particles according to any one of (1) to (3) above. (5) The method for producing alumina particles according to the above (4), in which the gaseous vaporized aluminum chloride and the oxidizing gas are preheated at 50,000 t: before the high-temperature oxidation. (6) — A method for producing alumina particles, wherein the ejection flow rates 导入 of the gas (raw material gas) containing chlorinated gas and the oxidizing gas introduced into the reactor are 10 m / s or more, respectively, and the oxidizing gas flow rate / The flow rate of the raw material gas is 0 · 2 or more and less than 10, and the amount of oxidizing gas is more than double the amount of oxidizing gas necessary for the stoichiometric oxidation of aluminum chloride.贽 Printed by a cooperative 〇 (7) The method for producing alumina particles as described in any one of (4) to (6) above, which comprises 5 to 90% by volume of aluminum chloride in vaporized aluminum chloride gas . (8) The method for producing alumina particles according to any one of (4) to (7) above, wherein the ratio of oxygen to water vapor in the oxidizing gas is oxygen heat 0 to 90% by volume 'water vapor 1 〇- 100 % by volume, oxygen and ^ paper standards are applicable to Chinese national standards (〇 Gangga 4 specifications (21 () \ 297mm) 590987 A7 ___B7 V. Description of the invention (5) The sum of water vapor is 1 〇 ~ 100% by volume. (Please read the precautions on the back before filling this page) (9) The method for producing alumina particles as described in any one of (4) to (8) above, where high temperature oxidation is a reaction The residence time in the device is performed for 1 second or less. (1 0) —Alumina particles obtained by the method for producing alumina particles according to any one of (4) to (9) above. (1 1) A composition containing the alumina particles according to any one of (1) to (3) and (10) above. (1 2) —Alumina slurry for honing, comprising the above (1) ~ Alumina particles according to any one of (3) and (10). The above and other objects, effects, features, and characteristics of the present invention and The points can be clarified by referring to the following description of the drawings. Brief description of the drawings Figure 1 is a block diagram showing an example of a suitable device flow for the production of the oxide particles of the present invention. The best form for implementing the invention is described below in detail with reference to the accompanying drawings. One embodiment of the present invention is described in detail. The present invention is not limited by this embodiment. Fig. 1 shows the production of alumina particles according to the present invention. An example of a suitable device flow, the device is composed of a raw material feeder 1, a raw material sublimator 2, an inert gas preheater 3, a raw material gas heater 4, an oxidizing gas heater 5, a reactor 6, a cooler 7 and Composed of product trap 8. This paper size is applicable to China National Standard (CNS) A4 specification (210X297 mm) -8- 590987 A7 B7 V. Description of the invention (6) (Please read the precautions on the back before filling in this (Page) First, the production strategy of the alumina particles of the present invention will be described. Aluminum chloride A is supplied to the raw material sublimator 2 through the raw material feeder 1. At the same time, the inert gas B is also inert. After the body preheater 3 is preheated, it is supplied to the raw material sublimator 2. The raw material gas C discharged from the raw material sublimator 2 is continuously introduced into the raw material gas heater 4. The raw material sublimer 2 is integrated with the raw material gas heater 4. Anyway. The raw material gas C containing the aluminum chloride gas thus heated is introduced into the reactor 5. On the other hand, the oxidizing gas D is heated through the oxidizing gas heater 6 and is introduced into the reactor 5. After the aluminum oxide is completely oxidized in the vessel 5, a large amount of the cooling gas E is introduced into the cooler 7, so that the reaction is forcibly terminated. The trap 8 is collected by a bag filter or the like to obtain a product P. The exhaust is sent to an exhaust treatment unit (not shown). The alumina particles of the present invention are aluminas obtained by vaporizing aluminum chloride as a raw material and oxidizing them with an oxidizing gas in a gaseous phase. The crystalline form is amorphous so-called transition alumina such as r, 5, and β. These particles printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs are composed of various particle sizes, with an average primary particle size of 5 to 100 nm, the primary particles are weakly agglomerated, and form a particle with a size of 50 to 800 nm Secondary particles of average particle size. The "average primary particle diameter" here is the converted particle diameter determined by the specific surface area measured by the BET method, that is, the converted specific surface area (j IS r 1 6 2 6) measured by the BET point method. The average particle diameter means an average secondary particle diameter, which is an average particle diameter obtained by a laser-based particle size measuring apparatus. The procedure for measuring the particle size distribution is described below. That is, 50 ml of pure water and 100 ml of 100% hexametaphosphate soda aqueous solution are added to 0.05 g of titanium oxide. The paper size is in accordance with Chinese National Standard (CNS) A4 (210X297 mm). " '-9- 590987 A7 __B7 __ 5. In the description of the invention (7) (please read the precautions on the back before filling out this page), irradiate the ultrasonic wave (4 6 KH z, 6 5 W) for 3 minutes. This slurry was measured for particle size distribution using a laser diffraction type particle size distribution measuring device (Shimadzu Corporation S A L D — 20000 J). From the particle size distribution thus measured, the average secondary particle size can be calculated. If the average primary particle size is less than 5 nm and the average secondary particle size is less than 50 nm, the honing force is insufficient, and if the average primary particle size exceeds 100 nm and the average secondary particle size exceeds 800 nm, then The frequency of scratches in honing becomes higher. Although the reason why the alumina particles of the present invention are suitable for CMP honing is printed by the employee's consumer cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs, it is estimated that the primary or secondary particle size is moderately large, and the shape is Aggregating particles into a complex shape is very effective for increasing the honing speed. Regarding particles that cause scratches, the alumina of the present invention is a primary particle that is weakly agglomerated to form secondary particles. Therefore, if the average particle diameter is within the above range, even coarse particles can be produced by honing. Stress is easily dissipated. It is preferred to minimize the disintegration of coarse particles. For example, add 50 grams of powder to 0. 3 liters of pure water, and make the slurry that is dispersed by ultrasound for 2 minutes after stirring, and the pores in the sieving and sieving in water will open more than 4 5 // m (more than 45 // m particles) is preferably 0.05% by mass or less. The weak agglutination of the primary particles is a property unique to the particles produced by the gas phase method described in the present invention. In addition, since the alumina of the present invention is amorphous, T, 5, 0, and the like, the hardness of the particles themselves is also lower than that of α-alumina particles, and scratches are less likely to occur. As described above, the alumina particles of the present invention are obtained by subjecting aluminum chloride gas to high temperature oxidation with an oxidizing gas. The raw material of gasification gas is chloride powder (usually anhydrous aluminum chloride) which is powder at normal temperature. Therefore, the imported materials are sublimated. The paper size is subject to the Zhongguanjia standard ([Gangba 4wuji (21 (^ 297mm) ' — -10-590987 A7 B7 — — ———-------- — V. Description of the invention (8) Gasification in device 2. (Please read the precautions on the back before filling this page) At this time Aluminium chloride gas can be diluted by diluent gas. The diluent gas can be selected not to react with aluminum chloride and is not oxidized. Inert gas B is preferably used as a carrier gas. This inert gas B can also be used as a raw material introduction Sealing gas at the time. Examples of the inert gas B include nitrogen, ammonia, argon, etc., but are not limited thereto. The inert gas B can effectively vaporize aluminum chloride A, so it can be heated in advance before introducing the raw material sublimator 2. The inert gas The preheating temperature of B is 30 ° C or higher, preferably 50 ° C or higher, and more preferably 200 ° C or higher. It is desirable that the temperature difference between preheating is as cold as possible. The size is selected so that the preheating temperature difference does not exceed the range of 300 t. Sublimation of raw materials The amount of inert gas introduced into the vessel 2 is A 1 C 1 3 / CA 1 C 1 3 + inert) is 5 to 90% by volume, more preferably 5 to 80% by volume 'more preferably 7 to 80% by volume %. This concentration is closely related to productivity, and is also the primary particle size of alumina as the control factor. That is, if the concentration of aluminum chloride (A 1 C 1 3) is 5 to 90% by volume or more Many homogeneous nuclei occur, and because the reactivity becomes higher, it is difficult to form particles that grow through CVD control and obtain particles with a narrow particle size distribution. Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs, it may also contain inertia The aluminum chloride gas, that is, the raw material gas C, is introduced into the raw material gas heater 4 connected to the raw material sublimator 2 and heated. The glass and ceramic heaters are used for heating. Moreover, if the raw material gas is heated Filling the heat transfer medium in the device 4 can promote the heat transfer more effectively for the stomach body C. The heat transfer medium is heat-resistant materials such as ceramics and glass: especially quartz glass and alumina ceramics are suitable. The shape is Consider heat transfer efficiency Honeycomb type, Laxihuan, etc. are preferred. The size of this paper is applicable to China National Standard (CNS) A4 (210X297 mm) -11-590987 A7 B7 V. Description of the invention (1〇) 〇 2 The gas flow in the reactor 5 is significantly lower, and it occurs on the wall surface of the reactor 5 and the trap 8 and the like. Aluminum chloride adheres to the reactor 5 and the trap 8 and contaminates the product. Above 10, there is a poor balance between the flow rate of the raw material gas and the flow rate of the oxidizing gas. Therefore, on the nozzle side of the raw material gas with a small flow rate, the oxidizing gas with a large flow rate flows back, and scale occurs near the nozzle, and Causes nozzle clogging. At the same time, the ejection flow rate of each gas is set to 10 m / s or more, preferably 20 to 200 m / s, more preferably 30 to 150 m / s, and the oxidizing gas is aluminum chloride. The stoichiometric amount necessary for the oxidation is more than 1 time, preferably 1 to 10 times, and more preferably 1 to 4 times. Alas, the gas flow rate is calculated from the flow rate and temperature, and the nozzle ejection area. The raw material gas C and the oxidizing gas D are introduced into the reactor 5. If the composition of each gas and the proportion of the two components are within the above range, the gas introduction method may be any of co-current, co-current, direct AC, and oblique AC. Both types can be oxidized quickly, and it is preferable to use a coaxial co-current method with a coaxial double casing nozzle using an oxidizing gas on the outer side of the inlet port for the introduction and the use of a raw material gas at the center. In addition, for the purpose of preventing aluminum chloride from contaminating the product, in any case, the amount of the oxidizing gas D is not less than the chemical amount necessary to oxidize the aluminum chloride. Regarding the reactor 5, the gas flow rate introduced into the reactor 5 is calculated by converting the amount of generated gas after the oxidation reaction into a standard state, and dividing the reactor residence time by the volume of the reactor 5 is preferably 1 second. Less than 0 minutes, more preferably 0. 1 second or less, and particularly preferably 0. 07 seconds or less. This paper size is determined by the Chinese National Standard (CNS) A4 specification (21〇 > < 297 cm). (Please Read the notes on the back before filling out this page), printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs, -13-590987 A7 B7 5. Description of the invention (μ) The size of the reactor. The residence time is closely related to the alumina particles, that is, the secondary particle size, so changing the residence time will change the appropriate particle size. If it exceeds 1 second, the secondary particle size will increase, and coarse particles will increase, so it is not good. . The shape of the reactor 5 used in the present invention is arbitrary, but it is advantageous to have a cylindrical shape in terms of suppressing scale adhesion and the like. The material can be determined by the heat resistance during the oxidation reaction of aluminum chloride gas, and the corrosion resistance of the oxidizing gas atmosphere. The preferred materials are metallic titanium, black lead (water-cooled), quartz glass, and the like. The oxidation reaction of the aluminum chloride gas is performed in the reactor 5 at a high temperature. First: In the present invention, the flow rate of the gas introduced into the reaction tube in the reaction tube is in order to make the mixing of the gas complete, preferably the larger flow rate, especially the average flow rate of 5 m / sec or more. If the flow velocity of the gas in the reaction tube is 5 m / sec or more, the mixing in the reaction tube can be sufficiently performed, and the number of particles grown by CV D domination will be small, and particles with a wide particle size distribution will not be generated. In order to control the secondary particle size after the oxidation reaction, it must be quenched. Specifically, a method in which a cooler 7 is connected to the reactor 5 and a gas after the reaction is introduced into the cooler 7 and a cooling gas E is introduced therein and water is sprayed. The cooling gas E can be air, nitrogen, etc., and the average gas temperature of the cooler 7 is 100 ° C or more and 4 50 ° t or less, preferably 100 ° C or more and 400 ° C or more. More preferably, it is 100 t: the cooling gas is blown in at a temperature of 3 to 50 ° C or more. The lower the temperature, the better, but it needs a large amount of cooling gas' and can be in the above temperature range for the purpose of preventing moisture condensation in the gas. In this way, the alumina used to stop particle growth is applicable to the Chinese National Standard (CNS) A4 size (210X297 mm) (please read the precautions on the back before filling out this page). System-14-590987 A7 B7 V. Description of the invention (12) (Please read the precautions on the back before filling out this page) The traps are collected by the trap 8 such as a bag filter. At the same time, the exhaust gas is discharged from the trap 8 and sent to an exhaust treatment device (not shown). Alas, the primary particle diameter and secondary particle diameter of aluminum oxide can be controlled by changing the temperature of the raw material gas C, the oxidizing gas D, the concentration of the raw material gas, the residence time of the reactor, and the discharge flow rate. The alumina captured by the trap 8 such as a bag filter can also be reduced by heating (C 1). It can use electric furnace, external thermal rotary inspection and so on. At this time, the heating temperature is 150 ° C ~ 850 ° C, preferably 150 ° C ~ 550 ° C, and more preferably 200 ° C ~ 500 ° C. If the heating temperature is less than 150 ° C, chlorine cannot be sufficiently removed, and if it is more than 850 ° C, the quality of the alumina product is reduced, which is not good. By adopting the above manufacturing conditions and device structure, it is possible to continuously obtain a primary particle diameter of 5 nm to 100 nm, a secondary particle diameter of 50 nm to 800 nm, and a transition alumina in particular. Amorphous, r, (5, or Θ) alumina particles. Printed by the Consumers' Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs to disperse the oxide particles in water, and add PΗ regulators, honing accelerators, etc. according to known methods , It can be used as a suitable honing slurry for honing semiconductor substrates, etc. In addition, alumina particles can be mixed with organic solvents (for example, alcohols, ketones, etc.) to form a composition, and can be used as It is also possible to use a coating agent for paper and the like. Examples' The examples and comparative examples are used to illustrate the present invention, but the present invention is not limited to these examples only. This paper standard is applicable to the China Standard (CNS) A4 specification ( 21GX297 mm) — -15- 590987 Printed by the Consumers ’Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs A7 B7_V. Description of Invention (13) Evaluation of Honing 1) Honing Method Hydrate (Kanto Chemical Corporation, the reagent special grade) 3.5% by mass was dissolved in water 'Order 2 mass% of alumina in the aqueous solution is uniformly dispersed. Honing performance is evaluated based on the honing rate and selection ratio and damage. The selection ratio refers to the ratio of the honing rate of a metal such as tungsten to be honed to the honing rate of an insulating film that is preferably not honed. The larger ratio is gold, because it is honing and the insulating film is not honing, so it has excellent performance as a honing slurry. 2) Evaluation of honing rate The evaluation of the honing rate was performed in the following manner. Five tungsten plates (purity: 99. 9% by mass) with a diameter of 20 mm and a thickness of 5 mm were attached to a glass substrate with a diameter of 110 mm and a thickness of 5 mm to form a material to be honed. The honing heat used was a two-layer type semiconductor device honing heat (IC 1000 / Suba 400 by Rodel Nita Co., Ltd.). The honing machine is a single-side polishing machine manufactured by Jiuben Industrial Co., Ltd. Models 7941-338 with a fixed disc diameter of 320 mm. The honing conditions were 60 r p m, processing pressure 39 · 2 k P a, and honing slurry feed rate 10 m 1 / m i η. After 15 minutes of honing under these conditions, the honing rate was converted to the thickness from the change in the weight of the material to be honed and calculated. 3) Evaluation of selection ratio This paper size applies the Zhongguanjia Standard (CNS) A4 specification (210X297mm) " -16- (Please read the precautions on the back before filling this page) Order 590987 A7 B7 V. Description of the invention (彳 4) (Please read the precautions on the back before filling in this page) The selection ratio is evaluated by honing the thermal oxide film formed on the silicon substrate, and thus the honing rate and the honing rate of the aforementioned tungsten plate are Figure it out. A thermal oxide film formed on a silicon wafer with a diameter of 6 inches and a thickness of 6 2 5 // m is used as the material to be honed, and the honing pad is a two-layer type semiconductor device honing pad (manufactured by Rodel Nita Co., Ltd.) IC 100 / Suba 400). The honing machine is a single-sided polishing machine for honing using a SH-24 model manufactured by Speedfam Co., Ltd. and a fixed disc diameter of 320 mm. The honing conditions were 30 r p m, a processing pressure of 39 2 k P a, and a honing slurry feed rate of 10 m 1 / m i η. After honing for 1 minute under these conditions, the honing rate was calculated using an optical interference film thickness measuring device. 4) Evaluation of damage Evaluation of damage was performed by observing (50 times) with a differential interference microscope, and 'the number of damage per 10 fields of view' was measured and evaluated in five stages. The evaluation criteria are as follows: 1: 0 ~ 1 damage 2: 2 ~ 10 damage 2 Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs 3: Damage 1 0 ~ 50 0 4: Damage 5 0 ~ 100 5 : More than 100 damage [Example 1] Nitrogen heated at 500 ° C 9 · 4Nm3 / hr (N means standard state) as carrier gas, and anhydrous aluminum chloride 5 1逋 Use Chinese National Standard (CNS) A4 specification (210X297 mm). _59090 A7 B7 V. Description of the invention (15) (Please read the precautions on the back before filling this page) kg / hr is supplied to the raw material sublimator. The gas containing the aluminum chloride gas discharged from the sublimator is introduced into the heater. This heater is a silica block filled with external heat. The temperature of the raw material gas obtained here was 850 ° C with respect to the ejection port of the reactor, and the raw material concentration was 48% by volume, and the ejection speed was 83 m / sec. Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs. On the other hand, an oxidizing gas meter with a water vapor of 95% by volume and oxygen of 5% by volume is heated by an external heating heater of 6 Nm 3 / hr. The heater is filled with silica blocks. The temperature of the oxidizing gas heated by it was 850,000 t: for the reactor, and the ejection speed was 34 m / s. The ejection pattern of the two gases is a double-pipe coaxial parallel flow, and the ratio between the oxidizing gas flow rate and the raw material gas flow rate is 0.41. The average residence time in the reactor is 0.3 seconds. If room temperature air is blown in immediately behind the reactor outlet, the gas temperature can be lower than 300 ° C. Thereafter, the alumina captured in the bag filter was r alumina having an average primary particle diameter of 45 nm and an average secondary particle diameter of 300 nm. When this alumina was sieved in water with an opening of 4 5 // m, the sieve was 0. 0 05 mass%. When honing evaluation was performed using this alumina, the honing rate of tungsten was 7 1 0 0 A / m i η, the selection ratio was 5 1 0, and the evaluation of damage was 2. [Example 2] Nitrogen gas heated at 1 500 ° C was used as a carrier gas, and anhydrous aluminum chloride 47 g / h r was supplied to a raw material sublimator. The gas containing the aluminum chloride gas discharged from the sublimator is introduced into the heater. This heater is a silica block filled with external heat. The paper size of the raw material gas obtained here applies to Chinese national standards (CNS> A4 size (210X297 mm) 590987 A7 B7 Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs 5. Description of the invention (16) The discharge port is 830 ° C, the raw material concentration is 41% by volume, and the discharge speed is 7 2m / sec .. On the other hand, the water vapor is 100% by volume of oxidizing gas other than 1 1 8Nm3 / hr. The heater is used for heating. The heater is filled with silica blocks. The temperature of the oxidizing gas heated by it is 8 3 5 C for the ejection outlet of the reactor. The ejection speed is 1 7 9πί / second. Two gases The ejection pattern is a double-tube coaxial parallel flow, and the ratio of the oxidizing gas flow rate / the raw material gas flow rate is 2.5. The average residence time in the reactor is 0.4 seconds and it is blown into the chamber directly behind the reactor outlet. Warm air can make the gas temperature below 300 ° C. After that, the alumina captured in the bag filter is an average primary particle size of 30 nm and an average secondary particle size of 150 nm. r Alumina. This oxide is sieved in water with an opening of 4 5 vm. On the sieve, it was 0.002% by mass. When honing evaluation was performed using this alumina, the honing rate of tungsten was 5 3 0 0 A / mi η, the selection ratio was 4 2 0, and the evaluation of damage was 1. [Example 3] Nitrogen heated at 500 ° C 1 1 · 4 Nm3 / hr was used as the carrier gas, and anhydrous aluminum chloride 47 kg / hr was supplied to the raw material sublimator. The chlorinated gas discharged from the sublimator The gas of aluminum gas is introduced into the heater. This heater is a silica block filled with external heat. The temperature of the raw material gas obtained here is 8 3 0 ° C for the reactor outlet, and the raw material concentration is 4 1% by volume, and the ejection speed is 72m / s. On the other hand, the water vapor is 80% by volume and the oxygen is 20% by volume (please read the precautions on the back before filling this page). Standard (CNS) A4 (210X297 mm) 590987 A7 B7 V. Description of the invention (17) Oxidizing gas meter 1 4 8 N m 3 / hr for heating by an external heat type heater. The heater is filled with silica blocks The temperature of the oxidizing gas heated by it is 8 30 ° C for the ejection outlet of the reactor, and the ejection speed 2 ◦0m / sec. The discharge pattern of the two gases is a double-pipe coaxial parallel flow, and the ratio of the oxidizing gas flow rate / feedstock gas flow rate is 2 · 8. The average residence time in the reactor is 0 · 0 3 seconds, Injecting room-temperature air directly behind the reactor outlet can make the gas temperature below 300 ° C. After that, the alumina captured in the bag filter has an average primary particle diameter of 20 nm and an average of two Grade alumina is 80 nm. When this alumina was sieved with 4 5 # m openings in water, the sieve was 0. 06 mass%. When this alumina was used for honing evaluation, the honing rate of tungsten was 5 2 0 A / mi η, the selection ratio was 460, and the evaluation of damage was 2. [Example 4] Nitrogen 3, 1 Nm3 / hr heated at 500 ° C was used as a carrier gas, and anhydrous aluminum chloride 4 3 g / h r was supplied to a raw material sublimator. The gas containing the aluminum chloride gas discharged from the sublimator is introduced into the heater. This heater is a silica block filled with external heat. The temperature of the raw material gas obtained here was 800 ° C for the ejection outlet of the reactor, the raw material concentration was 19% by volume, and the ejection speed was 150 m / s. On the other hand, an oxidizing gas with 60% by volume of water vapor and 40% by volume of oxygen was heated to 1 8 N m 3 / h r by an external heating heater. The heater is filled with silica blocks. The temperature of the oxidizing gas heated by it is 800 ° C for the ejection outlet of the reactor, and the ejection speed is 90. This paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm) (please read the back first) Note for re-filling this page) Order printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs -20- 590987 A 7 B7 V. Description of the invention (18 m / s. The two gas ejection patterns are dual-tube coaxial parallel flow, The ratio of the flow rate of the oxidizing gas / the flow rate of the raw material gas is 0. 60. The average residence time in the reactor is 0.22 seconds. If room temperature air is blown directly behind the reactor outlet, the gas temperature can be 30 Below 0 ° C. After that, the alumina captured in the bag filter is a y oxide bromide with an average primary particle size of 15 nm and an average secondary particle size of 7 0 π m. This oxide bromide has openings 4 5 // m when sieved in water, the sieve is 0. 0 0 3 mass%. When honing evaluation is performed using this alumina, the honing rate of tungsten is 4 0 0 0 A / min, and the selection ratio is < 5 6 0, the damage evaluation is 1. (Please read the precautions on the back before filling in this ) Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs [Example 5] Nitrogen heated at 500 ° C 30 Nm3 / hr as the carrier gas, and anhydrous aluminum chloride 4 5 kg / hr is supplied to the raw material sublimator The gas containing the aluminum chloride gas discharged from the sublimator is introduced into the heater. This heater is an externally-heated silica block. The temperature of the raw material gas obtained here is for the ejection outlet of the reactor as follows: At 80 ° C, the raw material concentration is 2 〇 || volume%, and the ejection speed is 14 3 m / sec. On the other hand, 100% by volume of water vapor is oxidizing gas 4 500 N m 3 / hr. The oxidizing gas heater is used for heating. The oxidizing gas heater is a block filled with an alumina sintered body. The temperature of the oxidizing gas heated by its households is 8 8 0t for the reactor's ejection outlet. The speed is 1 2 7m / sec. The discharge pattern of the two gases is a bi-axial parallel flow, and the ratio of the flow rate of the oxidizing gas / the flow rate of the raw material gas is 1 · 1. The average residence time in the reactor is 0 · 0 1 second. The paper size applies to Chinese National Standard (CNS) A4 (210X29 7mm :) -m Γ Μ -21-590987 A 7 B7 V. Description of the invention (19) (Please read the precautions on the back before filling in this page) Blow in room temperature air directly behind the exit of the device, which can make the gas The temperature is below 300 ° C. Thereafter, the alumina captured in the bag filter is r alumina having an average primary particle diameter of 12 nm and an average secondary particle diameter of 300 nm. When the opening 4 5 // m is sieved in water, the sieve is 0.05% summer quality. To 100 g of this alumina, 900 g of a 40 mass aqueous solution of polyvinyl alcohol (12H: manufactured by CULARE Co., Ltd.) was added. This slurry was disintegrated in a homomixer (TKRobomix: manufactured by Special Machinery Co., Ltd.) at 11,000 rpm for 30 minutes. A coating liquid was prepared, and the coating liquid was mixed with a rod. The applicator is coated on a resin-coated paper and dried to a dry film thickness of 20 / m. There were no cracks on the coating film after drying. When a color printer (BJC-645J: Canon Co., Ltd.) was used to perform a printing test on its recording paper, the ink's absorbency and color development were excellent. When the base material is a polyethylene terephthalate film (100 // m: manufactured by Donglei Co., Ltd.) and the same test is performed, the transparency of the coating film is also good. [Example 6] Printed by the Consumers Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs, heated nitrogen at 1 500 ° C 1 1 · 4 Nm3 / hr (N is the standard state) as the carrier gas, and the anhydrous chloride name 4 7 kg / hr is supplied to the raw material sublimator. The gas containing the aluminum chloride gas discharged from the sublimator is introduced into the heater. This heater is a silica block filled with external heat. The temperature of the raw material gas obtained here was 830 ° C for the ejection port of the reactor, the raw material concentration was 41 vol%, and the ejection speed was 7 2 m / sec. This paper size is applicable to Chinese National Standard (CNS) A4 (210/297 mm) -22-590987 A7 B7 V. Description of Invention (21) Test. The honing rate of tungsten is 4 2 0 0 A / m i η, the selection ratio is 1 2 0, and the evaluation of damage is 4. [Comparative Example 2] Aluminium hydroxide having a crystalline average secondary particle size of 40 0 / m of bayerite was calcined to obtain 0 alumina. This was pulverized by ball milling using alumina balls as a pulverizing medium. The alumina obtained by static classification was 0 aluminum oxide having an average primary particle diameter of 35 nm and an average secondary particle diameter of 15 00 nm. When this oxyaluminum was sieved in water with an opening of 4 5 # m, the sieve was 0.8% by mass. A honing test was performed using this alumina. The honing rate of tungsten is 5 1 0 0 A / mi η, the selection ratio is 3 1 0, and the evaluation of damage is 5 0. The preparation conditions of Examples 1 to 4 and Comparative Examples 1 and 2 and the properties of the obtained products are shown in Table 1. The preparation conditions of Examples 5 and 6 and the properties of the products obtained are shown in Table 2. (Please read the notes on the back before filling in this page) The paper size printed by the Employees' Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs applies the Zhongguanjia standard. Comparative Example 2 Printed by the Property Cooperative Consumer Cooperatives Zhao W. Mysterious ^ 3 drive. ^ 6 «^« 5¾ | ^ 11 One μ? Yuling® 茗 Honey_⑴ ^ ^ 蟀 β Comparative Example 1 Iff ^, ΝAGE nuclear nucleus 1. Dynamic fflf 鵾 S exhaust mine and 3 classes Φ honey_secret. ® _ Example 4-§ 2 2 § S 〇, 〇22 § 〇1 〇〇 ^ 0.60 0.02 Example 3 11.4 500 47 41 830 72 g 〇 ^ ^ OOOO CN ^ QQ ^ 〇〇0.03 Example 2 11.4 500 47, 41 830 ί 72 〇〇〇ν〇σ > i-H ι-Η OO τ-Η un CN 0.04 Example 1 os ^ ^ S ^ ^ 1 0.41 cn ^ N □ 33 | fg 5 5 Yi® Zhao I Teng & i Han Han g IS Tao 8 boat touch g g jealous 鲥 Gong Gong listening g Gong _ oyster sun double □ 33 ma $ ^ S is «Laozuka I ^ hg | _ sound f $ 涵 铤 劲 ^ w δ series · Aluminum Chain Teng Gu Β ^ sg 堠 agger» ratio of average oxidation residence time (secret oxidizing gas flow rate) / (raw material gas flow rate) (seconds) (Please read the notes on the back before filling this page)

本紙張尺度適用中國國家標準(CNS ) A4規格(210X297公釐) -25- 590987 A7 B7 五、發明説明( 23 經濟部智慧財產局員工消費合作社印製 (il)I 撇 CX1 m 鎰 Ϊλ 〇 〇〇 Φ co un 〇 〇 r—Η un 〇 1—( cn VO τ-Η 鎰 ^ ^ S Ο g r-H 寸 寸 辑 ΙΚ {H- ^ R 8 * 05 ο ο S ν〇 r—Η CO 辑 IK ^ ^ g 8 〇 ο CNl Ό s 寸 CN (XI U .^ S § 〇 ο cn ν〇 寸 r—Η τ—Η 舞 U ^ § 1 Ο ,_ _ Η 〇 to CN 1ft Ή 媞 媞 ε s ^ s s 务 起.¾ 曰 到 运 11 3 鵾 < 砍 切 ^ 祕 /—\ 〇C Ιί 1πΐ| )S m ΛΛ Kt m .擊 寒 (請先閲讀背面之注意事項再填寫本頁)This paper size applies to Chinese National Standard (CNS) A4 (210X297 mm) -25- 590987 A7 B7 V. Description of Invention (23 Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs (il) I Excluding CX1 m 镒 Ϊλ 〇〇 〇Φ co un 〇〇r—Η un 〇1— (cn VO τ-Η 镒 ^ ^ S 〇 g rH Inch series IK {H- ^ R 8 * 05 ο ο S ν〇r—Η CO series IK ^ ^ g 8 〇ο CNl Ό s inch CN (XI U. ^ S § 〇ο cn ν〇inch r—Η τ—Η 舞 U ^ § 1 〇, _ _ Η 〇to CN 1ft Ή 媞 媞 ε s ^ ss From ¾ to arrival 11 3 鵾 < 切切 ^ Secret / — \ 〇C Ιί 1πΐ |) S m ΛΛ Kt m. Cold (please read the precautions on the back before filling this page)

本紙張尺度適用中國國家標準(CNS ) A4規格(210X 29<7公釐) -26- 590987 Β7 五、發明説明(24 ) 經濟部智慧財產局員工消費合作社印製 表2 實施例5 實施例6 原料氣體 *.· 氮氣流速(Nm3/hr) 30 11.4 溫度(°C) 500 500 原料流速(kg/hr) 45 47 原料濃度(體積%) 20 41 氣體溫度(反應器噴出口)(°0 ) 800 830 (噴出速度(m/秒) 143 72 氧化性氣體 組成水蒸氣(體積%) 100 100 酵素(體積%) • 0 0 流速(Nm3/hr) 450 118 氣體溫度(對於反應器之噴出n)(°c ) 880 835 噴出速度(m/秒). 127 179 (氧化性氣體流速)/(原料氣體流速)之比 0.1 1.5 平均滯留時間(秒) 0.01 0.04 氧化鋁 結晶型 7 r 平均初級粒徑(nm) , 12 30 平均二級粒徑(nm) 300 150 開孔45 // m水中過篩篩上(質量%) 0.005 0.002 塗佈膜(20 // m)乾燥後之裂縫發生 並 j \ \\ — 油墨吸收性 良好 — 油墨發色性 良好 一 、 與平均粒徑5 0 0 // m之聚丙烯酸鈉做爲 未察見 主成分之吸水性樹脂粉末之混合物(混 樹脂之 合率:〇.3質量%)於3 5 °C,相對濕度90%,24 融粘 小時放置後之性狀 (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(21 O X 297公釐) 590987 A7 B7 五、發明説明(25 ) 產業上之利用領域 本發明之氧化錦粒子爲由初級粒子以弱的凝集力,形 成二級粒徑,爲較低硬度之無定型’或過渡氧化鋁,故不 僅爲C Μ P硏磨用途,且亦可使用於期待配合碎屑效果之 平滑觸感的化粧材料。又,微粒之初級粒子爲適度凝集, 故亦兼具化學物質的吸附力。因此,使用做爲紙和高分子 薄膜等基材之塗佈液時’不會影響基材之色調且爲透明, 油墨吸收性佳,故可取得不會滲出油墨之優良的記錄媒體 。又,亦可適於使用於代替先前的活性氧化鋁。 本發明在不超脫其本質的特徵下,可於其他特定之實 施態樣中實施。因此,本實施形態於所有點中僅爲例示性 的,並非限定性,且本發明範圍爲由上述說明及所附之申 請專利範圍而示出,因此於申請專利範圍之均等範圍中所 有之變更爲被包含於本發明中。 (請先閱讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 本紙張尺度適用中國國家標準(CNS ) Α4規格(210X297公釐) -28-This paper size applies the Chinese National Standard (CNS) A4 specification (210X 29 < 7 mm) -26- 590987 B7 V. Description of the invention (24) Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs 2 Example 5 Example 6 Feed gas *. · Nitrogen flow rate (Nm3 / hr) 30 11.4 Temperature (° C) 500 500 Feed flow rate (kg / hr) 45 47 Feed concentration (vol%) 20 41 Gas temperature (reactor ejection port) (° 0) 800 830 (discharge rate (m / s) 143 72 oxidizing gas composition water vapor (vol%) 100 100 enzyme (vol%) • 0 0 flow rate (Nm3 / hr) 450 118 gas temperature (for ejection n of the reactor) (° c) 880 835 Ejection speed (m / s). 127 179 (oxidizing gas flow rate) / (raw material gas flow rate) ratio 0.1 1.5 Average residence time (seconds) 0.01 0.04 Alumina crystal type 7 r average primary particle size (Nm), 12 30 Average secondary particle size (nm) 300 150 Opening holes 45 // m sieve on water (mass%) 0.005 0.002 Coating film (20 // m) cracks after drying and j \ \\ — Good ink absorption — Good color development of ink I, and average particle size 5 0 0 // m of sodium polyacrylate is a mixture of water-absorbent resin powder with no main component (combined resin ratio: 0.3% by mass) at 35 ° C, 90% relative humidity, and left for 24 hours after melting Later properties (please read the precautions on the back before filling this page) This paper size is applicable to the Chinese National Standard (CNS) A4 specification (21 OX 297 mm) 590987 A7 B7 V. Description of the invention (25) Industrial application fields The oxidized brocade particles of the present invention are formed from primary particles with weak agglutination force to form a secondary particle size, and are amorphous or transition alumina with lower hardness. Therefore, they are not only used for CMP honing, but also can be used in A cosmetic material with a smooth feel that matches the effect of debris is expected. The primary particles of the fine particles are moderately agglomerated, so they also have the ability to absorb chemicals. Therefore, they are used as coating liquids for substrates such as paper and polymer films. It does not affect the hue of the substrate, is transparent, and has good ink absorption, so it can obtain an excellent recording medium that does not bleed out of the ink. It is also suitable for use in place of the previous activated alumina. Detached The essential features can be implemented in other specific implementation forms. Therefore, this embodiment is merely illustrative and not limitative in all points, and the scope of the present invention is defined by the above description and the scope of the attached patent application. It is shown that, therefore, all the changes in the equal scope of the patent application scope are included in the present invention. (Please read the notes on the back before filling out this page) Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs This paper applies the Chinese National Standard (CNS) Α4 specification (210X297 mm) -28-

Claims (1)

590987590987 々、申請專利範圍 第891 281 93號專利申請案 中文申請專利範圍修正本 民國92年9月5日修正 1 · 一種氧化鋁粒子,其爲由氯化鋁以氣相法所得之氧 化鋁粒子,該氧化鋁之結晶型爲無定型或過渡氧化纟g,且平 均初級粒徑爲5〜1 0 0 n m,初級粒子凝集而成之平均二 級粒徑爲5 0〜8 0 0 nm,其中大於4 5 //m之粒子爲 0 . 05質量%以下。 2 · —種氧化錦粒子,其爲由氯化銘以氣相法所得之氧 化鋁粒子,該粒子之結晶型爲無定型,r、5、θ之任一種 或其混合型,平均初級粒徑爲5〜1 0 0 n m,初級粒子凝 集而成之平均二級粒徑爲5 0〜8 0 0 nm, 其中大於4 5 //m之粒子爲0 . 0 5質量%以下。 3 · —種製造如申請專利範圍第1或2項之氧化鋁粒子· 的方法,其中係令氯化鋁汽化,並以氧化性氣體將其高溫氧 化,而於高溫氧化前,係將氯化鋁汽化之氣體及氧化性氣體 於5 0 0 t以上預熱。 4 . 一種製造如申請專利範圍第1或2項之氧化鋁粒子 的方法,其中對反應器導入含氯化鋁之氣體(原料氣體)及 氧化性氣體之噴出流速値分別爲1 0 m/秒以上,且氧化性 氣體流速/原料氣體流速之値爲0 . 2以上而未達_ 1 〇,且 氧化性氣體量爲令氯化鋁化學計量性地氧化上所必要之氧化 性氣體量之1倍以上。 5 ·如申請專利範圍第3項之氧化鋁粒子之製造方法, 本紙張尺度適用中國國家榇準(CNS ) A4規格(210 X 297公釐) (請先閲讀背面之注意事項再填寫本頁) 、τ 經濟部智慧財產局員工消費合作社印製 590987 A8 B8 C8 D8 ----------- 六、申請專利範圍 其中於汽化之氯化鋁氣體中係含有5〜9 0體積%之氯化鋁 〇 6 .如申請專利範圍第4項之氧化鋁粒子之製造方法, (請先閎讀背面之注意事項再填寫本頁) 其中於汽化之氯化鋁氣體中係含有5〜9 0體積%之氯化鋁 〇 7 .如申請專利範圍第3項之氧化鋁粒子之製造方法, 其中氧化性氣體中之氧氣與水蒸氣之比例爲氧氣0 - 9 0體 積%、水蒸氣1 〇 - 1 〇 〇體積%,而氧氣與水蒸氣之和爲 1〇〜1 0〇體積% 〇 8 .如申請專利範圍第4項之氧化鋁粒子之製造方法, 其中氧化性氣體中之氧氣與水蒸氣之比例爲氧氣0 - 9 0體 積%、水蒸氣1 〇 - 1 〇 〇體積%,而氧氣與水蒸氣之和爲 1 0〜1 0 0體積%。 9 .如申請專利範圍第3項之氧化鋁粒子之製造方法, 其中高溫氧化係於反應器內之滯留時間爲1秒鐘以下進行。 1 〇 .如申請專利範圍第4項之氧化鋁粒子之製造方法 ,其中高溫氧化係於反應器內之滯留時間爲1秒鐘以下進行 經濟部智慧財產局員工消費合作社印製 〇 1 1 . 一種化學機械硏磨漿體,其係由氧化金屬鹽、水 係溶劑與均勻懸濁於其中之無機粒子所成者,該無機粒子爲 如申請專利範圍第1或2項之氧化鋁粒子。 本紙張尺度適用中國國家標準(CNS ) A4規格(210X297公釐) -2 -々 Application for Patent Scope No. 891 281 No. 93 Chinese Patent Application for Amendment of the Chinese Patent Amendment on September 5, 1992 1. Alumina particles, which are alumina particles obtained from aluminum chloride by gas phase method, The crystalline form of the alumina is amorphous or transition oxide g, and the average primary particle size is 5 to 100 nm. The average secondary particle size of the agglomerated primary particles is 50 to 800 nm, where 4 5 // m particles are 0.05 mass% or less. 2 · —A kind of oxidized brocade particles, which are alumina particles obtained by the gas phase method from chlorinated amine, the crystal form of the particles is amorphous, any of r, 5, and θ or a mixed type thereof, and the average primary particle diameter It is 5 to 100 nm, and the average secondary particle size of the primary particles is 50 to 800 nm, in which the particles larger than 4 5 // m are 0.5 mass% or less. 3 · A method for manufacturing alumina particles such as those in the scope of patent application No. 1 or 2 · In which aluminum chloride is vaporized and oxidized with an oxidizing gas at high temperature, and before high temperature oxidation, chlorination is performed The vaporized aluminum and oxidizing gas are preheated above 500 t. 4. A method for manufacturing alumina particles such as those in item 1 or 2 of the scope of patent application, wherein the ejection flow rates of the aluminum chloride-containing gas (raw gas) and the oxidizing gas are introduced into the reactor at 10 m / s, respectively. Above, and the ratio of the flow rate of the oxidizing gas / the flow rate of the raw material gas is 0.2 or more and less than -10, and the amount of the oxidizing gas is 1 of the amount of the oxidizing gas necessary for the stoichiometric oxidation of aluminum chloride. Times more. 5 · If the method of manufacturing alumina particles according to item 3 of the scope of patent application, this paper size is applicable to China National Standard (CNS) A4 (210 X 297 mm) (Please read the precautions on the back before filling this page) , Τ printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs 590987 A8 B8 C8 D8 ----------- 6. Scope of Patent Application Among them, the vaporized aluminum chloride gas contains 5 ~ 90% by volume Aluminium chloride 〇6. If the method of manufacturing alumina particles according to item 4 of the patent application, (please read the precautions on the back before filling this page) where the vaporized aluminum chloride gas contains 5 ~ 9 0% by volume of aluminum chloride 0. The method for manufacturing alumina particles according to item 3 of the patent application, wherein the ratio of oxygen to water vapor in the oxidizing gas is 0 to 90% by volume of oxygen and 1% of water vapor. -100% by volume, and the sum of oxygen and water vapor is 10 ~ 100% by volume. 8) The method for manufacturing alumina particles according to item 4 of the patent application, wherein oxygen and water in the oxidizing gas The proportion of steam is 0-90% by volume Steam 1 billion --1 billion billion vol%, while the oxygen and steam to a sum 0~1 00% by volume. 9. The method for producing alumina particles according to item 3 of the scope of patent application, wherein the residence time of the high temperature oxidation in the reactor is 1 second or less. 1 〇. The manufacturing method of alumina particles according to item 4 of the scope of patent application, wherein the residence time of the high-temperature oxidation system in the reactor is less than 1 second and printed by the Consumer Cooperative of Intellectual Property Bureau of the Ministry of Economic Affairs A chemical-mechanical honing slurry is formed by oxidizing a metal salt, an aqueous solvent, and inorganic particles uniformly suspended therein. The inorganic particles are alumina particles such as those in the first or second scope of the patent application. This paper size applies to China National Standard (CNS) A4 (210X297 mm) -2-
TW89128193A 1999-12-27 2000-12-27 Alumina particles, method for producing the same, composition comprising the same, and alumina slurry for chemical mechanical polishing TW590987B (en)

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