TW200422258A - Method for producing α-alumina powder - Google Patents

Method for producing α-alumina powder Download PDF

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Publication number
TW200422258A
TW200422258A TW093103878A TW93103878A TW200422258A TW 200422258 A TW200422258 A TW 200422258A TW 093103878 A TW093103878 A TW 093103878A TW 93103878 A TW93103878 A TW 93103878A TW 200422258 A TW200422258 A TW 200422258A
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TW
Taiwan
Prior art keywords
aluminum
alumina
producing
item
patent application
Prior art date
Application number
TW093103878A
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English (en)
Inventor
Hajime Maki
Yoshiaki Takeuchi
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Sumitomo Chemical Co
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Publication date
Application filed by Sumitomo Chemical Co filed Critical Sumitomo Chemical Co
Publication of TW200422258A publication Critical patent/TW200422258A/zh

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    • H01B7/00—Insulated conductors or cables characterised by their form
    • H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/6303—Inorganic additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
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    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
    • C01F7/308—Thermal decomposition of nitrates
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    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
    • C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
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  • Condensed Matter Physics & Semiconductors (AREA)
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  • Spectroscopy & Molecular Physics (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Description

200422258 玖、發明說明： 【發明所屬之技術領域】 本發明是有關於一種氧化銘粉末的製造方法。 【先前技術】
α -氧化鋁粉末是一種鋁化合物’其化學式係爲 Α1203，而且其係廣泛用於作爲’例如，生產例如透明管 之燒結體的生材料。氧化鋁粉末需具有高含量的α相 以及相對高的BET特定表面積，如此才容易獲得高強度 的燒結體，且這樣的α-氧化鋁粉末可以較容易的分散在 水中。 已知的生產α-氧化鋁粉末的方法，例如是在一晶種 結晶存在之情況下鍛燒氫氧化銘（Mineralogy Association magazine νο1·19，Νο·1，ρρ·21·41，日本專利申請號(JP_A) 62-128918)。然而，上述之方法難以製得具有高含量相 以及相對高BET特定表面積的氧化鋁粉末。 【發明內容】 本發明之發明人硏發出一種氧化鋁粉末的製造方 法’並且已經可以兀全的完成本發明。 本發明是提出一種α-氧化鋁粉末的製造方法，其包 括在一晶種結晶存在時於攝氏6〇〇度至890度中鍛燒一鋁 rr^cf — ·" 鹽° 【實施方式】 用於本發明之生產方法中的銘鹽包括，例如，一無機 麵’胃如ΤΗίΙ酸纟肖、硫酸、硫__、碳銨氫氧 化物，或是上述之氫氧化物；一有機鋁鹽，例如是草酸鋁、 13150pif.doc/008 4 醋酸鋁、硬脂酸鋁、乳酸鋁以及月桂酸鋁，或是上述之氫 氣化物；而較佳的是無機鋁鹽或是其氫氧化物，更佳的是 硝酸鋁或是其氫氧化物。 晶種結晶之實例包括金屬氧化物，例如是氧化鋁 (Αΐ2〇3)、水鋁石(Α100Η)、氧化鐵(Fe2〇3)、氧化鉻(Cr2〇3) 以及氧化鈦（Ti〇2)。這些晶種結晶可以單獨使用或是兩個 或多個合倂使用。而此晶種結晶較佳的是具有小的平均主 ^頼粒直徑，一般的平均主要顆粒直徑是約〇.〇1微米或更 咼以及0.5微米或更低，而且通常其bet特定表面積是12 m2/g或更高以及150 m2/g或更低。作爲晶種結晶的α _氧 化鋁的製備方法，例如是先預鍛燒氫氧化鋁，其中氫氧化 錦是藉由水解異丙氧基鋁以製得，然後碾磨锻燒的氫氧化 銘，然後再鍛燒氫氧化銘並且再碾磨之，即可製得。而氧 化鐵、氧化鉻以及氧化鈦的製備方式，例如是碾磨一般市 售的產品即可。 晶種結晶的含量通常是1份重量或更多，較佳的是2 份重量或更多，更佳的是4份重量或更多以及24份重量 或更低，其係針對每100份重量的銘鹽總含量而言，且晶 種結晶通常是金屬成分之氧化物。 依據本發明之生產α-氧化鋁粉末的方法，上述之銘 鹽係於晶種結晶#在時鍛燒。 在此生產方法中，晶種結晶較佳的是與上述之錫鹽混 合。而混合方式的進行，例如是，將一銘鹽加入一溶劑中， 以取得一溶液或是一泥漿，之後再將晶種結晶加入。然後 再移除溶劑。若使用上述之方法混合，可以使得晶種，結晶 13150pif.doc/008 5 200422258 均勻的分散在鋁鹽中。 在混合時，晶種結晶在加入至上述的溶劑或泥漿之 前，可能已經分散於一溶劑中。之後，再移除溶劑。 再者，混合的方式亦可以是將晶種結晶加入鋁鹽中， 之後再攪拌此混合物。上述之攪拌動作可以利用一設備來 進行，其例如是一垂直制粒機及韓蘇混合機。在此混合步 驟中，晶種結晶於加入上述之鋁鹽之前可能是分散在一溶 劑中，之後再移除溶劑。 鍛燒步驟的溫度是攝氏600度或更高，較佳的是攝氏 % 700度或更高以及攝氏890度或更低，較佳的是攝氏890 度或更低。鍛燒的步驟一般是在空氣中或是鈍氣（氮氣、 氬氣或類似物）中進行。锻燒步驟可以在有控制局部蒸汽 壓的空氣中進行，例如是在具有局部蒸汽壓600 Pa或更低 的空氣中進行。鍛燒的時間是能使鋁鹽轉換成α -氧化鋁 的時間，因此其係依照鋁鹽生材料的種類及量的不同、後 續會描述到的爐形式、鍛燒溫度及鍛燒大氣壓，而有差異。 一般是約10分鐘或更高以及約24小時或更低。用來鍛燒 的設備必須是可以使鋁鹽在上述之條件中進行鍛燒的設 9 備，其可以是靜態的爐、流體基座爐及類似的爐。這些設 備可以是批次式的或是連續式的。特別的鍛燒爐實例包括 | 箱型電子爐、隧遣Μ、紅外線爐、微波爐、井窯、反射窯、 | 旋轉窯、滾動爐床窯及類似的爐。 藉由鍛燒以製成的α -氧化鋁粉末是爲了獲得高密度 的燒結體。而碾磨之步驟可以利用一介質硏磨機，其例如 是震動硏磨機、球硏磨機或是空氣流硏磨機其例如是噴射 13150pif.doc/008 6 200422258 硏磨機。再者，藉由锻燒以製得的α -氧化銘粉末或是以 上述方法碾磨的α -氧化銘粉末便可以加以分類。 利用本發明之方法所生產的α "氧化銘粉末之ΒΕΤ特 定表面積通常是約13 m2/g或更高’較佳的是約15 m2/g 或更高。另一方面，若α-氧化銘粉末之BET特定表面積 過高，在某些例子中，於水中的分散性會降低’因此 氧化鋁粉末之BET特定表面積較佳的是約30 m2/g或更 低。再者，在α -氧化鋁粉末中，主要的晶相是α相，且 α -比例通常約93%或更高’較佳的是95%或更高。另外’ % α-氧化鋁粉末係爲細緻顆粒型態’且其平均主要顆粒直 徑是約0.05微米或更高以及約1微米或更低。 以本發明之生產方法所製得的α-氧化銘粉末具有高 BET特定表面積以及如上述之高α-比例，因此其可以用 來作爲生產α-氧化鋁燒結體之生材料。而所製得的α-氧 化鋁燒結體適合作爲具有高強度需求的組成構件，例如是 切割工具、生物瓷器以及防彈板。此種α-氧化鋁燒結體 由於其化學穩定性，例如是具有絕佳的抗腐蝕力，因此可 以用來作爲生產半導體元件（例如是晶圓處理器）之設備的 φ 一部份；電子構件(例如是氧感應器）；半透明管(例如是鈉 燈以及金屬鹵素燈）；或是陶瓷過濾器。陶瓷過濾器可以 · 用在移除包含在排出氣體中的固體成分、鋁熔化物的過 ’ 濾、食物的過濾（例如是啤酒）、或是對石油製程所產生的 氣體或一氧化碳、二氧化碳、氮氣、氧氣、氫氣作選擇性 的滲透。 以本發明之方法所生產的α -氧化鋁粉末可以用來作 13150pif.doc/008 7 200422258 爲添加劑、調色劑或是樹脂過濾劑，以改善頭淸洗性質(head cleaning property)以及抗摩擦性，其係藉由力氧化鋁 粉末至應用型態的磁性介質的應用層。氧化鋁粉末還 可以用來作爲硏磨材料，例如將氧化鋁粉末分散在一 介質中（例如是水)以製成泥漿，便可以用於半導體CMP製 程的硏磨以及硬碟基板的硏磨。硏磨帶可以藉由塗佈❹― 氧化鋁粉末於帶狀物的表面上，其係適於硬碟以及磁頭的 精確硏磨。
再者，α -氧化鋁粉末還可以作爲陶瓷的添加物、揉 碎機的內襯的添加物、或是催化媒介物，更可以用來作爲 導電燒結體以及導熱燒結體的材料。 實例 以下之實例係用來詳細說明本發明，但並非用以限定 本發明之範圍。α-氧化鋁粉末之物理性質是依照以下之 方法來量測。 α -比例(％): 利用X-光繞射儀量測繞射光譜，以取得氧化鋁α相 (012)基面的波峰強度Ια(1()2)，以及氧化鋁0相（440)基面 的波峰強度IM44〇y，然後以下列式（1)計算α-比例。 -比例（％) = I α (102)/( I α (102) + I (9 (44G))X 1 〇〇% ( 1 ) BET特定表面積(m2/g): 其係以氮吸附法來判定。 13150pif.doc/008 8 平均主要顆粒直徑(微米）： 在α-氧化鋁粉末之穿透式電子顯微鏡圖片中，沿著 任20個或更多個的各主要顆粒之固定方向量測其最大直 徑，並計算量測値的平均値。 實例1 [製備晶種結晶泥漿] 先水解異丙氧基鋁而取得氫氧化鋁，再將氫氧化鋁預 鍛燒以製得過渡氧化鋁，其主要晶相爲0相且含有3%重 量百分比的α -氧化鋁。之後，上述過渡氧化鋁經噴射硏 磨機磨碎之後，即可取得具有體密度爲0.21 g/cm3之粉末。 將100 g的此粉末置入具有8公升體積的管狀電子爐 (Motoyama K.K·所製造，商標名是”Tubular atmospheric furnace”），並且以1 L/min的流速引入具有攝氏-15度露點 的乾燥空氣（局部水蒸氣壓：165 Pa)至爐中，然後將此粉 末加熱至攝氏1170度，並維持此溫度3小時，儘管需保 持爐內的大氣露點在攝氏-15度。之後再逐漸冷卻，即可 以取得鍛燒氧化鋁物質。之後利用震動硏磨機（硏磨媒介 物：氧化鋁）磨碎此鍛燒氧化鋁物質，以取得α-氧化鋁， 其BET特定表面櫝爲16 m2/g。 將20份重量的α -氧化鋁加入80份重量pH 4的硝酸 中，之後利用塡有2 mm直徑之氧化鋁珠的球硏磨機進行 分散步驟3小時，以取得晶種結晶泥漿。 13150pif.doc/008 9 200422258 [α-氧化鋁粉末之製備] 將357.13克（1莫爾）的硝酸鋁氫氧化物[Α1(Ν〇3)3· 9Η20，由 Wako Pure Chemical Industries，Ltd.製造]溶在純 水中，以取得1000 cm3的硝酸鋁水溶液。然後在100 cm3 的硝酸鋁水溶液中加入2.83克的上述晶種結晶泥漿(Al2〇3 份量：0.566克），之後將此混合物置入旋轉蒸餾器之容器 中。接著，降低此容器中的壓力，並且將此容器以水加熱 至攝氏75度，以移除混合物中的水，而取得粉末。而1〇〇 份重量的粉末中係含有ίο份重量的氧化鋁(ai2o3)晶種結 晶。之後，將此粉末置入一氧化鋁熔化爐中，並且將此氧 化鋁熔化爐係放置在一箱型電子爐中。之後，在攝氏850 度的空氣中鍛燒3小時。而所製得的α -氧化鋁粉末之平 均主要顆粒直徑是96 nm。此α-氧化鋁粉末之α-比例以 及BET特定表面積係列示於表1 ’而此α-氧化鋁粉末之 圖片係如圖1所示。 表1 α -比例 BET特定表面積 (%) _ (m2/g) 實例1 98 15.9 實例2 … 97 13.3 比較例1 99 10.1 實例2 實例2之操作步驟與實例1相似，除了鍛燒的溫度改 13150pif.doc/008 10 200422258 成攝氏890度以外。而所製得之α_氧化鋁粉末之性質係 列示於表1。 比較例1 比較例1之操作步驟與實例1相似，除了锻燒的溫度 改成攝氏925度以外。而所製得之α-氧化鋁粉末之性質 係列示於表1。 實例3 將100克的硝酸鋁氫氧化物[Α1(Ν〇3)3· 9Η20,由Wako Pure Chemical Industries，Ltd·製造]以及 1.5 克的氧化銘利 用硏缽混合以取得一粉末，其中此氧化鋁係於實例1之[製 備晶種結晶泥漿]步驟中所製得’且具有BET特定表面積 16.0 m2/g。而100份重量的粉末係含有1〇份重量的氧化 銘(A1203)晶種結晶。 之後，將此粉末置入一氧化銘熔化爐中’並且將此氧 化鋁熔化爐係放置在一箱型電子爐中。之後，在攝氏870 度的空氣中锻燒3小時。而所製得的a-氧化鋁粉末之平 均主要顆粒直徑是110 nm。此α -氧化鋁粉末之α -比例以 及BET特定表面積係列示於袠2 ° 實例4 實例4之操作步驟與實例3相似，除了鍛燒的溫度改 成攝氏850度以外。而所製得之氧化錦粉末之性質係 列示於表2。 13150pif.doc/008 200422258 表2 α -比例(％) BET特定表面積 (m2/g) 實例3 96 17.4 實例4 97 18.9 比較例2 將未添加晶種結晶之硝酸鋁氫氧化物[ai(no3)3 · 9H2〇，由 Wako Pure Chemical Industries，Ltd·製造]置入一 氧化鋁熔化爐中，並且將此氧化鋁熔化爐係放置在一箱型 電子爐中。之後在攝氏870度的空氣中锻燒3小時。而所 製得之粉末的x_光繞射光譜圖中沒有^相的波峰存在。此 粉末之性質係列示於表3。 比較例3 比較例3之操作步驟與比較例2相似，除了锻燒的溫 度改成攝氏900度以外。而所製得之粉末之性質係列示於 表3。 比較例4 比較例4之操作步驟與比較例2相似，除了鍛燒的溫 度改成攝氏950度以外。而所製得之粉末之性質係列示於 表3。 13150pif.doc/008 12 200422258 比較例5 比較例3之操作步驟與比較例2相似，除了鍛燒的溫 度改成攝氏970度以外。而所製得之粉末之性質係列示於
α _比例(％) BET特定表面積 (m2/g) 比較例2 0 111 比較例3 0 107 比較例4 91 41 比較例5 98 9.9 【圖式簡單說明】 圖1是於實例1中所製得的α-氧化鋁粉末的穿透式 電子顯微鏡圖片。 圖2是於實例1中所製得的α -氧化鋁粉末的X-光繞 射光譜圖。 【圖式標示說明】 Μ j \ \\ 13150pif.doc/008 13

Claims (1)

  1. 200422258 拾、申請專利範圍： 1· 一種α-氧化鋁的製造方法，包括在一晶種結晶存在 時，於攝氏600度至890度中鍛燒一鋁鹽。 2·—種α-氧化鋁的製造方法，包括： 將一銘鹽與一晶種結晶混合以取得一混合物；以及 於攝氏600度至890度中鍛燒該混合物。 3·如申請專利範圍第1項或第2項所述之氧化鋁的 製造方法，其中該鋁鹽至少選自無機鋁鹽、該無機錦鹽之 氫氧化物、有機鋁鹽以及該有機鋁鹽之氫氧化物所組成之 族群其中之一。 4·如申請專利範圍第3項所述之α-氧化鋁的製造方 法，其中該無機鋁鹽至少選自硝酸鋁、硫酸鋁、硫酸銘銨、 碳酸鋁銨氫氧化物所組成之族群其中之一。 5·如申請專利範圍第3項所述之氧化鋁的製造方 法，其中該有機鋁鹽至少選自草酸鋁、醋酸鋁、硬脂酸錫、 乳酸鋁以及月桂酸鋁所組成之族群其中之一。 6·如申請專利範圍第4項所述之α-氧化鋁的製造方 法，其中該無機鋁鹽係爲硝酸鋁。 7·如申請專利範圍第1項或第2項所述之以-氧化鋁的 製造方法，其中該晶種結晶至少選自α -氧化鋁、水鋁石、 氧化鐵、氧化鉻以及氧化鈦組成之族群其中之一。 8·如申請專利範圍第1項或第2項所述之〇： _氧化鋁的 製造方法，其中該晶種結晶之BET特定表面積係爲12m2/g 或更高。 9·如申請專利範圍第8項所述之α-氧化鋁的製造方 13150pif.doc/008 14 200422258 法，其中該晶種結晶之BET特定表面積係爲 m2/g 〇 13150pif.doc/008 15
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