JP4834809B2 - 溶融酸化アルミニウムを基礎とする球状コランダム粒子並びにその製造方法 - Google Patents

溶融酸化アルミニウムを基礎とする球状コランダム粒子並びにその製造方法 Download PDF

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JP4834809B2
JP4834809B2 JP2008530412A JP2008530412A JP4834809B2 JP 4834809 B2 JP4834809 B2 JP 4834809B2 JP 2008530412 A JP2008530412 A JP 2008530412A JP 2008530412 A JP2008530412 A JP 2008530412A JP 4834809 B2 JP4834809 B2 JP 4834809B2
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アラリ，ジャン−アンドレ
ザクサ，セバスチャン
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Description

本発明は、粒径０．００１〜５ｍｍ、酸化ナトリウムの最大含量０．５重量％及び酸化チタンの最大含量０．５重量％を有する溶融酸化アルミニウムを基礎とする球状コランダム粒子並びにその製造方法に関する。
球状コランダムは既に約７５年前から知られており、かつ約３０年前から大量生産されている。例えば米国特許第１，８７１，７９２号明細書及び米国特許第１，８７１，７９３号明細書には圧縮空気又は蒸気を用いた還元条件下での液状コランダムの注ぎ噴流のブローが記載されている。その場合には約０〜５ｍｍの直径を有するコランダム中空球が生じる。上記米国刊行物には今日なお用いられている製造方法の全ての重要な工程が既に記載されている。
中空球状コランダムは、球の中に閉じ込められた空気領域のために著しくわずかな熱伝導性を示すことからおもに耐火物として使用される。さらに中空球状コランダムは化学的に攻撃的な高温の気体及び液体のための濾材として適用される。
しかしながら中空球状コランダムのほかに、圧力、衝撃及び摩耗に対する高い機械的抵抗性をもつ中実の球も工業的に重要である。
球状コランダムの物理的性質はとりわけ粒度（粒径）、球の壁厚及び球状コランダムを構成する酸化アルミニウム一次結晶のクリスタリットの大きさによって特徴づけられる。適用に応じて実に様々な要求が球状コランダムの性質に課される。例えば過去には、球状コランダムの性質に使用原料の変化、溶融物への添加剤によってかあるいはまた注ぎにおけるプロセス工学的な変化（注ぎ量、注ぎ噴流の操作、空気圧もしくは蒸気圧、ノズル形状等）によって影響を及ぼす数多くの試みが記述されてきた。
ブローによる高密度の酸化アルミニウム球の製造が米国特許第２，２６１，６３９号明細書に記載されており、その際、溶融物への酸化ナトリウム１〜１０％の添加及び引き続いてのブローによって高密度の球が得られる。米国特許第２，３４０，１９４号明細書には溶融物への酸化チタン１〜１．５％の添加が記載されており、この添加によって比較的壁厚の耐圧性中空球が得られる。しかしながら、この方法に従って製造された酸化アルミニウム球には、外来イオン（ナトリウム、チタン）によって汚染されているという欠点がある。このことは特に、この材料が研磨材として使用すべき場合に欠点として現れる可能性がある、というのもこの外来イオンが処理すべき表面との望ましくない反応を生じさせる可能性があるからである。不純物としての酸化ナトリウムの場合にはさらにアルミン酸ナトリウムが生成されるということが加わり、その研磨作用はわずかでしかない。
欧州特許第１１５７０７７号明細書には多結晶砥粒子の製造が記載されており、その場合、液状のコランダムが注ぎ出され、かつその冷却がこの溶融酸化アルミニウムを超音波の使用下に微細な液滴に分散させることによって促進される。その場合には１ｍｍより小さな平均直径を有する高密度の粒子が得られる。粒子が比較的小さく、そのことによってその使用分野が限定されることは別として、この方法は比較的費用を要しかつ超音波の使用は大量生産に適当ではない。
独国特許第６９００５９７５Ｔ２号には球状の酸化アルミニウム粒子が記載されており、その際、微粉砕されたα酸化アルミニウムと粘土の水性懸濁液が噴霧乾燥及び引き続いての熱処理によって凝集粒子へと加工される。球状の酸化アルミニウム粒子のこの製造方法は著しく費用を要しかつ高価な原料を必要とする。
従って、容易に実施可能で効果の大きい方法で製造することができる高密度の酸化アルミニウム球がさらに求められている。
従って本発明の課題は、十分に高密度の酸化アルミニウム球並びに従来技術の欠点を有さないその製造方法を提供することである。
この課題は、請求項１の特徴を有する球状コランダム粒子並びに請求項８又は請求項９の特徴を有する方法によって解決される。本発明の理論のさらなる発展は、従属請求項２〜７の対象である。
意外にも、酸化条件下での酸化ケイ素０．１〜１重量％、又は酸化ケイ素０．２〜０．６％の添加下に電気アーク炉で溶融し、次に溶融酸化アルミニウムを１００ｋｇ／分より少ない注ぎ量で注ぎ出し、かつその注ぎ噴流を圧力３〜１０バール空気を用いてブローする場合に、かさ密度１．５ｋｇ／ｌ〜２．５ｋｇ／ｌを有する直径０．００１〜５ｍｍ、酸化ナトリウムの最大含量０．５重量％、酸化チタンの最大含量同じく０．５重量％、９８重量％より大きな酸化アルミニウム含量を有する酸化アルミニウム球を得ることができることが確認された。
これに比べ市販の中空球状コランダムのかさ密度は０．５〜１．２ｋｇ／ｌである。
液状コランダムのブローの際に空気のみが使用され、かつ水の添加が省略される場合に有利であることがさらに見いだされた。
ＳｉＯ2の添加によって第一に該溶融物の粘度に影響が及ぼされ、その際ＳｉＯ2は融剤として用いられかつＳｉＯ2は該溶融物の粘度を低下させる。さらに、生成物の色も溶融物中のＳｉＯ2含量によって影響が及ぼされることが確認された。ＳｉＯ2含量０．８重量％を有する生成物が純白の外観を有するのに対し、０．５重量％未満のＳｉＯ2含量を有する生成物は顕著な黄色の着色を示す。生成物の密度へのＳｉＯ2の影響はあまり強く示されておらず、おそらく、製造条件がＳｉＯ2の添加で改善された流動性によって改善されかつ従って生成物のより高い密度もまたより高いＳｉＯ2含量の場合に得られることにもっぱら基づいている。
しかしながら、ＳｉＯ2含量は球状コランダムの物理的性質への比較的大きな影響を有すると思われる。例えばＳｉＯ2０．４％の平均的な含量で粒子破壊強度の最大値が得られる。このことは、この条件下で溶融した材料の場合には全細孔容積に対する３μｍ未満の細孔容積のミクロ細孔の比較的高い割合が得られることに起因する可能性がある。均一に分布したミクロ細孔のこの高い割合というよりむしろ大きな細孔のわずかな割合が球状コランダムの相応の強度を生じさせており、この強度は粒子破壊強度の測定によって数値的に表現することができる。
３μｍ未満のミクロ細孔の比容積約０．５％を有する市販の中空球状コランダムに対して、ＳｉＯ2０．４％とともに溶融された本発明による球状コランダムは約４０％の全細孔容積でミクロ細孔の相対的な割合約１３％を達成する。検査の範囲内で、３μｍ未満のミクロ細孔の比容積が粒子破壊強度と相互に関連していることが見いだされた。従って同じ全細孔容積でミクロ細孔の高い割合を有する材料の場合に最大の粒子破壊強度が得られる。
市販の中空球状コランダムと本発明による球状コランダムの違いが特にはっきりとわかるのはデジタル画像解析においてである。図１は約９０％の細孔容積を有する従来の中空球状コランダムの顕微鏡写真を示す。はっきりとこの場合にはこの中空球状コランダムの薄壁であることがわかる。これに対し図２は約４０％の細孔容積を有する本発明による球状コランダムの磨き出し面を示す。この場合には、細孔が球全体にわたってほぼ均一に分布していることがきわめてよくわかる。製造条件に応じて本発明による球状コランダムについての細孔容積は２５〜５０％であり、それに対して従来の球状コランダムの細孔容積は８５〜９５％である。特に際立っているのが高密度の球状コランダムのわずかな比表面積である。例えば球直径に応じて０．００５〜０．０５ｍ2／ｇの比表面積が得られる。これに対し従来の中空球状コランダムの比表面積はおよそ１０％高くかつ０．０５〜０．５ｍ2／ｇの範囲内で変動し、その際、粒径が大きくなるにつれて比表面積は小さくなる。比表面積はＢＥＴに従って計算された。
図１及び図２の像によって、本発明による球状コランダム粒子と従来の球状コランダムとの構造における相違が明確にされる。この相違は物理的な測定方法に基づいて明示することもできる。この測定のための特に適当な方法はその場合にはフォルシュテート社による粒子破壊強度の測定である。この方法は、個々の粒子の大きさ及び形状の分析を伴ったコンピュータ制御された単粒子強度試験である。
装置の主要部分は空気圧式加力装置、精密力覚センサ、ステップモーター並びに組込みカメラ及び照明並びに補助的な観察用カメラを備える特殊顕微鏡である。この測定方法の機能原理は、特定数の粒子がキャリヤテープに載せられ、次にこのキャリヤテープを測定装置が通過することに基づいている。その際に顕微鏡を用いて粒子の大きさ、形状及び位置パラメータが測定され、次にこの粒子は超硬のプランジャ間の厳密に規定された位置に運ばれる。次にここで個々の粒子に、粒子の破壊が起こるまで一定増の力が及ぼされる。この破壊力は検出され、これら粒子についての既に測定したパラメータのリストに追加される。
上記方法に従って従来の球状コランダムについて粒度３６で１〜５Ｎの粒子破壊強度を確認したのに対して、本発明による高密度のコランダム粒子は２０Ｎ以上、特に４０Ｎ以上の粒子破壊強度を示した。
次に本発明をいくつかの選び出された実施例につき説明する。
実施例１〜３．
酸化アルミニウム１０００ｋｇと石英砂各８ｋｇ、４ｋｇないしは１ｋｇとの混合物を直径約１．８ｍ、出力１．２ＭＷ及び電圧１７２Ｖである蓋付きの電気アーク炉（傾注炉）で溶融させた。混合物が完全に液状になると直ちに炉を傾けこの液状のコランダムを注湯口を経て注いだ。注いでいる間に注ぎ噴流を、その先端にノズル及び付加的に圧縮空気供給が備えられた槍形の管から本質的になる送風機を用いてブローし、その際、ノズルは注ぎ噴流に向けられており、圧縮空気が広げられかつ液状のコランダムの注ぎ噴流が分散された。使用した空気圧は８バールであった。このようにして得たコランダム球を底部が水冷される鋼板からなるいわゆるブローチャンバに受けた。そこから該球を空気を用いてブローチャンバにつながった冷却管内に送り込んだ。続いてコランダム球を篩別ステーションに輸送し、その直径に応じて個々の分級物に篩い分けした。次の表１にはこのようにして得られたコランダム球の物理データがまとめられている。比較のため従来の中空球状コランダムを記載する。
Figure 0004834809
表１の実施例からわかるようにＳｉＯ2含量はとりわけ粒度分布及び粒子破壊強度に影響を及ぼす。ＳｉＯ2の含量が高ければ高いほど溶融物はますます希薄になりかつブローにより得られるコランダム粒子はますます微細になる。これに対し、かさ密度及び比表面積は比較的ＳｉＯ2含量に依存していないように思われる。ＳｉＯ2含量へのミクロ細孔の比容積の依存ははっきりとわかり、そのことによって明白に粒子破壊強度も示される。
表１からさらにわかるように、かさ密度及び比表面積は粒度が大きくなるにつれて減少する。際立っているのは粒度分布へのＳｉＯ2の影響である。
例えば本発明による方法に従った高密度の球状コランダムの製造においてＳｉＯ2含量０．８％の場合には粒群０〜０．５ｍｍにおける５０％以上の割合が得られる。
実施例４（ブラスト試験）．
高密度の球状コランダムの重要な使用分野はサンドブラストである。球状コランダムの性能レベルを試験するために、実施例１〜３の材料を市販の通常の研磨材と比較した。その際に次の試験条件を定めた。
鋼板（材料、ＳＴ３７）に研磨材５ｋｇを８ｍｍノズルを使用して圧力４．５バール及び噴射角約６０°で距離２５ｍｍで噴射した。表面積能力、ダスト生成、粒子摩耗、表面粗度並びに表面構造を測定した。
表面積能力は、鋼板ＳＴ３７の１ｍ2を均一にブラストするのに必要とされる研磨材の量によって特徴づけられる。すなわちこの値が低ければ低いほど、少ない研磨材が必要とされかつ研磨材の表面積能力は高いということである。
この試験では粒群０．５〜１ｍｍを使用した。市販の鋼粒子ジルブラスト（登録商標）（ＳｉＯ2３１％＋酸化ジルコニウム６１％、分級物４２５〜５００μｍ）及びソビテック社（ＳＯＶＩＴＥＣ）ガラスビーズ（分級物４２５〜８００μｍ）と比較した。試験の結果は表２にまとめられている。
Figure 0004834809
表２では、本発明による高密度のコランダム球が上記ガラスビーズに匹敵する表面積能力を示すことが示されている。上記ガラスビーズに対する本発明によるコランダム球の利点は、コランダム球が使用される場合には石英含有の健康を害するダストを生じないことに示される。酸化ジルコニウム含有の球に比べ、本発明によるコランダム球はたしかに顕著により大きな摩耗と同時により低い表面積能力を示すが、しかしながら、この場合には本発明によるコランダム球の利点は明らかに低い価格にある。
高密度の球状コランダムのもう１つの利点は、この高密度の本発明による球状コランダムを用いてわずかな凹みと球の跡で特徴づけられる表面の特別な構造化が達成されることに示されており、従ってこの球状コランダムは表面仕上げに好適である。
約９０％の細孔容積を有する従来の中空球状コランダムの顕微鏡写真。 約４０％の細孔容積を有する本発明による球状コランダムの磨き出し面を示す顕微鏡写真。

Claims (9)

  1. 粒径０．００１〜５ｍｍ、酸化ナトリウムの最大含量０．５重量％、酸化チタンの最大含量０．５重量％、及びかさ密度１．５ｋｇ／ｌ〜２．５ｋｇ／ｌを基礎とする球状コランダム粒子において、
    球状コランダムの比表面積（ＢＥＴ）０．００５〜０．０５ｍ 2 ／ｇで、細孔容積が２５〜５０％であることを特徴とする球状コランダム粒子。
  2. プランジャ間に配置された単粒子に破壊が起こるまで一定増の力をかけることで測定される粒子破壊強度が、粒子破壊強度≧２０Ｎを示す
    ことを特徴とする、請求項１記載の球状コランダム粒子。
  3. プランジャ間に配置された単粒子に破壊が起こるまで一定増の力をかけることで測定される粒子破壊強度が、粒子破壊強度≧４０Ｎを示す
    ことを特徴とする、請求項１又は２記載の球状コランダム粒子。
  4. 細孔容積４０％以下、を示すことを特徴とする、請求項１から３のいずれか１項に記載の球状コランダム粒子。
  5. 細孔容積３０％以下、を示すことを特徴とする、請求項１から３のいずれか１項に記載の球状コランダム粒子。
  6. 全細孔容積３０〜４０％に対する３μｍ未満の比細孔容積５％以上、
    を示すことを特徴とする、請求項１から５のいずれか１項に記載の球状コランダム粒子。
  7. 全細孔容積３０〜４０％に対する３μｍ未満の比細孔容積１５％以上、
    を示すことを特徴とする、請求項１から５のいずれか１項に記載の球状コランダム粒子。
  8. ａ）酸化アルミニウムを出発物質の全重量に対して石英砂０．１〜１％、の添加下に電気アーク炉で溶融し、
    ｂ）その溶融物を１００ｋｇ／分以下の注ぎ量で注ぎ出しかつ
    ｃ）その注ぎ噴流を圧縮空気を用いて圧力３〜１０バールでブローすることによる、
    請求項１から７のいずれか１項に記載の、球状コランダム粒子を製造する方法において、
    溶融を酸化条件下に実施する
    ことを特徴とする球状コランダム粒子の製造方法。
  9. ａ）酸化アルミニウムを出発物質の全重量に対して石英砂０．２〜０．６％、の添加下に電気アーク炉で溶融し、
    ｂ）その溶融物を１００ｋｇ／分以下の注ぎ量で注ぎ出しかつ
    ｃ）その注ぎ噴流を圧縮空気を用いて圧力３〜１０バールでブローすることによる、
    請求項１から７のいずれか１項に記載の、球状コランダム粒子を製造する方法において、
    溶融を酸化条件下に実施する
    ことを特徴とする球状コランダム粒子の製造方法。
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BRPI0614845B1 (pt) 2016-12-13
CN101268014A (zh) 2008-09-17
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US7654323B2 (en) 2010-02-02
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WO2007033787A1 (de) 2007-03-29
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