JP2017520678A - 実質的に球状の金属粉末の製造 - Google Patents
実質的に球状の金属粉末の製造 Download PDFInfo
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- JP2017520678A JP2017520678A JP2016567400A JP2016567400A JP2017520678A JP 2017520678 A JP2017520678 A JP 2017520678A JP 2016567400 A JP2016567400 A JP 2016567400A JP 2016567400 A JP2016567400 A JP 2016567400A JP 2017520678 A JP2017520678 A JP 2017520678A
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- sintering
- powder
- alloy
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Abstract
Description
本出願は、2014年5月13日に出願された米国特許仮出願番号第61/992,692号、2014年9月2日に出願された米国特許仮出願番号第62/044,781号、及び2014年12月2日に出願された米国特許仮出願番号第62/086,524号に関し、これらはそれぞれ参照により本明細書に組み込まれる。
無し
本発明の記載及び特許請求において、以下の用語を使用する。本明細書で使用するとき、「空隙体積」は、グリーン体、予備焼結集合(pre-sintered mass)又は部分的に焼結された脆弱体における、固体顆粒同士の間の空間の体積を指す。したがって、空隙体積の百分率は、固体顆粒が占めていない集合全体又は部分的に焼結された脆弱体の体積のパーセントである。空隙体積は、例えば空気、真空、又は他の流体が占めていてもよい。
粉末冶金は、従来の融解及び展伸冶金技術に対する低コストの代案である。しかし、粉末冶金も課題を提示する。いくつかの原料金属では、原料として使用される粉末の製造コストが非常に高いことがあり、粉末冶金アプローチの利点及び競争力を最小化する。特に、チタン金属は、粉末冶金のための良好な候補であるが、チタン金属粉末は、製造が非常に高価であり得る。
a)CaCl2、CaBr2、CaI2を含むハロゲン化カルシウム塩、
b)CaCl2−LiCl、CaCl2−KCl、CaCl2−MgF2、CaCl2−LiF、CaCl2−KF、CaCl2−NaF、CaCl2−NaBr、CaCl2−LiBr、CaCl2−KBr、CaCl2−NaI、CaCl2−LiI、CaCl2−KI、CaBr2−LiCl、CaBr2−KCl、CaBr2−MgF2、CaBr2−LiF、CaBr2−KF、CaBr2−NaF、CaBr2−NaBr、CaBr2−LiBr、CaBr2−KBr、CaBr2−NaI、CaBr2−LiI、CaBr2−KI、CaI2−LiCl、CaI2−KCl、CaI2−MgF2、CaI2−LiF、CaI2−KF、CaI2−NaBr、CaI2−LiBr、CaI2−KBr、CaI2−NaI、CaI2−LiI、CaI2−KIを含むハロゲン化カルシウム−ハロゲン化アルカリ共晶塩、
c)CaCl2−CaBr2、CaCl2−CaI2、CaCl2−CaF2、CaBr2−CaI2、CaBr2−CaF2、CaI2−CaF2を含むハロゲン化カルシウム−ハロゲン化カルシウム共晶塩、
d)a)、b)又はc)で記述した3以上の塩から形成される共晶塩であって、1つのカルシウム塩を少なくとも含有する共晶塩。
UGSからのTiH2の調製
TiO2粉末を調製し、Mgを使用してTiO2を還元し、TiH2を製造する例を、以下に記載する。平均サイズが200マイクロメートルより大きい、入手したままのUGSをボールミリングして、包まれたSiを露出させ、再浸出を容易にする。ミリングされたUGSのサイズは、容易に数マイクロメートル、例えば1〜5マイクロメートルに達し得る。次に、100グラムのミリングされたUGSを、200g/LのNaOHを含むアルカリ性溶液で、100℃で2時間、体積−質量比(volume-to-mass ratio)を2:1に制御しながら予備浸出させる。予備浸出の後、スラリーを固液分離し、おおよそ100グラムの残渣の固体を乾燥させて、ロースト加工の用意をする。その後、100グラムの予備浸出した残渣を、150グラムの商業用NaOH固体と、タンブラーによって30分間混合し、混合物をInconel反応器内に入れる。反応器を上部負荷箱形炉(top-loaded box furnace)内に置く。炉を加熱し、熱電対を使用して、混合物の温度プロファイルを追跡する。500℃で1時間維持した後、反応器を冷却して炉から取り出し、ローストされた製品を粉末に粉砕する。250グラムのローストされた粉末を、500mLの50℃の水で30分間、撹拌しながら洗浄した後、固液分離する。溶液のpH値がおおよそ12に達するまで、洗浄手順を数回繰り返す。主成分がチタン酸である泥状材料を得る。この材料を、濃度がおおよそ6mol/Lの希釈HCl溶液中で浸出させる。チタン及び他のアルカリ不溶性遷移金属種、例えばFeは、同時に溶解する。浸出液を濾過して、加水分解の前に、他の不溶性粒子を除去する。TiCl4を含む溶液を、封止された晶析装置内に移し、溶液中に存在する第二鉄イオンを、Ti3+イオンによって、第一鉄イオンに還元する。晶析装置を、温度が100℃に設定された油浴内に置く。還流冷却器を晶析装置に取り付けて、加水分解中の水及びHClの蒸発を回避する。その後、連続的に撹拌しながら、沈殿を100℃で15時間維持する。得られた沈殿物を、60℃の水で、液体が中性pHに達するまで洗浄する。沈殿物は、粒径が9〜30マイクロメートルのピロタン酸である。沈殿物を更に、600℃で2時間仮焼して、水を除去し、アナターゼを生成した後、900℃で2時間仮焼して、ルチルを生成する。
噴霧乾燥したTiH2顆粒の調製
TiH2微粒子をバインダー及び溶媒と混合し、混合物を噴霧乾燥させて、球状の顆粒を形成することにより、顆粒を調製した。図7は、球状TiH2顆粒のSEM写真である。顆粒は、サイズが約40マイクロメートル〜約100マイクロメートルの範囲である。
部分的に焼結された顆粒の調製
TiH2微粒子をバインダー及び溶媒と混合し、混合物を噴霧乾燥させて、球状の顆粒を形成することにより、顆粒を調製した。顆粒を、温度範囲250〜400℃で9時間、チューブ炉のアルゴンフロー中で脱バインダーした。脱バインダー段階の後、温度を700℃に上昇させ、脱水素及び部分的な焼結のために、同じチューブ炉内で30分間保持した。図8は、部分的に焼結された顆粒のSEM写真である。
Ti−6Al−4V球状粉末の調製
球状の顆粒の噴霧乾燥、脱バインダー、及び焼結の例を、以下に記載する。この例で使用される原料金属は、Ti−6Al−4V合金スクラップから作製された、2000グラムの−325メッシュのTi−6Al−4V水素化物である。噴霧乾燥用のスラリーは、粉末を、500mLの水、1500mLのエチルアルコール、及び30gのポリビニルアルコール溶液中で、アトライタ(Union Process lab attritor HD−1)に、回転速度300rpmでボールミリングすることによって調製した。ミリング後、水素化物の粉末の粒径は、10マイクロメートル未満に減少した。造粒は、Buchi Mini Spray Dryer B−290に、入口温度210℃で行い、Ti−6Al−4V水素化物の顆粒を形成した。スラリーを、噴霧乾燥機に供給する間、電磁撹拌器によって撹拌した。乾燥させた顆粒を、CaOと、1:1の質量比で混合した後、混合物を冷間等方圧加圧(CIP:cold isostatic press)により、圧力50MPaでプレスした。CIPを行ったパートを、同じチューブ炉のアルゴンフロー中、温度範囲250〜400℃で9時間脱バインダーし、1300℃で1分間焼結した。脱バインダー及び焼結の後、希釈塩酸(chloride acid)及び水を使用して、CaOを浸出させた。乾燥後、球状のTi−6Al−4V粒子を回収した。焼結されたままのTi−6Al−4V顆粒の形態を図9に示す。図9は、焼結された顆粒のSEM写真である。
脱酸素プロセス
3.91重量%の酸素を含むTi焼結球状粉末を、CaCl2−KCl共晶塩で脱酸素した。サイズが20〜45マイクロメートルの焼結された球状の粉末を10グラム秤量し、2グラムの6メッシュ顆粒状カルシウム、8.5グラムの無水CaCl2粉末、及び1.5グラムの無水KCl粉末と混合し、Moるつぼ内に入れた。その後、混合物を収容したるつぼを、チューブ炉内に置いた。加熱前に、炉のチューブを評価し、標準の実験室用純アルゴンを3回流した。その後、炉を800℃まで、加熱速度10℃/分で加熱し、Arフロー雰囲気中で12時間保持した。その後、炉を室温に冷却し、開放した。その後、処理された製品をるつぼから取り出し、200mLの希釈HClで2時間浸出させた。溶液のpH値を、2〜5に制御した。その後、浸出させた製品を水で3回洗浄し、エタノールですすぎ、最後に真空で12時間乾燥させた。Ti球状粉末の酸素含有量は、初期値3.91重量%から最終濃度0.0740重量%まで、98.1%減少した。
脱酸素プロセス
0.22重量%の酸素を含むニオブ(Nb)−30重量%ハフニウム(Hf)(C103合金)粉末を、CaCl2−LiCl共晶塩を融解塩として使用して脱酸素した。サイズが<37マイクロメートルのNb−30重量%Hf粉末を10グラム秤量し、0.5グラムの6メッシュ顆粒状カルシウム、及び7グラムのCaCl2粉末、及び3グラムのLiCl粉末と混合し、ステンレス鋼るつぼ内に入れた。混合物を収容したるつぼを、チューブ炉内に置いた。加熱前に、炉のチューブを評価し、標準のアルゴンを3回流した。その後、炉を700℃まで、加熱速度10℃/分で加熱し、Arフロー雰囲気中で1時間保持した。その後、炉を室温に冷却し、開放した。その後、処理された製品をるつぼから取り出し、200mLの希釈HNO3で2時間浸出させた。酸のpH値を、2〜5に制御した。その後、浸出させた製品を水で3回洗浄し、エタノールですすぎ、最後に真空で乾燥させた。Nb−30重量%Hf粉末の酸素含有量は、初期値0.22重量%から最終濃度0.055重量%まで、75%減少した。
Claims (37)
- 実質的に球状の金属粉末を製造する方法であって、
一次微粒子を含み、平均出発粒径を有する微粒子原料金属を準備することと、
前記微粒子原料金属を、バインダー及び任意の溶媒と混合して、スラリーを形成することと、
前記スラリーを造粒して、実質的に球状の顆粒を形成することであって、それぞれの顆粒が微粒子原料金属の凝集物を含む、ことと、
脱バインダー温度で前記顆粒を脱バインダーし、前記顆粒のバインダー含有量を低下させて、脱バインダーした顆粒を形成することと、
それぞれの顆粒内の粒子が一緒に融合し、部分的に又は完全に焼結された顆粒を形成するように、前記脱バインダーした顆粒を、焼結温度で少なくとも部分的に焼結することと、
前記焼結された顆粒を回収して、前記実質的に球状の金属粉末を形成することと、
を含む、方法。 - 前記顆粒をサイズによって選別することを更に含む、請求項1に記載の方法。
- 前記実質的に球状の金属粉末が、約1〜約1000マイクロメートルの平均最終粒径を有する、請求項1に記載の方法。
- 前記実質的に球状の金属粉末が、チタン、ジルコニウム、ハフニウム、トリウム、バナジウム、ニオブ、タンタル、クロム、モリブデン、タングステン、ニッケル、アルミニウム、鉄、上記の金属同士の合金、上記の金属と他の金属との合金、上記の金属と非金属との合金、CP−Ti合金、Ti−6Al−4V合金、ニッケル系高温合金、ステンレス鋼、及びこれらの組み合わせからなる群から選択される、請求項1に記載の方法。
- 前記実質的に球状の金属粉末が、約1.5未満の平均粒子アスペクト比を有する、請求項1に記載の方法。
- 前記微粒子原料金属が、チタン、水素化チタン、Al−V母合金、酸化チタン、又はこれらの混合物を含む、請求項1に記載の方法。
- 前記微粒子原料金属が、ジルコニウム、ハフニウム、トリウム、バナジウム、ニオブ、タンタル、クロム、モリブデン、タングステン、ニッケル、アルミニウム、鉄、上記の金属同士の合金、上記の金属と他の金属との合金、上記の金属と非金属との合金、CP−Ti合金、Ti−6Al−4V合金、ニッケル系高温合金、ステンレス鋼、これらの水素化物、これらの酸化物、これらの混合物、及びこれらの組み合わせを含む、請求項1に記載の方法。
- 前記微粒子原料金属を、チタンスラグ、高級チタンスラグ、二酸化チタン、スクラップチタン、スクラップチタン合金、又はこれらの組み合わせから選択される原料から作製することを更に含む、請求項1に記載の方法。
- 前記一次微粒子の前記平均出発粒径が、0.1〜100マイクロメートルである、請求項1に記載の方法。
- 前記微粒子原料金属を、バインダーと混合することが、前記微粒子原料金属及び前記バインダーを前記溶媒中で湿式ボールミリングすることを更に含む、請求項1に記載の方法。
- 前記スラリーを造粒することが、噴霧乾燥、回転乾燥、振動ペレット化、凍結造粒及び乾燥、又はこれらの組み合わせを含む、請求項1に記載の方法。
- 前記顆粒が、前記実質的に球状の金属粉末の平均最終粒径よりも約20%〜約50%大きい平均顆粒サイズを有する、請求項1に記載の方法。
- 前記顆粒が、10マイクロメートルよりも大きい平均顆粒サイズを有する、請求項1に記載の方法。
- 前記脱バインダー温度が約50℃〜約600℃である、請求項1に記載の方法。
- 前記脱バインダーした顆粒を焼結することが、不活性ガス雰囲気下で行われる、請求項1に記載の方法。
- 焼結中に顆粒がCaO粉末によって分離されるように、前記脱バインダーした顆粒がCaO粉末と混合される、請求項1に記載の方法。
- 前記焼結温度が約700℃〜約1400℃である、請求項1に記載の方法。
- 前記焼結温度が約900℃〜約1000℃である、請求項1に記載の方法。
- 前記脱バインダーした顆粒を焼結することが、約1秒〜約100時間の焼結時間で行われる、請求項1に記載の方法。
- 前記脱バインダーした顆粒を焼結することが、それぞれの焼結された顆粒が65%よりも高い相対密度に達するまで行われる、請求項1に記載の方法。
- 前記脱バインダーした顆粒を焼結することが、それぞれの焼結された顆粒が、実質的に互いに結合しない状態まで行われる、請求項1に記載の方法。
- 前記脱バインダーした顆粒を焼結することが、前記脱バインダーした顆粒が、前記脱バインダーした顆粒同士の間の接触点で一緒に融合するが、前記脱バインダーした顆粒が平均で少なくとも約20%の非融合表面積を保つまで行われる、請求項1に記載の方法。
- 前記少なくとも部分的に焼結することが、前記顆粒が互いに接続され、少なくとも部分的に焼結された顆粒の脆弱体を形成するように行われ、前記分離が、前記脆弱体を砕いて、前記実質的に球状の金属粉末を回収することにより達成される、請求項1に記載の方法。
- 前記脆弱体を砕くことが、前記脆弱体をボールミリングすることを含む、請求項20に記載の方法。
- 酸素含有量を0.3重量%未満まで低下させるために十分な脱酸素剤を使用して、前記焼結された顆粒を脱酸素することを更に含む、請求項1に記載の方法。
- 前記脱酸素剤が、カルシウム(Ca)及び水素化カルシウム(CaH2)のうちの少なくとも1つを含む、請求項25に記載の方法。
- 前記焼結された顆粒を脱酸素する前に、前記焼結された顆粒及び前記脱酸素剤を塩と混合することを更に含む、請求項25に記載の方法。
- 前記脱酸素することが、900℃未満の温度で行われる、請求項25に記載の方法。
- 前記脱酸素剤が、ハロゲン化カルシウム塩、ハロゲン化カルシウム−ハロゲン化アルカリ共晶塩、ハロゲン化カルシウム−ハロゲン化カルシウム共晶塩、又はこれらの組み合わせを含む塩である、請求項25に記載の方法。
- 前記脱酸素剤が、CalCl2及びKClから構成される共晶塩である、請求項25に記載の方法。
- 前記脱酸素剤が、カルシウム(Ca)の融点未満の融点を有する共晶塩を含む、請求項25に記載の方法。
- 前記脱酸素剤が、焼結中に酸素を前記脱バインダーした顆粒から除去し、前記焼結された顆粒が、焼結中に互いに分離したままである、請求項25に記載の方法。
- 請求項1に記載の方法により形成される実質的に球状の金属顆粒の回収。
- 前記金属顆粒が、チタン、ジルコニウム、ハフニウム、トリウム、バナジウム、ニオブ、タンタル、クロム、モリブデン、タングステン、ニッケル、アルミニウム、鉄、上記の金属同士の合金、上記の金属と他の金属との合金、上記の金属と非金属との合金、CP−Ti合金、Ti−6Al−4V合金、ニッケル系高温合金、ステンレス鋼、及びこれらの組み合わせからなる群から選択される部材を含む、請求項33に記載の回収。
- 前記金属顆粒がチタンを含む、請求項33に記載の回収。
- 前記金属顆粒が、1%〜35%の相対密度を有する多孔質である、請求項33に記載の回収。
- 前記金属顆粒が、デンドライトを実質的に含まず、焼結された微細構造を有する、請求項33に記載の回収。
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US20160074942A1 (en) | 2016-03-17 |
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