JP7448955B2 - 球状タンタル粉末、それを含有する製品、及びその作製方法 - Google Patents
球状タンタル粉末、それを含有する製品、及びその作製方法 Download PDFInfo
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- JP7448955B2 JP7448955B2 JP2020546438A JP2020546438A JP7448955B2 JP 7448955 B2 JP7448955 B2 JP 7448955B2 JP 2020546438 A JP2020546438 A JP 2020546438A JP 2020546438 A JP2020546438 A JP 2020546438A JP 7448955 B2 JP7448955 B2 JP 7448955B2
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- tantalum powder
- tantalum
- powder
- microns
- ppm
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- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 3
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- 238000012546 transfer Methods 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000002061 vacuum sublimation Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/047—Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/02—Inorganic materials
- A61L31/022—Metals or alloys
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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- B33Y10/00—Processes of additive manufacturing
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- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
- B33Y40/10—Pre-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
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- B33Y80/00—Products made by additive manufacturing
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
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- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/12—Materials or treatment for tissue regeneration for dental implants or prostheses
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/10—Formation of a green body
- B22F10/12—Formation of a green body by photopolymerisation, e.g. stereolithography [SLA] or digital light processing [DLP]
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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- B22F10/25—Direct deposition of metal particles, e.g. direct metal deposition [DMD] or laser engineered net shaping [LENS]
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- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
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- B22F10/60—Treatment of workpieces or articles after build-up
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- B22F12/00—Apparatus or devices specially adapted for additive manufacturing; Auxiliary means for additive manufacturing; Combinations of additive manufacturing apparatus or devices with other processing apparatus or devices
- B22F12/10—Auxiliary heating means
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Description
約5ミクロン~約25ミクロンのD10径、
約20ミクロン~約80ミクロンのD90径、及び/又は、
(粉末の重量に対して)約20 ppm~約1000 ppm、例えば、約100 ppm~約1000 ppm、又は100 ppm~約250 ppmの酸素含量。
a)約4 g/cc~約12.3 g/ccの見掛け密度、
b)約5ミクロン~約25ミクロンのD10粒径、
c)約20ミクロン~約50ミクロンのD50粒径、
d)約30ミクロン~約100ミクロンのD90粒径、及び/又は、
e)約0.05 m2/g~約20 m2/gのBET表面積。
タンタル粉末は、以下の性質の少なくとも1つを有することができる:
a)約9 g/cc~約12.3 g/ccの見掛け密度、
b)約12ミクロン~約25ミクロンのD10粒径、
c)約20ミクロン~約40ミクロンのD50粒径、
d)約30ミクロン~約70ミクロンのD90粒径、及び/又は、
e)約0.1 m2/g~約15 m2/gのBET表面積。
純度レベル:
酸素含量は、約20 ppm~約60000 ppm、又は約100 ppm~約60000 ppm、例えば、約20 ppm~約1000 ppm、又は約40 ppm~約500 ppm、又は約50 ppm~約200 ppm、又は約250 ppm~約50000 ppm、又は約500 ppm~約30000 ppm、又は約1000 ppm~約20000 ppmである。BET(m2/g)に対する酸素(ppm)の割合は、約2000~約4000、例えば、約2200~約3800、約2400~約3600、約2600~約3400、又は約2800~約3200等とすることができる。
炭素含量は、約1 ppm~約100 ppmであり、より好ましくは約10 ppm~約50 ppm、又は約20 ppm~約30 ppmである。
窒素含量は、約5 ppm~約20000 ppm、又は約100 ppm~約20000 ppm以上であり、より好ましくは約1000 ppm~約5000 ppm、又は約3000 ppm~約4000 ppm、又は約3000 ppm~約3500 ppmである。
水素含量は、約1 ppm~約1000 ppm、約10 ppm~約1000 ppmであり、より好ましくは約300 ppm~約750 ppm、又は約400 ppm~約600 ppmである。
鉄含量は、約1 ppm~約50 ppmであり、より好ましくは約5 ppm~約20 ppmである。
ニッケル含量は、約1 ppm~約150 ppmであり、より好ましくは約5 ppm~約100 ppm、又は約25 ppm~約75 ppmである。
クロム含量は、約1 ppm~約100 ppmであり、より好ましくは約5 ppm~約50 ppm、又は約5 ppm~約20 ppmである。
ナトリウム含量は、約0.1 ppm~約50 ppmであり、より好ましくは約0.5 ppm~約5 ppmである。
カリウム含量は、約0.1 ppm~約100 ppmであり、より好ましくは約5 ppm~約50 ppm、又は約30 ppm~約50 ppmである。
マグネシウム含量は、約1 ppm~約50 ppmであり、より好ましくは約5 ppm~約25 ppmである。
リン(P)含量は、約1 ppm~約500 ppm、又は約5 ppm~約500 ppmであり、より好ましくは約100 ppm~約300 ppmである。
フッ化物(F)含量は、約1 ppm~約500 ppmであり、より好ましくは約25 ppm~約300 ppm、又は約50 ppm~約300 ppm、又は約100 ppm~約300 ppmである。
+60#が、約0.0%~約1%、好ましくは約0.0%~約0.5%、より好ましくは0.0%又は約0.0%である。
60/170が、約45%~約70%、好ましくは約55%~約65%、又は約60%~約65%である。
170/325が、約20%~約50%、好ましくは約25%~約40%、又は約30%~約35%である。
325/400が、約1.0%~約10%、好ましくは約2.5%~約7.5%、例えば、約4%~約6%である。
-400が、約0.1%~約2.0%、好ましくは約0.5%~約1.5%である。
市販のKTa2F7(KTAF)とナトリウムとを使用して、標準工業プロセスを利用するKTAFのナトリウム還元を用いて、タンタル粉末を得た。副生成塩は、洗浄工程、及び酸浸出工程、及び乾燥工程によって除去した。得られたタンタル粉末は、約0.1 m2/gのBET表面積を有していた。このタンタルは、基本ロットタンタル粉末とした。図1Aに、この出発タンタル粉末のSEM画像を示す。出発タンタル粉末を、3つの粉末ロット、すなわち、ロットA、ロットB、及びロットCに分割し、以下の通り、各々別々に、プラズマ処理した。
この例では、実施例1と同様の基本ロットタンタル粉末(ナトリウム還元粉末)を使用した。この基本ロットタンタル粉末は、0.1 m2/gのBET表面積を有していた。基本ロットタンタル粉末をプレスし、約1000℃の焼結温度で、1時間、圧粉体ログへと焼結した。圧粉体ログを、電子ビーム炉へと供給し、そこで、坩堝を用いて金属を溶融した。金型を通して溶融物を延伸し、これにより、タンタルが凝固し、インゴットを形成した。水素雰囲気を有する高温炉を用いて、タンタルインゴットを水素化し、水素化後は室温まで冷却した。次いで、水素化したインゴットを(ジョークラッシャー、次いで、ロールクラッシャーを用いて)破砕し、-20 #の篩サイズ(size)にスクリーニングした。破砕後のインゴットを、望ましいサイズカット、すなわち、ロットAでは10ミクロン~25ミクロン(又は、ロットBでは35ミクロン~75ミクロン)にスクリーニングした。次いで、スクリーニング後の各ロット用の粉末を酸浸出した。次いで、粉末を、マグネシウムを用いて脱酸素化し、酸素レベルを500 ppm未満に低減した。この出発タンタル粉末のSEM画像を図2Aに示す。次いで、ロットA及びロットBを、各々別々に、実施例1と同様の方法で、プラズマ処理した。
実施例2のタンタル粉末を、3D印刷プロセス、すなわち、積層造形プロセスに用いた。具体的には、タンタル造形を、直径100 mm×100 mmの造形容積、及び175 Wの最大レーザー出力で、Trumpf TruPrint 1000において行った。使用するベースプレートは、316型のオーステナイト系クロムニッケルステンレス鋼とした。
この例では、実施例1と同様の基本ロットタンタル粉末(ナトリウム還元粉末)を使用した。この基本ロットタンタル粉末は、0.1 m2/gのBET表面積を有していた。基本ロットタンタル粉末をプレスし、2500℃~3000℃の焼結温度で、3時間、圧粉体ログへと焼結した。圧粉体ログを、電子ビーム炉へと供給し、そこで、坩堝を用いて金属を溶融した。金型を通して溶融物を延伸し、これにより、タンタルが凝固し、インゴットを形成した。水素雰囲気を有する高温炉を用いて、タンタルインゴットを水素化し、水素化後は室温まで冷却した。次いで、水素化したインゴットを(ジョークラッシャー、次いで、ロールクラッシャーを用いて)破砕し、-20 #の篩サイズ(size)にスクリーニングした。破砕後のインゴットを、望ましいサイズカット、すなわち、ロットA2及びロットD2では10ミクロン~25ミクロン、又はロットE2及びロットF2では15ミクロン~40ミクロン、又はロットB2、ロットC2では35ミクロン~105ミクロンにスクリーニングした。次いで、スクリーニング後の各ロット用の粉末を酸浸出した。次いで、各ロット用の粉末を、マグネシウムチップを用いて(700℃で2時間)脱酸素化し、酸素レベルを、表6に示すような全て1000 ppm未満の様々なレベルへと低減した。標準酸素不純物粉末(A2、D2)及び低酸素不純物粉末(B2、E2)を製造した。次いで、ロットA2~ロットF2を、各々別々に、実施例1と同様の方法で、プラズマ処理した。ロットC2及びロットF2に対しては、ロットB2及びロットE2において行った初期脱酸素化に加えて、球状化後に追加の脱酸素化(マグネシウムチップ、700℃、2時間)を行って(脱酸素化を2回)、超低酸素不純物粉末(ロットC2、ロットF2)を得た。A2、D2、B2、及びE2において酸素量が異なるのは、表7に示すように、各ロットの粒度分布によるものである。
この例では、円筒形のバー又はロッドの形状を有するタンタル引張バーを数本作製した。これらのバー又はロッドは、その間に円筒形状を有する2つの平らな端面を有している。サンプル5.1は比較例であり、この例では、型内で、タンタル角状粉末(Global Advanced Metals USA, IncのKDELとして市販)を真空アーク溶融することによって加工タンタルバーを作製した。
1.
a.1.0~1.25の平均アスペクト比を有する球状形状を有し、
b.ガス不純物を除くタンタル粉末の全重量に対して、少なくとも99.99重量%Taのタンタル純度を有し、
c.約0.5ミクロン~約250ミクロンの平均粒径を有し、
d.16 g/cc~16.6 g/ccの真密度を有し、
e.約4 g/cc~約12.3 g/ccの見掛け密度を有し、かつ、
f.20秒以下のホールフローレートを有する、タンタル粉末。
2. プラズマ熱処理されている、任意の上記又は下記の実施形態/特徴/態様のタンタル粉末。
3. 400 ppm未満の酸素レベルを有する、任意の上記又は下記の実施形態/特徴/態様のタンタル粉末。
4. 20 ppm~250 ppmの酸素レベルを有する、任意の上記又は下記の実施形態/特徴/態様のタンタル粉末。
5. 前記平均アスペクト比が1.0~1.1である、任意の上記又は下記の実施形態/特徴/態様のタンタル粉末。
6. 前記平均アスペクト比が1.0~1.05である、任意の上記又は下記の実施形態/特徴/態様のタンタル粉末。
7. 前記純度が少なくとも99.995重量%Taである、任意の上記又は下記の実施形態/特徴/態様のタンタル粉末。
8. 前記平均粒径が約0.5ミクロン~約10ミクロンである、任意の上記又は下記の実施形態/特徴/態様のタンタル粉末。
9. 前記平均粒径が約5ミクロン~約25ミクロンである、任意の上記又は下記の実施形態/特徴/態様のタンタル粉末。
10. 前記平均粒径が約15ミクロン~約45ミクロンである、任意の上記又は下記の実施形態/特徴/態様のタンタル粉末。
11. 前記平均粒径が約35ミクロン~約75ミクロンである、任意の上記又は下記の実施形態/特徴/態様のタンタル粉末。
12. 前記平均粒径が約55ミクロン~約150ミクロンである、任意の上記又は下記の実施形態/特徴/態様のタンタル粉末。
13. 前記平均粒径が約105ミクロン~約250ミクロンである、任意の上記又は下記の実施形態/特徴/態様のタンタル粉末。
14. 以下の性質のうち少なくとも1つを有する、任意の上記又は下記の実施形態/特徴/態様のタンタル粉末:
a.約5ミクロン~25ミクロンのD10径、
b.約20ミクロン~80ミクロンのD90径、及び/又は、
c. 約100 ppm~約1000 ppm、例えば約100 ppm~約250 ppmの酸素含量。
15. 任意の上記又は下記の実施形態/特徴/態様のタンタル粉末を含む物品。
16. 物理蒸着プロセス用のコイルセットのボスである、任意の上記又は下記の実施形態/特徴/態様の物品。
17. 前記ボスが、連続気泡構造と、中実構造とを含む、任意の上記又は下記の実施形態/特徴/態様の物品。
18. 物理蒸着プロセス用のコイルセット又はその部品である、任意の上記又は下記の実施形態/特徴/態様の物品。
19. 整形外科用インプラント又はその部品である、任意の上記又は下記の実施形態/特徴/態様の物品。
20. 歯科用インプラントである、任意の上記又は下記の実施形態/特徴/態様の物品。
21. 物品を形成する方法であって、任意の上記又は下記の実施形態/特徴/態様のタンタル粉末を利用して、物品又はその部品の形状を形成することによって、物品を積層造形することを含む、方法。
22. 前記積層造形が、レーザー粉末床溶融を含む、任意の上記又は下記の実施形態/特徴/態様の方法。
23. 前記積層造形が、電子ビーム粉末床溶融を含む、任意の上記又は下記の実施形態/特徴/態様の方法。
24. 前記積層造形が、指向性エネルギー堆積を含む、任意の上記又は下記の実施形態/特徴/態様の方法。
25. 前記積層造形が、粉末又はワイヤーを介したレーザークラッディングを含む、任意の上記又は下記の実施形態/特徴/態様の方法。
26. 前記積層造形が、材料噴射を含む、任意の上記又は下記の実施形態/特徴/態様の方法。
27. 前記積層造形が、シート積層を含む、任意の上記又は下記の実施形態/特徴/態様の方法。
28. 前記積層造形が、液槽光重合を含む、任意の上記又は下記の実施形態/特徴/態様の方法。
29. 任意の上記又は下記の実施形態/特徴/態様のタンタル粉末を作製する方法であって、
a.不活性雰囲気中で、出発タンタル粉末をプラズマ熱処理して、該出発タンタル粉末の少なくとも外表面を少なくとも部分的に溶融し、熱処理済タンタル粉末を得ることと、
b.不活性雰囲気中で、前記熱処理済タンタル粉末を冷却して、タンタル粉末を得ることと、
を含む、方法。
30. 前記出発タンタル粉末がナトリウム還元タンタル粉末である、任意の上記又は下記の実施形態/特徴/態様の方法。
31. 前記出発タンタル粉末が基本ロットタンタル粉末である、任意の上記又は下記の実施形態/特徴/態様の方法。
32. 前記出発タンタル粉末が第1の粒度分布を有しており、前記タンタル粉末が第2の粒度分布を有しており、前記第1の粒度分布と前記第2の粒度分布とが、互いに10%以内である、任意の上記又は下記の実施形態/特徴/態様の方法。
33. 工程aに先立って、第1のタンタル粉末を焼結して焼結粉末を得て、次いで、該焼結粉末を電子ビーム溶融してインゴットを得て、次いで、該インゴットを出発タンタル粉末へと粉末化することにより、前記出発タンタル粉末を形成する、任意の上記又は下記の実施形態/特徴/態様の方法。
図1B
Spherical Tantalum Powder 球状タンタル粉末
図2A
T-Powder T粉末
図2B
Spherical Tantalum Powder 球状タンタル粉末
図11
X-direction X方向
Y-direction Y方向
Z-direction Z方向
Claims (17)
- a.1.0~1.25の平均アスペクト比を有する球状形状を有し、
b.ガス不純物を除くタンタル粉末の全重量に対して、少なくとも99.99重量%Taのタンタル純度を有し、
c.i)0.5ミクロン~250ミクロンの平均粒径を有し、かつ400ppm未満の酸素レベルを有し、又はii)0.5ミクロン~10ミクロン若しくは5ミクロン~25ミクロン若しくは105ミクロン~250ミクロンの平均粒径を有し、又はiii)5ミクロン~25ミクロンのD10径を有し、
d.4g/cc~12.3g/ccの見掛け密度を有し、
e.16g/cc~16.6g/ccの真密度を有し、かつ、
f.20秒/50 g以下のホールフローレートを有する、タンタル粉末。 - 0.5ミクロン~10ミクロン若しくは5ミクロン~25ミクロン若しくは15ミクロン~45ミクロン若しくは35ミクロン~75ミクロン若しくは55ミクロン~150ミクロン若しくは105ミクロン~250ミクロンの平均粒径を有し、かつ400ppm未満の酸素レベルを有する、請求項1に記載のタンタル粉末。
- 前記平均アスペクト比が1.0~1.1である、請求項1に記載のタンタル粉末。
- 前記平均粒径が15ミクロン~45ミクロンであり、かつ400 ppm未満の酸素レベルを有する、請求項1に記載のタンタル粉末。
- 前記平均粒径が35ミクロン~75ミクロンであり、かつ400 ppm未満の酸素レベルを有する、請求項1に記載のタンタル粉末。
- 以下の性質のうち少なくとも1つを有する、請求項1に記載のタンタル粉末:
a.5ミクロン~25ミクロンのD10径、
b.20ミクロン~80ミクロンのD90径、又は、
c. 100ppm~1000ppmの酸素含量。 - 請求項1に記載のタンタル粉末を積層造形することにより形成される物品。
- 整形外科用インプラント又はその部品である、請求項7に記載の物品。
- 前記整形外科用インプラントが、連続気泡構造と、中実構造とを含む、請求項8に記載の物品。
- 物品を形成する方法であって、請求項1に記載のタンタル粉末を利用して、物品又はその部品の形状を形成することによって、物品を積層造形することを含む、方法。
- 前記積層造形が、レーザー粉末床溶融を含む、請求項10に記載の方法。
- 前記積層造形が、電子ビーム粉末床溶融を含む、請求項10に記載の方法。
- 請求項1に記載のタンタル粉末を作製する方法であって、
a.不活性雰囲気中で、出発タンタル粉末を15kW~35 kWの電力でプラズマ熱処理して、該出発タンタル粉末の少なくとも外表面を少なくとも部分的に溶融し、熱処理済タンタル粉末を得ることと、
b.不活性雰囲気中で、前記熱処理済タンタル粉末を冷却して、タンタル粉末を得ることと、
を含む、方法。 - 工程aに先立って、第1のタンタル粉末を焼結して焼結粉末を得て、次いで、該焼結粉末を電子ビーム溶融してインゴットを得て、次いで、該インゴットを出発タンタル粉末へと粉末化することにより、前記出発タンタル粉末を形成する、請求項13に記載の方法。
- 前記出発タンタル粉末が第1の粒度分布を有しており、前記タンタル粉末が第2の粒度分布を有しており、前記出発タンタル粉末の粒度分布が、D10径及び/又はD90径が、出発タンタル粉末のD50径の50%以内になるものである、請求項13に記載の方法。
- 前記出発タンタル粉末が第1の粒度分布を有しており、前記タンタル粉末が第2の粒度分布を有しており、前記出発タンタル粉末の粒度分布が、D10径及び/又はD90径が、出発タンタル粉末のD50径の25%以内になるものである、請求項13に記載の方法。
- 前記出発タンタル粉末が第1の粒度分布を有しており、前記タンタル粉末が第2の粒度分布を有しており、前記出発タンタル粉末の粒度分布が、D10径及び/又はD90径が、出発タンタル粉末のD50径の10%以内になるものである、請求項13に記載の方法。
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