JP6412251B2 - コンデンサグレード粉末の製造方法及び前記方法から得られたコンデンサのグレード粉末 - Google Patents
コンデンサグレード粉末の製造方法及び前記方法から得られたコンデンサのグレード粉末 Download PDFInfo
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- JP6412251B2 JP6412251B2 JP2017508046A JP2017508046A JP6412251B2 JP 6412251 B2 JP6412251 B2 JP 6412251B2 JP 2017508046 A JP2017508046 A JP 2017508046A JP 2017508046 A JP2017508046 A JP 2017508046A JP 6412251 B2 JP6412251 B2 JP 6412251B2
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- powder
- slurry
- tantalum
- spray dryer
- microns
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- 229910052715 tantalum Inorganic materials 0.000 claims description 37
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- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
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- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
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- 241000723346 Cinnamomum camphora Species 0.000 description 1
- 101100504379 Mus musculus Gfral gene Proteins 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
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- 229910004529 TaF 5 Inorganic materials 0.000 description 1
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- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
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- 229910052786 argon Inorganic materials 0.000 description 1
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- 229960000846 camphor Drugs 0.000 description 1
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- 150000004678 hydrides Chemical class 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical group [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
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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 1
- 238000002844 melting Methods 0.000 description 1
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- 239000007769 metal material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- BFRGSJVXBIWTCF-UHFFFAOYSA-N niobium monoxide Inorganic materials [Nb]=O BFRGSJVXBIWTCF-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
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- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
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- 150000003481 tantalum Chemical class 0.000 description 1
- YRGLXIVYESZPLQ-UHFFFAOYSA-I tantalum pentafluoride Chemical compound F[Ta](F)(F)(F)F YRGLXIVYESZPLQ-UHFFFAOYSA-I 0.000 description 1
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- C01G33/00—Compounds of niobium
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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Description
a)スコット密度が約14g/in3〜約35g/in3である、
b)D10粒度が約5ミクロン〜約25ミクロンである、
c)D50粒度が約20ミクロン〜約50ミクロンである、
d)D90粒度が約30ミクロン〜約100ミクロンである、及び/又は、
e)BET表面積が約0.5m2/g〜約20m2/gである。
又は、コンデンサグレード粉末は下記の特性の少なくとも1つを有することができる。
a)スコット密度が約20g/in3〜約35g/in3である、
b)D10粒度が約12ミクロン〜約25ミクロンである、
c)D50粒度が約20ミクロン〜約40ミクロンである、
d)D90粒度が約30ミクロン〜約70ミクロンである、及び/又は、
e)BET表面積が約0.7m2/g〜約15m2/gである。
スラリーは前記スラリーの総質量を基準として約35wt%〜約70wt%のコンデンサグレード粉末を含む。
スラリーは水性スラリーである。
回転式アトマイザディスクは約10,000rpm〜約50,000rpmで回転する。
回転式アトマイザディスクは約20mm〜約200mmの直径を有する。
スプレイドライヤは約100℃〜約200℃の入口温度を有する。
スプレイドライヤは入口温度よりも少なくとも40℃低い出口温度を有する。
スラリーは前記スプレイドライヤに少なくとも0.5kg/時のフィード速度でフィードされ、そして、
熱処理は少なくとも800℃の温度である。
1.コンデンサグレード粉末を製造する方法であって、
回転式アトマイザディスクを含むスプレイドライヤ中に粉末のスラリーをフィードし、そして乾燥した凝集粉末を形成すること、及び、
前記乾燥した凝集粉末を熱処理して、前記コンデンサグレード粉末を形成すること、
を含み、前記粉末はタンタル、ニオブ又はニオブ亜酸化物である、方法。
2.前記粉末はタンタル金属粉末である、任意の先行の又は後続の実施形態/特徴/態様の方法。
3.前記粉末はニオブ金属粉末である、任意の先行の又は後続の実施形態/特徴/態様の方法。
4.前記粉末はNbOx(式中、xは0.7〜1.2である)であるニオブ亜酸化物粉末である、任意の先行の又は後続の実施形態/特徴/態様の方法。
5.前記粉末はNbOx(式中、xは0.8〜1である)であるニオブ亜酸化物粉末である、任意の先行の又は後続の実施形態/特徴/態様の方法。
6.前記スラリーは、前記スラリーの総質量を基準として、約35wt%〜約70wt%のタンタル粉末を含む、任意の先行の又は後続の実施形態/特徴/態様の方法。
7.前記スラリーは水性スラリーである、任意の先行の又は後続の実施形態/特徴/態様の方法。
8.前記スラリーは水スラリーである、任意の先行の又は後続の実施形態/特徴/態様の方法。
9.前記スラリーは、前記スラリーの総質量を基準として、約40wt%〜約70wt%のタンタル粉末を含む、任意の先行の又は後続の実施形態/特徴/態様の方法。
10.前記スラリーは、前記スラリーの総質量を基準として、約45wt%〜約65wt%のタンタル粉末を含む、任意の先行の又は後続の実施形態/特徴/態様の方法。
11.前記回転式アトマイザディスクは5,000rpm以上で回転する、任意の先行の又は後続の実施形態/特徴/態様の方法。
12.前記回転式アトマイザディスクは10,000rpm以上で回転する、任意の先行の又は後続の実施形態/特徴/態様の方法。
13.前記回転式アトマイザディスクは約10,000rpm〜約50,000rpmで回転する、任意の先行の又は後続の実施形態/特徴/態様の方法。
14.前記回転式アトマイザディスクは約15,000rpm〜約40,000rpmで回転する、任意の先行の又は後続の実施形態/特徴/態様の方法。
15.前記回転式アトマイザディスクは直径が少なくとも20mmである、任意の先行の又は後続の実施形態/特徴/態様の方法。
16.前記回転式アトマイザディスクは直径が約20mm〜約200mmである、任意の先行の又は後続の実施形態/特徴/態様の方法。
17.前記回転式アトマイザディスクは直径が約35mm〜約150mmである、任意の先行の又は後続の実施形態/特徴/態様の方法。
18.前記回転式アトマイザディスクは直径が約50mm〜約125mmである、任意の先行の又は後続の実施形態/特徴/態様の方法。
19.前記スプレイドライヤは入口温度が少なくとも100℃である、任意の先行の又は後続の実施形態/特徴/態様の方法。
20.前記スプレイドライヤは入口温度が約100℃〜約200℃である、任意の先行の又は後続の実施形態/特徴/態様の方法。
21.前記スプレイドライヤは入口温度が約120℃〜約170℃である、任意の先行の又は後続の実施形態/特徴/態様の方法。
22.前記スプレイドライヤは入口温度が約130℃〜約150℃である、任意の先行の又は後続の実施形態/特徴/態様の方法。
23.前記スプレイドライヤは出口温度が入口温度よりも少なくとも10℃だけ低い、任意の先行の又は後続の実施形態/特徴/態様の方法。
24.前記スプレイドライヤは出口温度が入口温度よりも少なくとも20℃だけ低い、任意の先行の又は後続の実施形態/特徴/態様の方法。
25.前記スプレイドライヤは出口温度が入口温度よりも少なくとも30℃だけ低い、任意の先行の又は後続の実施形態/特徴/態様の方法。
26.前記スプレイドライヤは出口温度が入口温度よりも少なくとも50℃だけ低い、任意の先行の又は後続の実施形態/特徴/態様の方法。
27.前記スプレイドライヤは出口温度が入口温度よりも約10℃〜約100℃だけ低い、任意の先行の又は後続の実施形態/特徴/態様の方法。
28.前記スプレイドライヤは出口温度が入口温度よりも約50℃〜約100℃だけ低い、任意の先行の又は後続の実施形態/特徴/態様の方法。
29.前記スラリーは少なくとも0.5kg/時のフィード速度で前記スプレイドライヤ中にフィードされる、任意の先行の又は後続の実施形態/特徴/態様の方法。
30.前記スラリーは少なくとも1kg/時のフィード速度で前記スプレイドライヤ中にフィードされる、任意の先行の又は後続の実施形態/特徴/態様の方法。
31.前記スラリーは少なくとも2kg/時のフィード速度で前記スプレイドライヤ中にフィードされる、任意の先行の又は後続の実施形態/特徴/態様の方法。
32.前記スラリーは約0.5kg/時〜約5kg/時のフィード速度で前記スプレイドライヤ中にフィードされる、任意の先行の又は後続の実施形態/特徴/態様の方法。
33.前記スラリーは約1kg/時〜約4kg/時のフィード速度で前記スプレイドライヤ中にフィードされる、任意の先行の又は後続の実施形態/特徴/態様の方法。
34.前記コンデンサグレード粉末を乾燥し、さらに湿分含有率を低減することをさらに含む、任意の先行の又は後続の実施形態/特徴/態様の方法。
35.前記乾燥は少なくとも50℃の温度で少なくとも1時間である、任意の先行の又は後続の実施形態/特徴/態様の方法。
36.前記乾燥は少なくとも70℃の温度で少なくとも3時間である、任意の先行の又は後続の実施形態/特徴/態様の方法。
37.前記コンデンサグレード粉末を乾燥し、さらに湿分含有率を、前記コンデンサグレード粉末の質量を基準として0.5wt%未満の湿分含有率まで低減することをさらに含む、任意の先行の又は後続の実施形態/特徴/態様の方法。
38.前記熱処理は少なくとも800℃の温度である、任意の先行の又は後続の実施形態/特徴/態様の方法。
39.前記熱処理は少なくとも1,000℃の温度である、任意の先行の又は後続の実施形態/特徴/態様の方法。
40.前記熱処理は約800℃〜約1,300℃の温度である、任意の先行の又は後続の実施形態/特徴/態様の方法。
41.前記熱処理は約1,000℃〜約1,300℃の温度である、任意の先行の又は後続の実施形態/特徴/態様の方法。
42.前記熱処理は少なくとも10分である、任意の先行の又は後続の実施形態/特徴/態様の方法。
43.前記熱処理は少なくとも30分である、任意の先行の又は後続の実施形態/特徴/態様の方法。
44.前記熱処理は約10分〜2時間の時間である、任意の先行の又は後続の実施形態/特徴/態様の方法。
45.前記コンデンサグレード粉末に少なくとも1回の脱酸素化を受けさせることをさらに含む、任意の先行の又は後続の実施形態/特徴/態様の方法。
46.前記脱酸素化は前記コンデンサグレード粉末を少なくとも1種の酸素ゲッターの存在下で約500℃〜1,000℃の温度に付すことを含む、任意の先行の又は後続の実施形態/特徴/態様の方法。
47.前記脱酸素化は少なくとも1種の酸素ゲッターを使用することを含む、任意の先行の又は後続の実施形態/特徴/態様の方法。
48.前記酸素ゲッターはマグネシウム金属である、任意の先行の又は後続の実施形態/特徴/態様の方法。
49.前記スラリー中の前記粉末はリンドープされている、任意の先行の又は後続の実施形態/特徴/態様の方法。
50.前記スラリー中の前記粉末は少なくとも50ppmのレベルにリンドープされている、任意の先行の又は後続の実施形態/特徴/態様の方法。
51.前記スラリー中の前記粉末は少なくとも100ppmのレベルにリンドープされている、任意の先行の又は後続の実施形態/特徴/態様の方法。
52.前記スラリー中の前記粉末は約50ppm〜約500ppmのレベルにリンドープされている、任意の先行の又は後続の実施形態/特徴/態様の方法。
53.前記粉末はナトリウム還元されたタンタル粉末である、任意の先行の又は後続の実施形態/特徴/態様の方法。
54.前記粉末は酸洗浄された粉末である、任意の先行の又は後続の実施形態/特徴/態様の方法。
55.前記粉末は酸洗浄されかつ真空乾燥された粉末である、任意の先行の又は後続の実施形態/特徴/態様の方法。
56.前記粉末はナトリウム還元されたタンタル粉末であって、前記スラリーを形成する前に酸洗浄されかつ真空乾燥されたものである、任意の先行の又は後続の実施形態/特徴/態様の方法。
57.前記スラリーを形成する前に前記粉末を破砕することをさらに含む、任意の先行の又は後続の実施形態/特徴/態様の方法。
58.前記破砕はミルを通して前記粉末をフィードすることを含む、任意の先行の又は後続の実施形態/特徴/態様の方法。
59.前記破砕はMicrotrac(マイクロトラック)により測定して、粒度を5ミクロンより大きいD50から2.5ミクロン未満の粒度までに低減する、任意の先行の又は後続の実施形態/特徴/態様の方法。
60.前記コンデンサグレード粉末はスコット密度(Scott density)が少なくとも14g/in3である、任意の先行の又は後続の実施形態/特徴/態様の方法。
61.前記コンデンサグレード粉末はスコット密度が少なくとも20g/in3である、任意の先行の又は後続の実施形態/特徴/態様の方法。
62.前記コンデンサグレード粉末はスコット密度が少なくとも25g/in3である、任意の先行の又は後続の実施形態/特徴/態様の方法。
63.前記コンデンサグレード粉末はスコット密度が約20g/in3〜約405g/in3である、任意の先行の又は後続の実施形態/特徴/態様の方法。
64.前記コンデンサグレード粉末はスコット密度が約14g/in3〜約40g/in3である、任意の先行の又は後続の実施形態/特徴/態様の方法。
65.前記コンデンサグレード粉末は下記の特性の少なくとも1つ:
a)スコット密度が約14g/in3〜約40g/in3である、
b)D10粒度が約5ミクロン〜約25ミクロンである、
c)D50粒度が約20ミクロン〜約50ミクロンである、
d)D90粒度が約30ミクロン〜約100ミクロンである、
e)BET表面積が約0.5m2/g〜約20m2/gである、
を有する、任意の先行の又は後続の実施形態/特徴/態様の方法。
66.前記コンデンサグレード粉末は下記の特性の少なくとも1つ:
a)スコット密度が約20g/in3〜約37g/in3である、
b)D10粒度が約12ミクロン〜約25ミクロンである、
c)D50粒度が約20ミクロン〜約40ミクロンである、
d)D90粒度が約30ミクロン〜約70ミクロンである、
e)BET表面積が約0.7m2/g〜約15m2/gである、
を有する、任意の先行の又は後続の実施形態/特徴/態様の方法。
67.前記スラリーは前記スラリーの総質量を基準として約35wt%〜約70wt%のタンタル粉末を含み、
前記スラリーは水性スラリーであり、
前記回転式アトマイザディスクは約10,000rpm〜約50,000rpmで回転し、
前記回転式アトマイザディスクは直径が約20mm〜約200mmであり、
前記スプレイドライヤは入口温度が約100℃〜約200℃であり、
前記スプレイドライヤは出口温度が入口温度よりも少なくとも35℃だけ低く、
前記スラリーは前記スプレイドライヤ中に少なくとも0.5kg/時のフィード速度でフィードされ、
前記熱処理は少なくとも800℃の温度である、任意の先行の又は後続の実施形態/特徴/態様の方法。
68.前記回転式アトマイザディスクは少なくとも25m/秒の外周速度で回転する、任意の先行の又は後続の実施形態/特徴/態様の方法。
69.前記回転式アトマイザディスクは少なくとも30m/秒の外周速度で回転する、任意の先行の又は後続の実施形態/特徴/態様の方法。
70.前記回転式アトマイザディスクは約25m/秒〜約125m/秒の外周速度で回転する、任意の先行の又は後続の実施形態/特徴/態様の方法。
71.前記回転式アトマイザディスクは約30m/秒〜約100m/秒の外周速度で回転する、任意の先行の又は後続の実施形態/特徴/態様の方法。
Claims (10)
- 粉末を製造する方法であって、
回転式アトマイザディスクを含むスプレイドライヤ中に粉末のスラリーをフィードし、そして乾燥した凝集粉末を形成すること、及び、
前記乾燥した凝集粉末を熱処理して、前記粉末を形成すること、
を含み、前記粉末はタンタル、ニオブ又はニオブ亜酸化物であり、前記粉末は下記の特性の少なくとも1つ:
a)スコット密度が14g/in 3 〜40g/in 3 である、
b)D10粒度が5ミクロン〜25ミクロンである、
c)D50粒度が20ミクロン〜50ミクロンである、
d)D90粒度が30ミクロン〜100ミクロンである、
e)BET表面積が0.5m 2 /g〜20m 2 /gである、
を有する、方法。 - 前記粉末はタンタル金属粉末である、請求項1記載の方法。
- 前記スラリーは、前記スラリーの総質量を基準として、35wt%〜70wt%のタンタル粉末を含む、請求項1記載の方法。
- 前記スラリーは水性スラリーである、請求項3記載の方法。
- 前記回転式アトマイザディスクは10,000rpm〜50,000rpmで回転し、
前記回転式アトマイザディスクは直径が20mm〜200mmであり、
前記スプレイドライヤは入口温度が100℃〜200℃であり、
前記スプレイドライヤは出口温度が入口温度よりも50℃〜100℃だけ低く、
前記回転式アトマイザディスクは25m/秒〜125m/秒の外周速度で回転する、請求項1記載の方法。 - 前記スラリーは0.5kg/時〜5kg/時のフィード速度で前記スプレイドライヤ中にフィードされる、請求項1記載の方法。
- 前記粉末を乾燥し、さらに湿分含有率を低減することをさらに含む、請求項1記載の方法。
- 前記粉末に少なくとも1回の脱酸素化を受けさせることをさらに含む、請求項1記載の方法。
- 前記粉末はナトリウム還元されたタンタル粉末である、請求項1記載の方法。
- 前記スラリーは前記スラリーの総質量を基準として35wt%〜70wt%のタンタル粉末を含み、
前記スラリーは水性スラリーであり、
前記回転式アトマイザディスクは10,000rpm〜50,000rpmで回転し、
前記回転式アトマイザディスクは直径が20mm〜200mmであり、
前記スプレイドライヤは入口温度が100℃〜200℃であり、
前記スプレイドライヤは出口温度が入口温度よりも少なくとも35℃だけ低く、
前記スラリーは前記スプレイドライヤ中に少なくとも0.5kg/時のフィード速度でフィードされ、
前記熱処理は少なくとも800℃の温度である、請求項1記載の方法。
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