CN100547695C - 耐高温的铌导线、生产方法及其应用 - Google Patents
耐高温的铌导线、生产方法及其应用 Download PDFInfo
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- CN100547695C CN100547695C CNB2005100544020A CN200510054402A CN100547695C CN 100547695 C CN100547695 C CN 100547695C CN B2005100544020 A CNB2005100544020 A CN B2005100544020A CN 200510054402 A CN200510054402 A CN 200510054402A CN 100547695 C CN100547695 C CN 100547695C
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- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000010955 niobium Substances 0.000 claims abstract description 31
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 24
- 239000003990 capacitor Substances 0.000 claims abstract description 14
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 13
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 12
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 9
- 239000011574 phosphorus Substances 0.000 claims abstract description 9
- 229910000484 niobium oxide Inorganic materials 0.000 claims abstract description 5
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 11
- 238000005245 sintering Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 4
- 238000010894 electron beam technology Methods 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 3
- 229910001257 Nb alloy Inorganic materials 0.000 description 2
- ROSDCCJGGBNDNL-UHFFFAOYSA-N [Ta].[Pb] Chemical compound [Ta].[Pb] ROSDCCJGGBNDNL-UHFFFAOYSA-N 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910001096 P alloy Inorganic materials 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001033 granulometry Methods 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- BFRGSJVXBIWTCF-UHFFFAOYSA-N niobium monoxide Chemical compound [Nb]=O BFRGSJVXBIWTCF-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
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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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/052—Sintered electrodes
- H01G9/0525—Powder therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- Mechanical Engineering (AREA)
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- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Powder Metallurgy (AREA)
- Insulated Conductors (AREA)
- Superconductors And Manufacturing Methods Therefor (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Organic Insulating Materials (AREA)
- Inorganic Insulating Materials (AREA)
Abstract
富集磷的耐高温铌导线,适用于作为铌、氧化铌或钽电容器的连线使用。
Description
技术领域
本发明涉及高温条件下保持稳定的铌金属导线的生产方法及其与铌-或氧化铌或钽电容器连接时的应用。
背景技术
为了能与金属粉末-电容器连接,需要采用耐高温金属材料做成的导线,而铌电容器是采用颗粒更粗、价格更便宜的铌粉,在1400℃以上温度条件下进行烧结而成的。一般情况下,钽导线也能承受这一高温,然而由于钽的比重大约是铌的两倍,因此材料消耗大。粉末材料部分主要是由铌构成的已加工好的电容器以及烧结毛坯的下脚料不能与钽分开,因此不能将铌提供一个经济的再生循环过程。采用铌导线就能解决这一问题。此外,由于市场上钽的价格波动很厉害,以致于使原材料成本难以控制,因此人们希望获得价格低廉的以铌为基材的代用材料。再有,由于作为原材料,铌的价格稳定,因此也希望在钽电容器上采用铌作为连接导线。
对于未掺杂的铌,作为在1600℃温度下钽(Ta)和钨(W)的焊接材料已为人们所熟悉(请参看Werner Espe的《高真空技术的工业材料学》第一册,“金属与导电金属材料”VED德国科学出版社,1959),但在这项应用中,对材料既不要求它在往复弯曲载荷下具有晶粒稳定性,也不要求对脆化和断裂显示出稳定性。
有人曾推荐采用铌导线来连接粉末阳极,例如,在US6358625B1中就对于用铌或钽做成的阳极导线作了介绍。为改善它们附着性,用氧进行处理,使其表面大约50nm深度范围内约有35%的原子获得富集。正常情况下铌-钽导线只包含少量的氧,对于钽一般规定含氧量在50-600微克/克。表面富集对于一般性能(如导电性)并不会产生影响,但其粘附性将会升高。烧结温度规定为1250℃左右。正如尚未授权的德国专利申请DE10304756认为,掺杂氧的铌导线,它们在大约1300℃时就达到了使用极限。
因此在技术上取决于找到一种以铌为基体的合适材料,使它们在使用温度超过1400℃时不构成粗晶粒,同时其导电性能可与纯铌相比,并能不会因此而脆化或断裂,以便承受电容器生产过程的弯折程序。
现已发现,只需极少量的磷掺混其中就会对铌的重结晶温度及铌晶粒的开始形成和形成的进程产生很大影响。
掺杂有P(磷)的铌在1400℃下灼热20分钟才显示出ASTM9中要求的颗粒粒径,这相当于1200℃下含氧铌的颗粒粒径及在900℃下无掺杂的铌颗粒粒径。NbP颗粒明显粗化是在1600℃以上才出现的。
另外,在1600℃时将到达ASTM5中的粒度标准。
发明内容
按照本发明的材料,连接铌电容器的铌导线具有广泛的应用性,由于这种材料即使在1600℃也不会有大量的颗粒形成、不变脆,而且,能承受在钽电容器上的应用,这一点对于微型结构特别引人注目,因为,在这种情况下,它有助于明显降低钽导线的成本。
可通过以下程序实现铌的掺杂(Dotierung):
-加入P或含P预合金,借助于电子束熔化;
-加入P或含P预合金,借助于电弧熔化;
-在Nb-粉末中加入P或含P预合金,生产烧结块;或者,
-将已掺杂P的Nb粉末生产烧结块。
生成的含P合金可以在室温条件下加工成直径为0.15-0.4mm的导线。这种导线最适合于作为铌或氧化铌或钽电容器上的连接导线使用。这种电容器是用金属粉末生产出来的。通过烧结(和导线一起)金属就会被“固定”在表面上,即被阳极氧化,与此同时就会形成极薄一层Nb2O5或Ta2O5作为电介质。
附图说明
图1至图3显示机械性能(强度及延伸性),按照本发明制成的直径为0.24mm的含P铌导线的在各种不同温度条件下经过20分钟烧结后的粒度(ASTM标准)和弯曲次数。
具体实施方式
以下将通过实施例对本发明作进一步的详细阐述,但并不限于例中内容:
在铌-熔融块中均匀地加入含P10%的预合金,通过电子束熔融过程将P掺杂,即获得一含P量为100-2000微克/克的铌合金,这样制得的铌合金可以在室温条件下被拉制成直径为0.15-0.4mm的铌导线。
借助于退火试验,模拟电容器生产过程中烧结的真实条件,以证实这种合金能承受高温加工处理。用Nb(标准Nb)和掺杂有3000微克/克氧(即“NbO”)的铌作为对比样。
试验结果汇总于下表中:
Nb的质量 | 退火温度 | ASTM标准的最终粒度规格 | 往复弯曲次数 |
标准Nb标准Nb | 900℃1000℃ | 74 | >105 |
NbONbONbO | 90012001300 | 1274 | >1082 |
NbPNbPNbPNbPNbPNbPNbPNbPNbPNbP | 900120013001400150016001700180019002000 | 形变结构999874 | 未确定>40>40>40>40>20>20151212 |
这项实验表明,在大约1500℃以前颗粒是稳定的,而从1600℃起颗粒开始粗糙化。在1600℃温度时烧结的机械性能(弯曲数)也足以保证在电容器生产过程中顺利加工处理的需要。
本文图1至图3显示了机械性能(强度及延伸性),这是指按照本发明制成的直径为0.24mm的含P铌导线的在各种不同温度条件下经过20分钟烧结后的粒度(ASTM标准)和弯曲次数。这种典型导线中的含P量为350微克/克。
(图中,Rm=抗拉强度;Rp0.2=0.2%屈服点;Al254=相对于原长度254mm的断裂伸长率)
Claims (5)
1、耐受高温铌导线,其特征是含有磷,铌导线中含磷量在50-2000微克/克范围内。
2、根据权利要求1所述的耐受高温铌导线的生产方法,其特征是:
a)将铌在加入磷或含磷合金条件下通过电子束熔融或电弧熔化或烧结来掺杂磷;或
b)将已掺杂磷的铌粉烧结;
并将所获材料拉制成导线。
3、按照权利要求2所述的方法,其特征是,拉成的导线直径在0.2-0.4mm范围内。
4、按照权利要求2所述的方法,其特征是,导线是在室温条件下拉制成的。
5、根据权利要求1所述的耐受高温铌导线的应用,其特征是作为铌或氧化铌、或钽电容器的连线使用的。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102004011214A DE102004011214A1 (de) | 2004-03-04 | 2004-03-04 | Hochtemperaturbeständiger Niob-Draht |
DE102004011214.2 | 2004-03-04 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1828781A CN1828781A (zh) | 2006-09-06 |
CN100547695C true CN100547695C (zh) | 2009-10-07 |
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Application Number | Title | Priority Date | Filing Date |
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CNB2005100544020A Expired - Fee Related CN100547695C (zh) | 2004-03-04 | 2005-03-04 | 耐高温的铌导线、生产方法及其应用 |
Country Status (14)
Country | Link |
---|---|
US (1) | US7704448B2 (zh) |
EP (1) | EP1571228B1 (zh) |
JP (1) | JP4886199B2 (zh) |
CN (1) | CN100547695C (zh) |
AT (1) | ATE353984T1 (zh) |
BR (1) | BRPI0500699A (zh) |
DE (2) | DE102004011214A1 (zh) |
DK (1) | DK1571228T3 (zh) |
ES (1) | ES2281032T3 (zh) |
IL (1) | IL167218A (zh) |
PL (1) | PL1571228T3 (zh) |
PT (1) | PT1571228E (zh) |
RU (1) | RU2341577C2 (zh) |
SI (1) | SI1571228T1 (zh) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108778573A (zh) * | 2016-03-03 | 2018-11-09 | H.C.施塔克公司 | 通过增材制造制备金属部件 |
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DE102005038551B3 (de) * | 2005-08-12 | 2007-04-05 | W.C. Heraeus Gmbh | Draht und Gestell für einseitig gesockelte Lampen auf Basis von Niob oder Tantal sowie Herstellungsverfahren und Verwendung |
JP2009505412A (ja) | 2005-08-19 | 2009-02-05 | エイブイエックス リミテッド | ポリマーベースの固体コンデンサおよびその製造方法 |
GB0517952D0 (en) * | 2005-09-02 | 2005-10-12 | Avx Ltd | Method of forming anode bodies for solid state capacitors |
DE102007046899B3 (de) * | 2007-09-28 | 2009-02-12 | W.C. Heraeus Gmbh | Stromdurchführung durch Keramikbrenner in Halogen-Metalldampflampen |
US7760487B2 (en) * | 2007-10-22 | 2010-07-20 | Avx Corporation | Doped ceramic powder for use in forming capacitor anodes |
US7852615B2 (en) | 2008-01-22 | 2010-12-14 | Avx Corporation | Electrolytic capacitor anode treated with an organometallic compound |
US7760488B2 (en) * | 2008-01-22 | 2010-07-20 | Avx Corporation | Sintered anode pellet treated with a surfactant for use in an electrolytic capacitor |
US7768773B2 (en) * | 2008-01-22 | 2010-08-03 | Avx Corporation | Sintered anode pellet etched with an organic acid for use in an electrolytic capacitor |
US8203827B2 (en) * | 2009-02-20 | 2012-06-19 | Avx Corporation | Anode for a solid electrolytic capacitor containing a non-metallic surface treatment |
KR20130027785A (ko) * | 2011-09-08 | 2013-03-18 | 삼성전기주식회사 | 탄탈 캐패시터 |
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US4084965A (en) * | 1977-01-05 | 1978-04-18 | Fansteel Inc. | Columbium powder and method of making the same |
US5171379A (en) * | 1991-05-15 | 1992-12-15 | Cabot Corporation | Tantalum base alloys |
US6165623A (en) * | 1996-11-07 | 2000-12-26 | Cabot Corporation | Niobium powders and niobium electrolytic capacitors |
US20030164225A1 (en) * | 1998-04-20 | 2003-09-04 | Tadashi Sawayama | Processing apparatus, exhaust processing process and plasma processing |
US6051044A (en) * | 1998-05-04 | 2000-04-18 | Cabot Corporation | Nitrided niobium powders and niobium electrolytic capacitors |
DE19847012A1 (de) * | 1998-10-13 | 2000-04-20 | Starck H C Gmbh Co Kg | Niobpulver und Verfahren zu dessen Herstellung |
US6375704B1 (en) * | 1999-05-12 | 2002-04-23 | Cabot Corporation | High capacitance niobium powders and electrolytic capacitor anodes |
US6593532B1 (en) * | 1999-10-11 | 2003-07-15 | H. C. Starck, Inc. | Electrode lead wires |
US6358625B1 (en) | 1999-10-11 | 2002-03-19 | H. C. Starck, Inc. | Refractory metals with improved adhesion strength |
JP3718412B2 (ja) * | 2000-06-01 | 2005-11-24 | キャボットスーパーメタル株式会社 | ニオブまたはタンタル粉末およびその製造方法 |
JP2002343687A (ja) * | 2001-03-16 | 2002-11-29 | Showa Denko Kk | コンデンサ用ニオブ、及び該ニオブ焼結体を用いたコンデンサ |
WO2003019592A2 (en) * | 2001-08-22 | 2003-03-06 | Showa Denko K.K. | Tantalum capacitor with niobium alloy lead wire |
CA2473845A1 (en) * | 2002-01-24 | 2004-01-08 | H.C. Starck Inc. | Capacitor-grade lead wires with increased tensile strength and hardness |
DE10304756B4 (de) * | 2003-02-05 | 2005-04-07 | W.C. Heraeus Gmbh | Sauerstoffangereicherter Niob-Draht |
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- 2004-03-04 DE DE102004011214A patent/DE102004011214A1/de not_active Withdrawn
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- 2005-02-23 ES ES05003832T patent/ES2281032T3/es active Active
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- 2005-03-03 RU RU2005106079/02A patent/RU2341577C2/ru not_active IP Right Cessation
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108778573A (zh) * | 2016-03-03 | 2018-11-09 | H.C.施塔克公司 | 通过增材制造制备金属部件 |
CN108778573B (zh) * | 2016-03-03 | 2021-11-16 | H.C.施塔克公司 | 通过增材制造制备金属部件 |
Also Published As
Publication number | Publication date |
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ATE353984T1 (de) | 2007-03-15 |
PT1571228E (pt) | 2007-04-30 |
PL1571228T3 (pl) | 2007-07-31 |
DE502005000370D1 (de) | 2007-03-29 |
EP1571228A1 (de) | 2005-09-07 |
IL167218A (en) | 2011-08-31 |
ES2281032T3 (es) | 2007-09-16 |
RU2005106079A (ru) | 2006-08-10 |
DE102004011214A1 (de) | 2005-10-06 |
BRPI0500699A (pt) | 2005-11-08 |
EP1571228B1 (de) | 2007-02-14 |
JP4886199B2 (ja) | 2012-02-29 |
SI1571228T1 (sl) | 2007-06-30 |
IL167218A0 (en) | 2009-02-11 |
JP2005264330A (ja) | 2005-09-29 |
RU2341577C2 (ru) | 2008-12-20 |
CN1828781A (zh) | 2006-09-06 |
US7704448B2 (en) | 2010-04-27 |
DK1571228T3 (da) | 2007-04-10 |
US20050199321A1 (en) | 2005-09-15 |
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