CN1212910C - 铌粉末及固体电解电容器 - Google Patents
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- 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
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/045—Alloys based on refractory metals
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Abstract
本发明公开了一种固体电解电容器，通过在铌粉末中添加微量成分，制造使固体电解电容器的漏电流减小、使静电容量提高、静电容量大、损耗系数小的电解电容器。具体解决措施如下：将含有1ppm以上、600ppm以下的氢；1ppm以上、200ppm以下的碳或1ppm以上、50ppm以下的镍；其余量实质上是铌的铌粉末的原料制成烧结体，并将此烧结体制成固体电解电容器(10)内部的阳极。
Description
技术领域
本发明涉及铌粉末组成以及使用这种粉末制成的固体电解电容器。
背景技术
近年来铌作为具有高静电容量的固体电解电容器的阳极倍受关注。图1中示意地表示固体电解电容器的纵向剖面图。固体电解电容器10由铌11、氧化铌12、固体电解质13、石墨14、银15层叠而构成。该固体电解电容器10的制造工艺如下：将铌粉末在约1000～1400℃烧结，制成多孔性烧结体后，进行化成处理，使得在铌11的表面形成氧化铌。接着，形成固体电解质13、石墨14、银15。接着，将阳极18(外部端子)连接于铌11，将阴极19(外部端子)通过导电性粘结剂16连接于银15，最后，加装树脂模17，经过老炼工艺而制成。
以往，如特开昭64-73009号公报及特开平6-25701号公报中所记载的那样，要求用于固体电解电容器的铌粉末是高纯度的。一般认为纯度越高越好。特开昭64-73009号公报中没有给出有关纯度的具体数值。特开平6-25701号公报中的记载为：氧不超过100ppm或者不超过5000ppm；非氧化物杂质的总和不超过200ppm或者不超过5000ppm。但没有记载有关具体的非氧化物杂质名称及含量。
另一方面，特开2000-226607号公报中指出，如果在铌粉末中添加特定元素，就会提高所制成的阳极的容量。即，其记载为：“添加从氮、磷、硼、硫、硅、氟、钇、镁等公知的元素中选择的一种以上的参杂剂。这些元素在铌粉末的烧结过程中起抑制剂作用，从而起到提高阳极容量的作用，还具有改善化成氧化膜的膜质的效果。这些元素以氩气或氢气为载气，以单体或由氢还原的化合物的形式添加。添加量通常为对铌1000ppm以下”。但没有定量给出添加物的种类、量及其具体效果。
发明内容
本发明的目的是，通过在铌粉末中适量添加氢、碳、或镍，提供一种适用于制造漏电流小而静电容量大的固体电解电容器的铌粉末、以及使用这种铌粉末的固体电解电容器。
以往，没有完全公开的关于在铌粉末中添加氢、碳、或镍的记载。本发明者们发现了通过在铌粉末中适量添加氢、碳、或镍，就能够达到上述目的，并完成了本发明。即，本发明的第1个发明为一种铌粉末，其特征是：含有1ppm以上、600ppm以下的氢，其余量实质上是铌。氢的含量不到1ppm时，漏电流大、而且静电容量不够大，因此规定1ppm以上；在1～600ppm的范围内时，漏电流小、静电容量出现最大值；氢的含量超过600ppm时，反而漏电流增加、静电容量减小，因此，以600ppm为上限。
本发明的第2个发明为一种铌粉末，其特征是：含有1ppm以上、200ppm以下的碳，其余量实质上是铌。碳的含量不到1ppm时，漏电流大、静电容量不够大；而碳的含量超过200ppm时，反而漏电流增加、静电容量减小，因此以200ppm为上限。
本发明的第3个发明为一种铌粉末，其特征是：含有1ppm以上、50ppm以下的镍，其余量实质上是铌。镍的含量不到1ppm时，漏电流大、静电容量不够大；而镍的含量超过50ppm时，反而漏电流增加、静电容量减小，因此以50ppm为上限。
本发明的第4个发明为一种铌粉末，其特征是：含有从氢：1ppm以上、600ppm以下、碳：1ppm以上、200ppm以下、镍：1ppm以上、50ppm以下之中所选择的2种以上，其余量实质上是铌。
还有，本发明的第5个发明是提供一种固体电解电容器，其特征是：将以上述含有1ppm以上、600ppm以下的氢的铌粉末、含有1ppm以上、200ppm以下的碳的铌粉末、含有1ppm以上、50ppm以下的镍的铌粉末；或含有从氢：1ppm以上、600ppm以下、碳：1ppm以上、200ppm以下、镍：1ppm以上、50ppm以下之中所选择的2种以上，其余量实质上是铌为特征的铌粉末之中的任何一种作为原料的烧结体制成电容器内部的阳极。
以往公知的铌粉末其1次粒子的平均粒径小，例如不到50nm(0.050μm)或50～150nm(0.050～0.150μm)，如果将这样细微的铌粉末烧结、制成阳极，则存在用作烧结体的粒子过小的缺点，在化成处理工艺中，铌将成为氧化铌而损失掉，导致未氧化的铌的量减少。因而，电极面积减小，不能获得超高容量的电容器。此处，在本发明的第1～第3个发明中，理想的是，1次粒子的平均粒径为0.150μm以上、2μm以下。如果铌粉末粒子过大，在制造烧结体时就难以进行烧结。另外，1次粒子是指在SEM显微镜下观察，能够作为单体粒子看到的、没有凝聚的粒子。平均粒径是指在粒度分布图中个数累积达50％时的粒径。
附图说明
图1是固体电解电容器的剖面示意图。
具体实施方式
以下对本发明的具体实施方式进行说明。
采用铌粉末、根据以下所述方法制作固体电解电容器，并测量其漏电流和静电容量。将用于阳极的φ0.5mm的铌线材埋入0.2g的铌粉末中并压制成型，制成颗粒。压制时的压强为50～150MN/m2，压制体的体积密度为2800～3200kg/m3。将制成的颗料在炉内压强1×10-3以下、温度1000～1400℃烧成。将烧成后的样品浸泡在0.8质量％的磷酸水溶液中，加6小时20V的电压，使得在颗料表面生成化成被膜。此后，用40质量％的硫酸水溶液测量铌电容器的漏电流和静电容量。在测量电压14V测定5分钟后漏电流的电流值。在偏置电压为1.5V的条件下测量静电容量。
固体电解电容器用铌粉末的制造方法包括由镁、钠、或氢将五氯化铌还原、由钠将氟化铌还原、由碳或铝将氧化铌还原等等。
以下，列举实施例并对本发明的具体实施例进行说明。
(实施例1～3、比较例1～2)
由氢还原五氯化铌而制成铌粉末。将这种铌粉末置于氢气氛围中、在1100℃的温度下、改变时间进行加热处理，并调整氢向铌粉末的导入量。采用热传导式气体分析仪，测量氢的量。此后，制作如上所述的电容器、测量电容器的漏电流和静电容量的值。结果如表1所示，氢含量在1ppm～600ppm的范围内时，漏电流小、静电容量大；在此上下限之外的结果则不理想。
(实施例4～5、比较例3～4)
通过氧化铌的铝还原制成铌粉末。使添加到这种铌粉末的萘的添加量进行各种变化、在1100℃的温度下、按规定的时间进行加热处理，并调整碳向铌粉末的导入量。用燃烧红外吸收分析仪来测量碳的量。此后，制作如上所述的电容器、测量电容器的漏电流和静电容量的值。结果如表2所示，碳含量在1ppm～200ppm的范围内时，漏电流小、静电容量大；如果不到1ppm或超过200ppm，则漏电流增大、静电容量减小。
(实施例6～7、比较例5～6)
由铝还原氧化铌而制成铌粉末。使添加到这种铌粉末的羰基镍的添加量进行各种变化、在1100℃的温度下、按规定的时间进行加热处理，并调整镍向铌粉末的导入量。用等离子体激发质量分析仪测量镍的量。此后，制作如上所述的电容器、测量电容器的漏电流和静电容量的值。结果如表3所示，镍含量在1ppm～50ppm的范围内时，漏电流小、静电容量大，结果好；在此范围之外则性能变差。
工业实用性
本发明根据在铌粉末中按规定量添加特定的成分，能够获得漏电流小且静电容量大的固体电解电容器。
表1
| 氢含有率(ppm) | 漏电流(μA/μF) | 静电容量(μFV/g) | 1次粒子的平均粒径(μm) | |
| 比较例1 | 0.5 | 0.015 | 70,500 | 0.5 |
| 实施例1 | 5 | 0.0088 | 75,000 | 0.7 |
| 实施例2 | 200 | 0.0083 | 76,000 | 0.5 |
| 实施例3 | 550 | 0.0087 | 75,500 | 0.6 |
| 比较例2 | 700 | 0.018 | 69,000 | 0.6 |
表2
| 碳含有率(ppm) | 漏电流(μA/μF) | 静电容量(μFV/g) | 1次粒子的平均粒径(μm) | |
| 比较例3 | 0.5 | 0.015 | 70,500 | 0.3 |
| 实施例4 | 3 | 0.0080 | 77,000 | 0.4 |
| 实施例5 | 180 | 0.0087 | 78,000 | 0.4 |
| 比较例4 | 250 | 0.020 | 73,500 | 0.4 |
表3
| 镍含有率(ppm) | 漏电流(μA/μF) | 静电容量(μFV/g) | 1次粒子的平均粒径(μm) | |
| 比较例5 | 0.5 | 0.012 | 70,000 | 0.4 |
| 实施例6 | 2 | 0.0088 | 75,000 | 0.4 |
| 实施例7 | 40 | 0.0086 | 75,000 | 0.4 |
| 比较例6 | 60 | 0.028 | 65,500 | 0.5 |
Claims (3)
1.一种铌粉末，其特征在于，含有1ppm以上、600ppm以下的氢，其余量实质上是铌。
2.一种铌粉末，其特征在于，含有氢：1ppm以上、600ppm以下，进而含有碳：1ppm以上、200ppm以下和/或镍：1ppm以上、50ppm以下，其余量实质上是铌。
3.一种固体电解电容器，其特征在于，将以权利要求1或2中所述的铌粉末为原料的烧结体制成电容器内部的阳极。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002011824A JP2003213301A (ja) | 2002-01-21 | 2002-01-21 | ニオブ粉末及び固体電解コンデンサ |
| JP11824/2002 | 2002-01-21 |
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| Publication Number | Publication Date |
|---|---|
| CN1533312A CN1533312A (zh) | 2004-09-29 |
| CN1212910C true CN1212910C (zh) | 2005-08-03 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB038006871A Expired - Fee Related CN1212910C (zh) | 2002-01-21 | 2003-01-21 | 铌粉末及固体电解电容器 |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US20040244531A1 (zh) |
| EP (1) | EP1502680A4 (zh) |
| JP (1) | JP2003213301A (zh) |
| KR (1) | KR20040079403A (zh) |
| CN (1) | CN1212910C (zh) |
| TW (1) | TWI266661B (zh) |
| WO (1) | WO2003061881A1 (zh) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PL370639A1 (en) * | 2002-01-24 | 2005-05-30 | H.C.Starck Inc. | Capacitor-grade lead wires with increased tensile strength and hardness |
| CN107924763B (zh) * | 2015-08-12 | 2020-04-17 | 株式会社村田制作所 | 电容器及其制造方法、基板和电容器集合基板 |
| CN106868370A (zh) * | 2017-02-09 | 2017-06-20 | 武汉华智科创高新技术有限公司 | 一种抗氧化的铌合金粉末配方 |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1471183A (fr) * | 1965-12-31 | 1967-03-03 | Kuhlmann Ets | Procédé pour l'obtention de poudres métalliques ou composites par réduction directe des halogénures correspondants |
| EP0532658B1 (en) * | 1990-06-06 | 1997-09-10 | Cabot Corporation | Tantalum or niobium base alloys |
| WO2000049633A1 (fr) * | 1999-02-16 | 2000-08-24 | Showa Denko K.K. | Poudre de niobium, element fritte a base de niobium, condensateur renfermant cet element et procede de fabrication de ce condensateur |
| CN100381234C (zh) * | 1999-03-19 | 2008-04-16 | 卡伯特公司 | 通过研磨制备铌和其它金属粉末 |
| DE19953946A1 (de) * | 1999-11-09 | 2001-05-10 | Starck H C Gmbh Co Kg | Kondensatorpulver |
| US6423110B1 (en) * | 1999-12-08 | 2002-07-23 | Showa Denko K.K. | Powder composition for capacitor and sintered body using the composition, and capacitor using the sintered body |
| DE10030387A1 (de) * | 2000-06-21 | 2002-01-03 | Starck H C Gmbh Co Kg | Kondensatorpulver |
-
2002
- 2002-01-21 JP JP2002011824A patent/JP2003213301A/ja active Pending
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2003
- 2003-01-21 EP EP03701817A patent/EP1502680A4/en not_active Withdrawn
- 2003-01-21 TW TW092101259A patent/TWI266661B/zh not_active IP Right Cessation
- 2003-01-21 WO PCT/JP2003/000459 patent/WO2003061881A1/ja not_active Application Discontinuation
- 2003-01-21 US US10/485,295 patent/US20040244531A1/en not_active Abandoned
- 2003-01-21 KR KR10-2004-7000852A patent/KR20040079403A/ko not_active Application Discontinuation
- 2003-01-21 CN CNB038006871A patent/CN1212910C/zh not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| US20040244531A1 (en) | 2004-12-09 |
| TWI266661B (en) | 2006-11-21 |
| EP1502680A1 (en) | 2005-02-02 |
| CN1533312A (zh) | 2004-09-29 |
| WO2003061881A1 (fr) | 2003-07-31 |
| KR20040079403A (ko) | 2004-09-14 |
| JP2003213301A (ja) | 2003-07-30 |
| EP1502680A4 (en) | 2007-04-04 |
| TW200302144A (en) | 2003-08-01 |
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