CN1997774A - 制备具有提高的电导率的氧化镍表面的方法 - Google Patents
制备具有提高的电导率的氧化镍表面的方法 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 36
- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 18
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 90
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- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 5
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
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- 239000002184 metal Substances 0.000 claims description 6
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- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 3
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- MVYYDFCVPLFOKV-UHFFFAOYSA-M barium monohydroxide Chemical compound [Ba]O MVYYDFCVPLFOKV-UHFFFAOYSA-M 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
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- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 1
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- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
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- H01M4/24—Electrodes for alkaline accumulators
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Abstract
本发明涉及一种由含镍的材料制备导电氧化镍表面的方法，在此首先对镍表面脱脂，随后在约1％盐酸溶液中表面粗糙化约10分钟，在此过程中通过添加过氧化氢溶液加速该过程并察觉到电解液变成淡绿色，快速洗涤镍表面，镍材料浸入到由与约10％过氧化氢混合的3.5摩尔浓度的碱液构成的溶液中和保持10分钟，这样形成的氢氧化镍表面在随后的热过程中脱水和随后进一步氧化成氧化镍。此外本发明还包括根据上述的方法制备的导电界限层以及由其制备的电极和电极在氯－碱电解中，在燃料电池中和在蓄电池中的用途。
Description
本发明的对象是一种通过用碱金属氧化物化学掺杂氧化镍而制备导电的氧化镍表面的方法，特别是镍用于电化学应用中。
在电化学过程中通过外部的电流而控制化学反应。在电化学电池内部必须有导电的、稳定的和价格低的导体输送电子。在此镍证实是用于电极的理想的材料。然而不足的是要形成不导电的或导电差的镍表面，假如电极在氢氧化镍的电势以上工作的话。由于该电势是不高的，所以在许多过程中都要形成氢氧化物。
例如当纯镍在电解时用作为氧发生电极时，这种不导电的或导电差的氢氧化物层是不利的。然而在其中镍作为导电的组织、板网或薄片与催化活性的材料，如碳、铂化的碳等联合的体系中，对绝缘层也产生不利的作用。所以氢氧化物层在耗氧电极时也阻碍了最佳的电流。
由于在镍表面处的欧姆损失而使得整个体系的效率变差，如锌/空气-和镍/金属氢化物-电池，在氯碱电解时的氧阴极或在碱性燃料电池中氧电极。
已知的是，采用机械的方法对镍表面粗糙化，以产生在镍和电极的其他组成部件如活性碳之间更好的电接触。然而最初较小的电阻在工作时非常快地增大，因为镍表面被不导电的氢氧化镍覆盖了。
另一种方法是成套电极的多小时还原。主要对于直接与碳接触的镍，还原不仅只导致不导电的表面的去除，而且也导致在金属镍和碳之间较稳定的结合。这种方法的缺点是，例如不可能将成品的锌/空气-电池的空气电极-由活性碳、二氧化锰和镍组织构成-在氢电势下还原几个小时。
在开放的体系中这种方法是可能的，然而这样生成的镍和碳的化合物不是特别稳定的。特别地对于氧发生时最迟要在一个月之后再重复还原，因为在活性碳和镍组织之间已构成了新的氢氧化镍层。
已知的是，导电差的氧化镍由于少量的氧化锂而使得电导率显著增加[P.J.Fensham，J.Amer.Soc.，76，969(1954)Li2O的溶解度]。然而在施加时，必需非常高的温度。然而对于电化学应用，必需复杂的镍部件，如组织、板网或电池杯，其不允许承受高的温度负载，因为否则它们可以非常容易变形。
另外已知一种用导电的氧化镍涂覆玻璃的溶液，在此掺杂入锂和这样生成导电的涂层。这用在复印机，然而也用于工业玻璃机(Glaessern)中。这方法的缺点又是高温，如在DE 692 12 528中所描述的。
在电池技术中镍的电导率不仅对于碱性的镍/镉型蓄电池而且对于镍/金属氢化物型都是重要的，如在DE 697 21 136中描述的那样。对于锂电池，在镍中加入锂也是已知的，在此也参见DE 691 24 158。
除了高温方法也还已知低温方法，在该方法中一个活性的镍电极通过在由KOH、NaOH、BaOH和过氧化氢构成的混合物中处理而改善。然而在此只是描述了对活性电极的处理，也没有描述对纯的金属表面的处理。
这一任务的解决方案在于，提出一种方法，其使得可以在较低的温度下通过用碱金属氧化物化学掺杂氧化镍而制备导电的氧化镍表面。
这一任务通过根据权利要求1的方法而解决。本发明解决这一任务是通过
·首先对镍表面脱脂，
·随后在约1％盐酸溶液中粗糙化约10分钟，在此过程中
·通过添加过氧化氢溶液加速该过程并察觉到电解液变成淡绿色，
·快速洗涤镍表面，
·镍材料浸入到由与约10％过氧化氢混合的3.5摩尔浓度的碱液构成的溶液中和在其中保持10分钟，
·这样形成的氢氧化镍表面在随后的热过程中脱水，
·和随后进一步氧化成氧化镍。
这样生成的、掺杂的氧化镍表面以下称为导电界限层和具有优越的电导率。
在把镍材料浸入到由3.5摩尔浓度的碱液构成的溶液中时镍发生强烈的氧化，在此过程中同时掺入碱金属离子。不仅可以用氢氧化钾溶液而且可以用氢氧化钠溶液或氢氧化锂溶液作为碱液。
在本方法的一个构成中，在把镍材料浸入由3.5摩尔浓度的碱液构成的溶液中时还可以加入胶体的碳或铁、钴、钛、铱或铂的氢氧化物。在本方法的另一个构成中，脱水和进一步氧化在180℃下进行。在本方法的另一个构成中，所用的镍含有50％重量的铝或10％重量的钛或同时含有铝和钛二种金属的合金元素。
以下用两个实施例更清楚地解释本发明。实施例1根据图1和图2示出了在碱性电解液中镍表面对空气电极的电流/电压特性的作用效果，实施例2示出了掺杂的可能性。
实施例1：在图1中示出了镍放电器(Ableiter)的表面对空气电极的电化学容许负荷的影响。由活性碳和碳根据“反应混合”方法构成的混合物制备成为催化活性材料。随后这种材料棍压成金属放电器。在图1中示出的是对于未处理过的镍、还原的镍、具有导电界限层的镍、和银的电化学值。非常清楚地，当不用常用的镍组织而用具有导电界限层的镍组织可观察到极大的功率增益。因此，空气电极的功率是可与在银放电器材料上的空气电极相比较的。
当不用碳而用银作为活性材料时，显示出类似的图形。因为银催化剂本身可以参与导电，所以镍腐蚀的作用就没有如图1中所示出的那么显著。然而掺杂的氧化镍层还是有有利的影响，如在图2中所示出的那样。
实施例2：氧化镍是一种已知的用于氧发生的催化剂。所以常常在电解装置中使用Raney-镍-催化剂。现在条件是已知的，在该条件下氧发生电极应具有尽可能小的电阻。在这种情况下迄今为止具有氧化铱的涂层的镍组织用作为催化剂。
对于在此所提出的掺杂的导电界限层，有目的地将其他的催化剂加入到氧化镍中是可能的。所以可通过加入钴、铁、铱或铂在形成氢氧化物层时这些层附加地用催化活性材料掺杂。通过改变作用时间而确定导电界限层的厚度。以这种方式涂覆镍组织，那么已经达到了比例如在Raney-镍气体扩散电极小得多的电阻。在此，制备氧化镍表面时的较低的温度导致非常活泼的镍催化剂。
根据本发明的导电界限层不仅在氯-碱电解中而且在燃料电池和蓄电池中可优越地用作为电极。
Claims (7)
1、一种用来由含镍的材料制备导电的氧化镍表面的方法，其特征在于，
·首先对镍表面脱脂，
·随后在约1％盐酸溶液中粗糙化约10分钟，在此过程中
·通过添加过氧化氢溶液加速该过程并察觉到电解液变成淡绿色，
·短时间洗涤镍表面，
·镍材料浸入到由与约10％过氧化氢混合的3.5摩尔浓度的碱液构成的溶液中和在其中保持10分钟，
·这样形成的氢氧化镍表面在随后的热过程中脱水，
·和随后进一步氧化成氧化镍。
2、根据权利要求1的方法，其特征在于，在镍材料浸入3.5摩尔浓度的碱液中时也还加入胶体的碳或加入铁、钴、钛、铱或铂的氢氧化物。
3、根据权利要求1或2之一的方法，其特征在于，所形成的氢氧化镍表面的脱水和进一步氧化是在180℃的温度下进行的。
4、根据权利要求1-3之一的方法，其特征在于，所使用的镍含有50％重量的铝或10％重量的钛或同时含有铝和钛二种金属的合金元素。
5、一种导电界限层，其是根据权利要求1-4之一的方法制备的。
6、一种电极，其含有根据权利要求5的导电界限层。
7、根据权利要求6的电极在氯-碱电解中、在燃料电池中或在蓄电池中的用途。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102004034886.3 | 2004-07-19 | ||
| DE102004034886A DE102004034886A1 (de) | 2004-07-19 | 2004-07-19 | Verfahren zur Herstellung von Nickeloxidoberflächen mit erhöhter Leitfähigkeit |
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| CN1997774A true CN1997774A (zh) | 2007-07-11 |
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| CNA2005800243695A Pending CN1997774A (zh) | 2004-07-19 | 2005-07-09 | 制备具有提高的电导率的氧化镍表面的方法 |
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| Country | Link |
|---|---|
| US (1) | US8057713B2 (zh) |
| EP (1) | EP1771604A2 (zh) |
| JP (1) | JP4746618B2 (zh) |
| KR (1) | KR20070040794A (zh) |
| CN (1) | CN1997774A (zh) |
| BR (1) | BRPI0513480A (zh) |
| CA (1) | CA2574170A1 (zh) |
| DE (1) | DE102004034886A1 (zh) |
| RU (1) | RU2383659C2 (zh) |
| WO (1) | WO2006008012A2 (zh) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103492616A (zh) * | 2011-01-10 | 2014-01-01 | 蒂森克虏伯伍德公司 | 用于电解池的金属池元件材料的涂层 |
| CN110952111A (zh) * | 2019-10-31 | 2020-04-03 | 南通安思卓新能源有限公司 | 一种两步氧化合成的电解水阳极及其制备方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2015086420A (ja) * | 2013-10-29 | 2015-05-07 | 国立大学法人横浜国立大学 | アルカリ水電解用陽極 |
| RU2758442C1 (ru) * | 2020-12-08 | 2021-10-28 | Федеральное государственное бюджетное учреждение науки Институт проблем химической физики Российской Академии наук (ФГБУН ИПХФ РАН) | Композитный катодный материал и способ его получения |
| CN115044862B (zh) * | 2022-06-17 | 2023-03-10 | 长沙特耐金属材料科技有限公司 | 一种镍基合金表面硬化方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| DE8305885U1 (de) * | 1983-03-02 | 1997-07-24 | Faber Matthias Dipl Ing | Neuartige Nickelelektrode zum Einsatz in alkalischen, elektrochemischen Energiespeichersystemen |
| JPS6074272A (ja) * | 1983-09-30 | 1985-04-26 | Agency Of Ind Science & Technol | 溶融炭酸塩型燃料電池の製造方法 |
| EP0297316B1 (de) * | 1987-07-01 | 1992-01-22 | Messerschmitt-Bölkow-Blohm Gesellschaft mit beschränkter Haftung | Einrichtung zur Stromzuführung in die poröse Anode einer bipolaren Platte eines Zellenstapels in Filterpressenanordnung |
| DE68926642T2 (de) * | 1988-01-22 | 1996-11-28 | Japan Storage Battery Co Ltd | Alkalische batterien und verfahren zur herstellung |
| US5264201A (en) | 1990-07-23 | 1993-11-23 | Her Majesty The Queen In Right Of The Province Of British Columbia | Lithiated nickel dioxide and secondary cells prepared therefrom |
| IT1247908B (it) | 1991-05-08 | 1995-01-05 | Eniricerche Spa | Elettrodo di ossido di nichel intercalato con litio e dispositivi elettrocromici che lo incorporano |
| JP3289358B2 (ja) * | 1993-01-28 | 2002-06-04 | 株式会社村田製作所 | 磁性酸化物粉末の製造方法 |
| JP3664519B2 (ja) * | 1995-05-29 | 2005-06-29 | クロリンエンジニアズ株式会社 | 活性陰極の製造方法 |
| US6007946A (en) | 1996-06-26 | 1999-12-28 | Sanyo Electric Co., Ltd. | Non-sintered nickel electrode for alkaline storage battery, alkaline storage battery including the same, and method for production of non-sintered nickel electrode for alkaline storage battery |
| US5905000A (en) * | 1996-09-03 | 1999-05-18 | Nanomaterials Research Corporation | Nanostructured ion conducting solid electrolytes |
| US6586483B2 (en) * | 2001-01-08 | 2003-07-01 | 3M Innovative Properties Company | Foam including surface-modified nanoparticles |
| JP2003045420A (ja) * | 2001-07-30 | 2003-02-14 | Hitachi Maxell Ltd | 非焼結式正極、その製造方法および前記正極を用いたアルカリ蓄電池 |
| JP2003045422A (ja) * | 2001-07-30 | 2003-02-14 | Hitachi Maxell Ltd | アルカリ蓄電池 |
| JP2003068293A (ja) * | 2001-08-23 | 2003-03-07 | Hitachi Maxell Ltd | 非焼結式正極、その製造方法および前記正極を用いたアルカリ蓄電池 |
| JP3884768B2 (ja) * | 2002-06-21 | 2007-02-21 | 日立マクセル株式会社 | 電気化学素子用の電極およびこれを用いた電池 |
| WO2004020128A1 (ja) * | 2002-08-28 | 2004-03-11 | Toho Titanium Co., Ltd. | 金属ニッケル粉末及びその製造方法 |
-
2004
- 2004-07-19 DE DE102004034886A patent/DE102004034886A1/de not_active Withdrawn
-
2005
- 2005-07-09 WO PCT/EP2005/007464 patent/WO2006008012A2/de active Application Filing
- 2005-07-09 BR BRPI0513480-3A patent/BRPI0513480A/pt not_active IP Right Cessation
- 2005-07-09 CN CNA2005800243695A patent/CN1997774A/zh active Pending
- 2005-07-09 RU RU2007105880/15A patent/RU2383659C2/ru not_active IP Right Cessation
- 2005-07-09 JP JP2007521844A patent/JP4746618B2/ja not_active Expired - Fee Related
- 2005-07-09 KR KR1020077001404A patent/KR20070040794A/ko not_active Application Discontinuation
- 2005-07-09 EP EP05772399A patent/EP1771604A2/de not_active Withdrawn
- 2005-07-09 US US11/632,790 patent/US8057713B2/en not_active Expired - Fee Related
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103492616A (zh) * | 2011-01-10 | 2014-01-01 | 蒂森克虏伯伍德公司 | 用于电解池的金属池元件材料的涂层 |
| CN110952111A (zh) * | 2019-10-31 | 2020-04-03 | 南通安思卓新能源有限公司 | 一种两步氧化合成的电解水阳极及其制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20070040794A (ko) | 2007-04-17 |
| JP4746618B2 (ja) | 2011-08-10 |
| CA2574170A1 (en) | 2006-01-26 |
| RU2007105880A (ru) | 2008-08-27 |
| US8057713B2 (en) | 2011-11-15 |
| RU2383659C2 (ru) | 2010-03-10 |
| DE102004034886A1 (de) | 2006-02-16 |
| JP2008506845A (ja) | 2008-03-06 |
| WO2006008012A2 (de) | 2006-01-26 |
| WO2006008012A3 (de) | 2006-06-22 |
| BRPI0513480A (pt) | 2008-05-06 |
| EP1771604A2 (de) | 2007-04-11 |
| US20080280204A1 (en) | 2008-11-13 |
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