JPH08157902A - Production of bulk and powder of hydrogen storage alloy and intermetallic compound having active surface layer - Google Patents
Production of bulk and powder of hydrogen storage alloy and intermetallic compound having active surface layerInfo
- Publication number
- JPH08157902A JPH08157902A JP6294869A JP29486994A JPH08157902A JP H08157902 A JPH08157902 A JP H08157902A JP 6294869 A JP6294869 A JP 6294869A JP 29486994 A JP29486994 A JP 29486994A JP H08157902 A JPH08157902 A JP H08157902A
- Authority
- JP
- Japan
- Prior art keywords
- hydrogen
- powder
- alloy
- hydrogen storage
- bulk
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 35
- 239000001257 hydrogen Substances 0.000 title claims abstract description 35
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 28
- 239000000956 alloy Substances 0.000 title claims abstract description 28
- 239000000843 powder Substances 0.000 title claims abstract description 9
- 229910000765 intermetallic Inorganic materials 0.000 title claims description 16
- 239000002344 surface layer Substances 0.000 title claims description 5
- 238000004519 manufacturing process Methods 0.000 title description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 13
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 12
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 11
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 11
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 230000000694 effects Effects 0.000 claims abstract description 10
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 10
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 7
- 239000003513 alkali Substances 0.000 claims abstract description 6
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 6
- 229910052741 iridium Inorganic materials 0.000 claims abstract description 5
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 4
- 238000003795 desorption Methods 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 150000002739 metals Chemical class 0.000 claims description 3
- 238000009713 electroplating Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 238000007772 electroless plating Methods 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 229910052763 palladium Inorganic materials 0.000 abstract description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract 2
- 239000011232 storage material Substances 0.000 abstract 2
- 239000007868 Raney catalyst Substances 0.000 abstract 1
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 abstract 1
- 229910000564 Raney nickel Inorganic materials 0.000 abstract 1
- 230000001747 exhibiting effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 239000007773 negative electrode material Substances 0.000 abstract 1
- 238000004381 surface treatment Methods 0.000 abstract 1
- 229910008340 ZrNi Inorganic materials 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000010306 acid treatment Methods 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 229910000756 V alloy Inorganic materials 0.000 description 1
- 229910001093 Zr alloy Inorganic materials 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000005211 surface analysis Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
- Chemically Coating (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、成分として含まれるT
i、Zr、Hf、V、Mo、W、Al、Znなどが合金および金属間
化合物の表面に形成する不活性酸化物を、フッ化水素酸
などの酸あるいはアルカリで溶解除去し、従来より欠点
とされていたそれらの低い水素の吸収−放出速度を向上
させる技術に利用分野をもつ。The present invention relates to T contained as an ingredient.
Inactive oxides formed on the surface of alloys and intermetallic compounds such as i, Zr, Hf, V, Mo, W, Al, and Zn are dissolved and removed with acid or alkali such as hydrofluoric acid It has been applied to the technology for improving those low hydrogen absorption-desorption rates.
【０００２】[0002]
【従来の技術】成分としてTi、Zr、Hf、V、Mo、W、Al、
Znなどを含む合金あるいは金属間化合物では、上述の通
り水素吸蔵容量の点で優れている反面、表面がこれらの
成分の不活性酸化物で覆われているために水素の吸収−
放出速度は極めて遅い。しかしこれへの対処としては、
単に水素化を繰り返し多少の活性向上をはかっているの
が現状である。2. Description of the Related Art As components Ti, Zr, Hf, V, Mo, W, Al,
Alloys or intermetallic compounds containing Zn or the like are excellent in terms of hydrogen storage capacity as described above, but on the other hand, since the surface is covered with an inert oxide of these components, hydrogen absorption-
The release rate is extremely slow. However, in order to deal with this,
The present situation is that hydrogenation is simply repeated to improve the activity to some extent.
【０００３】[0003]
【発明が解決しようする課題】従来の技術では、表面に
生成したTi、Zr、Hf、V、Mo、W、Al、Znなどの不活性酸
化物を除去することができず、根本的な反応活性の阻害
要因を取り除くことは不可能であった。更に、最も多量
に水素を吸蔵できる(Ti,Zr)V2合金などでは、水素の吸
収−放出反応に活性なNi、Co、Feなどの成分を全く含ん
でおらず、従来の活性化をいくら施しても水素の吸収−
放出速度の改善には全く無意味であった。In the prior art, it was not possible to remove the inactive oxides such as Ti, Zr, Hf, V, Mo, W, Al and Zn formed on the surface, which caused a fundamental reaction. It was not possible to remove the inhibitor of activity. In addition, (Ti, Zr) V 2 alloys that can store the largest amount of hydrogen do not contain components such as Ni, Co, and Fe that are active in the absorption-desorption reaction of hydrogen at all, and the conventional activation is no matter how much. Absorption of hydrogen-
There was no point in improving the release rate.
【０００４】[0004]
【課題を解決するための手段】前記の目的を達成するた
めには、合金ならびに金属間化合物の表面に生成したT
i、Zr、Hf、V、Mo、W、Al、Znなどの不活性酸化物を除
去することが不可欠であり、除去にはこれら不活性酸化
物に対し高い溶解能をもつフッ化水素酸などの酸あるい
はアルカリが極めて有効である。また、この処理に際し
て内部のTi、Zr、Hf、V、Mo、W、Al、Znなどの金属も溶
解し、これに伴い合金および金属間化合物内に含まれる
Ni、Co、Feなどが表面に残り、水素の吸収−放出反応に
高い活性を示す多孔質層を形成することになる。一方、
水素の吸収−放出反応に対し更に高い活性もつPt、Ir、
Pdなどの貴金属を処理した表面に担持することで、飛躍
的に水素の吸収−放出速度を向上させることが可能とな
る。In order to achieve the above-mentioned object, T formed on the surface of alloys and intermetallic compounds
It is indispensable to remove inert oxides such as i, Zr, Hf, V, Mo, W, Al and Zn. The acids or alkalis are extremely effective. In addition, internal metals such as Ti, Zr, Hf, V, Mo, W, Al, and Zn are also dissolved during this treatment, and along with this, contained in the alloy and intermetallic compound.
Ni, Co, Fe, etc. remain on the surface, forming a porous layer having high activity for hydrogen absorption-desorption reaction. on the other hand,
Pt, Ir, which has higher activity for hydrogen absorption-desorption reaction,
By loading a noble metal such as Pd on the treated surface, it becomes possible to dramatically improve the absorption-desorption rate of hydrogen.
【０００５】[0005]
【作用】本発明では、Ti、Zr、Hf、V、Mo、W、Al、Znな
どを成分として含む水素吸蔵性合金および金属間化合物
を、フッ化水素酸などの酸あるいはアルカリで処理する
ことで、表面に形成されたそれら成分の不活性酸化物を
効果的に溶解除去することができ、これにより良好な水
素の吸収−放出反応活性を発現することができる。In the present invention, the hydrogen storage alloy and the intermetallic compound containing Ti, Zr, Hf, V, Mo, W, Al and Zn as components are treated with an acid such as hydrofluoric acid or an alkali. In this way, the inactive oxides of those components formed on the surface can be effectively dissolved and removed, and thereby good hydrogen absorption-release reaction activity can be expressed.
【０００６】また、表面近傍のTi、Zr、Hf、V、Mo、W、
Al、Znなどの金属も酸あるいはアルカリ処理により溶出
し、表面にはNi、Co、Feなどの高活性成分から成る多孔
質層が形成され、水素の吸収と放出速度は更に一段と向
上することになる。In addition, Ti, Zr, Hf, V, Mo, W near the surface,
Metals such as Al and Zn are also eluted by acid or alkali treatment, and a porous layer composed of highly active components such as Ni, Co and Fe is formed on the surface, and the absorption and desorption rates of hydrogen are further improved. Become.
【０００７】更に、上記で処理した合金および金属間化
合物を、水素化により活性化すると共に、金属を電解メ
ッキあるいは内部に吸蔵した水素で還元メッキすること
で、水素の吸収−放出反応を一層効率よく進めることが
可能となる。Further, the alloy and intermetallic compound treated as described above are activated by hydrogenation, and at the same time, the metal is electrolytically plated or reduction-plated with hydrogen occluded inside, so that the absorption-desorption reaction of hydrogen is more efficient. It is possible to proceed well.
【０００８】[0008]
【実施例】以下に本発明の実施例を示すが、本発明はこ
れに限定されるものではない。EXAMPLES Examples of the present invention will be shown below, but the present invention is not limited thereto.
【０００９】図１に示す製造工程により、活性表面層を
有する水素吸蔵性合金および金属間化合物バルクあるい
は粉末を製造することができる。By the manufacturing process shown in FIG. 1, a hydrogen storage alloy having an active surface layer and an intermetallic compound bulk or powder can be manufactured.
【００１０】製造はまず、Ti、Zr、Hf、V、Mo、W、Al、
Znなどを成分として含む水素吸蔵性合金ならびに金属間
化合物バルクおよび粉末を、フッ化水素酸などの酸ある
いはアルカリで処理することで、表面に形成された上記
成分の不活性酸化物を溶解除去する。これを洗浄、乾燥
後オートクレーブ内で水素化することで、活性表面層を
有する水素吸蔵性合金および金属間化合物のバルクおよ
び粉末試料が得られる。また、更に水素の吸収−放出速
度を高める必要がある場合は、これらの反応に高活性な
Pt、Ir、Pdなどを合金ならびに金属間化合物の活性化処
理済みの表面へ、電解メッキあるいは吸蔵水素による還
元メッキにより担持する。The manufacturing process is as follows: Ti, Zr, Hf, V, Mo, W, Al,
By treating the hydrogen storage alloy containing Zn as a component and the intermetallic compound bulk and powder with an acid such as hydrofluoric acid or an alkali, the inactive oxides of the above components formed on the surface are dissolved and removed. . This is washed, dried, and then hydrogenated in an autoclave to obtain a bulk and powder sample of a hydrogen storage alloy having an active surface layer and an intermetallic compound. Also, when it is necessary to further increase the absorption-desorption rate of hydrogen, it is highly active in these reactions.
Pt, Ir, Pd, etc. are supported on the surface of the alloy and the intermetallic compound that has been activated by electrolytic plating or reduction plating with absorbed hydrogen.
【００１１】表１は、ZrNi2合金のXPSによる表面分析の
結果をまとめたものである。まずエッチング前の合金表
面はZrO2で完全に覆われており、Niのシグナルは全く観
察されなかった。また、5nmのエッチング後でも、Niの
シグナルは観察されず、表面は依然ZrO2で覆われたまま
であった。これに対し、25nmのエッチング後では、ZrO2
のシグナル強度が低下し、これに伴ってZr金属およびNi
金属に帰属できるシグナルが観測された。以上より、通
常の方法で作製されたZrNi2合金表面はかなりの厚さのZ
rO2層で完全に覆われていることがわかる。Table 1 summarizes the results of surface analysis of ZrNi 2 alloy by XPS. First, the alloy surface before etching was completely covered with ZrO 2 , and no Ni signal was observed. In addition, no Ni signal was observed even after etching to 5 nm, and the surface was still covered with ZrO 2 . On the other hand, after etching 25 nm, ZrO 2
Signal intensity of Zr metal and Ni decreases.
A signal attributable to the metal was observed. From the above, the surface of the ZrNi 2 alloy prepared by the usual method is
It can be seen that it is completely covered by the rO 2 layer.
【００１２】[0012]
【表１】 [Table 1]
【００１３】図２は、XPSのシグナル強度から求めたフ
ッ酸処理前後のZrNi2の深さ方向依存性を示したもので
ある。未処理のものに比べ、フッ化水素酸で処理した合
金では、Niの濃度が著しく高くなっており、またその領
域も合金内部まで続いていることがわかる。これより、
フッ化水素酸処理により表面には一種の多孔質（ラネ
ー）層が形成されると結論される。FIG. 2 shows the dependence of ZrNi 2 in the depth direction before and after hydrofluoric acid treatment, which was determined from the XPS signal intensity. It can be seen that the concentration of Ni in the alloy treated with hydrofluoric acid is significantly higher than that of the untreated one, and that region continues to the inside of the alloy. Than this,
It is concluded that the hydrofluoric acid treatment forms a kind of porous (Raney) layer on the surface.
【００１４】表２は、フッ化水素酸で処理したNi-V合金
と水酸化ナトリウムで処理したNi-A1合金の表面粗度
（ラフネスファクター）と水電解（1M、KOH水溶液中、
室温）時の交換電流密度を示す。類似した表面粗度にお
いてNiV合金の交換電流密度が大きいことより、良好な
水素吸蔵能を与えるV系の合金の方がかえって電極とし
ての比活性は高いことがわかった。同様の傾向はTiおよ
びZr系の合金においても見られた。また、これらの電極
に更にPr,Ir,Pdを担持することで、交換電流密度は５〜
１０倍程増大することも明かとなった。Table 2 shows the surface roughness (roughness factor) of Ni-V alloy treated with hydrofluoric acid and Ni-A1 alloy treated with sodium hydroxide and water electrolysis (1M in KOH aqueous solution,
The exchange current density at room temperature) is shown. Since the exchange current density of NiV alloy is high at similar surface roughness, it was found that the V-type alloy that gives a good hydrogen storage capacity has a higher specific activity as an electrode. A similar tendency was found in Ti and Zr alloys. Moreover, by further supporting Pr, Ir, and Pd on these electrodes, the exchange current density is 5 to 5.
It was also revealed that it would increase about 10 times.
【００１５】[0015]
【表２】 [Table 2]
【００１６】[0016]
【発明の効果】本発明は、本来優れた水素吸蔵能を有す
る反面、構成成分であるTi、Zr、Hf、V、Mo、W、Al、Zn
などにより表面に形成された不活性酸化物のために低い
水素の吸収および放出速度しか示さない合金あるいは金
属間化合物に対して、水素の吸収−放出速度を飛躍的に
向上させる顕著な効果がある。EFFECTS OF THE INVENTION The present invention originally has an excellent hydrogen storage capacity, but on the other hand, the constituents of Ti, Zr, Hf, V, Mo, W, Al and Zn.
For alloys or intermetallic compounds that show only a low hydrogen absorption and desorption rate due to the inactive oxide formed on the surface, etc., it has a remarkable effect of dramatically improving the hydrogen absorption-desorption rate. .
【図１】活性表面層を有する水素吸蔵性合金および金属
間化合物バルクあるいは粉末の製造工程図である。FIG. 1 is a manufacturing process diagram of a hydrogen storage alloy having an active surface layer and an intermetallic compound bulk or powder.
【図２】フッ化水素酸処理前後のZrNi2合金において、X
PSシグナルから求めたNi/Zr原子比の深さ方向依存性で
ある。[Fig. 2] X in ZrNi 2 alloy before and after hydrofluoric acid treatment
Depth dependence of Ni / Zr atomic ratio obtained from PS signal.
Claims (2)
活性酸化物を形成し易い成分を含む合金ならびに金属間
化合物バルクおよび粉末をフッ化水素酸などの酸あるい
はアルカリで処理し、これらの成分を溶解除去すること
で表面にNi、Co、Feなどの水素の吸収−放出反応に活性
な成分からなる清浄でかつ多孔質な表面層を形成させた
水素吸蔵性合金ならびに金属間化合物のバルクおよび粉
末を製造する技術。1. An alloy containing a component that easily forms an inactive oxide such as Ti, Zr, Hf, V, Mo, W, Al, and Zn, and an intermetallic compound bulk and powder are treated with an acid such as hydrofluoric acid or the like. By treating with an alkali and dissolving and removing these components, a clean and porous surface layer consisting of components active in the absorption-desorption reaction of hydrogen such as Ni, Co, Fe is formed on the surface. Techniques for making bulk and powder alloys and intermetallics.
した合金ならびに金属間化合物バルクおよび粉末表面
に、水素の吸収−放出反応に対し更に高活性なPt、Ir、
Pdなどの金属を電解あるいは無電解メッキする技術。2. Pt, Ir, which has a higher activity for hydrogen absorption-desorption reaction, on the alloy and intermetallic compound bulk and powder surfaces whose surface has been cleaned or made porous by the above treatment.
Technology for electrolytic or electroless plating of metals such as Pd.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6294869A JPH08157902A (en) | 1994-11-29 | 1994-11-29 | Production of bulk and powder of hydrogen storage alloy and intermetallic compound having active surface layer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6294869A JPH08157902A (en) | 1994-11-29 | 1994-11-29 | Production of bulk and powder of hydrogen storage alloy and intermetallic compound having active surface layer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH08157902A true JPH08157902A (en) | 1996-06-18 |
Family
ID=17813306
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6294869A Pending JPH08157902A (en) | 1994-11-29 | 1994-11-29 | Production of bulk and powder of hydrogen storage alloy and intermetallic compound having active surface layer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH08157902A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6322925B1 (en) | 1997-08-28 | 2001-11-27 | Sanyo Electric Co., Ltd. | Metal hydride alkaline storage cell |
| JP2002363605A (en) * | 2001-06-11 | 2002-12-18 | Sumitomo Metal Ind Ltd | Manufacturing method of hydrogen storage alloy |
| EP1093673A4 (en) * | 1999-04-08 | 2007-03-28 | Ovonic Battery Co | Active electrode compositions comprising raney based catalysts and materials |
-
1994
- 1994-11-29 JP JP6294869A patent/JPH08157902A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6322925B1 (en) | 1997-08-28 | 2001-11-27 | Sanyo Electric Co., Ltd. | Metal hydride alkaline storage cell |
| US6852447B2 (en) | 1997-08-28 | 2005-02-08 | Sanyo Electric Co., Ltd. | Metal hydride alkaline storage cell and manufacturing method thereof |
| US6902588B2 (en) | 1997-08-28 | 2005-06-07 | Sanyo Electric Co., Ltd | Manufacturing method of metal hydride alkaline storage cell |
| EP1093673A4 (en) * | 1999-04-08 | 2007-03-28 | Ovonic Battery Co | Active electrode compositions comprising raney based catalysts and materials |
| JP2002363605A (en) * | 2001-06-11 | 2002-12-18 | Sumitomo Metal Ind Ltd | Manufacturing method of hydrogen storage alloy |
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