JP2002343351A - Hydrogen storage alloy powder - Google Patents
Hydrogen storage alloy powderInfo
- Publication number
- JP2002343351A JP2002343351A JP2001141952A JP2001141952A JP2002343351A JP 2002343351 A JP2002343351 A JP 2002343351A JP 2001141952 A JP2001141952 A JP 2001141952A JP 2001141952 A JP2001141952 A JP 2001141952A JP 2002343351 A JP2002343351 A JP 2002343351A
- Authority
- JP
- Japan
- Prior art keywords
- hydrogen storage
- storage alloy
- alloy powder
- gas
- powder
- 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.)
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Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、Ｎｉ−水素二次電
池負極用材料として使用される電気化学特性に優れた水
素吸蔵合金粉末に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a hydrogen storage alloy powder having excellent electrochemical properties and used as a negative electrode material for a Ni-hydrogen secondary battery.
【０００２】[0002]
【従来の技術】従来、水素吸蔵合金粉末の作製方法とし
ては、ガスアトマイズ法や鋳造粉砕法などが提案されて
いるが、鋳造粉砕粉末は凝固時に成分偏析などが発生
し、電気化学特性に悪影響を及ぼす。一方、Ａｒ、Ｈｅ
などの不活性ガスでアトマイズした粉末は急冷凝固によ
り、成分偏析の少ない粉末が製作できる。また、雰囲気
ガスについては、例えば特開平２−２５３５５８号公報
のように、希ガスのような水素吸蔵合金と容易に反応す
ることのない不活性なものが望ましいとされている。こ
れは酸素または窒素を含有する雰囲気の場合には、高温
下ではそれぞれ水素吸蔵合金の構成金属の酸化物または
窒化物が生成して、水素の吸蔵・放出反応に関与する合
金の量が減少するという不都合が発生するからであると
している。2. Description of the Related Art Conventionally, a gas atomizing method or a casting and pulverizing method has been proposed as a method for producing a hydrogen storage alloy powder. However, the cast and pulverized powder causes segregation of components at the time of solidification and adversely affects electrochemical characteristics. Exert. On the other hand, Ar, He
Powder that has been atomized with an inert gas such as that described above can be rapidly solidified to produce powder with less component segregation. Further, it is considered that an inert gas which does not easily react with a hydrogen storage alloy, such as a rare gas, is desirable as disclosed in, for example, JP-A-2-253558. This is because, in an atmosphere containing oxygen or nitrogen, at high temperatures, oxides or nitrides of the constituent metals of the hydrogen storage alloy are generated, and the amount of the alloy involved in the hydrogen storage / release reaction decreases. This is because such a problem occurs.
【０００３】また、窒素を含むガスによるアトマイズと
しては、例えば特開平９−３０２４３１号公報に示すよ
うに、ミッシュメタル・ニッケル系水素吸蔵合金を溶解
後、０．１ｖｏｌ．％以上５０ｖｏｌ．％未満の窒素ガ
スを含み、残りは不活性ガスからなるアトマイズガスで
ガスアトマイズした後、該粉末を酸溶液中で表面処理す
ることを特徴とする水素吸蔵合金粉末の製造方法が開示
されている。As atomization by a gas containing nitrogen, for example, as disclosed in JP-A-9-302431, after dissolving a misch metal / nickel-based hydrogen storage alloy, 0.1 vol. % Or more and 50 vol. A method for producing a hydrogen-absorbing alloy powder is disclosed, which comprises subjecting the powder to gas atomization with an atomizing gas consisting of an inert gas containing less than 10% of nitrogen gas and then subjecting the powder to a surface treatment in an acid solution.
【０００４】一方、不活性ガスによるガスアトマイズ粉
末は慨して球状をしており、負極を形成した際に個々の
水素吸蔵合金粉末間の接触抵抗が大きいため負極内部抵
抗が大きく電気化学特性を劣化させる。そこで、ガスア
トマイズ粉末を不定形状化する方法として、例えば特開
平４−１２６３６１号公報のように、ガスアトマイズ法
で製作した水素吸蔵合金粉末を、さらに、ボールミルな
どで機械的に微粉砕したり、あるいは水素の吸蔵放出を
行わせて微粉砕して平均粒径が例えば１００μ以下の微
細な不定形状の水素吸蔵合金を製作するものが提案され
ている。On the other hand, the gas atomized powder by an inert gas is generally spherical, and when the negative electrode is formed, the contact resistance between the individual hydrogen storage alloy powders is large, so that the internal resistance of the negative electrode is large and the electrochemical characteristics are deteriorated. Let it. Therefore, as a method of forming the gas atomized powder into an irregular shape, for example, as disclosed in Japanese Patent Application Laid-Open No. 4-126361, a hydrogen-absorbing alloy powder produced by a gas atomizing method is further mechanically pulverized by a ball mill or the like. For producing a fine irregular-shaped hydrogen storage alloy having an average particle diameter of, for example, 100 μm or less, by performing occlusion and release.
【０００５】[0005]
【発明が解決しようとする課題】上記した特開平２−２
５３５５８号公報は、酸素や窒素を含有する雰囲気では
高温下で酸化物や窒化物を生成し、電気化学特性が劣化
するとしているが、本発明は窒素ガスを積極的に使用す
ることで、粉末形状を不定形状化し、電気化学特性が向
上するものであり、また、特開平９−３０２４３１号公
報に示される窒素ガスを混合したガスでアトマイズした
粉末は、窒素混合率を５０ｖｏｌ％未満にしているため
形状が球状または楕円形となっており、粉末間接触抵抗
が高い。SUMMARY OF THE INVENTION The above-mentioned Japanese Patent Application Laid-Open No. Hei 2-2
Japanese Patent No. 53558 discloses that in an atmosphere containing oxygen or nitrogen, oxides and nitrides are generated at a high temperature and the electrochemical characteristics are degraded. The shape is made indefinite, and the electrochemical characteristics are improved. Further, the powder mixed with nitrogen gas described in Japanese Patent Application Laid-Open No. 9-302431 has a nitrogen mixing ratio of less than 50 vol%. Therefore, the shape is spherical or elliptical, and the contact resistance between powders is high.
【０００６】さらに、特開平４−１２６３６１号公報
は、ガスアトマイズ粉末を不定形状化する方法として、
ガスアトマイズ法で製作した水素吸蔵合金粉末を、ボー
ルミルなどで機械的に微粉砕したり、あるいは水素の吸
蔵放出を行わせて微粉砕しているもので、アトマイズ工
程の後に別途粉砕工程を追加しなくてはならず、粉末製
造工程が煩雑になり、製造コスト高にもなる。上述のよ
うに、電気化学特性の良好な水素吸蔵合金粉末の作製方
法として、不活性ガスによるガスアトマイズ法等が提案
されてきたが、いずれの方法もそれぞれ問題がある。Further, Japanese Patent Application Laid-Open No. 4-126361 discloses a method for forming a gas atomized powder into an irregular shape.
Hydrogen storage alloy powder produced by the gas atomization method is mechanically finely pulverized with a ball mill or the like, or is finely pulverized by absorbing and releasing hydrogen, without adding a separate pulverization step after the atomization step. In addition, the powder manufacturing process becomes complicated and the manufacturing cost increases. As described above, a gas atomizing method using an inert gas or the like has been proposed as a method for producing a hydrogen-absorbing alloy powder having good electrochemical characteristics, but each method has a problem.
【０００７】[0007]
【課題を解決するための手段】上述のような問題を解消
するために、発明者らは鋭意開発を進めた結果、負極材
料として、不定形状のガスアトマイズ粉末を使用するこ
とで、別途粉砕工程を設けることなく、電気化学特性に
優れたＮｉ−水素二次電池用水素吸蔵合金粉末を提供す
ることにある。その発明の要旨とするところは、 （１）９１ｖｏｌ％以上の窒素ガスを含み、残部不活性
ガスからなるアトマイズガスでガスアトマイズし製造し
たことを特徴とする水素吸蔵合金粉末。Means for Solving the Problems In order to solve the above-mentioned problems, the present inventors have intensively developed and as a result, by using a gas atomized powder of irregular shape as a negative electrode material, a separate pulverizing step was carried out. An object of the present invention is to provide a hydrogen-absorbing alloy powder for a Ni-hydrogen secondary battery having excellent electrochemical characteristics without providing the same. The gist of the invention is as follows: (1) A hydrogen storage alloy powder characterized by being produced by gas atomizing with an atomizing gas consisting of an inert gas containing at least 91 vol% of nitrogen gas.
【０００８】（２）噴霧状態で３８μｍ未満、２５μｍ
以上に分級した粉末の平均比表面積が０．０４０ｍ2 ／
ｇ以上となる前記（１）記載の水素吸蔵合金粉末。 （３）アトマイズ後、熱処理を施した前記（１）または
（２）に記載の水素吸蔵合金粉末。 （４）アトマイズ粉末を熱処理した後、酸処理を施した
前記（１）〜（３）記載の水素吸蔵合金粉末にある。(2) When sprayed, less than 38 μm, 25 μm
The average specific surface area of the powder classified above is 0.040 m 2 /
g of the hydrogen storage alloy powder according to the above (1). (3) The hydrogen storage alloy powder according to (1) or (2), which has been subjected to heat treatment after atomization. (4) The hydrogen storage alloy powder according to the above (1) to (3), wherein the atomized powder is heat-treated and then subjected to an acid treatment.
【０００９】[0009]
【発明の実施の形態】以下、本発明について詳細に説明
する。本発明は、９１ｖｏｌ％以上、好ましくは９５ｖ
ｏｌ％以上の窒素ガスを含み、残部不活性ガスからなる
アトマイズガスを使用することにより、水素吸蔵合金粉
末を不定形状化する。これにより比表面積が増大し、粉
末間接触も面接触となる。この場合、９１ｖｏｌ％以上
の窒素ガス含有量にすることで、粉末の比表面積が急激
に増大し、水素吸蔵放出反応面積が増大する。また、負
極内部抵抗も減少し、結果として電気化学特性が向上す
る。BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail. In the present invention, 91 vol% or more, preferably 95 v%
The hydrogen storage alloy powder is formed into an irregular shape by using an atomizing gas containing at least ol% of nitrogen gas and a balance of inert gas. As a result, the specific surface area increases, and the contact between the powders also becomes the surface contact. In this case, by setting the nitrogen gas content to 91 vol% or more, the specific surface area of the powder rapidly increases, and the hydrogen storage / release reaction area increases. Further, the internal resistance of the negative electrode is reduced, and as a result, the electrochemical characteristics are improved.
【００１０】ここで、３８μｍ未満、２５μｍ以上の粉
末粒度を比表面積評価の対象とした理由は、アルゴンや
ヘリウムによる球状のガスアトマイズ粉末であっても、
５０μｍ以上になると噴霧条件によってはフレークや針
状粉末が多く入ることがあり、比表面積の評価が適切で
なくなる可能性があるためであり、また、評価粒度を狭
くしておかないと粒度分布（頻度）の影響が出てしまう
ため、２５μｍ未満の粉末を除外した。従って、噴霧状
態で３８μｍ未満、２５μｍ以上に分級した粉末を比表
面積、評価の対象とする。Here, the reason why the particle size of less than 38 μm and 25 μm or more was targeted for the specific surface area evaluation was that even a spherical gas atomized powder of argon or helium was used.
If the particle size is 50 μm or more, a large amount of flakes and needle-like powders may enter depending on the spraying conditions, and the evaluation of the specific surface area may not be appropriate. Also, if the evaluation particle size is not narrowed, the particle size distribution ( Frequency), powder having a particle size of less than 25 μm was excluded. Therefore, the powder classified as less than 38 μm and 25 μm or more in the spray state is the target of the specific surface area and evaluation.
【００１１】このような方法で製造した粉末のうち、噴
霧状態で３８μｍ未満、２５μｍ以上に分級した粉末の
平均比表面積が０．０４０ｍ2 ／ｇ以上になる場合にさ
らに良好な電気化学特性が得られる。さらに、熱処理に
より、アトマイズ時の急冷による凝固歪みを緩和するこ
とで、さらに均一組織の粉末が製造でき、良好な電気化
学特性が得られる。また、アトマイズ粉末を熱処理した
後、酸処理により、粉末表面の不純物層の除去およびＮ
ｉリッチ層の露出によって、さらに電気化学特性は向上
する。[0011] Among the powders produced by such a method, when the average specific surface area of the powder classified into less than 38 µm and 25 µm or more in a spray state becomes 0.040 m 2 / g or more, more excellent electrochemical characteristics can be obtained. Can be Furthermore, by heat treatment, solidification distortion due to rapid cooling during atomization is alleviated, whereby a powder having a more uniform structure can be produced, and good electrochemical characteristics can be obtained. After heat treatment of the atomized powder, removal of the impurity layer on the powder surface and N
The electrochemical properties are further improved by exposing the i-rich layer.
【００１２】[0012]
【実施例】以下、本発明について実施例によって具体的
に説明する。ミッシュメタル・ニッケル系水素吸蔵合金
を溶解後、窒素／アルゴン比を表１に示す混合ガスでア
トマイズし、得られた粉末を、−１０６μｍに分級し、
アルゴン気流中で１０００℃−２ｈ熱処理した。さらに
熱処理粉末をｐＨ１の塩酸で酸処理し、酸処理液濾過後
純水にて３回洗浄、濾過を繰り返した後真空乾燥炉中で
２４時間乾燥させる。評価法としては、走査型電子顕微
鏡による形状観察、ＢＥＴ法（粉体粒子の表面に吸着占
有面積の判った分子を液体窒素の温度で吸着させ、その
量から試料の比表面積を求める方法）による比表面積測
定、および電気化学特性の測定を実施した。The present invention will be specifically described below with reference to examples. After dissolving the misch metal / nickel hydrogen storage alloy, the nitrogen / argon ratio was atomized with a mixed gas shown in Table 1, and the obtained powder was classified into −106 μm.
Heat treatment was performed at 1000 ° C. for 2 hours in an argon stream. Further, the heat-treated powder is acid-treated with hydrochloric acid having a pH of 1, filtered with an acid-treated solution, washed three times with pure water, and filtered repeatedly, and then dried in a vacuum drying furnace for 24 hours. As the evaluation method, the shape is observed by a scanning electron microscope, and the BET method (a method in which molecules whose adsorption occupation area is known is adsorbed on the surface of powder particles at the temperature of liquid nitrogen and the specific surface area of the sample is determined from the amount). Specific surface area measurement and measurement of electrochemical properties were performed.
【００１３】また、電気化学容量として、上記方法で製
造された水素吸蔵合金粉末／ＰＴＦＥ粉（結着材）＝９
／１（重量比）で混合、混錬しペレット状にし１．０ｇ
φ２０の円盤状に切り出しＮｉメッシュに挟んで成形し
負極とした。この負極をこれより体積の充分大きい焼結
ニッケル電極と組み合わせアルカリ液に浸漬し、実験用
Ｎｉ−水素二次電池とした。負極中の水素吸蔵合金粉末
１．０ｇ当たり５０ｍＡとなる電流値で８時間充電し、
１時間休止の後、負極中の水素吸蔵合金粉末１．０ｇ当
たり２００ｍＡとなる電流値で放電し、正負極間の電位
差が０．６Ｖになったところで放電をストップした。続
けて負極中の水素吸蔵合金粉末１．０ｇ当たり５０ｍＡ
となる電流値で同じ要領で放電した。この時の２００ｍ
Ａおよび５０ｍＡの放電における合計放電量を負極中の
水素吸蔵合金粉末１．０ｇ当たりの量に換算したものを
電気化学容量とした。The electrochemical capacity is determined as follows: hydrogen storage alloy powder / PTFE powder (binder) = 9 produced by the above method.
/ 1 (weight ratio), knead and pelletize 1.0g
A negative electrode was obtained by cutting out into a disk shape of φ20 and sandwiching the Ni mesh. This negative electrode was combined with a sintered nickel electrode having a sufficiently large volume and immersed in an alkaline solution to obtain an experimental Ni-hydrogen secondary battery. Charged at a current value of 50 mA per 1.0 g of the hydrogen storage alloy powder in the negative electrode for 8 hours,
After the suspension for 1 hour, the battery was discharged at a current value of 200 mA per 1.0 g of the hydrogen storage alloy powder in the negative electrode, and the discharge was stopped when the potential difference between the positive and negative electrodes became 0.6 V. Continuously, 50 mA per 1.0 g of the hydrogen storage alloy powder in the negative electrode
The discharge was performed in the same manner at a current value of. 200m at this time
The electrochemical capacity was obtained by converting the total discharge amount in the discharge of A and 50 mA into the amount per 1.0 g of the hydrogen storage alloy powder in the negative electrode.
【００１４】[0014]
【表１】 [Table 1]
【００１５】[0015]
【表２】 [Table 2]
【００１６】表１および表２に示すように、試料Ｎｏ．
１〜４は本発明例であり、試料Ｎｏ．５〜１０は比較例
である。試料Ｎｏ．５〜１０はいずれも窒素量が９０％
以下であり、そのために平均比表面積が０．０４０ｍ2
／ｇ未満であり、電気化学容量が低下していることが判
る。これに対し、本発明はいずれも平均比表面積が０．
０４０ｍ2 ／ｇ以上であり、電気化学容量の値が高く、
電気化学特性の優れていることが判る。As shown in Tables 1 and 2, Sample No.
Sample Nos. 1 to 4 are examples of the present invention. 5 to 10 are comparative examples. Sample No. 5 to 10 are all 90% nitrogen
Or less, so that the average specific surface area is 0.040 m 2
/ G, which indicates that the electrochemical capacity is reduced. On the other hand, in the present invention, the average specific surface area is in all cases of 0.1.
040 m 2 / g or more, the value of electrochemical capacity is high,
It can be seen that the electrochemical properties are excellent.
【００１７】[0017]
【発明の効果】以上述べたように、本発明により電気化
学特性に優れたＮｉ−水素二次電池の負極材料に好適な
水素吸蔵合金粉末を提供することが出来る優れた効果を
奏するものである。As described above, the present invention has an excellent effect of providing a hydrogen storage alloy powder suitable for a negative electrode material of a Ni-hydrogen secondary battery having excellent electrochemical characteristics. .
───────────────────────────────────────────────────── フロントページの続き Ｆターム(参考） 4K017 AA04 BA03 BB12 DA09 EB05 FA03 4K018 BA04 BB10 BC01 BC09 BD07 5H050 AA19 BA14 CA03 CB16 DA03 DA15 FA17 GA02 GA06 GA14 HA01 HA07 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 4K017 AA04 BA03 BB12 DA09 EB05 FA03 4K018 BA04 BB10 BC01 BC09 BD07 5H050 AA19 BA14 CA03 CB16 DA03 DA15 FA17 GA02 GA06 GA14 HA01 HA07
Claims (4)
部不活性ガスからなるアトマイズガスでガスアトマイズ
し製造したことを特徴とする水素吸蔵合金粉末。1. A hydrogen storage alloy powder containing 91 vol% or more of nitrogen gas and gas atomized with an atomizing gas consisting of an inert gas as a balance.
に分級した粉末の平均比表面積が０．０４０ｍ2 ／ｇ以
上となる請求項１記載の水素吸蔵合金粉末。2. The hydrogen storage alloy powder according to claim 1, wherein the average specific surface area of the powder classified as less than 38 μm and 25 μm or more in a spray state is 0.040 m 2 / g or more.
または請求項２記載の水素吸蔵合金粉末。3. A heat treatment is performed after the atomization.
Or the hydrogen storage alloy powder according to claim 2.
を施した請求項１〜３記載の水素吸蔵合金粉末。4. The hydrogen storage alloy powder according to claim 1, wherein the atomized powder is heat-treated and then subjected to an acid treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001141952A JP2002343351A (en) | 2001-05-11 | 2001-05-11 | Hydrogen storage alloy powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001141952A JP2002343351A (en) | 2001-05-11 | 2001-05-11 | Hydrogen storage alloy powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2002343351A true JP2002343351A (en) | 2002-11-29 |
Family
ID=18988327
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2001141952A Withdrawn JP2002343351A (en) | 2001-05-11 | 2001-05-11 | Hydrogen storage alloy powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2002343351A (en) |
-
2001
- 2001-05-11 JP JP2001141952A patent/JP2002343351A/en not_active Withdrawn
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