JP2755661B2 - Manufacturing method of hydrogen storage alloy - Google Patents
Manufacturing method of hydrogen storage alloyInfo
- Publication number
- JP2755661B2 JP2755661B2 JP1050497A JP5049789A JP2755661B2 JP 2755661 B2 JP2755661 B2 JP 2755661B2 JP 1050497 A JP1050497 A JP 1050497A JP 5049789 A JP5049789 A JP 5049789A JP 2755661 B2 JP2755661 B2 JP 2755661B2
- Authority
- JP
- Japan
- Prior art keywords
- metal
- alloy
- hydrogen
- hydrogen storage
- storage alloy
- 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.)
- Expired - Lifetime
Links
- 229910045601 alloy Inorganic materials 0.000 title claims description 34
- 239000000956 alloy Substances 0.000 title claims description 34
- 239000001257 hydrogen Substances 0.000 title claims description 32
- 229910052739 hydrogen Inorganic materials 0.000 title claims description 32
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims description 28
- 238000003860 storage Methods 0.000 title claims description 10
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000002184 metal Substances 0.000 claims description 26
- 229910052751 metal Inorganic materials 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 8
- 229910000765 intermetallic Inorganic materials 0.000 claims description 5
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 238000010521 absorption reaction Methods 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- 238000007712 rapid solidification Methods 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 229910002515 CoAl Inorganic materials 0.000 description 4
- 239000003245 coal Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- 230000000171 quenching effect Effects 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 229910004247 CaCu Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 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
Landscapes
- Continuous Casting (AREA)
- Physical Vapour Deposition (AREA)
Description
【発明の詳細な説明】 （イ） 産業上の利用分野 本発明は、蓄熱、熱輸送システム等の熱利用システム
に用いる水素吸蔵合金の製造方法に関する。The present invention relates to a method for producing a hydrogen storage alloy used in a heat utilization system such as a heat storage and heat transport system.
（ロ） 従来の技術 熱利用システムに使用するこの種の水素吸蔵合金に
は、特に使用条件下で単位重量当りの水素吸収量が多い
ことが挙げられる。(B) Conventional technology This type of hydrogen storage alloy used in a heat utilization system has a large amount of hydrogen absorption per unit weight particularly under use conditions.
斯る条件を満足させるべく、特願昭63−218907号で
は、組成式Ａ−Ｂ（但し、Ａは水素を発熱吸収する型の
金属、Ｂは水素を吸熱吸収する型の金属）で表わされる
金属間化合物であって、金属Ｂに対する金属Ａの化学量
論比を増大させることを提案している。このものは、量
論比が1.3程度では水素吸収量の増加が認められる。In order to satisfy such conditions, in Japanese Patent Application No. 63-218907, the composition formula is represented by AB (where A is a metal of the type that exothermicly absorbs hydrogen and B is a metal of the type that endothermicly absorbs hydrogen). It is an intermetallic compound that proposes increasing the stoichiometric ratio of metal A to metal B. When the stoichiometric ratio is about 1.3, an increase in hydrogen absorption is observed.
（ハ） 発明が解決しようとする課題 しかし、従来例は、量論比が1.3を越えると、むしろ
水素吸収量が減少する。(C) Problems to be Solved by the Invention However, in the conventional example, when the stoichiometric ratio exceeds 1.3, the hydrogen absorption amount is rather reduced.
本発明は、斯る従来例を改良して水素吸収量の増大化
を図るものである。The present invention is intended to improve such a conventional example to increase the amount of hydrogen absorption.
詳しくは、従来例では水素の吸放出が容易な母相に対
して、母合金の化学量論比がずれすぎると、水素吸放出
の難しい結晶相が析出して合金中の母相部分が減少し、
合金の水素吸収量が減少していたことに着目し、この水
素吸放出の難しい結晶相の析出を量論比増大時にあって
も抑制せんとするものである。Specifically, if the stoichiometric ratio of the master alloy is too different from that of the parent phase, which is easy to absorb and release hydrogen in the conventional example, a crystal phase that is difficult to absorb and release hydrogen will precipitate and the mother phase portion in the alloy will decrease. And
Focusing on the fact that the amount of hydrogen absorbed by the alloy has been reduced, it is intended to suppress the precipitation of a crystal phase that is difficult to absorb and release hydrogen even when the stoichiometric ratio is increased.
（ニ） 課題を解決するための手段 本発明の組成式AxB5（但し、Ａは水素を発熱吸収する
型の金属、Ｂは水素を吸熱吸収する型の金属、ｘは金属
Ａの比率）で表される水素吸蔵合金の製造方法は、金属
間化合物を形成する化学両論比から金属Ｂに対して金属
Ａを増加させ、前記金属Ａの比率ｘを1.3≦ｘ≦1.9と
し、且つ急冷凝固させてなることを特徴とする。(D) Means for Solving the Problems The composition formula AxB 5 of the present invention (where A is a metal of the type that exothermicly absorbs hydrogen, B is a metal of the type that endothermicly absorbs hydrogen, and x is the ratio of metal A) The method for producing the hydrogen storage alloy represented is to increase the metal A with respect to the metal B from the stoichiometric ratio forming the intermetallic compound, set the ratio x of the metal A to 1.3 ≦ x ≦ 1.9, and rapidly solidify. It is characterized by becoming.
（ホ） 作用 急冷凝固することにより、化学量論比がずれても、合
金中の母相部分の減少及び不均質化現象を大幅に抑制で
き、化学量論比増大による水素吸収量増加効果を確保す
るものである。(E) Action By rapid solidification, even if the stoichiometric ratio deviates, the reduction of the parent phase in the alloy and the heterogeneous phenomenon can be greatly suppressed, and the effect of increasing the amount of hydrogen absorbed by increasing the stoichiometric ratio can be reduced. To ensure.
（ヘ） 実施例 ［実施例１］ Mm（La含有15wt％）、Ni、Co、Al及びMnの各市販金属
原料を使用し、アルゴン不活性雰囲気アーク炉を用い、
組成式AxByの金属間化合物である水素吸蔵合金を、ｘの
値を1.0〜2.0の範囲で変化させて作成した。但し、金属
ＡはMmであり、金属Ｂはｙの値を5.0とし、Ni3.2CoAl
0.2Mn0.6の組成式で表わされる。(F) Examples [Example 1] Using commercially available metal raw materials of Mm (La content 15 wt%), Ni, Co, Al and Mn, using an argon inert atmosphere arc furnace,
A hydrogen storage alloy which is an intermetallic compound of the composition formula AxBy was prepared by changing the value of x in the range of 1.0 to 2.0. However, metal A is Mm, metal B has a value of y of 5.0, and Ni 3.2 CoAl
It is represented by a composition formula of 0.2 Mn 0.6 .
以下、急冷凝固法として液体急冷法を用いた場合につ
いて説明する。まず、上記の合金を５〜15mm角程度の小
片に砕いた後に、透明石英ノズル（ノズル穴1.0mmφ）
の中に入れ、高純度アルゴンガス（4Nup）で置換し、こ
の後に高周波加熱コイルに200KHz、3KWの高周波を加え
ることにより、加熱した。合金が溶解した後、透明石英
ノズル内をアルゴンガスによって加圧し、アルゴンガス
雰囲気下（1atm）で、高速回転（200r.p.m）している大
容量の銅製ローラー（300mmφ、幅40mm）の上に、合金
溶湯を噴出させ、このローラー上で急冷させてリボン状
の水素吸蔵合金を得た。Hereinafter, the case where the liquid quenching method is used as the quenching and solidifying method will be described. First, after crushing the above alloy into small pieces of 5 to 15 mm square, a transparent quartz nozzle (nozzle hole 1.0 mmφ)
, And replaced with high-purity argon gas (4Nup), and then heated by applying a high frequency of 200 KHz and 3 KW to a high frequency heating coil. After the alloy is melted, pressurize the inside of the transparent quartz nozzle with argon gas and place it on a large-capacity copper roller (300 mmφ, width 40 mm) rotating at high speed (200 rpm) under argon gas atmosphere (1 atm). Then, a molten alloy was jetted out and quenched on the roller to obtain a ribbon-shaped hydrogen storage alloy.
この急冷凝固法で得られたＡ1.4Ｂの組成の合金と、
従来例で得られたＡ1.4Ｂの組成の合金とをＸ線回折分
析結果に基づいて考察した。尚、金属Ａは、Laを15wt％
含有のMm、金属ＢはNi3.2CoAl0.2Mn0.6である。An alloy having a composition of A 1.4 B obtained by the rapid solidification method,
The alloy having the composition of A 1.4 B obtained in the conventional example was considered based on the result of X-ray diffraction analysis. In addition, as for the metal A, 15 wt% of La
The contained Mm and metal B are Ni 3.2 CoAl 0.2 Mn 0.6 .
而して、本実施例の合金は、CaCu5型結晶構造だけを
観察できたが、従来例の合金ではCaCu5型結晶構造だけ
でなく、Ce2Ni7型及びPuNi3型結晶構造が顕著に観察で
きた。Thus, in the alloy of this example, only the CaCu 5 type crystal structure could be observed, but in the alloy of the conventional example, not only the CaCu 5 type crystal structure but also the Ce 2 Ni 7 type and PuNi 3 type crystal structures were remarkable. Could be observed.
更に、金属Ａの金属Ｂに対する化学量論比（ｘ）を、
１≦ｘ≦２の範囲として結晶構造を調べたが、本実施例
では全範囲に亘って均質性が保持され、従来例では1.4
以上の範囲で上記Ce2Ni7型結晶構造等が観察された。Further, the stoichiometric ratio (x) of metal A to metal B is
The crystal structure was examined in the range of 1 ≦ x ≦ 2. In the present embodiment, the homogeneity was maintained over the entire range.
In the above range, the Ce 2 Ni 7 type crystal structure and the like were observed.
斯る［実施例１］の水素吸収量比は第１表で示すとお
りであり、従来例に比して著しく改善されている。ま
た、熱伝導率について光交流法を用いて測定したとこ
ろ、従来の粉末状のものでは約0.5w/m・ｋであったが、
本実施例の合金では約20w/m・ｋに向上した。The ratio of the amount of hydrogen absorbed in [Example 1] is as shown in Table 1 and is remarkably improved as compared with the conventional example. In addition, when the thermal conductivity was measured using the photo-current method, it was about 0.5 w / m · k for the conventional powder,
In the case of the alloy of this example, the value was improved to about 20 w / mk.
［実施例２］ 急冷凝固法としてスパッタ法を用いた場合について説
明する。MmxNi3.2CoAl0.2Mn0.6の合金にあって、そのｘ
の値を1.0≦ｘ≦2.0の範囲で変化させた合金を各々スパ
ッタゲート（4inchφ×5mm tのディスク）に成型し、高
周波マグネトロンスパッタ装置により、アルゴンガス雰
囲気下（１×10-2Torr）でニッケル基板上に上記合金の
スパッタ膜を形成した。Example 2 A case where a sputtering method is used as the rapid solidification method will be described. MmxNi 3.2 CoAl 0.2 Mn 0.6 alloy x
The alloys having the values of 1.0 ≦ x ≦ 2.0 were each formed into a sputter gate (disk of 4 inchφ × 5 mm t), and were subjected to high-frequency magnetron sputtering under argon gas atmosphere (1 × 10 −2 Torr). A sputtered film of the above alloy was formed on a nickel substrate.
高周波電力は、出力500W、13.56MHzとし、スパッタリ
ングを10時間行なった後にニッケル基板をスパッタ装置
から取り出し、基板に付着した該合金のスパッタ膜を、
スクレーパー（ステンレス製）により剥離させ、該合金
の薄片を約8g得た。High-frequency power, output 500W, 13.56MHz, after performing sputtering for 10 hours, take out the nickel substrate from the sputtering apparatus, the sputtered film of the alloy adhered to the substrate,
The alloy was peeled off with a scraper (made of stainless steel) to obtain about 8 g of a flake of the alloy.
斯る［実施例２］の水素吸収量比は第１表で示すとお
りであった。The ratio of the amount of hydrogen absorbed in [Example 2] was as shown in Table 1.
［実施例３］ 急冷凝固法としてフラッシュ蒸着法を用いた場合につ
いて説明する。MmxNi3.2CoAl0.2Mn0.6の合金にあって、
その原料金属の粉末（純3Nup、100〜300mesh）をｘの値
が1.0≦ｘ≦2.0の範囲となるように、秤量後よく混合し
た。Example 3 A case where a flash evaporation method was used as the rapid solidification method will be described. MmxNi 3.2 CoAl 0.2 Mn 0.6 alloy,
The raw metal powder (pure 3Nup, 100-300 mesh) was weighed and mixed well so that the value of x was in the range of 1.0 ≦ x ≦ 2.0.
この混合粉末をフラッシュ蒸着装置に導入し、ニッケ
ル基板上に蒸着膜を形成させた。即ち、混合粉末は、ア
ルゴン雰囲気下（１×10-3Torr）で、1800℃に加熱され
たタングステンボート上に少量ずつ連続的に落下され、
約100μｍの膜厚の蒸着膜を形成する。そして、蒸着膜
をスクレーパー（ステンレス製）で剥離させ、該合金の
薄片を得た。This mixed powder was introduced into a flash vapor deposition apparatus, and a vapor deposition film was formed on a nickel substrate. That is, the mixed powder is continuously dropped little by little on a tungsten boat heated to 1800 ° C. under an argon atmosphere (1 × 10 −3 Torr),
A deposited film having a thickness of about 100 μm is formed. Then, the deposited film was peeled off with a scraper (made of stainless steel) to obtain a thin piece of the alloy.
斯る［実施例３］の水素吸収量比は第１表で示すとお
りであった。The ratio of the amount of hydrogen absorbed in [Example 3] was as shown in Table 1.
以上の［実施例１］、［実施例２］、［実施例３］、
［従来例］の水素吸収量比を比較したものが第１表であ
り、特性比較図である。[Example 1], [Example 2], [Example 3],
Table 1 shows a comparison of the hydrogen absorption ratios of the [conventional example], and is a characteristic comparison diagram.
次に、急冷凝固法としては［実施例１］で示す液体急
冷法を用い、合金種を変化させた他の実施例を［実施例
４］として、以下に説明する。 Next, another example in which the liquid quenching method shown in [Example 1] is used as the rapid solidification method and the alloy type is changed will be described as [Example 4].
［実施例４］ 組成式CaxNi5の合金を1.0≦ｘ≦2.0の範囲で急冷凝固
法により作製した。この結果は、第２表に示してあり、
水素吸収量は同合金の従来例（有効水素吸収量0.8wt
％）に比して増加した。Example 4 An alloy of the composition formula CaxNi 5 was produced by a rapid solidification method in a range of 1.0 ≦ x ≦ 2.0. The results are shown in Table 2,
The hydrogen absorption is the same as the conventional alloy (effective hydrogen absorption 0.8wt)
%).
（ト）発明の効果 本発明によれば、金属間化合物を形成する化学量論比
から金属Ａを金属Ｂに対して増加させても、合金の均質
性を保持でき、金属Ａの比率Ｘを1.3〜1.9の範囲とする
ことで、水素吸収量を増加させた水素吸蔵合金が得られ
る。従って、熱利用システムで使用することにより、シ
ステムの高性能化を図ることができるものである。 (G) Effects of the Invention According to the present invention, even if the metal A is increased with respect to the metal B from the stoichiometric ratio for forming an intermetallic compound, the homogeneity of the alloy can be maintained and the ratio X of the metal A can be reduced. By setting the range of 1.3 to 1.9, a hydrogen storage alloy with an increased amount of hydrogen absorption can be obtained. Therefore, by using the heat utilization system, it is possible to improve the performance of the system.
図は本発明方法による水素吸蔵合金の特性比較図であ
る。The figure is a characteristic comparison diagram of the hydrogen storage alloy according to the method of the present invention.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 ＦＩ // Ｃ２２Ｃ 19/00 Ｃ２２Ｃ 19/00 Ｆ (56)参考文献 特開 昭51−148634（ＪＰ，Ａ) 特開 昭57−177942（ＪＰ，Ａ) 特開 昭60−138036（ＪＰ，Ａ) 特開 昭62−136547（ＪＰ，Ａ)──────────────────────────────────────────────────続 き Continuation of front page (51) Int.Cl. 6 Identification symbol FI // C22C 19/00 C22C 19 / 00F (56) References JP-A-51-148634 (JP, A) JP-A-57-148 177942 (JP, A) JP-A-60-138036 (JP, A) JP-A-62-136547 (JP, A)
Claims (1)
る型の金属、Ｂは水素を吸熱吸収する型の金属、ｘは金
属Ａの比率）で表される水素吸蔵合金の製造方法であっ
て、金属間化合物を形成する化学両論比から金属Ｂに対
して金属Ａを増加させ、前記金属Ａの比率ｘを1.3≦ｘ
≦1.9とし、且つ急冷凝固させてなる水素吸蔵合金の製
造方法。1. Production of a hydrogen storage alloy represented by the composition formula AxB 5 (where A is a metal of the type that exothermicly absorbs hydrogen, B is a type of metal that absorbs and absorbs hydrogen, and x is the ratio of metal A) A method comprising: increasing metal A relative to metal B from a stoichiometric ratio forming an intermetallic compound;
A method for producing a hydrogen storage alloy which is ≦ 1.9 and is rapidly solidified.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1050497A JP2755661B2 (en) | 1989-03-01 | 1989-03-01 | Manufacturing method of hydrogen storage alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1050497A JP2755661B2 (en) | 1989-03-01 | 1989-03-01 | Manufacturing method of hydrogen storage alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02228434A JPH02228434A (en) | 1990-09-11 |
| JP2755661B2 true JP2755661B2 (en) | 1998-05-20 |
Family
ID=12860577
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1050497A Expired - Lifetime JP2755661B2 (en) | 1989-03-01 | 1989-03-01 | Manufacturing method of hydrogen storage alloy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2755661B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3212133B2 (en) * | 1992-05-21 | 2001-09-25 | 株式会社三徳 | Rare earth metal-nickel based hydrogen storage alloy ingot and method for producing the same |
| US5376474A (en) * | 1993-02-05 | 1994-12-27 | Sanyo Electric Co., Ltd. | Hydrogen-absorbing alloy for a negative electrode and manufacturing method therefor |
| DE69420104T2 (en) * | 1993-10-08 | 2000-01-20 | Sanyo Electric Co., Ltd. | Process for the evaluation of hydrogen-absorbing alloys for electrodes. |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51148634A (en) * | 1975-06-17 | 1976-12-21 | Mitsubishi Heavy Ind Ltd | Method of producing hydrogennoccluding metal |
| JPS57177942A (en) * | 1981-04-24 | 1982-11-01 | Toshiba Corp | Manufacture of material for storing hydrogen |
| JPS60138036A (en) * | 1983-12-26 | 1985-07-22 | Matsushita Electric Ind Co Ltd | Thin strip of ultra-quickly cooled nickel-titanium alloy and its production |
| JPS62136547A (en) * | 1985-10-28 | 1987-06-19 | エナ−ジ−・コンバ−シヨン・デバイセス・インコ−ポレ−テツド | Hydrogen storing material and its production |
-
1989
- 1989-03-01 JP JP1050497A patent/JP2755661B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02228434A (en) | 1990-09-11 |
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