JPH01129960A - Manufacture of thin film of hydrogen storage alloy - Google Patents
Manufacture of thin film of hydrogen storage alloyInfo
- Publication number
- JPH01129960A JPH01129960A JP28880687A JP28880687A JPH01129960A JP H01129960 A JPH01129960 A JP H01129960A JP 28880687 A JP28880687 A JP 28880687A JP 28880687 A JP28880687 A JP 28880687A JP H01129960 A JPH01129960 A JP H01129960A
- Authority
- JP
- Japan
- Prior art keywords
- hydrogen storage
- storage alloy
- substrate
- protective film
- hydrogen
- 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 40
- 239000001257 hydrogen Substances 0.000 title claims abstract description 40
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000003860 storage Methods 0.000 title claims abstract description 25
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 21
- 239000000956 alloy Substances 0.000 title claims abstract description 21
- 239000010409 thin film Substances 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000010408 film Substances 0.000 claims abstract description 23
- 230000001681 protective effect Effects 0.000 claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 18
- 230000035699 permeability Effects 0.000 claims abstract description 9
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 5
- 230000003647 oxidation Effects 0.000 claims abstract description 5
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 10
- 229910000831 Steel Inorganic materials 0.000 claims 1
- 239000010959 steel Substances 0.000 claims 1
- 238000004090 dissolution Methods 0.000 abstract description 5
- 229910001252 Pd alloy Inorganic materials 0.000 abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 3
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 abstract description 3
- 229910000990 Ni alloy Inorganic materials 0.000 abstract description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052725 zinc Inorganic materials 0.000 abstract description 2
- 239000011701 zinc Substances 0.000 abstract description 2
- 238000001312 dry etching Methods 0.000 abstract 2
- DOARWPHSJVUWFT-UHFFFAOYSA-N lanthanum nickel Chemical compound [Ni].[La] DOARWPHSJVUWFT-UHFFFAOYSA-N 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 239000010953 base metal Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 235000012149 noodles Nutrition 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910002335 LaNi5 Inorganic materials 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 210000002816 gill Anatomy 0.000 description 1
- 210000004907 gland Anatomy 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
げ）産業上の利用分野
本発明は、高純度の水素を精製する装置等で用いらｎる
水素吸蔵台金薄膜の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION G) Industrial Application Field The present invention relates to a method for manufacturing a hydrogen storage metal thin film used in an apparatus for refining high-purity hydrogen.
（ロ）従来の技術
半導体の還元工程等で大敵に使用さｎる高純度水素は、
例えば銀・パラジクム合金膜透過法を利用した水素精製
装置によ、て製造さｎている。(b) Conventional technology High-purity hydrogen, which is used as a major enemy in the reduction process of semiconductors, is
For example, it is manufactured by a hydrogen purification apparatus using a silver-palladium alloy membrane permeation method.
しかし、この装置ａ！は銀・パラジウム合金が高価であ
ること、＃製時に４００℃以上の高温が必要であること
と云う欠点がある。However, this device a! The disadvantages are that the silver/palladium alloy is expensive and that high temperatures of 400° C. or higher are required when manufacturing #.
そこで、銀・バラジクム蕾金に代る安価な水素吸蔵合金
を用いることが考えらｎ、更に形状加工を容易にするた
め、水素Ｎ展のゾロヤス速度七上げるために０．１〜３
０μｍ程度の厚さの水素吸蔵台金薄膜が要望さｎた。Therefore, it was considered to use an inexpensive hydrogen storage alloy instead of silver/baladicum gold, and to further facilitate shape processing, it was possible to increase the rate of hydrogen N expansion by 0.1 to 3
There was a demand for a hydrogen storage metal thin film with a thickness of approximately 0 μm.
そして、現状にあっては、特開昭６２−１９１４０２号
公報で示すＬうに、多孔性基板上にスパッタ法或いは蒸
着法で約３０ｐｍ程皮の水素吸蔵合金層１）！４ｔｆ′
Ｆ、戊している。At present, as shown in Japanese Unexamined Patent Publication No. 191402/1982, a hydrogen storage alloy layer 1) with a thickness of about 30 pm is formed on a porous substrate by sputtering or vapor deposition! 4tf'
F. It's empty.
ｃ／９ 発明が解決しようとする問題点しかし、斯る
薄膜は多孔性基板と云う担持体を有しているので、形状
加工が容易ではなく、水素透過性も悪く、平坦性が悪い
ので、膜厚が不均一となってピンホール金発生し易い。c/9 Problems to be solved by the invention However, since such a thin film has a carrier called a porous substrate, it is not easy to shape it, has poor hydrogen permeability, and has poor flatness. The film thickness becomes non-uniform and pinholes are likely to occur.
不発明は、加工性ｒ良好にすると共に水素透過性を維持
でき、更にピンホールの発生を抑えた水素吸蔵台金薄膜
の製造方法？提供するものである。What is uninvented is a method for manufacturing a hydrogen storage metal thin film that has good workability, maintains hydrogen permeability, and suppresses the formation of pinholes. This is what we provide.
に）問題点で＃決するための手段
不発明による解決手段は、基板の平坦面上に、耐酸化性
及び水素透過性の良好な呆ｆ！膜２均一に形成し、次い
でこの保護膜上に水素吸蔵台金層を均一に形成し、久い
てこの水素吸蔵合金層に上記保護膜を形成して両保護膜
間に水素吸蔵合金層を配置し、この後に上記基板ｒ溶解
除去して成る構成である。2) Means to Solve the Problem An inventive solution is to form a substrate with good oxidation resistance and hydrogen permeability on the flat surface of the substrate. A film 2 is uniformly formed, then a hydrogen storage base metal layer is uniformly formed on this protective film, and after a while, the above protective film is formed on this hydrogen storage alloy layer, and a hydrogen storage alloy layer is placed between both protective films. After this, the substrate r is dissolved and removed.
（ホ）作用
平坦な基板上に呆４鴫水票戎蔵台俊層、保護膜の順に均
一な厚さで形成し、基板を溶解除去すると、床敲映に侠
まｎた水素吸蔵台金が薄膜状態で形成される。こｎは、
徂？＃体が無いことから加工しや丁く、水素透過性も良
好となる。更に合金層及び保護腋を平坦な基板に利用し
て均一に形成していることから、凹凸によるピンホール
の発生が少く、とｎに呆−族が刀Ｕえらｎでいるのでめ
るから、溶解時及び溶解後に於ける酸化を防止すること
かできている。(e) Function: Form a uniform thickness layer and a protective film on a flat substrate in this order, and dissolve and remove the substrate. is formed in a thin film state. This is
Myself? # Since there is no body, it is easy to process and has good hydrogen permeability. Furthermore, since the alloy layer and the protective armpit are formed uniformly on a flat substrate, there are fewer pinholes caused by unevenness, and it is possible that there is a gap between the blades and the gills. Oxidation can be prevented during and after dissolution.
（へ）実施例
第１図に基づいて説明すると、５０μｍ厚の亜鉛板であ
る基板１の上面は切削、研磨等の処理で平坦面２として
６シ、この平坦＃！１２上には耐酸性、水素透過性で秀
ｎた銀・パラジウム合金（銀３０ａｔｎｎ＊）ｋＭｉ４
膜３として０．１μｍの厚さで均一に形成する。好まし
い形成方法としては、スパッタ法、イオンブレーティン
グ法、蒸着法が掲げられる。(f) Embodiment To explain based on FIG. 1, the upper surface of the substrate 1, which is a 50 μm thick zinc plate, is processed by cutting, polishing, etc. to form a flat surface 2. On top of No. 12 is a silver-palladium alloy (silver 30atnn*) kMi4 that has excellent acid resistance and hydrogen permeability.
The film 3 is formed uniformly to a thickness of 0.1 μm. Preferred forming methods include sputtering, ion blating, and vapor deposition.
次に、斯る保護＄３を約１００Ａ程度ドライエツチング
し、この後に保護膜３上にクンタンニッケル合金（Ｌａ
Ｎｉｓ）ｇ小素吸蔵合金Ｍ４として５６０μｍの厚さで
均一に形成する。形成方法は上述と同じ。Next, the protective film 3 is dry-etched at about 100A, and then a Kuntan nickel alloy (La
A Nis)g small element storage alloy M4 is uniformly formed with a thickness of 560 μm. The formation method is the same as above.
仄に、水素吸蔵合金層４ｔ−約ｌｏｏ ＡｓＢｔドライ
エツチングし、この後に水素吸蔵合金層４よに上述と同
じ銀・パラジウム含金を床岐展５として０、１ ｐ Ｍ
ｌの厚さで均一に形成する。形成方法は上述と同じ。At the same time, the hydrogen storage alloy layer 4t was dry-etched with approximately loo AsBt, and then the hydrogen storage alloy layer 4 was coated with the same silver and palladium containing metal as described above at a concentration of 0.1 pM.
Form it uniformly to a thickness of l. The formation method is the same as above.
そして、基板１−１希塩酸水溶液（５５Ｎ）でｇ解除去
し、順に水洗し、アセトン洗浄し、乾燥する。Then, the substrate 1-1 is removed by decomposition with a dilute aqueous hydrochloric acid solution (55N), washed with water, washed with acetone, and dried.
かくして、ｅｆ：、護膜３．５の間に水素吸蔵台金１ｍ
４を配した水素吸蔵台違薄膜６が得らｎた。この薄膜
６は、担持体が無く、平坦性及び可撓性を有するもので
あり、瑳厚も均一と成、ている。Thus, ef:, 1 m of hydrogen storage base between the protective film 3.5
A hydrogen-absorbing thin film 6 in which 4 was arranged was obtained. This thin film 6 has no carrier, has flatness and flexibility, and has a uniform thickness.
ドライエラをングは、腺よ、層上に生じる酸化膜Ｖｌ−
除去しているのであり、スパッタ法等を採用できる。When drying, the oxide film Vl- formed on the gland layer.
Therefore, a sputtering method or the like can be used.
基板ｌは、アルミニューム（ＡＪ）％ポリフ二二しンオ
キシド等の銅島性高分子材料を採用できるし、水素吸蔵
合金層４も既に知らｎた他の材料（希土類・ニッケル＆
会金、ｔタニワム基合衾、マグネシクム・ニッケル基台
金等）を採用できる。The substrate 1 can be made of a copper island polymer material such as aluminum (AJ)% polyphenylene oxide, and the hydrogen storage alloy layer 4 can also be made of other known materials (rare earth, nickel, etc.).
(Kaikin, Taniwam Kigoijuku, Magnesicum/Nickel base metal, etc.) can be adopted.
因みに１水素吸蔵含釡薄膜の不発明方法採用例と従来方
法採用例との特性比較をｖｃ表に示す。Incidentally, the VC table shows a comparison of the characteristics of a hydrogen-absorbing pot thin film using the uninvented method and an example using the conventional method.
秦水素吸７ＩＬ台金層として厚さ５０μｍでＬａＮｉ５
を用いた。LaNi5 with a thickness of 50 μm as the base metal layer for the Qin hydrogen absorbing 7IL.
was used.
※水素透過試験の条件は、１５０℃、ｌ久側水索圧力１
ａｔｍａｂ１２次側水素圧力ＯＢｔｍａｂである。*Hydrogen permeation test conditions are 150℃, 1 side water line pressure 1
atmab1 Secondary side hydrogen pressure OBtmab.
（）Ｊ発明の効果
本発明に威゛ｎば、晶板忙溶解除去したので、水素吸蔵
台盆博膜の加工性が同上すると共に水素透過性が良好と
なり、＊系吸賊台ｇｌＬ層を床−課で挾み且つ映、麺を
均一にしたので、溶解時及び離解後の飯化を防ぎ、ピン
ホールの発生を迎えることができるものである。()J Effects of the Invention The present invention has the advantage that since the crystal plate is removed by dissolution, the workability of the hydrogen storage tray HIROme is the same as above, and the hydrogen permeability is good. Since the noodles are sandwiched and rolled in the floor section to make them uniform, it is possible to prevent the noodles from becoming sticky during dissolution and after disintegration, and to prevent pinholes from forming.
第１図Ｕ】切Ｑ９に）（ホ）は本発明方法ｔｊ社に示す
断面図である。
１・・・基板、２・・・平担面、３．５・・・床＃！ｉ
１編、６・・・水巣吸ＩＲ菅釡淋展。FIG. 1 U] Cutting Q9) (E) is a sectional view showing the method of the present invention by TJ Company. 1...Substrate, 2...Flat surface, 3.5...Floor #! i
Part 1, 6... Mizusui IR Hinoki Kannobu.
Claims (1)
好な保護膜を均一に形成し、次いでこの保護膜上に水素
吸蔵合金層を均一に形成し、次いでこの水素吸蔵合金層
に上記保護膜鋼を形成して両保護膜間に水素吸蔵合金層
を配置し、この後に上記基板を溶解除去して成る水素吸
蔵合金薄膜の製造方法。(1) A protective film with good oxidation resistance and hydrogen permeability is uniformly formed on the flat surface of the substrate, then a hydrogen storage alloy layer is uniformly formed on this protective film, and then this hydrogen storage alloy layer is formed uniformly on the protective film. A method for manufacturing a hydrogen storage alloy thin film, which comprises forming the above-mentioned protective film steel, arranging a hydrogen storage alloy layer between both protective films, and then dissolving and removing the above-mentioned substrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28880687A JPH01129960A (en) | 1987-11-16 | 1987-11-16 | Manufacture of thin film of hydrogen storage alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28880687A JPH01129960A (en) | 1987-11-16 | 1987-11-16 | Manufacture of thin film of hydrogen storage alloy |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01129960A true JPH01129960A (en) | 1989-05-23 |
Family
ID=17734974
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28880687A Pending JPH01129960A (en) | 1987-11-16 | 1987-11-16 | Manufacture of thin film of hydrogen storage alloy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01129960A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995027315A1 (en) * | 1994-03-31 | 1995-10-12 | Motorola, Inc. | Improved metal hydride hydrogen storage electrodes |
| CN109680254A (en) * | 2019-02-28 | 2019-04-26 | 中国工程物理研究院化工材料研究所 | A kind of magnesium alloy carries hydrogen thin-film material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57137465A (en) * | 1981-01-16 | 1982-08-25 | Heraeus Gmbh W C | Manufacture of multilayer |
| JPS60100664A (en) * | 1983-11-07 | 1985-06-04 | Matsushita Electric Ind Co Ltd | Material for storing hydrogen |
-
1987
- 1987-11-16 JP JP28880687A patent/JPH01129960A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57137465A (en) * | 1981-01-16 | 1982-08-25 | Heraeus Gmbh W C | Manufacture of multilayer |
| JPS60100664A (en) * | 1983-11-07 | 1985-06-04 | Matsushita Electric Ind Co Ltd | Material for storing hydrogen |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995027315A1 (en) * | 1994-03-31 | 1995-10-12 | Motorola, Inc. | Improved metal hydride hydrogen storage electrodes |
| CN109680254A (en) * | 2019-02-28 | 2019-04-26 | 中国工程物理研究院化工材料研究所 | A kind of magnesium alloy carries hydrogen thin-film material and preparation method thereof |
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