JPH03232705A - Production of hydrogenated metal powder - Google Patents
Production of hydrogenated metal powderInfo
- Publication number
- JPH03232705A JPH03232705A JP3021990A JP3021990A JPH03232705A JP H03232705 A JPH03232705 A JP H03232705A JP 3021990 A JP3021990 A JP 3021990A JP 3021990 A JP3021990 A JP 3021990A JP H03232705 A JPH03232705 A JP H03232705A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- organic solvent
- crushing
- metal
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 47
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 35
- 239000002184 metal Substances 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims description 16
- 239000003960 organic solvent Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 229930195734 saturated hydrocarbon Natural products 0.000 claims abstract description 3
- 229910052987 metal hydride Inorganic materials 0.000 claims description 19
- 150000004681 metal hydrides Chemical class 0.000 claims description 19
- 125000004435 hydrogen atom Chemical group [H]* 0.000 abstract description 11
- 230000004913 activation Effects 0.000 abstract description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 24
- 239000001257 hydrogen Substances 0.000 description 11
- 229910052739 hydrogen Inorganic materials 0.000 description 11
- 239000002994 raw material Substances 0.000 description 11
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 238000005984 hydrogenation reaction Methods 0.000 description 8
- -1 niobium hydride Chemical compound 0.000 description 8
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 6
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 5
- 125000004430 oxygen atom Chemical group O* 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010494 dissociation reaction Methods 0.000 description 3
- 230000005593 dissociations Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 125000005843 halogen group Chemical group 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 239000010955 niobium Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 150000004678 hydrides Chemical class 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 239000011232 storage material Substances 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- YZCKVEUIGOORGS-UHFFFAOYSA-N Hydrogen atom Chemical compound [H] YZCKVEUIGOORGS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 150000001845 chromium compounds Chemical class 0.000 description 1
- 229910001320 chromium hydride Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000009849 vacuum degassing Methods 0.000 description 1
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、金属水素化物を用いた、水素貯蔵材料、水素
精製材料、水素貯蔵電極材料を作る方法において、その
金属水素化物粉末の製造方法に関するものである。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing a hydrogen storage material, hydrogen purification material, or hydrogen storage electrode material using a metal hydride, and a method for producing the metal hydride powder. It is related to.
従来、金属水素化物は、金属元素と水素ガスとの直接反
応によって製造されている。すなわち、固体の金属元素
をＭ、水素ガスをＨ２＋金属水素化物をＭＨゎとすると
、次の式で示される。Conventionally, metal hydrides are produced by direct reaction of metal elements and hydrogen gas. That is, assuming that M is a solid metal element, H2 is hydrogen gas, and MH is a metal hydride, it is expressed by the following formula.
Ｍ（固体） ＋ Ｈｔ （気体）＝ＭＨ，（固体）水素
ガスは金属元素と接触することにより、吸着、解離をお
こし原子状の水素を発生する。この水素原子は金属元素
の中へ溶は込み、いわゆる、固溶体を形成する。金属元
素の中における水素原子の溶解度は金属元素の種類、温
度、水素ガスの圧力によって一定の値を取る。従って、
これらの条件によって定まる濃度以上に水素原子が溶は
込んだ場合、もはや固溶体の形で水素原子を吸収するこ
とは不可能となり、金属元素との化合物を形成すること
になる。これが、金属水素化物である。M (solid) + Ht (gas) = MH, (solid) When hydrogen gas comes into contact with a metal element, it adsorbs and dissociates to generate atomic hydrogen. This hydrogen atom dissolves into the metal element and forms a so-called solid solution. The solubility of hydrogen atoms in metal elements takes a constant value depending on the type of metal element, temperature, and pressure of hydrogen gas. Therefore,
When hydrogen atoms are dissolved in a concentration higher than that determined by these conditions, it is no longer possible to absorb hydrogen atoms in the form of a solid solution, and a compound with a metal element is formed. This is a metal hydride.
しかし、上記の様な水素ガスとの直接反応による金属水
素化物の製造方法では次の操作が必要である。（１）高
温ならびに高圧状態における水素ガスの吸収が必要であ
る。（２）金属表面における水素ガスの吸着及び解離を
容易にするため、金属原料粉に対して、いわゆる活性化
処理が必要である。具体的に上記（１）に関して、例え
ば、マグネシウムの場合は、３００〜４００°Ｃにおい
て２４気圧〜４００気圧の加圧水素ガス中で製造を行う
必要がある。また、バナジウムの場合は、室温において
７０気圧の加圧水素ガス中で製造を行う必要がある。さ
らに、ランタンニンケルの場合は、室温で５０気圧〜６
０気圧の加圧水素ガス中で行う必要がある。上記（２）
の活性化処理の具体例としては、金属原料粉の表面にお
ける酸化被膜を除去する処理であるが、バナジウムの場
合は、金属原料粉を４５０°Ｃで真空中において脱ガス
処理を施したのち、室温で７０気圧の水素ガスによって
加圧処理をし、これを−７８°Ｃに冷却し、ついで水素
ガスを１気圧とし、再び、４５０°Ｃにおける真空脱ガ
ス処理を行う操作を少なくとも３回以上繰り返すことが
必要である。However, the method for producing metal hydrides by direct reaction with hydrogen gas as described above requires the following operations. (1) It is necessary to absorb hydrogen gas at high temperature and high pressure. (2) In order to facilitate the adsorption and dissociation of hydrogen gas on the metal surface, it is necessary to perform a so-called activation treatment on the metal raw material powder. Specifically regarding (1) above, for example, in the case of magnesium, it is necessary to manufacture it in pressurized hydrogen gas at 300 to 400°C and 24 atm to 400 atm. Furthermore, in the case of vanadium, it is necessary to manufacture it in pressurized hydrogen gas at 70 atmospheres at room temperature. Furthermore, in the case of lanterninkel, 50 atm to 6 atm at room temperature.
It is necessary to perform this in pressurized hydrogen gas at 0 atmospheres. Above (2)
A specific example of the activation treatment is a treatment to remove the oxide film on the surface of the metal raw material powder, but in the case of vanadium, the metal raw material powder is degassed in a vacuum at 450 ° C, and then Pressure treatment with hydrogen gas at 70 atm at room temperature, cooling to -78 °C, then increasing hydrogen gas to 1 atm, and vacuum degassing at 450 °C again at least three times. It is necessary to repeat.
以上のため、従来の技術は、耐高圧、耐高温真空系統な
ど製造装置及び反応装置が複雑化すると共に、製造技術
の工程自体が複雑であるという問題点を含んでいる。For this reason, the conventional technology has problems in that manufacturing equipment and reaction equipment such as high-pressure resistant and high-temperature resistant vacuum systems are complicated, and the manufacturing technology process itself is complicated.
本発明者は、従来の技術の（１）高温、高圧での処理及
び（２）活性化処理を行わなで、金属水素化物を製造す
る方法を検討した結果、水素原子を含有する液体状の有
機溶媒から水素原子を供給することにより、金属水素化
物の粉末を得ることが可能であることを見出、し、本発
明を完成したものである。The present inventor investigated a method for producing metal hydrides without performing (1) high temperature and high pressure treatment and (2) activation treatment in the prior art. The inventors have discovered that it is possible to obtain metal hydride powder by supplying hydrogen atoms from an organic solvent, and have completed the present invention.
本発明は、機械的破砕法により、金属粉を有機溶媒とと
もに撹拌破砕することを特徴とする金属水素化物粉末の
製造方法である。The present invention is a method for producing metal hydride powder, characterized by stirring and crushing metal powder together with an organic solvent by a mechanical crushing method.
即ち、本発明の特徴は、（１）水素原子の供給源として
、液体状態にある有機溶媒を用いること、（２）水素化
反応における原料粉末の活性な表面を得るため、機械的
破砕法を用いること、（３）成型体への加工を容易にす
るため機械的破砕法を用いることによりサブミクロン単
位の微細粉を得ること、の３点を特徴とする金属水素化
物粉末の製造方法である。That is, the features of the present invention are (1) using an organic solvent in a liquid state as a source of hydrogen atoms, and (2) using a mechanical crushing method to obtain an active surface of the raw material powder in the hydrogenation reaction. (3) Obtaining a fine powder of submicron size by using a mechanical crushing method to facilitate processing into a molded body. .
本発明における金属水素化物粉末の製造方法は、従来の
高温ならびに高圧の水素ガスを使用した製造方法とは全
く異なるものである。金属粉末を水素化するための水素
原子の供給源を、分子構造が鎖状をした飽和炭化水素系
の液体としている。製造装置としては、通常のボールミ
ル、例えば回転式ボールミルを使用する。ボールミル容
器内に、原料金属粉と水素供給源として有機溶媒を投入
する。原料としての金属粉は、粒度として１００メツシ
ユ以下であれば適する。これらを、ボールと共にミル、
即ち、粉砕することによって、室温において金属水素化
物粉末を得ることが可能となる。The method for producing metal hydride powder in the present invention is completely different from conventional production methods using high temperature and high pressure hydrogen gas. The source of hydrogen atoms for hydrogenating metal powder is a saturated hydrocarbon liquid with a chain-like molecular structure. As a manufacturing device, a normal ball mill, such as a rotary ball mill, is used. Raw metal powder and an organic solvent as a hydrogen supply source are placed in a ball mill container. The metal powder used as the raw material is suitable if it has a particle size of 100 mesh or less. Mill these together with the balls.
That is, by grinding, it becomes possible to obtain metal hydride powder at room temperature.
本方法の原理は、ボールミルによって金属粉の新生面を
創出し、この表面活性な新生面に対し、有機溶媒分子を
吸着及び解離させることによって、金属粉に対して水素
原子を供給し、金属水素化物の粉末を製造するものであ
る。The principle of this method is to create a new surface of the metal powder using a ball mill, and by adsorbing and dissociating organic solvent molecules to this surface active new surface, hydrogen atoms are supplied to the metal powder, and the metal hydride is produced. It produces powder.
さて、通常、金属粉はその表面が酸化物の層で覆われて
いるため、単に金属粉と有機溶媒では、金属水素化物を
製造することはできない。従って、酸化物で覆われてい
ない表面活性な新生面を得ること及び反応時間を短縮す
るため表面積の増大が必要である。湿式法のボールミル
はこの両者を満たしている。Now, since the surface of metal powder is usually covered with an oxide layer, metal hydride cannot be produced simply by using metal powder and an organic solvent. Therefore, it is necessary to increase the surface area in order to obtain a surface-active nascent surface that is not covered with oxides and to shorten the reaction time. The wet method ball mill satisfies both of these requirements.
破壊は金属の新生面を得る方法の一つとして知られてい
るが、この新生面は、瞬時にして再び酸化物層に覆われ
てしまう。しかし、有機溶媒と共に金属粉の粉砕を行っ
た場合、即ち、湿式法の粉砕においては、破砕によって
創出された新生面は有機溶媒の液によって保護されてい
るため酸化することがなく、有機溶媒分子の吸着及び解
離を促進する。さらに、粉砕によって新生面は供給され
続ける。従って、破砕が継続する限り、金属粉の水素化
反応は進行する。ここで、有機溶媒と金属原料粉の割合
が重要である。有機溶媒の量が少ない時は、金属粉の水
素化反応は、途中で止まってしまう。これは、有機溶媒
の水素原子供給能力がある一定の値、例えば、有機溶媒
分子１個に対して水素原子１個をとるためである。従っ
て、原料金属粉に対して、十分な有機溶媒を与える必要
がある。Destruction is known as one method of obtaining a new surface of metal, but this new surface is instantly covered with an oxide layer again. However, when metal powder is crushed together with an organic solvent, that is, in the wet method, the new surface created by crushing is protected by the organic solvent liquid, so it does not oxidize, and the organic solvent molecules Promotes adsorption and dissociation. Furthermore, the nascent surface continues to be supplied by the grinding. Therefore, as long as the crushing continues, the hydrogenation reaction of the metal powder will proceed. Here, the ratio of the organic solvent to the metal raw material powder is important. When the amount of organic solvent is small, the hydrogenation reaction of metal powder stops midway. This is because the ability of the organic solvent to supply hydrogen atoms is a certain value, for example, one hydrogen atom per organic solvent molecule. Therefore, it is necessary to provide a sufficient amount of organic solvent to the raw metal powder.
また、有機溶媒の選択に留意しなければならない。有機
溶媒としては、酸素原子を含む有機溶媒であるか否かが
重要である。即ち、酸素原子を含む有機溶媒の場合は、
有機溶媒分子の原料金属粉への吸着が酸素原子から起る
ため、金属表面における有機溶媒分子の吸着及び解離に
よる水素原子の放出が困難になるためである。さらには
、酸素原子を含む有機溶媒は、酸素原子による分極効果
のため、１００％の純粋な液体で得ることが不可能であ
り、水分子を含んでいる。この水分子は、金属原料粉の
表面を酸化させるため、金属粉はその表面が酸化物層で
覆われてしまい、有機溶媒分子の吸着を妨げ、金属粉の
水素化反応を困難にする。Also, care must be taken in the selection of organic solvents. It is important whether the organic solvent contains an oxygen atom or not. That is, in the case of an organic solvent containing oxygen atoms,
This is because adsorption of organic solvent molecules onto the raw metal powder occurs from oxygen atoms, making it difficult to release hydrogen atoms by adsorption and dissociation of organic solvent molecules on the metal surface. Furthermore, organic solvents containing oxygen atoms cannot be obtained as 100% pure liquids due to the polarization effect of oxygen atoms, and contain water molecules. These water molecules oxidize the surface of the metal raw material powder, so the surface of the metal powder is covered with an oxide layer, which prevents the adsorption of organic solvent molecules and makes the hydrogenation reaction of the metal powder difficult.
このような作用によって、本発明の方法によって得られ
る金属水素化物をＸ線回折法によって調査すると、破砕
時間とともに連続的に、純粋な金属粉から金属水素化物
に変化していることが確認される。Due to such an effect, when the metal hydride obtained by the method of the present invention is investigated by X-ray diffraction method, it is confirmed that the metal hydride continuously changes from pure metal powder to metal hydride with the crushing time. .
実施例（１） 原料として純ニオビウム粉（フルウチ化学製。 Example (1) The raw material is pure niobium powder (manufactured by Furuuchi Chemical).
１００メツシユ）を用いた。撹拌機としては回転式撹拌
機（ＳＵＳ３０４製、直径１００ＩＩＩＩｌｌ、高さ９
０ｍｍ）を使用した。破砕球としては超硬合金球（直径
１０ｎｕ＋＋）を使用した。水素供給源としてはへブタ
ンを使用した。純ニオビウム粉５０ｇとへブタン１００
ｃｃを破砕球１５０個とともに容器に投入し破砕を開始
した。100 mesh) was used. The stirrer is a rotary stirrer (made of SUS304, diameter 100IIIll, height 9
0 mm) was used. A cemented carbide ball (diameter 10 nu++) was used as the crushing ball. Hebutane was used as the hydrogen source. 50g pure niobium powder and 100g hebutane
cc was put into a container together with 150 crushed balls, and crushing was started.
この時、試料表面の保護のためアルキルナフタレン油を
１０％添加した。Ｘ線回折法によって破砕ならびにそれ
に伴う水素化の過程を調査したところ、破砕開始後３０
０時間で、純ニオビウムの回折強度が低下するとともに
、純ニオビウムの各回折ピークの低角側にニオビウム水
素化物の回折ピークが現れ始めた。破砕開始後１０００
時間で、純ニオビウムの回折ピークは完全に消失し、結
晶状態のニオビウム水素化物が得られた。走査型電子顕
微鏡の観察により、得られたニオビウム水素化物粉末は
サブミクロンサイズの粉末であることが確認された。At this time, 10% alkylnaphthalene oil was added to protect the sample surface. When we investigated the crushing and accompanying hydrogenation process using X-ray diffraction, we found that 30 minutes after the start of crushing.
At 0 hours, the diffraction intensity of pure niobium decreased, and a diffraction peak of niobium hydride began to appear on the lower angle side of each diffraction peak of pure niobium. 1000 after starting crushing
In time, the diffraction peak of pure niobium completely disappeared, and niobium hydride in the crystalline state was obtained. Observation with a scanning electron microscope confirmed that the obtained niobium hydride powder was a submicron-sized powder.
実施例（２）
原料として純クロム粉（フルウチ化学製、 −１００メ
、ンユ）を用いた。撹拌機としては回転式撹拌機（ＳＵ
Ｓ３０４製、直径１００ｎ＋ｍ、高さ９０ｍｍ）を使用
した。Example (2) Pure chromium powder (manufactured by Furuuchi Chemical Co., Ltd., -100mm) was used as a raw material. The stirrer is a rotary stirrer (SU
(made of S304, diameter 100n+m, height 90mm) was used.
破砕球としては超硬合金球（直径１０＋＋ｕａ）を使用
した。水素供給源としてはへブタンを使用した。純クロ
ム粉５０ｇとへブタン１００ｃｃを破砕球１５０個とと
もに容器に投入し破砕を開始した。この時、試料表面の
保護のためアルキルナフタレン油を１０％添加した。Ｘ
線回折法によって破砕ならびにそれに伴う水素化の過程
を調査したところ、破砕開始後３００時間で、クロムの
回折ピークはブロードとなり、破砕開始後約１０００時
間において、アモルファス合金に特有の、回折ピークの
ない、ハローパターンとなり、アモルファス状態のクロ
ム水素化物が得られた。走査型電子顕微鏡の観察により
、得られたクロム化合物はサブミクンサイズの粉末であ
ることが確認された。A cemented carbide ball (diameter 10++ ua) was used as the crushing ball. Hebutane was used as the hydrogen source. 50 g of pure chromium powder and 100 cc of hebutane were put into a container along with 150 crushed balls, and crushing was started. At this time, 10% alkylnaphthalene oil was added to protect the sample surface. X
When the crushing and accompanying hydrogenation process were investigated using a line diffraction method, the diffraction peak of chromium became broad 300 hours after the start of crushing, and about 1000 hours after the start of crushing, there was no diffraction peak, which is characteristic of amorphous alloys. , a halo pattern was formed, and chromium hydride in an amorphous state was obtained. Observation with a scanning electron microscope confirmed that the obtained chromium compound was a submicron-sized powder.
実施例（３）
原料として純マンガン粉（フルウチ化学製、−１００メ
ツシュ）を用いた。撹拌機としては回転式撹拌機（ＳＵ
Ｓ３０４製、直径１００ｍｍ、高さ９０ｍａ＋）を使用
した。Example (3) Pure manganese powder (manufactured by Furuuchi Chemical, -100 mesh) was used as a raw material. The stirrer is a rotary stirrer (SU
(made of S304, diameter 100 mm, height 90 ma+) was used.
破砕球としては超硬合金球（直径１０ｍｍ）を使用した
。水素供給源としてはへブタンを使用した。純マンガン
粉５０ｇとへブタン１００ｃｃを破砕球１５０個ととも
に容器に投入し破砕を開始した。この時、試料表面の保
護のためアルキルナフタレン油を１０％添加した。Ｘ線
回折法によって破砕ならびにそれに伴う水素化の過程を
調査したところ、破砕開始後１００時間で、マンガンの
回折ピークはブロードとなり、破砕開始後約１０００時
間において、アモルファス合金に特有の、回折ピークの
ない、ハローパターンとなり、アモルファス状態のマン
ガン水素化物が得られた。走査型電子顕微鏡の観察によ
り、得られたマンガン水素化物はサブミクロンサイズの
粉末であることが確認された。A cemented carbide ball (diameter 10 mm) was used as the crushing ball. Hebutane was used as the hydrogen source. 50 g of pure manganese powder and 100 cc of hebutane were put into a container along with 150 crushed balls, and crushing was started. At this time, 10% alkylnaphthalene oil was added to protect the sample surface. When we investigated the crushing and accompanying hydrogenation process using X-ray diffraction, we found that the diffraction peak of manganese became broad 100 hours after the start of crushing, and the diffraction peak of manganese became broad approximately 1000 hours after the start of crushing, which is characteristic of amorphous alloys. No, a halo pattern was formed, and manganese hydride in an amorphous state was obtained. Observation with a scanning electron microscope confirmed that the obtained manganese hydride was a submicron-sized powder.
実施例（４） 原料として純アルミニウム粉（フルウチ化学製。Example (4) Pure aluminum powder (manufactured by Furuuchi Chemical Co., Ltd.) is used as a raw material.
１００メツシユ）、純マンガン粉（フルウチ化学製。100 mesh), pure manganese powder (manufactured by Furuuchi Chemical).
１００メツシユ）、純シリコン（フルウチ化学製。100 mesh), pure silicon (manufactured by Furuuchi Chemical).
１００メツシユ）を用いた。撹拌機としては回転式撹拌
機（ＳｔｌＳ３０４製、直径１００ｍ＋１１．高さ９０
１）を使用した。破砕球としては超硬合金球（直径１０
ＩＩｌｌｌｌ）を使用した。水素供給源としてはへブタ
ンを使用した。純アルミニウム粉、純マンガン粉、純シ
リコン粉を合計５０ｇとへブタン１００ｃｃを破砕味１
５０個とともに容器に投入し破砕を開始した。この時、
試料表面の保護のためアルキルナフタレン油を１０％添
加した。Ｘ線回折法によって破砕ならびにそれに伴う水
素化の過程を調査したところ、破砕開始後５００時間で
、各金属元素の回折ピークはブロードになり始め、破砕
開始後約５０００時間において、アモルファス合金に特
有の、回折ピークのない、ハローパターンとなり、アモ
ルファス状態の（アルミニウムーマンガン−シリコン）
水素化物が得られた。走査型電子顕微鏡の観察により、
得られた（アルミニウムーマンガン−シリコン）水素化
物はサブミクンサイズの粉末であることが確認された。100 mesh) was used. As a stirrer, a rotary stirrer (made of StlS304, diameter 100m + 11.2cm, height 90cm) is used.
1) was used. Cemented carbide balls (diameter 10
IIllll) was used. Hebutane was used as the hydrogen source. Crushed 50g of pure aluminum powder, pure manganese powder, pure silicone powder and 100cc of hebutane
They were put into a container together with 50 pieces, and crushing was started. At this time,
10% alkylnaphthalene oil was added to protect the sample surface. When we investigated the crushing and accompanying hydrogenation process using X-ray diffraction, we found that 500 hours after the start of crushing, the diffraction peaks of each metal element began to become broad, and about 5,000 hours after the start of crushing, the diffraction peaks characteristic of amorphous alloys were observed. , a halo pattern with no diffraction peaks and an amorphous state (aluminum-manganese-silicon)
A hydride was obtained. By observation with a scanning electron microscope,
The obtained (aluminum-manganese-silicon) hydride was confirmed to be a submicron-sized powder.
〔発明の効果〕
本発明の製造方法は、高温、高圧での処理及び活性化処
理を必要としないで金属水素化物粉末を製造でき、得ら
れた粉末はサブミクロンサイズの粉末である特徴を有す
る。このため、成形体への加工が容易であり、水素貯蔵
材料、水素精製材料。[Effects of the Invention] The production method of the present invention is characterized in that metal hydride powder can be produced without the need for high-temperature, high-pressure treatment or activation treatment, and the obtained powder is a submicron-sized powder. . Therefore, it is easy to process into molded bodies, and is used as a hydrogen storage material and hydrogen purification material.
水素貯蔵電極材料等に有利に適用できる。It can be advantageously applied to hydrogen storage electrode materials, etc.
第１図は実施例（１）に対応するＸ線回折の結果を示し
たものである。第２図は実施例（２）に対応するＸ線回
折の結果を示したものである。第３図は実施例（３）に
対応するＸ線回折の結果を示したものである。第４図は
実施例（４）に対応するＸ線回折の結果を示したもので
ある。FIG. 1 shows the results of X-ray diffraction corresponding to Example (1). FIG. 2 shows the results of X-ray diffraction corresponding to Example (2). FIG. 3 shows the results of X-ray diffraction corresponding to Example (3). FIG. 4 shows the results of X-ray diffraction corresponding to Example (4).
Claims (2)
撹拌破砕することを特徴とする金属水素化物粉末の製造
方法。(1) A method for producing metal hydride powder, which comprises stirring and crushing metal powder together with an organic solvent by a mechanical crushing method.
とを特徴とする特許請求の範囲第１項に記載の金属水素
化物粉末の製造方法。(2) The method for producing metal hydride powder according to claim 1, characterized in that a chain-like saturated hydrocarbon is used as the organic solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3021990A JPH03232705A (en) | 1990-02-09 | 1990-02-09 | Production of hydrogenated metal powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3021990A JPH03232705A (en) | 1990-02-09 | 1990-02-09 | Production of hydrogenated metal powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03232705A true JPH03232705A (en) | 1991-10-16 |
Family
ID=12297610
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3021990A Pending JPH03232705A (en) | 1990-02-09 | 1990-02-09 | Production of hydrogenated metal powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03232705A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010142804A (en) * | 2008-12-19 | 2010-07-01 | Gkss Forschungszentrum Geesthacht Gmbh | Method for activating or regenerating hydrogen absorption material |
-
1990
- 1990-02-09 JP JP3021990A patent/JPH03232705A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010142804A (en) * | 2008-12-19 | 2010-07-01 | Gkss Forschungszentrum Geesthacht Gmbh | Method for activating or regenerating hydrogen absorption material |
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