TW201000645A - Method to produce high stoichiometric Mg2Ni hydrogen storage alloys and apparatus for the same - Google Patents

Method to produce high stoichiometric Mg2Ni hydrogen storage alloys and apparatus for the same Download PDF

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TW201000645A
TW201000645A TW97124474A TW97124474A TW201000645A TW 201000645 A TW201000645 A TW 201000645A TW 97124474 A TW97124474 A TW 97124474A TW 97124474 A TW97124474 A TW 97124474A TW 201000645 A TW201000645 A TW 201000645A
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magnesium
liquid
nickel
hydrogen storage
storage alloy
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TW97124474A
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TWI393787B (en
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Yuan-Pang Wu
Hui-Yun Bor
Rong-Ruey Jeng
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Chung Shan Inst Of Science
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Abstract

The present invention relates to the formation of high purity Mg2Ni hydrogen storage alloy having a stoichiometric composition. This is achieved by controlling the Mg-Ni composition between 23.5 and 50.2 wt% in nickel, as well as by its melt temperature between its solidus and liquidus line. Under this condition, only γ phase Mg2Ni compound will precipitates according to the equilibrium phase diagram. In this invention, a special apparatus is also designed such that the hot discard liquid, which is not pure γ phase but enriched in magnesium, can be directly re-used as a useful composition adjusting agent in the next run, and save much heating energy. Consequently, it can continuously produce high purity γ phase Mg2Ni hydrogen storage alloy.

Description

201000645 九、發明說明: 【發明所屬之技術領域】 本案所屬之技術領域主要為新能源科技之氫能固態储存技 術。另就發明所屬之製程技術觀點,亦與儲氫合金之冶煉技術 有關。 【先前技術】 自工業革命之後,隨著人類生產活動所產生大量排放的溫室氣 ,(如二氧化碳、甲烷、敗氯碳化物'一氧化二氮及臭氧等), 其中又以二氧化碳為最主要的人類排放溫室氣體,其貢獻度 高達六成,已形成嚴重的溫室效應,使得地球表面的平均溫$ 自十十世、己中期起就逐漸上升,造成全球暖化的現象。目前在 大規模使用石化能源下所產生之s〇2、c〇、Ν〇χ等有 等與It量二氧化碳造成之溫室效應,引發全 發ί #系問題下’世界各國莫不致力於新能源科技之開 室因文^產品只有水沒有二氧化碳,完全無污染又 -:被已被國際能源總署規劃為絲主要能源之 做為燃料,特別是革=生科技之一的燃料電池’也以氫 燃料電池更是以以^ =月匕燃燒效率的質子交換膜_F〇 氫氣之分子量太小燃料。但在實際應用上,因為 高壓方式儲存,但私^儲存體社過龐大,賴可採用超 此氫氣的儲存虚運法規與標準要求也相對嚴苛,因 傳統儲氫方成是否成功應用之關鍵。 氫氣,但鋼瓶儲存氫囊疋利用尚壓鋼瓶(氫氣瓶)來儲存 個大氣壓,所裝氫氣的皙^積小,瓶裏的氫氣即使加壓到150 有爆炸的危險;另二種‘二,不到虱氣瓶質量的1%,而且還 253°C變為液體進行儲;^法是儲存液態氫,將氣態氫降溫到〜 的絕熱裝置來隔埶,’但液體儲存箱非常龐大,需要極好 ,、、、才犯防止液態氫不會沸騰汽化。 5 201000645 ^到膽年代赠,可將氫賴態方式儲氫之職合金產^ ^之儲虱合金’無論是過渡金屬系AB2儲氮合金、或是 金屬系AB5儲士合金其儲氫重量密度仍嫌太低,不到2.0重詈 =比’ I^此南容量儲氫合金之研發乃目前國際發展之趨勢。 二Ϊ之ί糸儲氫合金’由於具有儲氫量高、質量輕、原料成本 低廉之優點,因此被視為相當有發展潛力之儲氫合金,但201000645 IX. Description of the invention: [Technical field to which the invention belongs] The technical field to which this case belongs is mainly the hydrogen energy solid state storage technology of the new energy technology. In addition, the viewpoint of the process technology to which the invention belongs is also related to the smelting technology of the hydrogen storage alloy. [Prior Art] Since the industrial revolution, a large amount of greenhouse gases (such as carbon dioxide, methane, chlorocarbons, nitrous oxide and ozone) have been produced with human production activities, among which carbon dioxide is the most important. Humans emit greenhouse gases, which contribute up to 60%, and have formed a serious greenhouse effect. The average temperature of the Earth's surface has gradually increased since the tenth century, and it has caused global warming. At present, under the large-scale use of petrochemical energy, s〇2, c〇, Ν〇χ, etc. have the greenhouse effect caused by the amount of carbon dioxide, and the whole world is caused by the problem. The opening room of the product ^ product only water without carbon dioxide, completely pollution-free - has been planned by the International Energy Agency as the main energy source of the fuel, especially the fuel cell of one of the science = also hydrogen The fuel cell is a proton exchange membrane with a combustion efficiency of ^ = 匕 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 However, in practical applications, because of the high-pressure storage, but the private storage body is too large, it is relatively strict to use the hydrogen storage regulations and standards, because the traditional hydrogen storage method is the key to successful application. . Hydrogen, but the cylinders store hydrogen sacs. They use a still-pressed cylinder (hydrogen cylinder) to store the atmospheric pressure. The hydrogen contained in the cylinder is small, and the hydrogen in the bottle is dangerous to explode even if it is pressurized to 150; the other two Less than 1% of the mass of the helium cylinder, and also 253 ° C into a liquid for storage; ^ method is to store liquid hydrogen, the gaseous hydrogen is cooled to ~ the insulation device to separate, 'but the liquid storage box is very large, need Excellent, and, to prevent liquid hydrogen from boiling and boiling. 5 201000645 ^When you give it to the gallbladder, you can use the hydrogen storage method to store hydrogen in the alloy. ^The storage alloy of the alloy is either the transition metal system AB2 nitrogen storage alloy or the metal alloy AB5 storage alloy. Still too low, less than 2.0 heavy 詈 = than I ^ This South capacity hydrogen storage alloy research and development is currently the trend of international development. Because of its high hydrogen storage capacity, light weight and low cost of raw materials, the hydrogen storage alloy is considered to be a hydrogen storage alloy with considerable development potential.

因活性大’表面易形成阻礙氫分子吸附之氧化層而影響氣原子 於合,表面擴散速率,導致純料錄活化、吸放氫動力差t 吸放氫溫度過高,因此無法成為實用之儲氫合金。 針對純鎂吸放氫動力學性倾差的_ 藉由,有催化效果之鎳的添加,可改善;= 孟中的吸放氫反應速率’同時對初始活化性能亦有催化之效 ^。而r相之Mg2Ni則為Mg-Ni儲氫合金系統中活化反應速率 最快、吸放氫性質最佳之儲氫合金。 疋千 但由於鎂⑽〇_(1455。〇兩種金屬的熔點差異很大,易 it成炫解不均勻’導致職合金成分不均勻之問題,且錐的基 軋壓很咼,易於熔融過程產生揮發,使初始配比成分產生嚴重 偏差’造成過多的共晶結構與不會吸氫之万相_2生成 解決上述熔煉過程中成分產生嚴重偏差問題,新一代之真空 紐雖然裝設桃上檢測魏,然㈣後Mg_Ni儲氫合金而 言丄卻因_上之天然雜,使得%_Ni熔融液,即使透過最 精岔之線上檢測功能,將成分準確控制在鎂與鎳原子比為2 : 1之情況下’凝固後仍然、無法得到職純的r相Mg2Ni。 因為根據鎭與鎳之二元平衡相圖,在此—成份下,早在高於 761°C r相MgWi之熔點溫度以上,熔點1147艽不會吸氫之石 相MgNi2已先行凝固析出。又因為沒相之_2其組成遠比^ 相之MgAi含有較高之則,因此造成其餘尚未凝固之Mg_Ni熔 融液偏離原本賴錄原子比為2 : 1之7相Mg2Ni組成,成為 6 201000645 富鎂狀態。此一富鎂狀態Mg-Ni熔融液,在降溫至低於76rc 後,根據鎂與鎳之二元平衡相圖,在此一成份下,不僅會生成 r才目之M_i,在507〇C之共晶溫度還會得到包括純鎂相在内 之八晶組織。也就是說,即使在巨觀組成完全符合7相之比例 下’其微觀之組織結構卻是在7相之Μ&Νί中摻雜有冷相之 相。所以傳統麟法無法製備活化反 快、吸放氫性質佳之高純度Mg2Ni儲氫合金。 【發明内容】 =明之目的之…在於提供—難造高純度_儲氫合金之 f法及其裝置,*需精確控獅成麟儲氫合金巾顯 置,即得到高純度鎂鎳儲氫合金。 ’、 it t目的之…在於提供—種製造高純度_儲氫合金之 裝置’回收析出反應後剩餘之富鎂液體,依照本發明 、方法連續製造尚純度鎂鎳儲氫合金。 到上述目的’本發明提供―種製造高純度麟儲氣合金 /及其裝置’該裝置包含—密閉艙體、—第—掛鋼、一加Due to the large activity, the surface is easy to form an oxide layer that hinders the adsorption of hydrogen molecules, which affects the gas atomization and the surface diffusion rate, resulting in pure material recording activation, hydrogen absorption and desorption, and high hydrogen absorption and desorption. Therefore, it cannot be a practical storage. Hydrogen alloy. The kinetic dip of hydrogen absorption and desorption of pure magnesium can be improved by the addition of nickel with catalytic effect; = the rate of hydrogen absorption and desorption in Mengzhong is also catalyzed by the initial activation performance. The r-phase Mg2Ni is the hydrogen storage alloy with the fastest activation reaction rate and the best hydrogen absorption and desorption properties in the Mg-Ni hydrogen storage alloy system.疋 thousand but due to magnesium (10) 〇 _ (1455. 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 Volatilization produces a serious deviation from the initial proportioning component', causing excessive eutectic structure and tens of thousands of phases that do not absorb hydrogen to solve the problem of serious deviation of the components in the above smelting process. After the detection of Wei, (M), after the Mg_Ni hydrogen storage alloy, the 丄 is naturally mixed, so that the %_Ni melt, even through the most accurate on-line detection function, accurately controls the composition of the atomic ratio of magnesium to nickel to 2: In the case of 1 'after the solidification, it is still unable to obtain the pure phase r-phase Mg2Ni. Because according to the binary equilibrium phase diagram of yttrium and nickel, under this composition, as early as above the melting point temperature of the 761 ° C r phase MgWi The melting point of 1147 艽 does not absorb hydrogen. The phase of MgNi2 has been coagulated and precipitated. Because the composition of _2 is far higher than the MgAi of the phase, the remaining Mg_Ni melt which has not yet solidified deviates from the original Recorded atomic ratio is 2 : 1 7-phase Mg2Ni composition, becoming 6 201000645 magnesium-rich state. This magnesium-rich Mg-Ni melt, after cooling to less than 76rc, according to the binary equilibrium phase diagram of magnesium and nickel, under this component, not only will The M_i is generated, and the eutectic temperature at 507 〇C also gives the octagonal structure including the pure magnesium phase. That is, even in the case where the macroscopic composition completely conforms to the ratio of the 7 phases, the microscopic structure The structure is doped with a phase of cold phase in the phase 7 & Νί. Therefore, the conventional lining method cannot prepare a high-purity Mg2Ni hydrogen storage alloy which is activated by anti-fast, good hydrogen absorption and desorption properties. [Summary of the invention] In order to provide - high-purity hydrogen storage alloy f method and its equipment, * need to accurately control the lion Chenglin hydrogen storage alloy towel display, that is, to obtain high-purity magnesium-nickel hydrogen storage alloy. ', it t purpose ... Providing a device for producing a high-purity hydrogen storage alloy, 'recovering the magnesium-rich liquid remaining after the precipitation reaction, and continuously producing a magnesium-hydrogen storage alloy of a purity according to the present invention. The above object provides the invention to produce high purity. Lin gas storage alloy / its device 'The device contains - closed cabin, - first - hanging steel, one plus

ΓΪί、—麟裝置及—第二獅,其方絲將—純鎂原料置 一=f Γ職内,並將盛有該顯料之該第—職送入已通入 全該ί 3體:,:用該加熱裝置將該鎂原料加熱 體。接下來再將一純鎳粉徐徐加入盛有該 用Hi—_,並以該獅裝置不斷施以機械賴拌與利 加熱升溫’使_粉全部充分賴,並與該鎂液 i均句之一_液體。相較於習知之複雜做法,本發明 錄ii完全無讎設精密之線上檢_,與精準控制錢 成f τ要所添加之鎳,其添加量佔全部鎂舰融 於23,5至5〇.2就能保證得到組成為 =M 是鎂與鎳原子比為2 : D完全純的γ 相MgWi儲虱合金,而無摻雜有任何其他雜相。 7 201000645 第-圖’係本發明之I置示意圖。如圖所示 閉搶體10、-第一掛鋼U、一加熱 -裳置包含-密 -第二掛鋼18、—吊掛機構17、乂有:巧拌裝置16、 ^ 10=-加料管⑽,而本實施例之密冷鋼 一析出至101及一坩鍋取出/送 系、分割為 脑取出/送人室1G3間分別設置至少=衫m及該 該析出室1(U不論進行分離或⑽,為了使 真空或惰性氣體下。 約取出/达入仍保持可保持在 讜第一坩鍋12、該加熱裝置14、該 麵Π、該水冷銅座⑽及 、該吊掛 之該析出室m中,該第___ 艙體ίο 該勝裝置16裝置14上, =:12對應’該吊掛機構17亦設於i密 該析出至101頂端,該水冷銅座 4閉艙體10之 該加料管H14貫穿該密閉艙體1〇/又“亥弟—掛鋼12-側, 利用本裝置製造高純度鎂鎳 該賴取出/送入室1〇5置入臉體1〇之 入-惰性㈣至該酬艙體,===12 ’並通 鎂原料之該第—掛供19… 由°亥吊掛機構17將盛有該 101 ’且置人該加触置二^以生氣體之該分析室 料之該第一_ 12,㈣二熱盛有該鎮原 該密閉艙體之該加料;^ 、料為—域體,再透過貫穿 第-坩鍋12。利m亥加埶裝置二盛有該鎂液體之該 液體之該第一坩銷π,:心14加熱盛有混合該鎳粉及該鎂 鎳粉熔解於該鎮液體產生裝置16進行授拌,使該 加熱溫度於一溫产區n 二〜夜體,控制該加熱裝置14之 合金,最後分離^第°—_^亥鎂錦液體析出—固態鎂鎳儲氫 "B剩餘之該液體及被析出之該固態 8 201000645 艘體in二"先將一鎂原料置入該第二掛銷18送至該密閉 驗體之該分離室103,姻該吊掛機構丨 ^閉 ㈣切第-_ 12吊至倒至該分 :具有可傾斜之功能,使該第一_二== 該第,8,再將該第一_ 12置於至 座刚,該水冷銅座100以冷卻水冷卻 ^銅ΓΪί, - 麟装置 and - the second lion, its square wire will be - pure magnesium raw materials set a = f Γ Γ , , , , , , , , , , , , , , , , , , , , , : : : : : : : : : : : ,: the magnesium raw material is heated by the heating device. Next, a pure nickel powder is slowly added to the Hi-_, and the lion device is continuously applied with mechanical simmering and heating to heat up the _ powder, and the magnesium solution is fully used. A liquid. Compared with the complicated practice of the prior art, the invention has no need to set up a precise on-line inspection _, and precisely adjusts the nickel added by the money into the f τ, and the addition amount accounts for 23, 5 to 5 全部 of all the magnesium ships. .2 can guarantee a composition of =M is a γ phase MgWi storage alloy with a magnesium to nickel atomic ratio of 2: D completely pure, without any other heterogeneous phase. 7 201000645 The first figure is a schematic diagram of the I of the present invention. As shown in the figure, the body 10 is closed, the first steel is U, and the heating-spot is contained - the second - the second steel 18, the hanging mechanism 17, the concrete: the mixing device 16, the ^ 10 = - feeding Tube (10), while the dense cold steel of the present embodiment is precipitated to 101, and a crucible is taken out/delivered, and divided into a brain extraction/delivery chamber 1G3, at least = shirt m and the deposition chamber 1 are respectively provided. Separating or (10), in order to make a vacuum or an inert gas. The extraction/intake is still maintained in the first crucible 12, the heating device 14, the surface crucible, the water-cooled copper seat (10), and the hanging of the suspension In the chamber m, the first ___ compartment ίο the device 16 on the device 14, =: 12 corresponds to 'the hanging mechanism 17 is also disposed at the top of the precipitation to 101, the water-cooled copper seat 4 of the closed body 10 The feeding pipe H14 runs through the closed compartment 1〇/“Haidi-hanging steel 12-side, and the device is used to manufacture high-purity magnesium-nickel. The take-out/feeding chamber 1〇5 is placed into the face 1-inert-inert (4) to the remuneration compartment, ===12 'and the first part of the magnesium raw material-hanging 19... The °H hanging mechanism 17 will hold the 101' and set the contact with the gas to generate gas The analysis room The first _ 12, (four) two heat contains the feed of the closed compartment of the town; ^, the material is - domain, and then through the first - crucible 12. The Lim Haijiao device 2 has The first pin π of the liquid of the magnesium liquid: the core 14 is heated to mix the nickel powder and the magnesium nickel powder is melted in the town liquid generating device 16 for mixing, so that the heating temperature is in a temperature producing area n two to night body, control the alloy of the heating device 14, and finally separate ^ ° - _ ^ Hai magnesium liquid precipitation - solid magnesium nickel hydrogen storage "B remaining liquid and precipitated solid 8 201000645 body In two " first put a magnesium raw material into the second hanging pin 18 to the separation chamber 103 of the closed inspection body, the hanging mechanism is closed (four) cut the first - _ 12 hanging to the point: The function of tilting enables the first _ two == the first, 8, and then the first _ 12 is placed in the seat, the water-cooled copper seat 100 is cooled by cooling water

1 ί於2ϋ ί從該第—職12取出該_鎂鎳儲氫合金。 金有該水冷銅座100,係因該鎂鎳儲氫合 声^化ιΊί1"7溫下空氣中非常容易與氧反應甚至於燃 生危險,因此必須要充分冷卻後才能由真 ;^下之該析出室而内取出。考慮到大量生產時, Γΐ百ΐ斤或輪以上之溶煉’單靠靜置該析出謂内待 所不足,因_制生產效(速)率。所以於該析 内設有具财冷卻循環水之該水冷銅座,銅之良 ===編咖_糧結之該第一增 由上述可知’本㈣提供―難造高純度_儲氫合金之裝置 及,法’可以製造南純度及具有良好吸放肋力學特性之鎮錄 儲氫合金,錢使科貴料之設備,能回收作析丨作用後剩 餘之液體,連續不斷㈣ώ具有良好吸放氫動力學躲及高純 度鎂鎳儲氫合金。 【實施方式】 茲為使貴審查委員對本發明之結構特徵及所達成之功效 有更進一步之瞭解與認識,謹佐以較佳之實施例及配合詳細之 說明,說明如後: 9 201000645 示,之—難實闕之流程示㈣。如圖所 裝置,其震種製造高純度之鎮錄儲氫合金之方法及其 梦詈u、一桃^3—密閉艙體10、一第一坩鍋12、一加熱 ^ sio,弁裝置16及一第二坩鍋18,韌用該裝置執行ί 為-鎂金屬雄,鎮原料置入該第一職12内’其中該鎮原料 點之金屬材料=該第—職12之材f為熔點超過鎮金屬溶 哕錯屌料夕^贫並通入一惰性氣體至該密閉艙體10,將盛有 ί性;二_12送至該密晴體1G内,其中通入該 密閉 u) 密賺體10,讓該 =體1G内後,執行步驟sn,將該第一掛 :i置14 ’利職加熱裝置14加熱該第一掛 :内之雜原料至完全轉,熔解為 熱為一電阻式加熱器,並具有調整加熱溫度=能 驟内之該鎮原料炫解為該魏體後,執行步 r 刚徐徐加人—鎳粉至盛有該鎌體之該 =用職拌裝置16鮮盛有該鎭液體及該鎳 __裝置14加熱盛有顏液體 ϊΐ==Γ12,使該第一_12内之簡液體溫 j升至攝氏761度以上’使該鎳粉完全炫解於該鎖液體中, 產生-混合均⑽麟賴。其巾賴縣置16係包 達(圖中未示)及-可升降之攪拌棒(圖中未示 ; 娜棒進行攪拌,而於該攪拌棒之—端設有_槳狀3=? 以增加擾拌面積及速度。而該_液體之鎳元素量 介於23. 5喊50· 2%之間,即表示加入該鎳粉之份量,如此 可使最後析出之-高純度固態鎂錄儲氫合金之鎭元素與錄元 201000645 素之成分比為2 : 1,並無摻雜有任何其他雜相。 當銻粉全數騎產生該鎮鎳液體後,執行步驟灿,控制該 加ΪΪΪΙ4之溫度於一溫度區間,使該鎂鎳液體之溫度於該 溫度區間中,該溫度區間為該鎂鎳液體形成固相之溫度之上, 與該麟液體形成液相之溫度之下,即介 761度之間,而該麟液體依照鎂 生成析出高純度鎂鎳儲氫合金,該_儲氫合金 純度與析^之溫度完全細。目此本發晴制之設備無須 使用精確叩貴之溫控系統。至於鎮錄儲Α合金之析出數(重、 則視,鎳㈣域以及析出溫度而定。—般而言在符合本㈣ 所述見廣之成份與溫度條件範咖,# 度愈,高純度_儲氫合金的析出量就愈多,-(重可依物理冶金之相圖槓桿定理計算得知。 ㈣tit出之麟儲氫合金之錄含量遠缺原本鎮鎳液 ’隨著析出反應的不斷進行,根據質量不滅定 律:殘留之·體形成富缝體。然:而鎳的密度(8 密度(1.74 g涛因此該固態鎮錄儲氫合金 賴12底部。當該鎂魏體完成或趨近完成 =敍沉於固態鎂錄儲氫合金後’執行步驟si4,分離3 狀織奴驗該第—_12絲之該固態 旦該第一職12内剩餘之該液體倒至該第二掛 _ Μ 將該第—賴12内剩餘之該液體倒至該第二 中,該第,2及該加熱裝置14 又土座上,當s亥基座產生傾倒時,該第一掛鋼12 ;5兮 =熱^^隨該基座傾倒,將剩餘之該液體倒至該第二^ 18 ’而束伽顧驗鎳儲氫合金留在卿—職12底部。 201000645 最後執行步驟SI5,從該加埶奘罢u山 12 ’冷卻盛有該固態鎮錦錢合金; 該加熱裝置Μ中取出談第一题,f储風合金。為了方便從 於該密閉搶體10内,該^掛機構且f設置一吊掛機構17 絞繩Π1固定於該第 ;絞謂,該些 ㈣從該力,裝置14取出。另== 該第-坩鍋12間之連接,該第一掛鍋12二吊掛機, 掛耳(圖中未示),而該吊掛機構17之該^ ° 2,數 別設有一掛勾(圖令未示),使該些絞繩17Γ之,此二分 該第一坩鍋12之該此掛耳,如心政之边二掛勾勾设於 坩鍋12間之連接。 * 0亥吊掛機構17與該第一 新回ί::一/進大=突破則是將原本剩餘之該液趙重 合金裝連續製造高純度鎮錄儲氣 ::構 -繼及該第二_8因二用金’上述該第 同的^連造ί’第二次及之後的製造與第一次的製造所不.1 ί于2ϋ ί Take the _magnesium nickel hydrogen storage alloy from the first job. Gold has the water-cooled copper seat 100, because the magnesium-nickel hydrogen storage sounds ^ ιΊί1"7 temperature is very easy to react with oxygen or even burning danger in the air, so it must be fully cooled before it can be true; Take it out of the room. Considering the large-scale production, the smelting of Γΐ ΐ 或 or the above-mentioned smelting ‘ s relying solely on the standing of the precipitation is insufficient, because of the production efficiency (speed) rate. Therefore, in the analysis, the water-cooled copper seat with the cooling cooling water is provided, and the first increase of the copper is determined by the above-mentioned (four) - difficult to make high purity _ hydrogen storage alloy The device and the method can manufacture the hydrogen storage alloy of the south purity and the mechanical properties of the absorbing and absorbing ribs. The equipment for the precious materials can be recovered as the liquid remaining after the precipitation, and the continuous absorption (4) has good absorption and release. Hydrogen kinetics hides high-purity magnesium-nickel hydrogen storage alloys. [Embodiment] In order to provide a better understanding and understanding of the structural features and the efficacies of the present invention, the preferred embodiment and the detailed description will be described as follows: 9 201000645 - The process of difficult to implement (4). As shown in the figure, the method for producing a high-purity town of hydrogen storage alloy and its dreams u, a peach ^ 3 - closed capsule 10, a first crucible 12, a heating ^ sio, a device 16 And a second crucible 18, toughly use the device to perform ί - magnesium metal male, the raw material of the town is placed in the first job 12 'where the metal material of the town's raw material point = the first - 12 material f is the melting point Exceeding the town, the metal is dissolved in the wrong material, and an inert gas is introduced into the closed chamber 10, which will contain ω; the second -12 is sent to the dense 1G, which is sealed into the closed u) dense After earning the body 10 and letting the body 1G inside, the step sn is performed, and the first hanging: i is set to 14 'the profit heating device 14 heats the first hanging: the inner raw material is completely rotated, and the melting is heat. Resistive heater, and has the adjustment heating temperature = the inner material of the town can be dazzled into the Wei body, the step r is just slowly added - the nickel powder to the body containing the body = the job mixing device 16 The sputum liquid and the nickel __ device 14 are heated to have a liquid ϊΐ == Γ 12, so that the simple liquid temperature j in the first _12 is raised to 761 degrees Celsius or more 'to make the nickel powder completely dazzle The lock in the liquid, resulting in - mixing both ⑽ Lin Lai. Its towel Lai County set 16 series package (not shown) and - lifting rod can be raised and lowered (not shown in the figure; Na stick is stirred, and at the end of the stirring rod is set - paddle 3 =? Increasing the scaffolding area and speed. The amount of nickel in the liquid is between 23.5 and 50%, which means that the amount of the nickel powder is added, so that the final precipitated high-purity solid magnesium can be stored. The composition ratio of the yttrium element of the hydrogen alloy to the recording element 201000645 is 2:1, and there is no other impurity phase. When the sputum powder is fully riding to produce the nickel liquid in the town, the step can be performed to control the temperature of the enthalpy 4 And in a temperature interval, the temperature of the magnesium-nickel liquid is in the temperature range, where the temperature range is above the temperature at which the magnesium-nickel liquid forms a solid phase, and the temperature at which the liquid phase forms a liquid phase, that is, 761 degrees Between the two, the lining liquid precipitates a high-purity magnesium-nickel hydrogen storage alloy according to magnesium, and the purity of the _ hydrogen storage alloy is completely finer than the temperature of the precipitation. Therefore, the apparatus of the present invention does not require the use of an accurate temperature control system. As for the number of precipitation in the town, the storage of the alloy (heavy, then, nickel (four) domain and precipitation temperature In general, in accordance with the provisions of this (four), see the ingredients and temperature conditions of the Fan, #度,, the higher the purity of the hydrogen storage alloy, the more precipitation, - (weight can be based on physical metallurgy phase diagram The calculation of the lever theorem is known. (4) The content of the hydrogen storage alloy of the Tit is not far from the original nickel liquid'. With the continuous precipitation reaction, according to the law of mass incompetence: the residual body forms a rich body. Density (8 density (1.74 g Tao, therefore the solid state of the hydrogen storage alloy lai 12 bottom. When the magnesium Wei body is completed or approaching completion = after sinking in the solid magnesium recording hydrogen storage alloy 'execution step si4, separating 3 woven The liquid of the first to the first job 12 is poured into the second hang _ Μ the liquid remaining in the first lag 12 is poured into the second, the first 2 and the heating device 14 is again on the earth seat, when the s-hai base is dumped, the first hanging steel 12; 5 兮 = heat ^ ^ with the base dump, the remaining liquid is poured to the second ^ 18' and the bunch of gamma test nickel storage hydrogen alloy stay in the bottom of the Qing - 12. 201000645 Finally, the implementation of step SI5, from the crown of the mountain u 1 2 'cooling contains the solid-state Jinjin alloy; the heating device removes the first question, f storage alloy. In order to facilitate the self-locking body 10, the hanging mechanism and f set a hanging mechanism 17 The twisted rope Π 1 is fixed to the first; the skein says that the (four) is taken out from the force, the device 14. The other = the connection of the first squat pot 12, the first hanging pot 12 hangs the hanging ear, Not shown in the figure, and the hook of the hanging mechanism 17 is provided with a hook (not shown), so that the twisted ropes 17 are twisted, and the two of the first crucibles 12 are Hanging ears, such as the side of the heart of the two hooks hooked in the connection of the shabu Shabu. * 0 Hai hanging mechanism 17 and the first new back ί:: one / Jinda = breakthrough is the original remaining liquid Zhaozhong Alloy Pack continuously manufactures high-purity Zhenshen gas storage::Construction- and subsequent the second_8 due to the second-use gold 'the above-mentioned second joint manufacturing ί' second and subsequent manufacturing and the first time Manufacturing is not.

儲氳合金114之產率,添加鎳粉ϋ H 50, .r〇i 5,6 wt: .5 it無摻雜有任何其他之雜相。因為剩餘 體為接近共日日組成(鎂含量% 5 t%)兮 好的成份輕劑,使得在無須精_ ;=分$為^ 夠使該賴㈣之雜永遠鱗在齡量為23. 5U二 201000645 的範圍。’ 鉍上所述,本發明係實為一具有新穎性、進步性及 應符合細專利法所規定之專利申請要件無疑,、 惟以上=二:早較; Y之顏,舉顺树===== 本發之均恤絲飾,均應包括於 【圖式簡單說明】 第一圖:本發明之裝置示意圖; 第二圖:本發明之流程示意圖。 【元件符號說明】 10 密閉艙體 100 水冷銅座 101 析出室 102 隔離閥 103 对鍋取出/送入室 104 加料管 12 第一时鋼 14 加熱裝置 16 攪拌裝置 165 槳狀葉片 17 吊掛機構 171 絞繩 18 第二坩鍋The yield of the storage alloy 114 was added with nickel powder H 50, .r〇i 5,6 wt: .5 it undoped with any other impurity phase. Because the remaining body is a light component close to the composition of the total day (magnesium content 5 t%), so that the _ _ = = $ is ^ enough to make the ( (4) of the eternal scale at the age of 23. 5U two 201000645 range. As stated above, the present invention is a novel, progressive and patent application requirement that should be in accordance with the fine patent law, but the above = two: early comparison; Y, Yan Shunshu == === The hairline of this hairdressing should be included in the simple description of the drawing. The first drawing: schematic view of the device of the present invention; the second drawing: the schematic flow chart of the present invention. [Description of Component Symbols] 10 Closed Cabin 100 Water-Cooled Copper Block 101 Precipitation Chamber 102 Isolation Valve 103 Dispensing/Feeding Room 104 Feeding Pipe 12 First Steel 14 Heating Device 16 Stirring Device 165 Paddle Blade 17 Hanging Mechanism 171 Winding Rope 18 second shabu-shabu

Claims (1)

201000645 十、申請專利範圍: 1. 一種製造高純度鎂鎳儲氫合金之方法,其包括: 於一惰性氣體下,加熱一鎂原料’並熔解該鎂原料為一鎂液體; 加入一鎳粉至該鎂液體中,並攪拌及加熱混有該鎳粉之該鎂液 體,以熔解該鎳粉於該鎂液體中; 待該鎳粉熔解於該鎂液體後,產生一鎂鎳液體; 控制該饍錄液體之溫度於一溫度區間,該鎂鎳液體析出一固態 鎂鎳儲氫合金;以及 &201000645 X. Patent application scope: 1. A method for manufacturing a high-purity magnesium-nickel hydrogen storage alloy, comprising: heating a magnesium raw material under an inert gas and melting the magnesium raw material into a magnesium liquid; adding a nickel powder to In the magnesium liquid, the magnesium liquid mixed with the nickel powder is stirred and heated to melt the nickel powder in the magnesium liquid; after the nickel powder is melted in the magnesium liquid, a magnesium nickel liquid is produced; Recording the temperature of the liquid in a temperature range, the magnesium nickel liquid is precipitated as a solid magnesium nickel hydrogen storage alloy; and & 分離剩餘之該液體及被析出之該固態鎂鎳儲氫合金,以得到該 固_鎮錄儲氮合金。 2. 如申請專娜圍第1項之方法,其巾分離剩餘之驗體及被析 出之該固態鎂鎳儲氫合金之步驟更包含冷卻該固態鎂鎳儲氫合 金。 ^ 3. 如申請專·圍第1項之方法,其巾該__儲氫合金帽 元素與鎳元素之成份比為2 : 1。 4. 如申请專利範圍第1項之方法,更包含: 加熱被分離出之剩餘之該液體,重覆加入該鎂原料 態鎂鎳儲氫合金之步驟,以連續得到該固態鎂鎳 5. 如申請專利範圍第丨項之方法,其中該顯料係—鎂:屬 6. 如申請專利範圍第丨項之方法,其找鎂鎳液體之鋅 量百分比介於23. 5%至50. 2%之間。 軌素之窒 "507 ^ 8. 如申請專利細第〗項之方法,其巾剩餘之該 9. -種製造高純度賴儲氫合金之裝置,其包含:^鎂液體。 一^割為-析出室及-義取出/送人室之 一第—坩鍋,設於該密閉艙體内; 腸遛, 14 201000545 加^裝置’設於該第一堆鋼; 及,,裝置,設於該密閉艙體内,位於該第一坩鍋上;以 側了第二坩鍋,設於該密閉艙體内’位於該第一坩鍋之一 10, it利範圍第9項之裝置,其中該第一賴及該第二堆 *之材質為熔點超過鎂之金屬材質。 m專利範圍第9項之裝置,其中製造高純度鎂錄儲氫合 艙雜允入—鎂原料至該第—職’通人—雜氣體至該密閉 哕該加熱裝置加熱盛有該鎂原料之該第一職,溶解 二二;―鎮液體’再加人―鎳粉至盛有該織體之該第 之彳】用該加熱裝置加熱盛有混合該鎳粉及該鎂液體 於,並利用該攪拌裝置進行攪拌’使該鎳粉熔解 声F 生—賴紐,控獅加餘置之加熱溫度於 八該_液體析出—固態鎂鎳儲氫合金,最後 =之該液體及被析_ _錦儲 H i鋼内剩餘之該紐倒至該第二_,並 ;= 内之該固態鎂鎳儲氫合金,待冷卻後,從該 i. 弟一掛練出該固態鎂鎳儲氫合金。 ^傻㈣ 12.如二請二,圍第11項之襄置,其中冷卻該第-坩鍋内之 顯儲氫合金’係由該加熱裝置取出該第待 π 從該第:_取出該_鎂鎳儲氫合金。 .體之;第利t第11項之裝置’更包含將盛有剩餘之該液 =解為二於:加熱输加入-鎂原料進行: 溶解為_鎂液體,再加人—鎳粉,湘該加 加熱,且利用該麟裝置進 二褒置進仃 制該加鄉罟命縣產生一鎮鎳液體,然後控 .f ^口熱裝置之加熱溫度於_溫度區間内, 一固祕齡金’錢分_第二賴_餘之 201000645 及被析出之該固態鎂鎳儲氫合金, 液體倒至該第一坩鍋,並冷卻該二弟一坩鍋内剩餘之該 氫合金,待冷卻後,從該第二掛錢^ ^内之該固態鎂錄儲 14·如申請專利範圍第U項之裝置,政〜固也鎂鎳儲氫合金。 性氣體前,係先利用該惰賴體將該^入該惰 15. 如申糊_ Η㈣置,其 性氣體後’係封閉該密閉艙體。T 4閉驗體通入該惰 16. =專利範圍第9項之裝置,其中該加熱裝置為-電阻式The remaining liquid and the solid magnesium-nickel hydrogen storage alloy which is precipitated are separated to obtain the solid-state nitrogen storage alloy. 2. If the method of claim 1 is applied, the step of separating the remaining test body and the precipitated solid magnesium-nickel hydrogen storage alloy further comprises cooling the solid magnesium-nickel hydrogen storage alloy. ^ 3. If you apply for the method of item 1, the ratio of the element of the __ hydrogen storage alloy cap to the nickel element is 2:1. 4. The method of claim 1, further comprising: heating the remaining liquid to be separated, and repeatedly adding the magnesium raw material magnesium-nickel hydrogen storage alloy to continuously obtain the solid magnesium nickel. 5%至50. 2%。 The percentage of the amount of zinc in the magnesium-nickel liquid is between 23.5% and 50. 2%, the method of the invention is the method of the invention. between.轨 窒 窒 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 One cut-to-precipitation chamber and one of the right-out-out/sending room--the crucible is set in the closed compartment; the intestinal fistula, 14 201000545 plus the device 'located in the first stack of steel; and, The device is disposed in the sealed cabin and is located on the first crucible; the second crucible is disposed on the side, and is disposed in the closed cabin, and is located in one of the first crucibles 10, The device, wherein the first material of the second stack* is made of a metal having a melting point exceeding that of magnesium. The device of item 9 of the patent scope, wherein the high-purity magnesium recording and storage hydrogen storage tank is mixed with the magnesium raw material to the first duty-passing human-gas to the sealed crucible, and the heating device is heated to hold the magnesium raw material. The first job, dissolving the second two; "the town liquid" plus the "nickel powder to the first layer of the texture" is heated by the heating device to mix the nickel powder and the magnesium liquid, and utilize The stirring device is stirred to make the nickel powder melt the sound F-Lai, the temperature of the control lion plus the remaining temperature is eight. The liquid precipitation - the solid magnesium nickel hydrogen storage alloy, and finally the liquid and the analysis _ _ The remaining one of the Jinhe H i steel is poured into the second _, and; = the solid magnesium-nickel hydrogen storage alloy inside, and after cooling, the solid magnesium-nickel hydrogen storage alloy is hung from the i. . ^傻傻(四) 12. If the second is the second, the eleventh item is placed, wherein the cooling hydrogen storage alloy in the first crucible is removed by the heating device. Magnesium nickel hydrogen storage alloy. The device of the eleventh item of the first item of 'lith t' contains the solution of the remaining liquid = two: heating and adding - magnesium raw material: dissolved into _ magnesium liquid, plus human-nickel powder, Xiang The heating is applied, and the nickel device is used to generate a nickel liquid in the township of the county, and then the heating temperature of the heat device is controlled within the temperature range. '钱分_Second _ _ 201000645 and the solid magnesium-nickel hydrogen storage alloy which is precipitated, the liquid is poured into the first crucible, and the hydrogen alloy remaining in the second dick is cooled, after cooling From the second hanging money ^ ^ the solid magnesium record storage 14 · as claimed in the scope of the U section of the device, the government ~ solid also magnesium nickel hydrogen storage alloy. Before the gas is used, the inertia is first used to set the inertia, such as the paste _ Η (4), and the gas is closed to close the closed capsule. The T 4 closed body is introduced into the idler 16. The device of claim 9 wherein the heating device is a resistive type 17.如申請專利範圍第9項之方法,更包含: 坩 加料管,穿設於該密閉餘體内,以加入 鍋及該第二坩鍋- 何讨至δ亥第一 18.如申請專利範圍第9項之裝置,其中之該析出室、兮 :该坩鍋取出/送入室之間設有至少一隔離閥,使得:: =取出/送人該_時,使析出室仍保持在真空或惰性^ 19. 如申請專觀_ u項之裝置,更包含—基座,該基座設 於該加熱裝置及該第—掛鋼之底部,並傾斜該第—掛鋼及該 加熱裝置’使該第一坩鍋將剩餘之該液體倒至該第二坩銷。 20. 如^請專利範圍f π項之裝置,更設有一吊掛機構,設於 _閉艙體内’以職第-細或該第二购(吊出/吊入該 加熱裝置。 ° 21. 士:申請專利範圍第2G項之裝置,其中該吊掛機構包含複數 絞,,該些絞繩之一端固定於該第一坩鍋或第二坩鍋,並使 該第一坩鍋或該第二坩鍋一端傾斜。 22. 如申請專利範圍第21項之裝置,其中該第一坩鍋及第二坩 鍋之開口周圍更分別設有複數掛耳,與該吊掛機構之該些絞 16 201000645 詞^紫'肩I兮rt罢_ 今此而該吊掛機構之該些絞繩分別設有一掛勾,使 該麵耳,使__之—_定於該第一 % 範圍第9項之裝置,其中該麟裝置包含一馬達 24如申#H ’達帶_攪拌棒進行職。 -槳'^葉23項之裝置,其中該攪拌棒之一端設有 H第U項之裝置,其中該密閉擒體更包含一 :金之;之水冷銅座’以冷卻盛有該固態鎂鎳儲氫 第11項之裝置’其中分離該第—_内剩 ^傾倒至鱗二购中前,該第二賴内可先添加 琢鎂原料。 概㈣26項H更包讀盛捕餘之鎌 伽二第—賴設_加熱^並加人—鎳粉進行加執,並 二襞置進行攪拌產生一鎂鎳液體,然後控制該加熱 溫_^,該鎂錦液體析出一固態鎮 離該第二掛銷内剩餘之該液體及被析出 节第=金’_第二__餘之該液體倒至 =第二购内之朗態_儲氯合金, 待4後,仗该第二掛銷取出該固態鎮錄儲氣合金。 1717. The method of claim 9, further comprising: a feeding tube disposed in the sealed body to be added to the pot and the second crucible - The device of claim 9, wherein the precipitation chamber and the crucible are provided with at least one isolation valve between the crucible removal/feeding chamber, so that:: = the removal/sending of the _, the precipitation chamber is still maintained Vacuum or inertia ^ 19. If the apparatus for applying the special item _ u further includes a base, the base is disposed at the bottom of the heating device and the first hanging steel, and tilts the first steel and the heating device 'Let the first crucible pour the remaining liquid to the second dowel. 20. If the device of the patent range f π is requested, there is also a hanging mechanism, which is located in the _ closed compartment, or the second purchase (lifting/lifting the heating device. ° 21 The device of claim 2G, wherein the hanging mechanism comprises a plurality of twists, and one of the twisted ropes is fixed to the first crucible or the second crucible, and the first crucible or the The second crucible is inclined at one end. 22. The apparatus of claim 21, wherein the first crucible and the second crucible are respectively provided with a plurality of mounting ears, and the windings of the hanging mechanism 16 201000645 The word ^紫' shoulder I兮rt _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ The device of the item, wherein the device comprises a motor 24 such as a #H '达带_搅拌棒. - a device of 23 blades of a paddle, wherein one end of the stirring bar is provided with a device of the Hth item, Wherein the sealed body further comprises: a gold-cooled copper seat to cool the device containing the solid magnesium-nickel hydrogen storage item 11 _Inside the remaining ^ before dumping to the second purchase, the second Lai can first add bismuth magnesium raw materials. (4) 26 items H more packaged to capture the remaining 镰 二 二 — 赖 赖 加热 _ heating ^ and add people - nickel The powder is added, and the second set is stirred to produce a magnesium-nickel liquid, and then the heating temperature is controlled, and the magnesium liquid liquid is precipitated in a solid state to leave the liquid remaining in the second hanging pin and to be precipitated. The liquid '_the second__the liquid is poured to the second state of the purchase _ storage of chlorine alloy, after 4, the second hanging pin to take out the solid state record gas storage alloy.
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* Cited by examiner, † Cited by third party
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