CN1397658A - Non-crystal rare-earht-Mg based hydrogen bearing alloy and its preparing process - Google Patents
Non-crystal rare-earht-Mg based hydrogen bearing alloy and its preparing process Download PDFInfo
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Abstract
一种非晶态稀土－镁基储氢合金及其制造方法，其特征是将预先设定的稀土－镁基合金成分通过熔炼制成晶态合金，该晶态合金在室温下粉碎成粉料，再将粉料与芳香族有机溶剂一起球磨形成非晶态合金，除去溶剂后即获得固体非晶态稀土－镁基储氢合金。该储氢合金的化学式为Re2－xMxMg17－yNy，式中，0≤x≤1；0≤y≤4；Re为稀土金属La、Ce、Pr、Nd、Sm、富铈混合稀土金属Mm、富镧混合稀土金属Ml中的一种；M为金属Ca、Ti、V、Zr中的一种；N为金属Ni、Co、Fe、Mn、Cu中的一种。同现有技术比较，本储氢合金的突出优点是：能在室温下吸收大量氢，用于制作氢燃料箱或储氢器具有结构简单、使用方便、能耗省、成本低的特点，特别适合于在氢燃料电池或燃氢发动机动力系统上应用。An amorphous rare earth-magnesium-based hydrogen storage alloy and its manufacturing method, which is characterized in that the preset rare earth-magnesium-based alloy components are smelted into a crystalline alloy, and the crystalline alloy is pulverized into powder at room temperature , and then ball mill the powder with an aromatic organic solvent to form an amorphous alloy, and obtain a solid amorphous rare earth-magnesium-based hydrogen storage alloy after removing the solvent. The chemical formula of the hydrogen storage alloy is Re 2－x M x Mg 17－y N y , where 0≤x≤1; 0≤y≤4; Re is the rare earth metal La, Ce, Pr, Nd, Sm, rich One of cerium mixed rare earth metal Mm and lanthanum rich mixed rare earth metal Ml; M is one of metals Ca, Ti, V, Zr; N is one of metals Ni, Co, Fe, Mn, Cu. Compared with the existing technology, the outstanding advantages of this hydrogen storage alloy are: it can absorb a large amount of hydrogen at room temperature, and it has the characteristics of simple structure, convenient use, low energy consumption and low cost when used to make hydrogen fuel tanks or hydrogen storage devices, especially It is suitable for application on hydrogen fuel cells or hydrogen-burning engine power systems.
Description
Technical field
The present invention relates to a kind ofly be main component with magnesium and be the Magnuminium of submember that the Asia relates to the structure that changes this alloy with cold process with the rare earth metal.
Background technology
Hydrogen Energy is reproducible desirable clear energy sources.At present, progressively applying such as fields such as vapour Trucks, power-assist Trucks, motor Trucks, mobile phone, communication, computer, pick up camera, power tool and military equipments with the fuel cell that hydrogen acts as a fuel, its hydrogen source is provided together that is storage, the transportation problem of hydrogen have become the task of top priority.Hydrogen storage material is safer and economical than technology such as present high pressure vessel, liquid hydrogen and methyl alcohol as Hydrogen Energy storage transmission carrier, is considered to hydrogen fuel cell and hydrogen engine one of fuel tank candidate material.So far, mainly be the hydrogen storage alloy that a class at room temperature can reversible hydrogen adsorption and desorption in the hydrogen storage material of practical application, as AB
5Rare earth system and the AB type and the AB of type
2The titanium alloy of type., the weight hydrogen-storage density of this class alloy is lower, only is 1.4～1.6% as the weight hydrogen-storage density of lanthanon hydrogen storage alloy, and the weight hydrogen-storage density of titanium base hydrogen storage alloy is 1.6～2.0%.Another kind of heavy body (higher 2～4 times than rare earth system and titanium alloy) hydrogen storage material is pure magnesium and Magnuminium, and wherein the maximum weight hydrogen-storage density of pure magnesium can reach 7.6%, but pure magnesium needs could inhale hydrogen usually under 320～400 ℃ of high temperature and 6.0MPa hydrogen pressure.In Magnuminium, hydrogen uptake condition demulcent the most is Mg
2The Ni alloy, under 200 ℃ and 1.4MPa can with H-H reaction, but its maximum storage hydrogen quantity only is 3.6%, no more than half of pure magnesium hydrogen-storage amount.Also have a class Magnuminium, they form intermetallic compound by rare earth element and magnesium, and typical composition has LnMg
12(Ln be among La, Ce, the Mm a kind of), Ln
2Mg
17(Ln is La or Ce) and Ce
5Mg
41The hydrogen-storage amount of this class Magnuminium is between pure magnesium and Mg
2Between the Ni, the weight hydrogen-storage density under 325 ℃ and 3.0MPa is 4.0～6.0%.All conventional preparations and the pure magnesium of handling without any modification and Magnuminium all are not inhale hydrogen or hydrogen is few at normal temperatures.
For the suction hydrogen discharging temperature that reduces pure magnesium and Magnuminium and improve its dynamic performance, various improvement technology have been proposed, wherein modal improvement project is an alloying, for example, to Mg
2The Ni alloy has been studied with Cr, Y, Zn, Ti, Mn, Al, Cu, Co, the various units of Fe and has usually partly been substituted Mg
2Ni among the Ni or Mg form ternary or multicomponent alloy, and the result is that hydrogen-storage amount reduces a lot, reduces seldom and inhale hydrogen discharging temperature; Another kind of improvement technology is in alloying, pure magnesium or Magnuminium is prepared into tiny nanocrystalline, provides a kind of mechanical alloying method to prepare ternary Mg as document [1]
1.9Ti
0.1Ni (Mg
2The Ni type) nanometer crystal alloy can and be inhaled hydrogen 3.2% in activation under 200 ℃ the lesser temps in 150 ℃ of next hours; Document [2-4] has proposed pure magnesium-graphite, pure magnesium-palladium blending aromatic organic solvent ball milling respectively and has prepared the nanocrystalline method of Mg, and the best result that these preparation methods obtain is to have 90% pure magnesium to be converted into hydride through 20 hours suction hydrogen process under 180 ℃ and the 6～7KPa hydrogen pressure; The another kind of complex-phase nano crystal alloy that document [5] provides is Mg-50wt%ZrFe
1.4Cr
0.6, this alloy is synthetic by the mechanical alloying method, and its weight hydrogen-storage density under 160～200 ℃ of temperature is 3.4%.But above-mentioned alloying or make the effect that nanocrystalline various improvement technology all fail to obtain to absorb under the room temperature a large amount of hydrogen.In addition, document [6] has been reported a kind of agglomerating multiphase alloy Mg-40wt%FeTi (Mn), this multiphase alloy by the pure magnesium of high temperature modification with normal temperature type FeTi (Mn) sintering, thereafter carry out pre-treatment under 400 ℃ of nitrogen atmosphere, so the multiphase alloy weight hydrogen-storage density at room temperature of preparation can reach 3.5%.Document [7] has reported that the Magnuminium that can inhale hydrogen under a kind of room temperature is MgH
2-5wt%V, this alloy adopt the preparation of mechanical ball milling method, and allow pure Mg suction hydrogen become MgH earlier
2, and then synthetic with pure vanadium ball milling, the hydrogen under its room temperature is weight 2.0wt%, although this alloy can at room temperature be inhaled hydrogen, its hydrogen only be pure magnesium when high temperature saturated hydrogen 26%.Being prepared into non-crystalline state also is to reduce to inhale the hydrogen temperature and improve the effective ways of inhaling hydrogen speed.Document [8] provides a kind of with Mg
2The Ni alloy mixes with 70wt%Ni and carries out ball milling and obtain a kind of amorphous Mg
2The Ni-Ni matrix material finds that its suction hydrogen speed is than as cast condition Mg
2The nanocrystalline M g of Ni alloy and ball milling
2The Ni alloy is much higher, can absorb the hydrogen of 2.4wt% under 30 ℃ and 3.0MPa hydrogen pressure, in this amorphous composite owing to added the Ni that do not inhale hydrogen in a large number, so the weight hydrogen-storage density reduces a lot.
Summary of the invention
The object of the present invention is to provide under a kind of room temperature and can absorb hydrogen storage alloy of a large amount of hydrogen and preparation method thereof.Hydrogen storage alloy of the present invention is a kind of amorphous binary or multielement rare earth-Magnuminium, the high advantage of hydrogen-storage amount that it had both kept the rare-earth and Mg base alloy of former crystalline structure to be had, having overcome former crystal alloy again must be in activation more than 300 ℃ and the shortcoming of inhaling hydrogen, owing at room temperature also can absorb a large amount of hydrogen, inhaling the hydrogen operation can carry out at ambient temperature, needn't be especially to the alloy heat temperature raising, therefore, the fuel tank or the storage hydrogen device that use this alloy to make are simple in structure, easy to operate, the saving energy, cost is low, is particularly suitable for using on hydrogen fuel cell or combustion hydrogen engine.
A kind of non-crystal rare-earht-Mg based hydrogen bearing alloy is characterized in that: the chemical formula of this hydrogen storage alloy is Re
2-xM
xMg
17-yN
y, in the formula, 0≤x≤1; 0≤y≤4; Re is a kind of among rare-earth metal La, Ce, Pr, Nd, Sm, cerium-rich mischmetal metal M m, the lanthanum rich norium Ml; M is a kind of among metal Ca, Ti, V, the Zr; N is a kind of among metal Ni, Co, Fe, Mn, the Cu.
A kind of manufacture method of non-crystal rare-earht-Mg hydrogen storage alloy, it is characterized in that: predefined rare-earth and Mg base alloying constituent is made crystal alloy by melting, crystal alloy at room temperature is ground into less than 200 powder materials, place the ball mill ball milling to form non-crystal rare-earht-Mg based alloy with the aromatic organic compounds solvent powder again, promptly obtain solid amorphous attitude rare-earth and Mg base hydrogen bearing alloy except that after desolvating; Solvent is selected one or several in tetrahydrofuran (THF), naphthane, naphthalene, toluene, benzene, ethylbenzene, tetrahydrobenzene, hexanaphthene, methylcyclohexane, the En, perylene for use.
Alloy of the present invention is equivalent to La before decrystallized
2Mg
17(2:17 type) phase structure.Be that a class is inhaled protium to rare earth element Re part alternate M element in the chemical general formula, they are all light than Re, and it is favourable to improving the weight hydrogen-storage density therefore to substitute the back; Be a class transition metal to Mg part alternate N element in the chemical formula, they substitute that to be decomposed into the reaction of hydrogen atom highly beneficial to improving alloy surface catalysis hydrogen molecule.
The preparation method of amorphous alloy of the present invention is characterized in that being prepared into crystal alloy by the chemical general formula composition of setting by the method for founding earlier, carries out ball milling until changing non-crystalline state in ball mill with the aromatic organic compounds solvent then.Just a kind of mechanical mill process of mechanical milling process, it is crucial to the non-crystalline state that the rare-earth and Mg base alloy is converted into tiny high-specific surface area; And the existence of aromatic organic compounds solvent also is very important, and at first, the existence of organic compound has protected the alloy particle surface to avoid or few oxidated, thereby has guaranteed the active surface chemical state that alloy is fresh; Secondly, the existence of solution of organic compound has changed transmission ofenergy and the distribution in the process of lapping system, thereby makes alloying pellet can obtain tiny amorphous rather than nanocrystalline in the shorter time; At last, electronic migration has taken place in the alloying element of organic compound and rare-earth and Mg base alloy surface in mechanical milling process, and has therefore formed many new complex catalysis active centre at alloy surface.Alloy of the present invention is a kind of rare-earth and Mg base binary or multicomponent alloy; And selected organic compound solvent be a class can and this class alloy produce and move between electronics, thereby can on these alloy surfaces, form the strong solvent in complex catalysis active centre, solvent is selected one or several in tetrahydrofuran (THF), naphthane, naphthalene, toluene, benzene, ethylbenzene, tetrahydrobenzene, hexanaphthene, methylcyclohexane, the En, perylene for use.If alloy is to select pure magnesium or MgH for use
2+ Ni, then the grinding of carrying out under the organic solvent dipping owing to magnesium can only obtain the nanocrystalline amorphous that is difficult to obtain; If that select for use is Mg
2Ni or Mg+Ni alloy can obtain Mg though then grind the back
2The Ni amorphous, but, therefore can not in the grinding under the organic compound dipping, produce more complex catalysis active centre because of this alloy does not contain rare earth metal and some other useful elements, then can not get a large amount of effects of inhaling hydrogen under the room temperature, and because Mg
2The maximum hydrogen of Ni only is 3.6%, and unit weight hydrogen-storage density itself is just on the low side.Weight hydrogen-storage density under the room temperature of the then decrystallized back of alloy of the present invention high more person of the weight hydrogen-storage density of original crystal alloy when high temperature before decrystallized is also high more; The complex catalysis active centre that employed organic compound solvent can form during its preparation amorphous is many more, then the at room temperature absorbent hydrogen of amorphous of this solvent preparation is many more, the big more then grinding of the specific inductivity of fragrant aromatics organic compound back non-crystaline amorphous metal surface complex catalytic center is also just many more, tetrahydrofuran (THF) for example, naphthane, naphthalene, toluene, benzene, the specific inductivity of ethylbenzene and hexanaphthene is respectively 7.8,2.7,2.5,2.4,2.3,2.3 with 2.1, the action effect of these aromatic organic compounds is tetrahydrofuran (THF)＞naphthane＞naphthalene＞toluene＞benzene＞ethylbenzene＞hexanaphthene in proper order.Non-crystal rare-earht-Mg based hydrogen bearing alloy of the present invention is the hydrogen storage alloy that can absorb a large amount of hydrogen under the class room temperature, and its hydrogen under 25 ℃, 3.0MPa hydrogen pressure reaches 3.8～4.2%, and this value is (AB for the normal temperature type rare earth
5) the hydrogen storage alloy hydrogen～3 times, be titanium system (AB and AB
2) 2～3 times of hydrogen storage alloy hydrogen, and general Magnuminium is not inhale hydrogen under the normal temperature condition.
Compared with the prior art, alloy of the present invention has following outstanding advantage: the hydrogen storage alloy of (1) and normal temperature type (can inhale hydrogen under the room temperature) compares, and hydrogen storage alloy of the present invention at room temperature hydrogen will exceed 2～3 times; (2) compare with conventional magnesium of making or Magnuminium, this hydrogen storage alloy can at room temperature be inhaled hydrogen, and the former need inhale hydrogen under 200～400 ℃ high temperature, therefore simple in structure with the fuel tank or the storage hydrogen device of the making of this hydrogen storage alloy, operate also more convenient, the saving energy, cost is low; (3) with previous Mg-graphite, Mg-palladium, the Mg-50wt%ZrFe that releases
1.4Cr
0.6, Mg-40wt%FeTi (Mn) and MgH
2The nanocrystalline comparison of magnesium such as-50wt%V and other element or alloy preparation, the hydrogen of amorphous rare-earth and Mg base alloy of the present invention when room temperature is more, and preparation process is then simpler; (4) and Mg
2The composite amorphous alloy ratio of Ni-70wt%Ni; Amorphous rare-earth and Mg base alloy of the present invention not only room temperature hydrogen exceeds a lot, and does not have material (and the Mg that can not inhale hydrogen in the alloy
2Among the Ni-70wt%Ni, the Ni that does not inhale hydrogen occupied gross weight 70%), fuel tank of making or the storage hydrogen amount of thinking highly of are lighter, volume is littler, efficient is higher.
Embodiment
Embodiment 1:
A kind of non-crystal rare-earht-Mg hydrogen storage alloy, its chemical general formula are Re
2-xM
xMg
17-yN
y, make that Re is La in the formula, x=0, y=1, N are Ni, then constituting chemical formula is La
2Mg
16The Ni ternary alloy by the weight proportion of this chemical formula calculating La, Mg and Ni, is smelted in the crucible oven of vacuum induction furnace that argon shield is arranged or slag making protection, and the back casting ingot-forming finishes.In the starting material, La is the lanthanoid metal of purity 〉=98% (weight percentage, together following), and Mg is the MAGNESIUM METAL of purity 〉=99%, and Ni is the electrolytic nickel of purity 〉=99.9%; Alloy pig is broken for fine powder in air, powder particle size is not more than 200 orders, with this fine powder ball grinder of packing into, put into the chemical pure tetrahydrofuran solvent of the inferior adding of abrading-ball by 30: 1 ratio of grinding media to material, till submergence alloy powder and abrading-ball, carry out ball milling then, the ball mill speed of mainshaft is 225 rev/mins, and be 60 minutes each running period, running in wherein preceding 50 minutes, back stall in 10 minutes, preventing that continuous operation from causing the alloy powder temperature too high, behind 20 hours interrupted ball millings, alloy changes tiny amorphous into, material behind the ball milling is vacuumized, promptly obtain non-crystalline state La behind the removal tetrahydrofuran (THF)
2Mg
16The Ni hydrogen storage alloy.This hydrogen storage alloy can be inhaled hydrogen under room temperature and 3.0MPa hydrogen pressure, the hydrogen actual measurement is 4.0% in 2 hours.
Embodiment 2:
Chemical formula is La in the preferred alloy of the present invention
1.8Ca
0.2Mg
16Ni (be that Re is La in the general formula, x=0.2, M are Ca, and y=1, N are Ni) is by the weight proportion of this chemical formula calculating La, Ca, Mg, Ni, and Ca is purity 〉=99% in the starting material, and is surplus with embodiment 1.The crystal alloy solvent is with embodiment 1.Milling parameters comprises that alloy granularity, ratio of grinding media to material, organic solvent, rotating speed, running period are all with embodiment 1.La
1.8Ca
0.2Mg
16The Ni crystal alloy changes tiny amorphous into behind 15 hours interrupted ball millings.Material behind the ball milling is vacuumized, promptly obtain non-crystalline state La behind the removal tetrahydrofuran (THF)
1.8Ca
0.2Mg
16The Ni alloy, its actual measurement of the hydrogen in 2 hours under room temperature and 3.0MPa hydrogen pressure is 4.2%.
Document [1]: J.Alloys and Compounds, 1999, Vol.282, pp286-290
Document [2]: J.Alloys and Compounds, 1996, Vol.232, pp218-223
Document [3]: J.Alloys and Compounds, 1997, Vol.253-254, pp34-37
Document [4]: J.Alloys and Compounds, 1999, Vol.293-295, pp564-568
Document [5]: J.Alloys and Compounds, 2000, Vol.297, pp240-243
Document [6]: J.Alloys and Compounds, 1992, Vol.184, pp1-9
Document [7]: J.Alloys and Compounds, 2000, Vol.305, pp239-245
Document [8]: J.Alloys and Compounds, 1999, Vol.285, pp246-249
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