CN101457321A - Magnesium base composite hydrogen storage material and preparation method - Google Patents

Magnesium base composite hydrogen storage material and preparation method Download PDF

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Publication number
CN101457321A
CN101457321A CNA2008101641159A CN200810164115A CN101457321A CN 101457321 A CN101457321 A CN 101457321A CN A2008101641159 A CNA2008101641159 A CN A2008101641159A CN 200810164115 A CN200810164115 A CN 200810164115A CN 101457321 A CN101457321 A CN 101457321A
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hydrogen
storage material
hydrogen storage
based composite
composite hydrogen
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CN101457321B (en
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王秀丽
涂江平
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention discloses a magnesium-based composite hydrogen storage material comprising the following compositions by weight percent: 1.0-10.0% of Al, 1.0-5.0% of Ni, and the balance of Mg. A preparation method thereof comprising the following steps: at first, smelting block-shaped metal Mg and Al by a medium frequency induction to prepare Mg17Al12 alloy which is crushed to 300 meshes; hydrogenising Mg powder at 340 DEG C under a hydrogen atmosphere of 4.0MPa to prepare MgH2; then blending Mg17Al12, MgH2, Ni powder in accordance with contents by weight percent for ball-grinding for 60 to 100 hours under an atmosphere of argon. The magnesium-based composite hydrogen storage material can reversely absorb and release hydrogen at low temperature, and has high hydrogen storage capacity, excellent activation performance and superior hydrogen absorbing and releasing kinetics property. The magnesium-based composite hydrogen storage material can be used for manufacturing hydrogen source to facilitate purification and storage and transportation of hydrogen, and can also used for hydrogen storage material for fuel cells.

Description

A kind of Mg-based composite hydrogen storage material and preparation method
Technical field
The present invention relates to a kind of light low temp reversible hydrogen storage material, particularly relate to a kind of Mg-based composite hydrogen storage material and preparation method thereof.
Background technology
Along with the minimizing day by day of petroleum resources, problem of environmental pollution is severe day by day, and Hydrogen Energy is because advantages such as its aboundresources, non-environmental-pollution become the ideal secondary energy.The major technique link that constitutes the Hydrogen Energy system comprises production, supply, storage, conversion and the use etc. of hydrogen, and wherein the storage of energy and conversion are the keys of energy effective utilization always.With the metal hydride storage of hydrogen is a kind of safety and the method that very high specific volume storage volume is arranged, and has irreplaceable effect in the secondary energy field, particularly in fuel cell, rechargeable cell research, has critical role.USDOE is defined as 6-7wt.% to the battery car that acts as a fuel with the hydrogen storage capability of hydrogen source.In various hydrogen storage materials, magnesium-base hydrogen storage material is big owing to its hydrogen-storage amount, light weight, cheap being subjected to are paid close attention to widely.The theoretical hydrogen-storage amount of Mg reaches 7.6wt.%, is the highest in all hydrogen storage alloys.Yet pure magnesium is poor as the dynamic performance that hydrogen storage material charges and discharge hydrogen, and hydrogen discharging temperature is than higher, if reach the acceptable hydrogen discharging speed, hydrogen discharging temperature must limit the practical application of Mg hydride more than 350 ℃.The intermetallic compound that generates Mg has effectively reduced inhales the temperature of putting hydrogen, however also obviously decline of hydrogen-storage amount, as the Mg of better performances 2Ni alloy theory hydrogen-storage amount has only 3.6wt.%.Thereby the Mg-base hydrogen-bearing matrix material is the emphasis of Recent study.With Mg compound compound Recent study more be to inhale the AB put hydrogen in room temperature 5Type rare earth-based alloy, yet LaNi 5After storing up for the first time the hydrogen circulation, decompose, generate irreversible LaH 3And Mg 2The hydride of Ni.Al is originally as light metal, in order to improve the unit mass hydrogen-storage amount, the compound also existing report of Al and Mg.Magnalium is that alloy has Mg 3Al 12, Mg 17Al 12, Mg 2Al 3Etc. type.With the Mg that studied 3Al 12, Mg 5Al 6, Mg-14Al all can realize reversible hydrogen adsorption and desorption, but it is poor to inhale the hydrogen discharge reaction dynamic performance, and hydrogen discharging temperature is all more than 300 ℃.Do not report nanocrystalline M g at present 17Al 12With Mg compound hydrogen storage material system.
Summary of the invention
The purpose of this invention is to provide a kind of reversible hydrogen adsorption and desorption, have the Mg-based composite hydrogen storage material and the preparation method of higher hydrogen-storage amount, good activation performance and good suction hydrogen desorption kinetics performance.
Mg-based composite hydrogen storage material of the present invention contains 1.0~10.0%Al by weight percentage, 1.0~5.0%Ni, and surplus is Mg.
Above-mentioned Al is with nanocrystalline M g 17Al 12There is grain-size 40~80nm mutually.
The preparation method of Mg-based composite hydrogen storage material, its step is as follows:
(1) reguline metal Mg and Al are prepared Mg by the Medium frequency induction melting 17Al 12Alloy is crushed to 300 orders;
(2) under 340 ℃ of hydrogen atmosphere 4.0MPa, the hydrogenation of Mg powder is made MgH 2
(3) with Powdered Mg 17Al 12, MgH 2, Ni is according to weight percent 1.0~10.0%Al, 1.0~5.0%Ni, surplus Mg mixes, ball milling is 60~100 hours under argon gas atmosphere, ratio of grinding media to material is 20:1, the Mg-Al-Ni composite hydrogen storage material.
Mg-based composite hydrogen storage material of the present invention since Al with intermetallic compound Mg 17Al 12Exist mutually, elemental metals Mg has good plasticity, Mg in matrix material 17Al 12Alloy has good fragility, and constantly particle welding, reflow process can cause Mg in mechanical milling process 17Al 12Alloying pellet is embedded in the Mg particle surface, when these particles are hydrogenated to hydride, and Mg 17Al 12Alloying pellet will be surrounded by Mg hydride layer, thereby plays the rapid passage effect of hydrogen atom diffusion, promotes the carrying out of hydrogenation.Mg behind the while ball milling 17Al 12Alloy has certain reversible hydrogen adsorption and desorption performance, has to inhale to put hydrogen activity, also is beneficial to the carrying out that promotes magnesium base composite material to inhale hydrogen discharge reaction.
The adding of Ni simple substance has good katalysis for the absorption and the desorption of hydrogen in Mg-based composite hydrogen storage material of the present invention.In addition, a large amount of crystal boundaries introduced in grain refining and the mechanical milling process and the existence of lattice imperfection have also promoted the raising of alloy hydrogen storage property.Magnesium base composite material of the present invention has inhales that hydrogen discharging temperature is low, the reversible hydrogen adsorption and desorption amount high and good suction hydrogen desorption kinetics performance and activation performance, can be used for making hydrogen source, is convenient to the purification and the accumulating of hydrogen, also can be used for the fuel cell hydrogen storage material.
Compared with prior art, the present invention has the following advantages: (1) Al is originally as light-weight metal, with the Mg after the Mg alloying 17Al 12Itself can reversible hydrogen adsorption and desorption, have certain hydrogen-storage amount; (2) Mg and Al have good plasticity, are difficult to realize grain refining, earlier Mg and Al are passed through the induction melting alloying among the present invention, generate compound Mg between friable metal 17Al 12, residue Mg powder generates MgH2 to improve its fragility by hydrogenation, makes ball milling refinement efficient improve greatly; (3) adding of Ni has been played good katalysis to the suction hydrogen discharge reaction of Mg; (4) compare with metal M g powder, this matrix material can be inhaled hydrogen under 120 ℃, and just can inhale at 260 ℃ and to put hydrogen, and it is functional to inhale hydrogen desorption kinetics, and activation easily.
Description of drawings
Fig. 1 is nanocrystalline M g 17Al 12The suction hydrogen curve of alloy (initial hydrogen pressure 4.0MPa).
Fig. 2 is nanocrystalline M g 17Al 12Alloy is put the hydrogen curve under 280 ℃, 0.1MPa hydrogen pressure.
Embodiment
Embodiment 1:
Reguline metal Mg, Al according to atomic ratio 17:12 proportioning, are prepared Mg by the Medium frequency induction melting under vacuum condition 17Al 12Alloy is through mechanical disintegration to 300 order.Ball milling obtained nanocrystalline M g in 80 hours under argon shield atmosphere 17Al 12Alloy powder.This alloy just can be inhaled hydrogen without any activation treatment under 200 ℃, 4.0MPa hydrogen pressure, and inhales hydrogen speed and improve with the rising of temperature.Nanocrystalline M g 17Al 12The suction hydrogen curve of alloy as shown in Figure 1, nanocrystalline M g 17Al 12Alloy put the hydrogen curve as shown in Figure 2.As seen from the figure, the nanocrystalline M g behind the ball milling 17Al 12Alloy has certain reversible hydrogen adsorption and desorption performance, has to inhale to put hydrogen activity, helps promoting magnesium base composite material to inhale the carrying out of hydrogen discharge reaction.
Embodiment 2:
With reguline metal Mg, Al Medium frequency induction smelting method for preparing Mg under vacuum condition 17Al 12Alloy is through mechanical disintegration to 300 order.Mg powder (200 order) (hydrogen pressure 4.0MPa) hydrogenation under 340 ℃ of hydrogen atmospheres makes MgH 2With Mg 17Al 12, MgH 2, Ni (300 order) is according to weight percent content 3.54%Al, 5.0%Ni, surplus Mg mixes.Ball milling is 80 hours under argon gas atmosphere, obtains the Mg-Al-Ni composite hydrogen storage material.This hydrogen storage material just can be inhaled H-H reaction under 120 ℃, hydrogen can reach 5.6wt.% in 160 ℃, 30 minutes, and 180 ℃, hydrogen reach more than 6.0%.Following 80 minutes hydrogen desorption capacities of 260 ℃, 1 atmospheric pressure reach 5.0wt.%.
Embodiment 3:
With reguline metal Mg, Al Medium frequency induction smelting method for preparing Mg under vacuum condition 17Al 12Alloy is through mechanical disintegration to 300 order.Mg powder (200 order) (hydrogen pressure 4.0MPa) hydrogenation under 340 ℃ of hydrogen atmospheres makes MgH 2With Mg 17Al 12, MgH 2, Ni (300 order) is according to weight percent content 9.5%Al, 1.0%Ni, surplus Mg mixes.Ball milling is 80 hours under argon gas atmosphere, obtains the Mg-Al-Ni composite hydrogen storage material.This hydrogen storage material just can be inhaled H-H reaction under 120 ℃, hydrogen can reach 5.05wt.% in 160 ℃, 30 minutes, and 180 ℃, hydrogen reach 5.82%.Following 80 minutes hydrogen desorption capacities of 260 ℃, 1 atmospheric pressure reach 4.85wt.%.
Embodiment 4:
With reguline metal Mg, Al Medium frequency induction smelting method for preparing Mg under vacuum condition 17Al 12Alloy is through mechanical disintegration to 300 order.Mg powder (200 order) (hydrogen pressure 4.0MPa) hydrogenation under 340 ℃ of hydrogen atmospheres makes MgH 2With Mg 17Al 12, MgH 2, Ni (300 order) is according to weight percent content 1.5%Al, 4.0%Ni, surplus Mg mixes.Ball milling is 80 hours under argon gas atmosphere, obtains the Mg-Al-Ni composite hydrogen storage material.This hydrogen storage material just can be inhaled H-H reaction under 120 ℃, hydrogen can reach 5.75wt.% in 160 ℃, 30 minutes, and 180 ℃, hydrogen reach more than 6.0%.Following 80 minutes hydrogen desorption capacities of 260 ℃, 1 atmospheric pressure reach 5.1wt.%.

Claims (3)

1, a kind of Mg-based composite hydrogen storage material is characterized in that containing by weight percentage 1.0~10.0%Al, 1.0~5.0%Ni, and surplus is Mg.
2, Mg-based composite hydrogen storage material according to claim 1 is characterized in that said Al is with nanocrystalline M g 17Al 12There is grain-size 40~80nm mutually.
3, the preparation method of Mg-based composite hydrogen storage material according to claim 1, its step is as follows:
(1) reguline metal Mg and Al are prepared Mg by the Medium frequency induction melting 17Al 12Alloy is crushed to 300 orders;
(2) under 340 ℃ of hydrogen atmosphere 4.0MPa, the hydrogenation of Mg powder is made MgH 2
(3) with Powdered Mg 17Al 12, MgH 2, Ni is according to weight percent 1.0~10.0%Al, 1.0~5.0%Ni, surplus Mg mixes, ball milling is 60~100 hours under argon gas atmosphere, ratio of grinding media to material is 20:1, the Mg-Al-Ni composite hydrogen storage material.
CN2008101641159A 2008-12-25 2008-12-25 Magnesium base composite hydrogen storage material and preparation method Expired - Fee Related CN101457321B (en)

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