CN102634714A - Copper-added magnesium-aluminum hydrogen storage alloy and preparation method thereof - Google Patents
Copper-added magnesium-aluminum hydrogen storage alloy and preparation method thereof Download PDFInfo
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- CN102634714A CN102634714A CN2012101181560A CN201210118156A CN102634714A CN 102634714 A CN102634714 A CN 102634714A CN 2012101181560 A CN2012101181560 A CN 2012101181560A CN 201210118156 A CN201210118156 A CN 201210118156A CN 102634714 A CN102634714 A CN 102634714A
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Abstract
The invention relates to a magnesium-aluminum hydrogen storage alloy and a preparation method thereof. The magnesium-aluminum hydrogen storage alloy is obtained by mechanical ball milling in a vacuum or inert atmosphere. The chemical composition of the magnesium-aluminum hydrogen storage alloy is 17Mg12Al-xCu, wherein 5<=x<=10. The magnesium-aluminum hydrogen storage alloy can effectively enhance the hydrogen adsorption capacity and hydrogen adsorption rate, and improves the hydrogen adsorption/desorption kinetic properties of magnesium. The invention can be used for filtration, purification, storage and transportation of hydrogen gas. The production method provided by the invention is simple and easy to implement, and has the advantage of low energy consumption.
Description
Technical field
The present invention relates to a kind of hydrogen storage material, particularly add the magnalium base hydrogen storage alloy and the preparation method of copper.
Background technology
Because the unlimited utilization of fossil oil and the rapid decay of the nature carbon energy, the CO2 emissions that combustion of fossil fuel brings are from 325 tons of rising to 2006 of 20,700,000,000 tons of nineteen ninety, and this numeral is than the rate of growth also fast 35% of expecting.Following energy system should be reliably, is easy to get, cleaning, flexibly, low consumed.Hydrogen is that occurring in nature is contained abundant element, and is the lightest a kind of fuel, and energy stored is bigger under the unit mass, and hydrogen is a kind of green energy resource, therefore it is believed that Hydrogen Energy is the developing direction of future source of energy.But the key element that is restricting the utilization of Hydrogen Energy is the storage of hydrogen.Searching out a kind of effective hydrogen storage material is the emphasis of recent people's research.Up to the present, most hydrogen storage alloy LaNi for example
5, TiFe, TiMn
2, hydrogen-storage amount all is lower than 2wt%, can not reach the target of Ministry of Energy's practical application.The hydrogenate of magnesium series is a kind of competitive hydrogen storage material candidate, and its theoretical hydrogen-storage amount can reach 7.6wt%.But because MgH
2Suction hydrogen desorption kinetics poor performance, though there is higher hydrogen not put into production use.In recent years, Mg-Al alloy liking because of its light weight, the low people of acquisition of cost.There is the scholar to report Mg
17Al
12Have and inhale the ability put hydrogen, and its hydrogen is 4.4wt%, compare Mg
2Hydrogen storage materials such as Ni, hydrogen has a certain upgrade, but Mg
17Al
12slow, the hydrogen of hydrogen-absorption speed can not reach theoretical value at short notice, have the investigator to use the method for BMA to prepare Mg
17Al
12, its performance is improved, and at 523K, the hydrogen that 5.3MPa inhales is 3.2wt%, also reaches theoretical hydrogen far away.Someone uses the ball milling method milled Mg
17Al
12, the Mg behind the observation 10-100h
17Al
12Hydrogen storage property, find its at ball milling behind 30h, 70h, the 100h its hydrogen sucking function just can reach 4.03wt%, 4.27wt%, 4.18wt% respectively, though its hydrogen near theoretical value, the ball milling overlong time is unfavorable for actual use.The somebody is at Mg simultaneously
17Al
12In added nano-TiO
2, but it is after 573K inhales hydrogen 1400min, and hydrogen is reduced to 3.5wt%, but because the nano material cost is higher, is difficult for obtaining.
Summary of the invention
The purpose of this invention is to provide a kind of magnalium base hydrogen storage alloy and preparation method who adds copper, the magnalium base hydrogen storage alloy of this interpolation copper can effectively promote its hydrogen and hydrogen-absorption speed, has improved the suction hydrogen desorption kinetics performance of magnesium.Can be used for filtration, purification and the accumulating of hydrogen.Working method according to the invention is easy, implements easily, and it is little to consume energy.
Technical scheme of the present invention is: add the magnalium base hydrogen storage alloy of copper, this magnalium base hydrogen storage alloy that adds copper obtains through mechanical ball milling under inert atmosphere, and its chemical composition is 17Mg12Al-xCu, wherein 5≤x≤10.
The magnalium base hydrogen storage alloy for preparing above-mentioned interpolation copper has following steps:
1) be to get each component powders at 17: 12 according to the atomic ratio of magnesium and aluminium, under inert atmosphere, ball-to-powder weight ratio 20: 1, mechanical ball milling 12h has obtained Mg
17Al
12Alloy;
2) according to 17Mg12Al-xCu, the stoichiometry of 5≤x≤10 takes by weighing the Mg of step 1) gained
17Al
12Alloy material and Cu metal-powder, under inert atmosphere, ball-to-powder weight ratio 20: 1, the mechanical ball milling time is 2 hours, obtains adding the magnalium base hydrogen storage alloy of copper.
Said mechanical ball milling rotating speed is 600rmp.
In the step 1) mechanical milling process, two hours mixed powders of every ball milling with Mg metal and Al metal place be full of be crushed to mortar under the inert atmosphere Powdered.
Said inert atmosphere is an argon gas atmosphere.
In the present invention, the effect of adding Cu is following: 1. transition metal Cu powder fully contacts in ball mill with the powder of mg-based material, because the powder comparatively small amt of transition metal Cu makes the fine particle of transition metal Cu be embedded in Mg
17Al
12Particle surface has played the effect that destroys the dense oxidation film of magnesium surface; 2. transition metal Cu has the effect of certain decomposition hydrogen molecule, makes it become Wasserstoffatoms at the material surface fast dissociating, and therefore, transition metal Cu can improve the surfactivity of magnalium material, and the hydrogen storage property that can improve the magnalium based material.The applicant can know through the XRD diffraction experiment, adds the Mg of Cu
17Al
12Sample after 623K inhales hydrogen, the Mg in the alloy
17Al
12Alloy phase disappears, and a large amount of MgH occurred
2Mutually with Al mutually, in addition, the intensity of the diffraction peak of Cu reduction, and MgCu occurred
2Phase.The MgCu that in inhaling the hydrogen process, generates
2In reaction process, played catalytic effect etc. cenotype.
Mg of the present invention, Al, three kinds of metal-powders of Cu are through after the ball-milling processing, and alloy can directly be used to charge and discharge hydrogen, need not activation.
The magnalium base hydrogen storage alloy of interpolation copper according to the invention is compared with the described Mg based hydrogen storage material of background technology, has higher hydrogen storage capability to reach hydrogen-absorption speed faster.
Preparing method of the present invention has following advantage:
1. do not use rare metal and precious metal, like palladium, platinum etc., use be aluminium, the copper that more cheaply is easy to get, reduced cost, be convenient to the extensive use of material.
2. produce easyly, implement easily, it is little to consume energy, and first ball milling 12h synthesizes Mg
17Al
12Subsequent use, only need ball milling 2h just can synthesize hydrogen storage alloy.
3. effectively promote the hydrogen and the hydrogen-absorption speed of alloy, as the Mg of control group
17Al
12Need be under the 623K temperature; Hydrogen is 4.1wt% behind the suction hydrogen 1400min; But its hydrogen at 240min is merely 3.1wt%, and the alloy of interpolation 5%Cu, 10%Cu is respectively 4.07wt%, 3.93wt% at the 240min hydrogen, and hydrogen and speed are well improved.
Magnalium base hydrogen storage alloy according to the invention can be used for filtration, purification and the accumulating of hydrogen.
In the magnesium powder according to the invention the content of magnesium be 99.5%, in the aluminium powder content of aluminium be 99%, the content 99.5% of copper in the copper powder.
The ball mill that the present invention adopts is the Pulverisett-5 type ball mill that German FRITSCH company produces.
Description of drawings
Fig. 1 is the XRD figure spectrum of magnalium base hydrogen storage alloy under different states, and wherein 1a is the Mg behind the ball milling 8h
17Al
12, 1b is the Mg behind the ball milling 12h
17Al
12, 1c is the Mg behind the ball milling 12h
17Al
12After inhaling hydrogen, 1d is the Mg behind the ball milling 12h
17Al
12After putting hydrogen;
Fig. 2 is Mg
17Al
12The XRD figure spectrum of+Cu under different states, wherein 2a is the Mg behind the ball milling 2h
17Al
12Before+5%Cu inhaled hydrogen, 2b was the Mg behind the ball milling 2h
17Al
12After+5%Cu inhales hydrogen; 2c is the Mg behind the ball milling 2h
17Al
12Before+10%Cu inhaled hydrogen, 2d was the Mg behind the ball milling 2h
17Al
12After+10%Cu inhales hydrogen;
Fig. 3 is Mg
17Al
12The suction hydrogen kinetic curve of the serial hydrogen storage alloy of+M (M=0,5%Cu, 10%Cu) under 350 ℃.
The practical implementation method
Embodiment 1
Insert in the stainless cylinder of steel that is full of argon gas after magnesium powder, aluminium powder mixed by atomic ratio at 17: 12, under rotating speed 600rmp, 20: 1 condition of ball-to-powder weight ratio,, obtained Mg with ball mill ball milling 12h
17Al
12Alloy.Because powdered alloy is bonded in easily on the ball milling tank skin and forms bulk, carries out for preventing the bonding synthetic effect that influences, reacting fully, and whenever places the vacuum glove box that is full of argon gas to carry out break process alloy at a distance from two hours, is crushed to Powdered.Respectively to 8h (referring to the 1a among Fig. 1), 12h (referring to the 1b among Fig. 1), inhale (referring to the 1c among Fig. 1) behind the hydrogen, put the Mg of (referring to the 1d among Fig. 1) behind the hydrogen
17Al
12Alloy carries out material phase analysis, and with the Mg for preparing
17Al
12Alloy (powder) is in 350 ℃ of inspiration promoting the circulation of qi attitude hydrogen storage property tests (referring to Fig. 3).
Embodiment 2
Get embodiment 1 described Mg
17Al
12Powdered alloy; Add mass percent then and be 5% Cu powder, two kinds of powder evenly are placed in the stainless cylinder of steel that is full of argon gas, with rotating speed 600rmp, 20: 1 condition of ball-to-powder weight ratio; With ball mill ball milling 2h, obtain adding the magnalium base hydrogen storage alloy of copper.
Get the magnalium base hydrogen storage alloy of the above-mentioned interpolation copper that makes, process Powderedly, make respectively and inhale before the hydrogen sample and inhale sample behind the hydrogen.Sample to (referring to the 2b among Fig. 2) behind (referring to the 2a among Fig. 2), the suction hydrogen before the suction hydrogen carries out material phase analysis, carries out gaseous state hydrogen storage property test (referring to Fig. 3) at 350 ℃.
Get the described Mg of embodiment
17Al
12Powdered alloy adds mass percent and is 10% Cu then, and two kinds of powder evenly are placed in the stainless cylinder of steel that is full of argon gas, with rotating speed 600rmp, 20: 1 condition ball milling 2h of ball-to-powder weight ratio, obtain adding the magnalium base hydrogen storage alloy of copper.
Get the magnalium base hydrogen storage alloy of the above-mentioned interpolation copper that makes, process Powderedly, make respectively and inhale before the hydrogen sample and inhale sample behind the hydrogen.Sample to (referring to the 2d among Fig. 2) behind (referring to the 2c among Fig. 2), the suction hydrogen before the suction hydrogen carries out material phase analysis (referring to the 2c among Fig. 2,2d) respectively, carries out gaseous state hydrogen storage property test (referring to Fig. 3) at 350 ℃.
Shown in Figure 1 is Mg and the XRD figure spectrum of Al mixed powder behind the 8-12h ball milling, and as can beappreciated from fig. 1, behind the ball milling 8h, powder has basically formed Mg
17Al
12Alloy phase, but wherein also have a spot of Mg and Al simple substance crystalline state diffraction peak.Behind the ball milling 12h (referring to Fig. 1 b), from the XRD diffraction curve, can find out to have only single Mg
17Al
12Alloy phase exists, and can think that Mg becomes Mg with Al powder combination without repetition
17Al
12Phase.In the process of ball milling, between magnesium powder and aluminium powder and abrading-ball repeatedly taking place clash into, powder produces violent viscous deformation, cold welding and Mg atomic diffusion take place in the lattice of Al in the continuous refinement of powder simultaneously between the particle, form Mg at last
17Al
12Phase.Fig. 1 c is the Mg behind the mechanical ball milling 12h
17Al
12Sample is inhaled the XRD figure spectrum behind the hydrogen under 623K, contain MgH in visible this sample
2, Al, Mg
17Al
12Deng the thing phase.Fig. 1 d is the XRD figure spectrum of alloy after 653K transfers hydrogen, it is thus clear that the product of putting behind the hydrogen is Mg
17Al
12Alloy phase.Know by above, at Mg
17Al
12Inhale in the hydrogen process MgH is arranged
2Generate with Al, put the hydrogen back alloying symphysis that finishes and become Mg
17Al
12This shows through behind the ball milling of 12h, be completed into Mg
17Al
12Phase, Mg
17Al
12It is reversible that the hydrogen process is put in the suction of phase.
Mg behind the ball milling 12h shown in Figure 2
17Al
12Powdered alloy add respectively 5% with 10%Cu after the different XRD figures put the hydrogen state under of inhaling compose.Visible by Fig. 2, add Cu ball milling 2h after, the principal phase of the alloy of gained still is Mg
17Al
12Single-phase, and have a spot of Cu simple substance.As the Mg that adds Cu
17Al
12Sample after 623K inhales hydrogen, the Mg in the alloy
17Al
12Alloy phase disappears, and a large amount of MgH occurred
2Reach the Al phase mutually, in addition, the intensity of the diffraction peak of Cu reduces, and MgCu occurred
2Phase.MgCu
2Can effectively improve the hydrogen storage property of alloy as catalyzer.
Fig. 3 is Mg
17Al
12And Mg
17Al
12The suction hydrogen dynamic performance test result of three kinds of alloys of+xCu (5≤x≤10) under the 623K temperature.Three kinds of alloys are respectively at the maximum hydrogen of 240min and are 3.1wt%, 4.07wt%, 3.93wt%, Mg
17Al
12Hydrogen 1200min must be inhaled and maximum hydrogen 4.17wt% could be arrived; After in alloy, adding Cu; Though the system hydrogen-storage amount slightly descends; But hydrogen-absorption speed improves greatly, as: the hydrogen behind interpolation 5%Cu, the 10%Cu is respectively 97%, 99% of theoretical hydrogen, and its hydrogen has just reached maximum when 240min.Through after the surperficial complex phase ball-milling processing, Mg
17Al
12Hydrogen storage property obtain more significantly improving, and along with the rising of temperature, its hydrogen constantly increases.The alloy activation of adding Cu is higher relatively, shows as to be easy to and hydrogen reaction, and the suction hydrogen time is shorter.
Think that through the experiment applicant ball milled can be accelerated the suction hydrogen discharging rate of Mg alloy, reduce the suction hydrogen discharging temperature of alloy.Through the Mg after the ball-milling processing
17Al
12Maximum hydrogen be 4.1wt%, compare the Mg of as cast condition
17Al
12(its maximum hydrogen is 1.3wt%) wants many.This is that active increasing accelerated H because ball milling increases granule surface area
2Decompose.Cu is a transition metal, and N Cu atom can make H
2Activation is with the H of absorption
2Molecule breaking is an atom, then the H atom is offered other reactant, thus the catalysis of realization response.Cu can improve dynamic performance, and hydrogen absorption capacity reduces.In the present embodiment, the MgCu that the Cu that adds in the test forms in the alloy hydrogen absorption and desorption process
2Possibly accelerate absorption hydrogen speed as the catalyzer of this experiment mutually, improve the hydrogen storage alloy hydrogen storage property.
The above results shows that the present invention can effectively improve Mg
17Al
12Suction hydrogen kinetics, accelerate hydrogen-absorption speed, what wherein play a major role is that alloy has formed new phase MgCu after adding Cu in the process of inhaling hydrogen
2, they improve the suction hydrogen dynamic performance of alloy.
Claims (5)
1. magnalium base hydrogen storage alloy that adds copper, it is characterized in that: the magnalium base hydrogen storage alloy of this interpolation copper obtains through mechanical ball milling under inert atmosphere, and its chemical composition is 17Mg12Al-xCu, wherein 5≤x≤10.
2. prepare the magnalium base hydrogen storage alloy of the described interpolation copper of claim 1, it is characterized in that following steps are arranged:
1) be to get each component powders at 17: 12 according to the atomic ratio of magnesium and aluminium, under inert atmosphere, ball-to-powder weight ratio 20: 1, mechanical ball milling 12h has obtained Mg
17Al
12Alloy;
2) according to 17Mg12Al-xCu, the stoichiometry of 5≤x≤10 takes by weighing the Mg of step 1) gained
17Al
12Alloy material and Cu metal-powder, under inert atmosphere, ball-to-powder weight ratio 20: 1, the mechanical ball milling time is 2 hours, obtains adding the magnalium base hydrogen storage alloy of copper.
3. method according to claim 2 is characterized in that: the mechanical ball milling rotating speed is 600rmp.
4. method according to claim 2 is characterized in that: in the step 1) mechanical milling process, two hours mixed powders of every ball milling with Mg metal and Al metal place be full of be crushed to mortar under the inert atmosphere Powdered.
5. method according to claim 2 is characterized in that: inert atmosphere is an argon gas atmosphere.
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Cited By (9)
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|---|---|---|---|---|
| CN105132838A (en) * | 2015-09-25 | 2015-12-09 | 广西大学 | Regulation method of Mg17Al12 hydrogenation |
| CN105514399A (en) * | 2015-12-21 | 2016-04-20 | 宁波高新区锦众信息科技有限公司 | Magnesium-based hydrogen storage alloy for Ni-MH secondary batteries and preparation method of magnesium-based hydrogen storage alloy |
| CN107760947A (en) * | 2017-09-18 | 2018-03-06 | 西北工业大学 | Mg Al Ni system's hydrogen storage particles and its catalytic modification preparation method |
| WO2020000610A1 (en) * | 2018-06-29 | 2020-01-02 | 邵鹏 | Catalyst-enhanced mgal-based hydrogen storage material |
| CN110697652A (en) * | 2019-11-20 | 2020-01-17 | 榆林学院 | Preparation method of yttrium/graphene modified magnesium-aluminum hydrogen storage composite material |
| CN110788331A (en) * | 2019-11-07 | 2020-02-14 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Copper-containing composite hydrogen storage alloy and preparation method thereof, composite solid hydrogen storage tank and hydrogen storage performance testing method |
| CN110788330A (en) * | 2019-11-07 | 2020-02-14 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Aluminum-containing composite hydrogen storage alloy and preparation method thereof, composite solid hydrogen storage tank and hydrogen storage performance testing method |
| CN111498800A (en) * | 2020-06-09 | 2020-08-07 | 世能氢电科技有限公司 | Magnesium-aluminum alloy composite hydrogen storage material and preparation method thereof |
| CN115383122A (en) * | 2022-08-25 | 2022-11-25 | 太原科技大学 | Hydrogen crushing preparation method of 2 |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105132838A (en) * | 2015-09-25 | 2015-12-09 | 广西大学 | Regulation method of Mg17Al12 hydrogenation |
| CN105514399A (en) * | 2015-12-21 | 2016-04-20 | 宁波高新区锦众信息科技有限公司 | Magnesium-based hydrogen storage alloy for Ni-MH secondary batteries and preparation method of magnesium-based hydrogen storage alloy |
| CN107760947A (en) * | 2017-09-18 | 2018-03-06 | 西北工业大学 | Mg Al Ni system's hydrogen storage particles and its catalytic modification preparation method |
| WO2020000610A1 (en) * | 2018-06-29 | 2020-01-02 | 邵鹏 | Catalyst-enhanced mgal-based hydrogen storage material |
| CN110788331A (en) * | 2019-11-07 | 2020-02-14 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Copper-containing composite hydrogen storage alloy and preparation method thereof, composite solid hydrogen storage tank and hydrogen storage performance testing method |
| CN110788330A (en) * | 2019-11-07 | 2020-02-14 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Aluminum-containing composite hydrogen storage alloy and preparation method thereof, composite solid hydrogen storage tank and hydrogen storage performance testing method |
| CN110788330B (en) * | 2019-11-07 | 2022-02-11 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Aluminum-containing composite hydrogen storage alloy and preparation method thereof, composite solid hydrogen storage tank and hydrogen storage performance testing method |
| CN110697652A (en) * | 2019-11-20 | 2020-01-17 | 榆林学院 | Preparation method of yttrium/graphene modified magnesium-aluminum hydrogen storage composite material |
| CN111498800A (en) * | 2020-06-09 | 2020-08-07 | 世能氢电科技有限公司 | Magnesium-aluminum alloy composite hydrogen storage material and preparation method thereof |
| CN115383122A (en) * | 2022-08-25 | 2022-11-25 | 太原科技大学 | Hydrogen crushing preparation method of 2 |
| CN115383122B (en) * | 2022-08-25 | 2023-07-14 | 太原科技大学 | Hydrogen crushing preparation method of 2:17 sintered samarium cobalt permanent magnet |
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Application publication date: 20120815 |