CN103556022B - A kind of Mg-In-Ag ternary hydrogen storage material and preparation method thereof - Google Patents
A kind of Mg-In-Ag ternary hydrogen storage material and preparation method thereof Download PDFInfo
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- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 99
- 239000001257 hydrogen Substances 0.000 title claims abstract description 99
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000011232 storage material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 52
- 239000000956 alloy Substances 0.000 claims abstract description 52
- 230000008018 melting Effects 0.000 claims abstract description 31
- 238000002844 melting Methods 0.000 claims abstract description 31
- 239000000126 substance Substances 0.000 claims abstract description 14
- 229910019015 Mg-Ag Inorganic materials 0.000 claims abstract description 11
- 229910002058 ternary alloy Inorganic materials 0.000 claims abstract description 11
- 229910002056 binary alloy Inorganic materials 0.000 claims abstract description 9
- 230000006698 induction Effects 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 15
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- 238000003860 storage Methods 0.000 abstract description 14
- 150000002431 hydrogen Chemical class 0.000 abstract description 9
- 238000007599 discharging Methods 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 7
- 239000000843 powder Substances 0.000 abstract description 5
- 238000005275 alloying Methods 0.000 abstract description 3
- 239000000470 constituent Substances 0.000 abstract 1
- 239000011777 magnesium Substances 0.000 description 40
- 238000000034 method Methods 0.000 description 19
- 229910052749 magnesium Inorganic materials 0.000 description 14
- 230000008569 process Effects 0.000 description 13
- 238000000498 ball milling Methods 0.000 description 10
- 229910052738 indium Inorganic materials 0.000 description 10
- 238000003795 desorption Methods 0.000 description 8
- 239000012071 phase Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 230000005496 eutectics Effects 0.000 description 5
- 230000004913 activation Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 229910001316 Ag alloy Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000005300 metallic glass Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000012254 powdered material Substances 0.000 description 2
- 230000007420 reactivation Effects 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 230000000930 thermomechanical effect Effects 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 229910003023 Mg-Al Inorganic materials 0.000 description 1
- 229910019086 Mg-Cu Inorganic materials 0.000 description 1
- 229910019083 Mg-Ni Inorganic materials 0.000 description 1
- 229910019403 Mg—Ni Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 1
- 241000720974 Protium Species 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 239000001996 bearing alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004455 differential thermal analysis Methods 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- SJCKRGFTWFGHGZ-UHFFFAOYSA-N magnesium silver Chemical compound [Mg].[Ag] SJCKRGFTWFGHGZ-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Abstract
The invention discloses a kind of novel Mg-In-Ag ternary hydrogen storage alloy system and preparation method thereof, belong to hydrogen storage material technical field.This hydrogen storage material composition consists of: the atomic percent of (Mg+In) is 80 ~ 85%, and wherein the accounting of In in (Mg+In) is 3 ~ 6%, and all the other are Ag.Take Mg block and Ag sheet by alloying constituent, adopt induction melting furnace first melting Mg-Ag binary low melting point alloy, then by proportioning take In block together with above-mentioned binary alloy again melting obtain Mg-In-Ag ternary alloy; Grind to form powdered alloy by after this alloy removing surface scale, then put into the ball grinder mechanical force and chemical being filled with hydrogen and prepare highly active powder hydrogen storage material, it can directly as final hydrogen storage material product use.Hydrogen storage material of the present invention has puts without the need to inhaling the feature that hydrogen activates, hydrogen-storage amount is high, suction hydrogen discharging temperature is low and suction hydrogen discharging rate is fast.
Description
Technical field
The present invention relates to hydrogen storage technology field, be specifically related to a kind of novel magnesium-base hydrogen storage material system and novel preparation method thereof.
Background technology
MAGNESIUM METAL has that density is little, hydrogen storage capacity is high (7.6 wt.%) as a kind of hydrogen storage material and aboundresources, the advantage such as cheap.Therefore Mg base hydrogen bearing alloy is the most promising a kind of hydrogen storage material.For now, Mg and Mg base alloy stores up hydrogen application widely and should solve following problem: (1) such alloy hydrogen absorption and desorption activation difficulty (generally needing the suction of 3 ~ 8 times to put hydrogen cyclic activation); (2) speed for hydrogen absorbing and releasing is comparatively slow, namely inhales hydrogen desorption kinetics poor performance; (3) inhale that to put hydrogen thermomechanical property poor, needs effectively could be inhaled at about 350 DEG C and put hydrogen usually.
Alloying improves the simple and effective means of one of Mg base hydrogenous alloy the problems referred to above, and the System Design of material, phase morphology control are directly connected to the quality of its hydrogen storage property.At present, the Mg base binary hydrogen storage alloy developed mainly contains the systems such as Mg-Ni, Mg-Cu, Mg-Al and Mg-In.The suction of compound to Mg alloy that wherein Ni, Cu, Al etc. and Mg are formed is put hydrogen and is had katalysis, and at MgH
2put the effect playing unstability medium in hydrogen process; And In and Mg formed Mg (In) sosoloid not only can improve suction hydrogen desorption kinetics, and can effectively improve suction put hydrogen thermomechanical property [
h. C. Zhong, H. Wang, J. W. Liu, D. L. Sun and M. Zhu, Scr. Mater., 65 (2011), 285].Based on Ni, Cu, Al and the In not same-action in the alloying of Mg, be developed Mg-Ni-In ternary hydrogen storage alloy recently, the hydrogen storage property of this alloy comparatively binary alloy improve significantly [
f. P. Luo, H. Wang, L. Z. Ouyang, M. Q. Zeng, J. W. Liu and M. Zhu, Int. J. Hydrogen Energy, 38 (2013), 10912; J. Cermak and L. Kral, J. Alloys Compd., 546 (2013), 129].Due to the fusing point of In low (156 DEG C), large (7.31 g/cm of density
2), simple melting method efficiently can not be adopted to prepare the Mg base hydrogenous alloy containing In.Therefore, people can only adopt high-energy ball milling+sintering two-step approach to prepare the hydrogen storage materials such as Mg-In, Mg-Ni-In at present.The method Ball-milling Time long (about 170 h) [
f. P. Luo, H. Wang, L. Z. Ouyang, M. Q. Zeng, J. W. Liu and M. Zhu, Int. J. Hydrogen Energy, 38 (2013), 10912], there is time consumption and energy consumption and long time ball milling bring the shortcomings such as tank skin impurity into; Follow-up sintering increases the consumption of preparation time and the energy further, and in sintering process, hydrogen storage material is easy to oxidation so that the control of sintering process difficulty, causes preparation cost significantly to increase.Therefore, the difficult problem in preparation is the Main Bottleneck containing the development and application of In ternary Mg base hydrogenous alloy.
Summary of the invention
In order to improve containing the Mg base hydrogenous alloy preparation method of In deficiency and improve hydrogen storage property, the invention provides a kind of novel Mg-In-Ag ternary hydrogen storage material system being suitable for melting and preparing, successfully prepare highly active Mg based hydrogen storage material powder in conjunction with mechanical force and chemical ball milling.Simple and the hydrogen storage property preparing material of the method preparation technology is largely increased.
The invention provides a kind of Mg-In-Ag ternary hydrogen storage material, this material component by atomic percent proportioning is: (Mg+In) is 80 ~ 85%, and wherein the accounting of In in (Mg+In) is 3 ~ 6%, and all the other are Ag.
Invention also provides a kind of preparation method of above-mentioned Mg-In-Ag ternary hydrogen storage material, the method concrete steps are as follows:
(1) molten alloy: take Mg block, In block and Ag tablet raw material by component proportion according to claim 1, the purity of raw material is all not less than 99.0 wt%, wherein Mg element is added to the scaling loss of 8 ~ 10 wt%; Then adopt induction melting furnace melting Mg-Ag binary low melting point alloy, then the In block taken by proportioning melting together with the Mg-Ag binary alloy of melting is obtained Mg-In-Ag ternary alloy;
(2) under nitrogen atmosphere, mechanical force and chemical prepares hydrogen storage material: ternary alloy step (1) melting obtained grinds to form powdered alloy except after descaling in glove box, then be placed on mechanical force and chemical in the ball grinder being filled with 2atm hydrogen and prepare highly active powder hydrogen storage material, be i.e. target product of the present invention: Mg-In-Ag ternary hydrogen storage material.
The principles of science of the present invention:
We develop a kind of Mg-Ag hydrogen storage material system of novelty first recently, put Mg-Ag compound in hydrogen process embody good katalysis in the suction of this material, thus make this system have excellent hydrogen storage property [
this front yard intelligence, Zhangjiang ripple, Liu Dongming, Zhang Qingan, a kind of preparation method of magnesium silver hydrogen storage material, number of patent application: 201210503872.0].In order to improve the hydrogen storage property of material further and the Mg base alloy melting difficulty overcome containing In, we successfully develop first and are a kind ofly applicable to the Mg-In-Ag ternary hydrogen storage material system prepared of common melting.According to binary Mg-Ag alloy low melting point (Mg+Mg
3ag) composition (eutectic transformation temperature is 472 DEG C) of eutectic, crucial being of successful melting preparation of Mg-In-Ag alloy selects the composition close to its ternary eutectic, thus the fusing point that when ensure that smelting solidification, alloy is low the temperature difference controlling liquid-solid phase line are within 10 DEG C; Make ternary alloy have good mobility when liquid phase, there are when solidifying excellent casting characteristics.In the atomization process of molten alloy, the present invention adopts hydrogenation mechanical force and chemical ball-milling technology, and this process makes material create the highly active product (MgH of amorphous+a small amount of
2), amorphous disordered state product facilitates In and puts diffusion in hydrogen process in suction subsequently, make In be all enriched in ternary alloy mutually in, thus cause material to activate (pure Mg and Mg without the need to Chu Qing
2ni alloy need the suction of 5 ~ 10 times put hydrogen cyclic activation [
d. M. Liu, T. Z. Si, C. C. Wang, Q. A Zhang, Scripta Materialia, 57 (2007), 389.]), there is low suction hydrogen discharging temperature and fast suction hydrogen desorption kinetics performance.
The invention has the beneficial effects as follows:
1, the selection of this alloy system composition achieves rich Mg(and inhales protium) alloy melting time liquid-solid phase line the temperature difference be less than 10 DEG C, thus both ensure that alloy had when high hydrogen storage capability (being greater than 2.5 wt.%) in turn ensure that this alloy graining and has excellent casting characteristics.Adopt first melting Mg-Ag binary alloy, the fusing point that the technique then adding In melting again reduces between ternary alloy raw material is poor; Thus further ensure the successful preparation of ternary alloy.Molten alloy technological operation is simple efficient, prepare with ball milling+sinter two steps compared with, greatly reduce energy consumption, improve production efficiency.
2, the mechanical force and chemical preparation technology under such alloy hydrogen storag powder end nitrogen atmosphere is simple to operation, without the annealing operation process of Conventional alloys, improves production efficiency; The high reactivity hydrogen storag powder end produced facilitates material In when hydrogen is put in follow-up suction and is all enriched in compound, and the Mg-In-Ag ternary compound of formation is to MgH
2hydrogen of putting there is splendid katalysis.
3, the hydrogen storage material system that prepared by the present invention has hydrogen storage capability high (being greater than 2.5 wt.%), without the need to Chu Qing activation, suction hydrogen discharging temperature low (260 DEG C), inhales the fast distinguishing feature of hydrogen discharging rate.
Accompanying drawing explanation
Fig. 1 is Mg81In4Ag15 molten alloy as-cast structure and line sweep energy spectrogram.
Fig. 2 is that mechanical force and chemical prepares Mg81In4Ag15 powdered alloy and hydrogen product X x ray diffration pattern x is put in suction;
Wherein: under (a), nitrogen atmosphere, mechanical force and chemical prepares Mg81In4Ag15 powdered alloy X-ray diffractogram; B hydrogen product X x ray diffration pattern x inhaled by (), Mg81In4Ag15 powdered alloy; C (), Mg81In4Ag15 powdered alloy put hydrogen product X x ray diffration pattern x.
Fig. 3 is that Mg81In4Ag15 powdered alloy puts hydrogen DSC(differential thermal analysis) curve.
Fig. 4 is that Mg-In-Ag ternary hydrogen storage material inhales hydrogen desorption kinetics figure at 260 DEG C.
Embodiment
In order to understand technology contents of the present invention further, below in conjunction with the drawings and specific embodiments, the invention will be further described, but the present invention is not limited to following embodiment.
embodiment 1: molten alloy gross weight is approximately 30 grams, takes Mg block (purity 99%, the scaling loss for Mg block many interpolations 9 wt%), Ag sheet (purity is 99.5 %) and In block (purity is 99.5 %) respectively by the composition of Mg81In4Ag15.The Mg block taken and Ag sheet are put into copper crucible induction melting under 15 KW power and obtain low melting point Mg-Ag binary alloy, then by In block together with binary alloy again melting obtain Mg81In4Ag15 ternary alloy, this alloy is by ((Mg, In)
3ag+Mg (In)) eutectic structure and proeutectic Mg (In) composition, In distributed components (as shown in Figure 1) in molten alloy.In glove box, grind to form 100 object powdered alloys with after sharpening machine removing molten alloy surface scale, powdered alloy mechanical force and chemical ball milling 30 h in the ball grinder being filled with 2atm hydrogen obtains a small amount of degradation production MgH
2with other non-crystaline amorphous metal phases (as Suo Shi Fig. 2 (a)); Wherein ratio of grinding media to material is 20:1, and drum's speed of rotation is 300 rpm.Powdered alloy after ball milling directly uses as hydrogen storage material.The powdered material that under nitrogen atmosphere prepared by mechanical force and chemical has high suction and puts hydrogen activity, and material is without the need to storing up hydrogen reactivation process; Amorphous disordered state product prepared by the method facilitates the diffusion of In in suction hydrogen process subsequently, and In is all enriched in (Mg, In) Ag alloy phase, and after causing inhaling hydrogen first, sample contains MgH
2(Mg, In) Ag two-phase (as Suo Shi Fig. 2 (b)), to put in hydrogen process (Mg, In) Ag phase first at 292 DEG C and MgH
2reaction is put hydrogen and is generated (Mg, In)
3ag phase (as Suo Shi Fig. 2 (c)), then (Mg, In)
3ag is to remaining MgH
2play good katalysis (hydrogen discharging temperature is 319 DEG C), two purer MgH of hydrogen discharging temperature
2decline respectively 75 and 48 DEG C (as shown in Figure 3).This powdered alloy just has excellent suction hydrogen desorption kinetics performance under 260 DEG C of low temperature, and it is substantially saturated that it inhaled hydrogen in 10 minutes; Hydrogen is put close to terminating (hydrogen desorption capacity reaches 3.1 wt%) in 25 minutes, and through the business MgH of same process ball milling
2the hydrogen (as shown in Figure 4) of 1.7 wt% is only put in 90 minutes.
embodiment 2: molten alloy gross weight is approximately 30 grams, takes Mg block (purity 99%, the scaling loss for Mg block many interpolations 9 wt%), Ag sheet (purity is 99.5 %) and In block (purity is 99.5 %) respectively by the composition of Mg75In5Ag20.The Mg block taken and Ag sheet are put into copper crucible induction melting under 15 KW power and obtain low melting point Mg-Ag binary alloy, then by In block together with binary alloy again melting obtain Mg75In5Ag20 ternary alloy, this alloy is by ((Mg, In)
3ag+Mg (In)) eutectic structure and proeutectic (Mg, In)
3ag forms, In distributed components in alloy.In glove box, grind to form 100 object powdered alloys with after sharpening machine removing molten alloy surface scale, powdered alloy mechanical force and chemical ball milling 30 h in the ball grinder being filled with 2atm hydrogen obtains a small amount of degradation production MgH
2with other non-crystaline amorphous metal phases; Wherein ratio of grinding media to material is 20:1, and drum's speed of rotation is 300 rpm.Powdered alloy after ball milling directly uses as hydrogen storage material.The powdered material that under nitrogen atmosphere prepared by mechanical force and chemical has high suction and puts hydrogen activity, and material is without the need to storing up hydrogen reactivation process; Material has low suction hydrogen discharging temperature, and it has excellent suction hydrogen desorption kinetics performance under 260 DEG C of low temperature, and it is substantially saturated that it inhaled hydrogen in 10 minutes; In 20 minutes, put hydrogen reach 2.6 wt%(as shown in Figure 4).
Claims (1)
1. a Mg-In-Ag ternary hydrogen storage material, is characterized in that, this material component by atomic percent proportioning is: (Mg+In) is 80 ~ 85%, and wherein the accounting of In in (Mg+In) is 3 ~ 6%, and all the other are Ag; This material is prepared by following steps:
(1) molten alloy: take Mg block, In block and Ag tablet raw material by said components proportioning, the purity of raw material is all not less than 99.0wt%, wherein adds the scaling loss of 8 ~ 10wt% to Mg element; Then adopt induction melting furnace melting Mg-Ag binary low melting point alloy, then the In block taken by proportioning melting together with the Mg-Ag binary alloy of melting is obtained Mg-In-Ag ternary alloy;
(2) under nitrogen atmosphere, mechanical force and chemical prepares hydrogen storage material: ternary alloy step (1) melting obtained grinds to form powdered alloy except after descaling in glove box, is then placed on mechanical force and chemical in the ball grinder being filled with 2atm hydrogen and prepares target product: Mg-In-Ag ternary hydrogen storage material.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967590A (en) * | 2010-10-26 | 2011-02-09 | 华南理工大学 | Magnesium indium solid solution and preparation method thereof |
| CN103014384A (en) * | 2012-12-02 | 2013-04-03 | 安徽工业大学 | Method for preparing magnesium-silver hydrogen storage material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101967590A (en) * | 2010-10-26 | 2011-02-09 | 华南理工大学 | Magnesium indium solid solution and preparation method thereof |
| CN103014384A (en) * | 2012-12-02 | 2013-04-03 | 安徽工业大学 | Method for preparing magnesium-silver hydrogen storage material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105603278A (en) * | 2016-01-06 | 2016-05-25 | 华南理工大学 | Mg-Ag-Al ternary hydrogen storage alloy and preparation method thereof |
| CN105603278B (en) * | 2016-01-06 | 2017-06-20 | 华南理工大学 | A kind of Mg-Ag-Al ternarys hydrogen bearing alloy and preparation method thereof |
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