CN100358624C - A nano-magnesium/graphite composite hydrogen storage material and its preparation method - Google Patents
A nano-magnesium/graphite composite hydrogen storage material and its preparation method Download PDFInfo
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- CN100358624C CN100358624C CNB2003101191775A CN200310119177A CN100358624C CN 100358624 C CN100358624 C CN 100358624C CN B2003101191775 A CNB2003101191775 A CN B2003101191775A CN 200310119177 A CN200310119177 A CN 200310119177A CN 100358624 C CN100358624 C CN 100358624C
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- magnesium
- hydrogen
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- hydrogen storage
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 102
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 102
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 71
- 239000010439 graphite Substances 0.000 title claims abstract description 71
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000011777 magnesium Substances 0.000 title claims abstract description 58
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 47
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 239000011232 storage material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000000498 ball milling Methods 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 14
- 238000011049 filling Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 239000000314 lubricant Substances 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 claims 1
- 239000012071 phase Substances 0.000 claims 1
- 238000003860 storage Methods 0.000 abstract description 8
- 239000012298 atmosphere Substances 0.000 abstract description 3
- 238000000713 high-energy ball milling Methods 0.000 abstract 1
- 238000000227 grinding Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 10
- 230000005540 biological transmission Effects 0.000 description 8
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000000446 fuel Substances 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 229910000861 Mg alloy Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- -1 graphite modified hydrogen Chemical class 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003534 oscillatory effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- Hydrogen, Water And Hydrids (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Fuel Cell (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention discloses magnesium / graphite composite hydrogen storage material and a preparation method thereof. The preparation method of the present invention comprises: crystalline graphite and magnesium powder are mixed, and prepared into the nanometer magnesium / graphite composite hydrogen storage material by using the reaction ball milling method (namely in a high energy ball milling mode in the high pure hydrogen atmosphere); the graphite is used as not only the catalyzing phase but also the lubricator; the content of the graphite is 5 to 30 mass%, preferably 8 to 12 mass%; the ball milling time is 15 minutes to 5 hours, preferably 25 to 35 minutes. The present invention has the advantage that the high hydrogen storage capacity of magnesium can be maintained and the dynamic properties of suction and release of hydrogen are greatly improved simultaneously after the crystalline graphite and the magnesium powder are treated in a ball milling mode in a short time.
Description
Technical field
The present invention relates to hydrogen storage material, specifically a kind of nanometer Mg/graphite composite hydrogen storage material and preparation method.
Background technology
A large amount of pollution and human energy crises that face of using fuel-engined vehicle to cause make national governments all put into effect the law and the regulation of a series of restricting vehicle exhaust emissions, and the fuel cell electric vehicle (FCEV) that many automakers also begin positive development " zero-emission " replaces traditional internal-combustion engines vehicle.Wherein clean, proton membrane fuel battery (PEMFC) automobile is acknowledged as the optimal selection that replaces the traditional combustion engine automobile efficiently.The numerous and confused R and D of supporting it of each main motor corporation of the world, the U.S. also will develop the PEMFC automobile as the strategic measure that reduces energy resource consumption and control environment and pollute.At present, Europe, the United States, add, day etc. state develop the sample car of PEMFC bus, car and minibus in succession.But how safely, easily PEMFC because the pure hydrogen of use is made fuel, so carry the key that the high density hydrogen source that can use just becomes the automobile-used PEMFC of development under temperate condition.And hydrogen storage material has characteristics such as capacity height, life-span be long, safe in utilization, is the main candidate material of on-board hydrogen source always.Estimate that according to relevant technologies tissue and department for the PEMFC automobile of a standard, travelling needs the hydrogen storage content of 5～6mass% about 500 kilometers.Mg and Mg based hydrogen storage material hydrogen storage content big (7.6mass%), volume ratio density height (134kgm
-3(H
2)), and cheap, promise to be following fuel cell hydrogen storage material.But suction hydrogen discharging rate that it is low excessively and too high operating temperature (～400 degree) have seriously restricted its practical application exploitation.In recent years, there are the various means of human that magnesium and magnesium alloy are carried out the modification processing to improve its dynamic performance.Wherein under reaction atmosphere ball milling (RBM) be promote magnesium and magnesium alloy solid-a kind of effective way of solid/liquid/gas reactions.In the RBM method, can be under nitrogen atmosphere directly ball-milling magnesium and magnesium alloy, also can be with it with the additive ball milling.Additive is divided three classes, and a class is as catalyst, and the effect that hydrogen is had catalytic decomposition is as Co, Ni etc.; Another kind of is as " hydrogen pump ", promptly at room temperature inhales the hydrogen storage material of putting hydrogen easily, as YNi, and Ce etc.; Also having a class is as grinding agent, can improve grinding efficiency, and effective refinement particle and crystal grain are as metal oxide Cr
2O
3, CeO
2Deng.Yet, adopt crystalline graphite under nitrogen atmosphere, to prepare magnesium at present or the magnesium alloy composite hydrogen storage material does not also appear in the newspapers as yet as additive.
The invention technology
The object of the present invention is to provide a kind of nanometer Mg/graphite composite hydrogen storage material and preparation method, after adopting the present invention to nanometer Mg/graphite composite hydrogen storage material process ball milling of short time, can be in the high hydrogen storage capability that keeps magnesium, improve its dynamic performance greatly, the practicability of on-vehicle fuel provides the candidate material of hydrogen source for future.
To achieve these goals, technical solution of the present invention is as follows:
Nanometer Mg/graphite composite hydrogen storage material: this composite hydrogen storage material is made up of magnesium and graphite, and the crystallite dimension of magnesium is 70nm～100nm, and the crystallite dimension of graphite is 7nm～16nm, and the content of graphite is 5～30mass%; The content of wherein said graphite is good with 8～12%.
The reaction ball milling method is adopted in its preparation, be specially: (purity is more than or equal to 99.0% with the Mg powder, granularity is 100 orders) and graphite (purity is more than or equal to 99.85%, and granularity is 450 orders) pack in the Spex8000 oscillatory type high energy ball mill in the ratio of 5～30mass%, ratio of grinding media to material is 10～50: 1; Vacuumize (1Pa～10 at ball grinder through 2～4 times
-2Pa), fill hydrogen operation after, charge into 0.2MPa～3MPa high-purity hydrogen and carry out ball milling to graphite and be evenly distributed on magnesium surface; The ball milling time is 15 minutes～5 hours, is good with 25～35 minutes.In preparation process, can monitor the ball grinder internal pressure in real time by pressure transmitter.
The principle of the invention is: because the structure of crystalline graphite can be held the hydrogen of physical absorption, graphite also is a kind of excellent lubrication agent simultaneously, can play the high-efficient grinding effect in mechanical milling process.Confirm that through ESEM, transmission electron microscope observing the crystallite dimension of magnesium can be 70～100nm in nanometer Mg of the present invention/graphite composite hydrogen storage material, the graphite that crystallite dimension can be 7～16nm is evenly distributed on magnesium surface.
The present invention has the following advantages:
1. preparation technology is simple, and preparation time is short, carries out in-situ activation in material preparation, for the on-vehicle fuel hydrogen source that develops high-energy-density provides an effective way.
2. composite of the present invention has good hydrogen storage property, in the high hydrogen storage capability that keeps Mg, improves its dynamic performance greatly.0.5 hour magnesium of ball milling/graphite composite material hydrogen sucking function is also better than 15 hours pure magnesium of ball milling under the same terms.
Description of drawings
Fig. 1 a is the SEM pattern picture of the composite of 10mass% for the graphite addition;
Fig. 1 b is the graphite composition energy spectrum analysis of elliptic region among Fig. 1 a;
Fig. 1 c is the TEM dark field image of graphite in the composite of 10mass% for the graphite addition;
Fig. 1 d is the TEM dark field image of magnesium in the composite of 10mass% for the graphite addition;
Fig. 2 is the suction hydrogen kinetic curve in the embodiment of the invention 1;
Fig. 3 is the suction hydrogen kinetic curve in the embodiment of the invention 2;
Fig. 4 is the suction hydrogen kinetic curve in the embodiment of the invention 3;
Fig. 5 is the suction hydrogen kinetic curve in the embodiment of the invention 4;
Fig. 6 is the suction hydrogen kinetic curve in the embodiment of the invention 5;
Fig. 7 is the suction hydrogen kinetic curve in the comparative example 1;
Fig. 8 is the activation kinetics curve in the comparative example 2.
The specific embodiment
Embodiment 1
The graphite addition is the composite of 10mass%, and the ball milling time is 0.5 hour, and ratio of grinding media to material is 30: 1; At ball grinder through vacuumizing (1Pa) 3 times, filling under the hydrogen (0.2MPa high-purity hydrogen) and carry out ball milling to graphite and be evenly distributed on magnesium surface.Described Mg powder purity is more than or equal to 99.0%, and granularity is 100 orders, and described graphite purity is more than or equal to 99.85%, and granularity is 450 orders.
At 573K, inhale hydrogen under the 1.2Mpa and test, the result shows, inhaled the hydrogen mark and reach (establishing suction hydrogen mark is, the mass percent of hydrogen is 7.6mass%, down together) more than 0.90 at 1 o'clock in 8 minutes, inhales the hydrogen mark in 30 minutes and reaches more than 0.999.Present embodiment SEM photo and TEM photo are referring to Fig. 1 a, Fig. 1 b, Fig. 1 c, Fig. 1 d, and as can be seen, after 0.5 hour, graphite has been evenly distributed on the surface of magnesium in the composite through ball milling from Fig. 1 b.And from Fig. 1 c and Fig. 1 d as can be seen, the crystallite dimension of magnesium is 100nm in this composite, the average grain size 10nm of graphite.Present embodiment is inhaled the hydrogen desorption kinetics curve and is seen Fig. 2.
Embodiment 2
Difference from Example 1 is: the ball milling time is 1 hour, and ratio of grinding media to material is 10: 1; Vacuumize (10 at ball grinder through 2 times
-1Pa), filling the 3MPa high-purity hydrogen carries out ball milling to graphite and is evenly distributed on magnesium surface.Confirm that through ESEM, transmission electron microscope observing the crystallite dimension of magnesium is 100nm, the average grain size of graphite is 9nm.
At 573K, inhale the hydrogen test under the 1.2Mpa.The result shows, inhaled the hydrogen mark and reach more than 0.81 in 30 minutes.Inhale the hydrogen kinetic curve and see Fig. 3.
Difference from Example 1 is: the ball milling time is 5 hours, and ratio of grinding media to material is 40: 1; Vacuumize (10 at ball grinder through 4 times
-2Pa), filling the 2MPa high-purity hydrogen carries out ball milling to graphite and is evenly distributed on magnesium surface.Confirm that through ESEM, transmission electron microscope observing the average grain size of magnesium is 80nm, the average grain size of graphite is 8nm.
At 573K, inhale the hydrogen test under the 1.2Mpa.The result shows, inhaled the hydrogen mark and reach more than 0.83 in 25 minutes.Inhale the hydrogen kinetic curve and see Fig. 4.
Embodiment 4
Difference from Example 1 is: the ball milling time is 0.5 hour, and the graphite addition is the composite of 20mass%, and ratio of grinding media to material is 50: 1; Vacuumize (1Pa) at ball grinder through 3 times, charge into the 1MPa high-purity hydrogen and carry out ball milling to graphite and be evenly distributed on magnesium surface.Confirm that through ESEM, transmission electron microscope observing the average grain size of magnesium is 90nm, the average grain size of graphite is 10nm.
At 573K, inhale the hydrogen test under the 1.2Mpa.The result shows, inhaled the hydrogen mark and reach more than 0.81 in 8 minutes, inhales the hydrogen mark in 30 minutes and reaches more than 0.95.Inhale the hydrogen kinetic curve and see Fig. 5.
Embodiment 5
Difference from Example 1 is: the ball milling time is 0.5 hour, and the graphite addition is the composite of 30mass%, and ratio of grinding media to material is 20: 1; Vacuumize (10 at ball grinder through 3 times
-1Pa), charging into the 0.5MPa high-purity hydrogen carries out ball milling to graphite and is evenly distributed on magnesium surface.Confirm that through ESEM, transmission electron microscope observing the average grain size of magnesium is 95nm, the average grain size of graphite is 10nm.
At 573K, inhale the hydrogen test under the 1.2Mpa.The result shows, inhaled the hydrogen mark and reach more than 0.66 in 8 minutes, inhales the hydrogen mark in 30 minutes and reaches more than 0.94.Inhale the hydrogen kinetic curve and see Fig. 6.
Embodiment 6
Difference from Example 1 is: the ball milling time is 25 minutes, and the graphite addition is the composite of 12mass%.Ratio of grinding media to material is 20: 1; Vacuumize (10 at ball grinder through 3 times
-2Pa), charging into the 0.2MPa high-purity hydrogen carries out ball milling to graphite and is evenly distributed on magnesium surface.Confirm that through ESEM, transmission electron microscope observing the crystallite dimension of magnesium is 100nm, the average grain size of graphite is 11nm.
At 573K, inhale the hydrogen test under the 1.2Mpa.The result shows, inhaled the hydrogen mark and reach more than 0.89 in 8 minutes, inhales the hydrogen mark in 30 minutes and reaches more than 0.98.
Embodiment 7
Difference from Example 1 is: the ball milling time is 35 minutes, and the graphite addition is the composite of 8mass%.Ratio of grinding media to material is 20: 1; Vacuumize (10 at ball grinder through 3 times
-2Pa), charging into the 0.2MPa high-purity hydrogen carries out ball milling to graphite and is evenly distributed on magnesium surface.Confirm that through ESEM, transmission electron microscope observing the average grain size of magnesium is 95nm, the average grain size of graphite is 10nm.
At 573K, inhale the hydrogen test under the 1.2Mpa.The result shows, inhaled the hydrogen mark and reach more than 0.88 in 8 minutes, inhales the hydrogen mark in 30 minutes and reaches more than 0.96.
Embodiment 8
Difference from Example 1 is: the ball milling time is 15 minutes, and the graphite addition is the composite of 5mass%.Ratio of grinding media to material is 20: 1; Vacuumize (10 at ball grinder through 3 times
-2Pa), charging into the 0.2MPa high-purity hydrogen carries out ball milling to graphite and is evenly distributed on magnesium surface.Confirm that through ESEM, transmission electron microscope observing the crystallite dimension of magnesium is 100nm, the average grain size of graphite is 15nm.
At 573K, inhale the hydrogen test under the 1.2Mpa.The result shows, inhaled the hydrogen mark and reach more than 0.76 in 8 minutes, inhales the hydrogen mark in 30 minutes and reaches more than 0.80.
Comparative example 1
Fig. 7 has provided in nitrogen atmosphere 15 hours pure magnesium of ball milling at 573K, inhales the kinetic curve of hydrogen test under the 1.2Mpa.Test result shows that suction hydrogen mark was lower than 0.72 in 30 minutes, was significantly less than the performance of the composite hydrogen storage material among the present invention.
Comparative example 2
Fig. 8 provided in hydrogen ball milling 0.5 hour, and the graphite addition is the composite activity function curve of 10mass%.As seen from the figure, just reach best, remain unchanged substantially through repeatedly inhaling the hydrogen storage property of putting the sample after hydrogen circulates through once inhaling the hydrogen storage property of putting hydrogen circulation sample.And in the present invention, the addition of graphite is that the composite activity function of 10mass% is than [S.Bouaricha such as S.Bouaricha, J.P.Dodelet, D.Guay, J.Huot, S.Boily, R.Schulz, Activationcharacteristics of graphite modified hydrogen absorbing materials, J.AlloysComp., 325 (2000) 245-251] activity function of the magnesium/graphite composite material of the same composition of preparation is significantly increased under argon atmospher, when other ball milling condition is identical.The graphite addition of ball milling preparation in argon gas such as S.Bouaricha be 10mass% composite inhale for the first time in the hydrogen process (T=300 ℃, P
H2=10bar), hydrogen reach 4,5 and time of 6mass% be respectively 0.73,1.97 and 10.5 hour; And the composite of the identical component that ball milling prepares in hydrogen in this experiment is being inhaled in the hydrogen process for the first time, and under the essentially identical condition of pressure and temperature (T=300 ℃, P
H2=1.2Mpa), hydrogen reach 4,5 and time of 6mass% be respectively 0.061h, 0.097h and 0.176h.This shows, be far superior to the performance of the same material of ball milling preparation under inert atmosphere with the composite activity function of the preparation of the reaction ball milling method under the hydrogen.
Claims (5)
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| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI400340B (en) * | 2008-08-25 | 2013-07-01 | Ind Tech Res Inst | Nanotization of magnesium-based hydrogen storage material |
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| CN109175349B (en) * | 2018-10-15 | 2020-10-09 | 微山钢研稀土材料有限公司 | High-performance double-rare-earth solid solution-based hydrogen storage material and preparation method thereof |
| CN112357916B (en) * | 2020-12-11 | 2022-09-06 | 安徽工业大学 | A method for improving the capacity of graphite electrode material |
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| US20020141939A1 (en) * | 2000-11-07 | 2002-10-03 | Hydro-Quebec | Method for rapidly carrying out hydrogenation of a hydrogen storage material |
| JP2003054901A (en) * | 2001-08-13 | 2003-02-26 | Sony Corp | Core-shell carbon nanofiber for hydrogen storage and process for preparing the fiber |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5541017A (en) * | 1994-01-28 | 1996-07-30 | Hong; Kuochih | Method for making high capacity rechargeable hydride batteries |
| US20020141939A1 (en) * | 2000-11-07 | 2002-10-03 | Hydro-Quebec | Method for rapidly carrying out hydrogenation of a hydrogen storage material |
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| Hydriding/dehydriging Properties of Advanced HydrogenStorage Mg /MWNTs Composites. CHEN，Dong.中山大学学报（自然科学版），第42卷. 2003 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI400340B (en) * | 2008-08-25 | 2013-07-01 | Ind Tech Res Inst | Nanotization of magnesium-based hydrogen storage material |
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