CN106191541B - A kind of hydrolytic hydrogen production aluminium alloy and preparation method thereof - Google Patents
A kind of hydrolytic hydrogen production aluminium alloy and preparation method thereof Download PDFInfo
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- CN106191541B CN106191541B CN201610564831.0A CN201610564831A CN106191541B CN 106191541 B CN106191541 B CN 106191541B CN 201610564831 A CN201610564831 A CN 201610564831A CN 106191541 B CN106191541 B CN 106191541B
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C21/00—Alloys based on aluminium
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- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
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Abstract
The present invention provides a kind of hydrolytic hydrogen production aluminium alloy and preparation method thereof.The present invention uses Mechanical Alloying, using the component including following mass content as raw material：Al 60~97wt%, Ga 0.5~10wt%, In0.5~10wt%, Sr 0.5~10wt%, SnCl21~10wt%, carry out ball milling and obtain the hydrolytic hydrogen production aluminium alloy with good hydrogen manufacturing performance.Test result indicates that, hydrolytic hydrogen production aluminium alloy prepared by preparation method provided by the invention can directly react after being contacted at normal temperatures with water, there is no Lag time, hydrogen output is up to 1210mL/g, hydrogen rate is produced up to 97.3%, real-time hydrogen manufacturing and real-time hydrogen supply can be reached, suitable for providing high-purity hydrogen source for hydrogen-oxygen fuel cell automobile.Preparation method cost provided by the invention is cheap, simple to operate, suitable for industrialized production.
Description
Technical field
The present invention relates to technical field of metal material, more particularly to a kind of hydrolytic hydrogen production aluminium alloy and preparation method thereof.
Background technology
The energy is important basic and guarantee, energy shortage and the environment that human society is depended on for existence and constantly advanced
Pollution turns into two hang-ups that have faced of contemporary mankind's social development, and world energy sources forms or with coal, oil, natural at this stage
Based on the great tradition energy of gas three.Because these fossil fuels are non-renewable, utilization clean energy resource is extremely urgent.Hydrogen Energy
Energy density is higher, and oxidation reaction product only has water, is a kind of more satisfactory fuel.Effective utilization of Hydrogen Energy can alleviate energy
Source crisis, reduce environmental pollution and promote regenerative resource and develop, be considered as 21 century most potential cleaning energy
Source.Therefore, the large-scale application of Hydrogen Energy meets the theory of " green " development, for global recycling economy and human society can
Sustainable development tool is of great significance.
At present, Hydrogen Energy industrialization is limited by three aspects such as hydrogen producing technology, hydrogen storage technology and fortune hydrogen technologies and is difficult to extensively
Implement.In terms of hydrogen manufacturing, mainly there are three kinds of water electrolysis hydrogen production, fossil fuel reformation hydrogen production and biological hydrogen production hydrogen production process at present, electricity
Solve that a kind of Technical comparing of water hydrogen manufacturing is ripe and one of widely used technology.Although the cost of the raw material needed for water electrolysis hydrogen production compared with
It is low, but water electrolysis hydrogen production needs to consume electric energy and energy consumption is larger, thus restrict its large-scale application；With fossil fuel reformation hydrogen production
Hydrogen production efficiency is not high, and produces CO therewith2、CO、SO2Environment is polluted Deng pernicious gas, does not meet the theory of Green Development.Storage
Aspect is deposited, not yet finds effective storing mode；It is such as low using storage Gaseous Hydrogen, bulky and energy density；Such as using storage
Liquified hydrogen is hidden, then requires ultralow temperature or super-pressure, storage tank manufacturing cost is high, and hydrogen container is heavy in itself, even if being filled in hydrogen container
Man Qing, storage hydrogen amount only account for the 5~7% of hydrogen container quality.In terms of hydrogen transport, although hydrogen has preferably potential transport
Defeated property, but it is easily leaked, and even if vacuum-packed fuel tank, daily slip is still up to 2%.Therefore, above mentioned problem is dissolved,
It is exactly to realize instant hydrogen manufacturing to realize one of approach that Hydrogen Energy effective and safe utilizes.
Energy-conservation and the focus that new-energy automobile is automobile industry development planning.The energy shape increasingly serious in face of global range
Gesture and environmental protection pressure, in recent years, World Main Auto production state all using development new-energy automobile as raising inter-industry competition ability,
Keep the vital measure of Sustainable Socioeconomic Development.2001, China formulated the science and technology of national energy-saving and new-energy automobile
Developing goal, plan are the time with 6~8 years, complete the industrialization of LEV.Hydrogen is to realize as the energy of automobile
One of China saves and the master of the science and technology object of new-energy automobile arranges, but before vehicle-mounted hydrogen production technology does not break through, vapour
Car only has the energy that could be using Hydrogen Energy as automobile using storage hydrogen, and uses storage hydrogen to increase automobile weight as energy source of car
Amount, is contradicted with current automotive light weight technology developing direction.Therefore, using relatively inexpensive controllable hydrogen manufacturing mode, hydrogen manufacturing at any time,
Use at any time, this is also to realize that hydrogen cell automobile extensive use has to solve the problems, such as.
Chinese patent CN102992263A discloses a kind of Al-Bi-NaCl- alkali metal or hydride hydrolytic hydrogen production composite wood
Material；CN102910582A discloses a kind of miniature hydrogen generating system and hydrogen production process based on aluminium alloy/borohydride hydrolytic reaction；
CN104190916A discloses a kind of oxidation resistant hydrolytic hydrogen production composite granule and preparation method thereof；CN103879959A is disclosed
A kind of aluminum-based composite hydrogen manufacturing material of high unit hydrogen output and its preparation and application；CN104401940A discloses a kind of aluminium and closed
The preparation method of gold/borohydride hydrogen making system；CN103861645A disclose a kind of aluminium/water react controllable catalyst for preparing hydrogen and
Its manufacture method.Although aluminium alloy hydrolytic hydrogen production technology, the hydrogen output and hydrogen-producing speed of alloy are utilized in the prior art
It is not high, it is difficult to meet the requirement of hydrogen cell automobile.
The content of the invention
It is an object of the invention to provide the high hydrolytic hydrogen production aluminium alloy of a kind of hydrogen output and hydrogen-producing speed and its preparation side
Method.
The invention provides a kind of preparation method of hydrolytic hydrogen production aluminium alloy, using the component including following mass content as original
Material：Al 60~97wt%, Ga 0.5~10wt%, In 0.5~10wt%, Sr 0.5~10wt%, SnCl21~
10wt%, carry out ball milling and obtain hydrolytic hydrogen production aluminium alloy.
Preferably, the raw material includes the component of following mass content：Al 70~93wt%, Ga 1~8wt%, In 1
~8wt%, Sr 1~8wt%, SnCl22~8wt%.
Preferably, the raw material includes the component of following mass content：Al 85~90wt%, Ga 2~5wt%, In 2
~5wt%, Sr 2~5wt%, SnCl23~5wt%.
Preferably, the Ga is liquid.
Preferably, the ball milling is carried out under inert gas shielding.
Preferably, the ratio of grinding media to material of the ball milling is 10~25:1.
Preferably, the time of the ball milling is 1~24h.
Preferably, the ball milling is carried out in ball mill, and the speed of mainshaft of the ball mill is 300~550r/min.
Present invention also offers a kind of hydrolytic hydrogen production aluminium alloy prepared according to above-mentioned technical proposal, the hydrolytic hydrogen production aluminium
The particle diameter of alloy is 100~200 μm.
The present invention uses Mechanical Alloying, using the component including following mass content as raw material：Al 60~
97wt%, Ga 0.5~10wt%, In 0.5~10wt%, Sr 0.5~10wt%, SnCl21~10wt%, carry out ball milling
Obtain hydrolytic hydrogen production aluminium alloy.In ma process, metal dust produced in the presence of mechanical force repeatedly plastic deformation,
Cold welding, broken etc., are mutually diffused generation solid-state reaction between atom, so that the powder surface of synthesis defect occurs, answered
Power increase, the increase of system free energy, and then improve the activity of aluminum-water reaction；Ga and In is low-melting-point metal, and Sr is active metal,
The fine and close oxide of aluminium surface is destroyed in mechanical milling process, improves the reactivity of aluminum-water reaction；In mechanical milling process, SnCl2Make
The agglomeration of aluminium powder is eliminated for grinding aid, and may be such that metallic aluminum surface produces substantial amounts of fresh surface and defect, is improved
The hydrolytic hydrogen production performance of material.Test result indicates that hydrolytic hydrogen production aluminium alloy prepared by preparation method provided by the invention is normal
Can directly it be reacted after being contacted under temperature with water, it is reachable up to 1210mL/g, production hydrogen rate without Lag time, hydrogen output
97.3%, real-time hydrogen manufacturing and real-time hydrogen supply can be reached, suitable for providing high-purity hydrogen source for hydrogen-oxygen fuel cell automobile.
Preparation method provided by the invention reduces the dosage of precious metal element, and cost is cheap, and technique is simple, suitable for work
Industry metaplasia is produced.
Embodiment
The invention provides a kind of preparation method of hydrolytic hydrogen production aluminium alloy, using the component including following mass content as original
Material：Al 60~97wt%, Ga 0.5~10wt%, In 0.5~10wt%, Sr 0.5~10wt%, SnCl21~
10wt%, carry out ball milling and obtain hydrolytic hydrogen production aluminium alloy.
In the present invention, the raw material includes Al, the preferably 70~93wt% that mass content is 60~97wt%, more excellent
Elect 85~90wt% as.In the present invention, the purity of the Al is preferably not lower than 99%.In the present invention, the Al is preferred
For Al powder；The Al powder is preferably dimensioned to be 100~200 mesh, more preferably 140~160 mesh.In the present invention, the Al warps
Generation hydrogen is reacted after activation with water.
In the present invention, the raw material includes Ga, the preferably 1~8wt% that mass content is 0.5~10wt%, more excellent
Elect 2~5wt% as.In the present invention, the purity of the Ga is preferably not lower than 99.9%.In the present invention, the Ga is preferred
For liquid.In the present invention, the Ga dissolves Al in mechanical milling process, and oxidation can not be formed by making to be dissolved into the Al surfaces in Ga
Film, improve the hydrolytic hydrogen production performance of aluminium alloy.
In the present invention, the raw material includes In, the preferably 1~8wt% that mass content is 0.5~10wt%, more excellent
Elect 2~5wt% as.In the present invention, the purity of the In is preferably not lower than 99.9%.In the present invention, the In is preferred
For In powder；The In powder is preferably dimensioned to be 100~200 mesh, more preferably 140~160 mesh.In the present invention, the In is
Low-melting-point metal, the fine and close oxide of aluminium surface is destroyed in mechanical milling process, improve the reactivity of aluminum-water reaction.
In the present invention, the raw material includes Sr, the preferably 1~8wt% that mass content is 0.5~10wt%, more excellent
Elect 2~5wt% as.In the present invention, the purity of the Sr is preferably not lower than 99.99%.In the present invention, the Sr is preferred
For Sr powder；The Sr powder is preferably dimensioned to be 100~200 mesh, more preferably 140~160 mesh.In the present invention, the Sr is
Active metal, the dense oxidation film of aluminium surface is changed into island shape in mechanical milling process, destroy the company of original dense oxidation film
Continuous property.
In the present invention, the raw material includes the SnCl that mass content is 1~10wt%2, preferably 2~8wt% is more excellent
Elect 3~5wt% as.In the present invention, the SnCl2Purity be preferably not lower than 99%.In the present invention, the SnCl2It is excellent
Elect powder as；The particle diameter of the powder is preferably 50~100 mesh.In the present invention, the SnCl2Aluminium powder is eliminated as grinding aid
Agglomeration, and may be such that metallic aluminum surface produces substantial amounts of fresh surface and defect, improve the hydrolytic hydrogen production of material
Energy.
The present invention carries out ball milling after raw material described in above-mentioned technical proposal is mixed, and obtains hydrolytic hydrogen production aluminium alloy.In this hair
In bright, the ball milling is preferably carried out under inert gas shielding.In the present invention, the ratio of grinding media to material of the ball milling be preferably 10~
25:1, more preferably 12~20:1, most preferably 14~16:1；The time of the ball milling is preferably 1~24h, more preferably 5~
20h, most preferably 10~15h.
In the present invention, the ball milling is carried out preferably in ball mill.In the present invention, the speed of mainshaft of the ball mill
Preferably 300~550r/min, more preferably 350~450r/min, most preferably 380~420r/min.
The present invention does not have special restriction to the species of the ball mill, using ball mill well known to those skilled in the art
.In the present invention, the ball mill is preferably one in planetary ball mill, stirring ball mill and vibrator
Kind, more preferably planetary ball mill.In an embodiment of the present invention, the ball mill can be specially the planetary balls of QM-3SP2
Grinding machine.
The present invention does not have special restriction to the ball grinder of the ball mill and the material of abrading-ball, using people in the art
The material of ball milling alloy known to member.In the present invention, the material of the ball grinder and abrading-ball is preferably all stainless steel, oxygen
Change aluminium ceramics or agate, more preferably aluminium oxide ceramics.
To prevent the hydrolytic hydrogen production aluminum alloy surface obtained after ball milling to be oxidized, the present invention is preferably after the completion of ball milling by institute
State the hydrolytic hydrogen production aluminium alloy that ball milling obtains and carry out vacuum or inert gas shielding.
Present invention also offers hydrolytic hydrogen production aluminium alloy prepared by preparation method described in a kind of above-mentioned technical proposal, the water
The particle diameter for solving hydrogen manufacturing aluminium alloy is 100~200 μm, preferably 120~150 μm.
In order to further illustrate the present invention, with reference to embodiment to hydrolytic hydrogen production aluminium alloy provided by the invention and its system
Preparation Method is described in detail, but they can not be interpreted as into limiting the scope of the present invention.
Embodiment 1:
Liquid Ga that the purity of Al powder, 2wt% using 89wt% 100 mesh purity as more than 99% is more than 99.9%,
Sr powder that In powder that 2wt% 100 mesh purity are more than 99.9%, 3wt% 100 mesh purity are more than 99.99%, 4wt%
Particle diameter be SnCl that 50 mesh purity are more than 99%2For raw material, raw material and abrading-ball are placed in the glove box full of argon gas
Sealed in ball grinder, ratio of grinding media to material 25:1, the material of ball grinder and abrading-ball is aluminium oxide ceramics, in the planetary balls of QM-3SP2
With 550r/min rotating speed ball milling 24h in grinding machine, the hydrolytic hydrogen production Al alloy powder that particle diameter is 200 μm is obtained.
Obtained hydrolytic hydrogen production Al alloy powder is mixed with 25 DEG C of water reaction is hydrolyzed, test hydrolytic hydrogen production performance.
The hydrolytic hydrogen production Al alloy powder occurs immediately upon vigorous reaction after being contacted with water, hydrolytic hydrogen production the performance test results are as shown in table 1.
Embodiment 2:
Liquid Ga that the purity of Al powder, 2wt% using 86wt% 150 mesh purity as more than 99% is more than 99.9%,
Sr powder that In powder that 3wt% 150 mesh purity are more than 99.9%, 4wt% 150 mesh purity are more than 99.99%, 5wt%
Particle diameter be SnCl that 100 mesh purity are more than 99%2For raw material, raw material and abrading-ball are placed in the glove box full of argon gas
Sealed in ball grinder, ratio of grinding media to material 15:1, the material of ball grinder and abrading-ball is aluminium oxide ceramics, in the planetary balls of QM-3SP2
With 500r/min rotating speed ball milling 20h in grinding machine, the hydrolytic hydrogen production Al alloy powder that particle diameter is 100 μm is obtained.
Obtained hydrolytic hydrogen production Al alloy powder is mixed with 25 DEG C of water reaction is hydrolyzed, test hydrolytic hydrogen production performance.
The hydrolytic hydrogen production Al alloy powder occurs immediately upon vigorous reaction after being contacted with water, hydrolytic hydrogen production the performance test results are as shown in table 1.
Embodiment 3:
Liquid Ga that the purity of Al powder, 3wt% using 88wt% 200 mesh purity as more than 99% is more than 99.9%,
Sr powder that In powder that 2wt% 200 mesh purity are more than 99.9%, 3wt% 200 mesh purity are more than 99.99%, 4wt%
Particle diameter be SnCl that 100 mesh purity are more than 99%2For raw material, raw material and abrading-ball are placed in the glove box full of argon gas
Sealed in ball grinder, ratio of grinding media to material 20:1, the material of ball grinder and abrading-ball is aluminium oxide ceramics, in the planetary balls of QM-3SP2
With 360r/min rotating speed ball milling 6h in grinding machine, the hydrolytic hydrogen production Al alloy powder that particle diameter is 150 μm is obtained.
Obtained hydrolytic hydrogen production Al alloy powder is mixed with 25 DEG C of water reaction is hydrolyzed, test hydrolytic hydrogen production performance.
The hydrolytic hydrogen production Al alloy powder occurs immediately upon vigorous reaction after being contacted with water, hydrolytic hydrogen production the performance test results are as shown in table 1.
Embodiment 4:
Liquid Ga that the purity of Al powder, 3wt% using 85wt% 180 mesh purity as more than 99% is more than 99.9%,
Sr powder that In powder that 3wt% 180 mesh purity are more than 99.9%, 4wt% 150 mesh purity are more than 99.99%, 5wt%
Particle diameter be SnCl that 50 mesh purity are more than 99%2For raw material, raw material and abrading-ball are placed in the glove box full of argon gas
Sealed in ball grinder, ratio of grinding media to material 10:1, the material of ball grinder and abrading-ball is aluminium oxide ceramics, in the planetary balls of QM-3SP2
With 400r/min rotating speed ball milling 2h in grinding machine, the hydrolytic hydrogen production Al alloy powder that particle diameter is 180 μm is obtained.
Obtained hydrolytic hydrogen production Al alloy powder is mixed with 25 DEG C of water reaction is hydrolyzed, test hydrolytic hydrogen production performance.
The hydrolytic hydrogen production Al alloy powder occurs immediately upon vigorous reaction after being contacted with water, hydrolytic hydrogen production the performance test results are as shown in table 1.
The hydrolytic hydrogen production aluminium alloy hydrogen manufacturing performance of the embodiment of the present invention of table 1
As can be seen from the above embodiments, hydrolytic hydrogen production aluminium alloy provided by the invention can immediate response in 25 DEG C of water
Hydrogen is produced, without Lag time, final hydrogen output is up to 1220mL/g, and final hydrogen rate of producing is up to 98.1%, Ke Yida
To real-time hydrogen manufacturing and real-time hydrogen supply.
Described above is only the preferred embodiment of the present invention, not makees any formal limitation to the present invention.Should
Point out, for those skilled in the art, under the premise without departing from the principles of the invention, if can also make
Dry improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (9)
- A kind of 1. preparation method of hydrolytic hydrogen production aluminium alloy, using the component of following mass content as raw material：60~97wt% of Al, Ga 0.5~10wt%, In 0.5~10wt%, Sr 0.5~10wt%, SnCl21~10wt%, carry out ball milling and hydrolyzed Hydrogen manufacturing aluminium alloy.
- 2. preparation method according to claim 1, it is characterised in that the raw material is the component of following mass content：Al 70~93wt%, Ga 1~8wt%, In 1~8wt%, Sr 1~8wt%, SnCl22~8wt%.
- 3. preparation method according to claim 2, it is characterised in that the raw material is the component of following mass content：Al 85~90wt%, Ga 2~5wt%, In 2~5wt%, Sr 2~5wt%, SnCl23~5wt%.
- 4. according to the preparation method described in claims 1 to 3 any one, it is characterised in that the Ga is liquid.
- 5. preparation method according to claim 1, it is characterised in that the ball milling is carried out under inert gas shielding.
- 6. preparation method according to claim 5, it is characterised in that the ratio of grinding media to material of the ball milling is 10~25:1.
- 7. the preparation method according to claim 5 or 6, it is characterised in that the time of the ball milling is 1~24h.
- 8. preparation method according to claim 7, it is characterised in that the ball milling is carried out in ball mill, the ball milling The speed of mainshaft of machine is 300~550r/min.
- 9. in a kind of claim 1~8 described in any one preparation method prepare hydrolytic hydrogen production aluminium alloy, particle diameter be 100~ 200μm。
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| CN111807322B (en) * | 2019-04-10 | 2022-06-10 | 吉林省氢汇新能源有限公司 | Method for preparing hydrogen and coproducing pseudo-boehmite and/or aluminum oxide by aluminum water reaction |
| CN110155943B (en) * | 2019-05-13 | 2020-09-08 | 湖北工业大学 | Ultrahigh-activity hydrolysis hydrogen production aluminum-based composite material and preparation method thereof |
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| CN101358310A (en) * | 2008-09-23 | 2009-02-04 | 河南四方超硬材料有限公司 | Hydrogen making Al base alloy composite materials, preparation and process of using thereof |
| CN102011030A (en) * | 2010-09-27 | 2011-04-13 | 中国计量学院 | Design of aluminum component for preparing hydrogen and preparation method thereof |
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| CN101358310A (en) * | 2008-09-23 | 2009-02-04 | 河南四方超硬材料有限公司 | Hydrogen making Al base alloy composite materials, preparation and process of using thereof |
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| CN102409202A (en) * | 2011-11-16 | 2012-04-11 | 湖北工业大学 | Al-Ga-In-Sn-Zn alloy as well as preparation method and application thereof |
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