CN101671788A - Method for nanocrystallization of magnesium-based hydrogen storage material - Google Patents
Method for nanocrystallization of magnesium-based hydrogen storage material Download PDFInfo
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- CN101671788A CN101671788A CN200810149139A CN200810149139A CN101671788A CN 101671788 A CN101671788 A CN 101671788A CN 200810149139 A CN200810149139 A CN 200810149139A CN 200810149139 A CN200810149139 A CN 200810149139A CN 101671788 A CN101671788 A CN 101671788A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention relates to a method for the nanocrystallization of a magnesium-based hydrogen storage material, which utilizes a nanocrystallization process for a nano-carbon material to prepare the magnesium-based hydrogen storage material to form monocrystal or polycrystal nano-particles so as to improve a specific surface area greatly and increase diffusion channels of hydrogen atoms in the hydrogen storage material. Therefore, the method can improve the effective hydrogen capacity of the hydrogen storage material, accelerate the hydrogen absorption and desorption of the hydrogen storage material, and reduce the temperature of the hydrogen absorption and desorption of the hydrogen storage material.
Description
Technical field
The invention relates to a kind of magnesium-base hydrogen storage material, more especially in regard to the method for nanometer magnesio compound.
Background technology
In the research of hydrogen storage material, for improving effective hydrogen-storage amount, acceleration suction hydrogen discharging rate, reaching to reduce and inhale hydrogen discharging temperature, material nanoization (nanotization) is the recent studies on direction.The material that present mechanically nanometer is ductile such as the high hardness material of magnesio compound or interpolation have its difficulty, reason is that the abrading-ball size is not a nanoscale and excessive with the relative dimension of abrasive substance, therefore is difficult to apply nano level stress in above-mentioned materials.For ductile material, though ball milling can destroy material, the material after destroying is easy to recrystallize into more large size, therefore can't effectively its crystalline size be contracted to nano level.For avoiding the recrystallize phenomenon, known method is a ductility of utilizing liquid nitrogen reduction ductile material such as al-based compound, but above-mentioned cryogrinding technology will increase cost.
In sum, still need new Ginding process to form the nano level hydrogen storage material at present.
Summary of the invention
The object of the present invention is to provide a kind of method for nanocrystallization of magnesium-based hydrogen storage material, form the nano level hydrogen storage material to adopt Ginding process.
For achieving the above object, method for nanocrystallization of magnesium-based hydrogen storage material provided by the invention comprises magnesio compound and nano carbon material is enclosed mixed grinding down in blunt atmosphere, forms the nano level magnesium-base hydrogen storage material; Wherein the size of this nano level magnesium-base hydrogen storage material is less than 100 nanometers.
Description of drawings
Fig. 1 is the storage hydrogen speed comparison diagram of embodiment 1 and comparing embodiment 1 among the present invention.
Embodiment
Method for nanocrystallization of magnesium-based hydrogen storage material provided by the invention comprises magnesio compound and nano carbon material is enclosed mixed grinding down in blunt atmosphere, forms the nano level magnesium-base hydrogen storage material.The nano level magnesium-base hydrogen storage material is defined as size less than 100 nanometers.
Above-mentioned magnesio compound is that magnesium or magnesium are main alloy such as Mg
1-xA
x, A is Li, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Al, Y, Zr, Nb, Mo, In, Sn, O, Si, B, C, F or Be, and 0＜x≤0.3.
Suitable nano carbon material can be carbon nanotube, carbon nano-powder or above-mentioned mixture.Carbon nanotube can be the single or multiple lift carbon nanotube, and its caliber is approximately between 12 to 15nm.In an embodiment of the present invention, carbon nanotube is available from aldrich.The particle diameter of carbon nano-powder is approximately between between the 10nm to 30nm.In an embodiment of the present invention, the carbon nano-powder is available from aldrich.
In an embodiment of the present invention, the weight ratio of magnesio compound and nano carbon material is between 100: 0.5 to 100: 1.Too much magnesio compound can cause hydrogen storage material to inhale rising of hydrogen temperature and the excessive phenomenon of grain boundary size, and too much nano carbon material can cause the decline of inhaling the hydrogen weight ratio.
Above-mentioned magnesio compound with after nano carbon material mixes, is carried out ball milling under rare gas element such as nitrogen, argon gas.The grinding bead of ball-milling technology is diameter 8～10mm wolfram steel ball, and temperature is between 27 to 40 ℃, and pressure is between 1.0 to 2.0atm, and the time is between 6 to 12 hours.When milling time during, will cause excessive grain to grow up, but during less than 6 hours, crystal grain can't be ground to nano level greater than 12 hours.
Behind above-mentioned grinding technics, promptly form so-called nano level magnesium-base hydrogen storage material.Since the present invention with littler, harder, and higher inflexible carbon nanotube as slurry, grinding bead can concentrate on nanoscale with grinding stress.High internal stress can make surface of fracture extend to magnesio compound inside rapidly, it is destroyed to nano-scale, and introduce a large amount of crystals stress and high angle crystal boundary at material internal.Thus, the structure of nano level magnesium-base hydrogen storage material has a lot of grain boundary defects, can be used as the rapid passage of hydrogen atom diffusion, helps hydrogen storage material to store fast or the release hydrogen atom.In application facet, can make effective hydrogen-storage amount approximation theory maximum storage hydrogen quantity, quicken to inhale hydrogen discharging rate, and reduce and inhale hydrogen discharging temperature.In an embodiment of the present invention, the suction hydrogen discharging rate of nano level magnesium-base hydrogen storage material between 150 ℃ to 300 ℃ is greater than 0.0073L/s.In another embodiment of the present invention, the nano level magnesium-base hydrogen storage material at the suction hydrogen discharging rate of room temperature (25 ℃) between between the 0.0051L/s to 0.0073L/s.
In another embodiment of the present invention, the high hardness material that can add high strength and non-ductility is to above-mentioned grinding technics.Grinding order is also unrestricted, can grind the mixture of high hardness material and nano carbon material earlier after, add magnesio compound again and grind.After also can grinding the mixture of magnesio compound and carbon nanometer material earlier, add high hardness material again and grind.Also can grind simultaneously magnesio compound, high hardness material, with the mixture of nano carbon material.After grinding, to less than 100nm, and the high hardness material of nanometer can be dispersed in the nano level magnesium-base hydrogen storage material size of high hardness material with nanometer.The purpose that imports high hardness material is to increase the physical strength of hydrogen storage material.High hardness material can be V, Ti, Fe, Co, Nb, Ca, Cs, Mn, Ni, Ca, Ce, Y, La, Pd, Hf, K, Rb, Rh, Ru, Zr, Be, Cr, Ge, Si or Li, or above-mentioned two or more mixture arbitrarily, or above-mentioned two or more alloy arbitrarily.When above-mentioned high hardness material was iron, titanium or nickel, the effect that can further have catalyzer was quickened hydrogen molecule is changed into hydrogen atom and stores hydrogen atom fast.The weight ratio of magnesio compound and high hardness material is between 100: 5 to 100: 30, if surpass this ratio, then too much high hardness material will reduce the performance of hydrogen storage material.
For making the clear more feature of the present invention of those skilled in the art, be schematically illustrated in following embodiment.
Embodiment 1
Get the magnesium (big this enterprise stock company limited) of 0.7g, the FeTi of 0.3g (rise U.S.A and reach international exploitation limited-liability company), and the carbon nanotube (aldrich) of 0.01g under argon gas, carry out ball-milling technology.The grinding bead of ball-milling technology is a wolfram steel, and temperature is 27, and pressure is 1atm, and the time is 6 hours.By XRD diffraction result and transmission electron microscope image analysis as can be known, the Mg behind the ball milling and average crystalline less than 100nm.On the other hand, its storage hydrogen speed of measuring stress, density of hydrogen and temperature coaptations such as (Pressure-Concentration-Temperature), the result is as shown in Figure 1.
Comparing embodiment 1
Roughly the same with embodiment 1, unique difference is not add carbon nanotube as slurry.By XRD diffraction result and transmission electron microscope image analysis as can be known, the average crystalline of the Mg behind the ball milling is less than 100nm.On the other hand, its storage hydrogen speed of measuring stress, density of hydrogen and temperature coaptations such as (Pressure-Concentration-Temperature), the result is as shown in Figure 1.
More as can be known, the formed hydrogen storage material of nanometer technology (embodiment 1) that adds carbon nanotube is arranged by the storage hydrogen speed ratio of Fig. 1, obviously be better than not adding the formed hydrogen storage material of nanometer technology (comparing embodiment 1) of carbon nanotube.
Though the present invention describes as above with several embodiment; right its is not in order to limit the present invention; those skilled in the art without departing from the spirit and scope of the present invention; when can changing arbitrarily and retouching, so protection scope of the present invention should be as the criterion with the claim scope content that be defined of application.
Claims (11)
1, a kind of method for nanocrystallization of magnesium-based hydrogen storage material comprises:
One magnesio compound and a nano carbon material are enclosed mixed grinding down in a blunt atmosphere, form a nano level magnesium-base hydrogen storage material;
Wherein the size of this nano level magnesium-base hydrogen storage material is less than 100 nanometers.
2, method for nanocrystallization of magnesium-based hydrogen storage material as claimed in claim 1, wherein, this magnesio compound comprises that magnesium or magnesium are main alloy.
3, method for nanocrystallization of magnesium-based hydrogen storage material as claimed in claim 1, wherein, this nano carbon material comprises carbon nanotube, carbon nano-powder or aforesaid combination.
4, method for nanocrystallization of magnesium-based hydrogen storage material as claimed in claim 1, wherein, this blunt atmosphere is enclosed and is comprised nitrogen or argon gas.
5, method for nanocrystallization of magnesium-based hydrogen storage material as claimed in claim 1, wherein, the weight ratio of this magnesio compound and this nano carbon material is between 100: 0.5 to 100: 1.
6, method for nanocrystallization of magnesium-based hydrogen storage material as claimed in claim 1, wherein, the time of this mixed grinding, temperature was between 27 to 40 ℃, and pressure is between between the 1atm to 2atm between 6 hours to 12 hours.
7, method for nanocrystallization of magnesium-based hydrogen storage material as claimed in claim 1, wherein, this nano level magnesium-base hydrogen storage material is between 100 ℃ to 200 ℃, and it inhales hydrogen discharging rate greater than 0.0073L/s.
8, method for nanocrystallization of magnesium-based hydrogen storage material as claimed in claim 1, wherein, the suction hydrogen discharging rate of this nano level magnesium-base hydrogen storage material under room temperature is between between the 0.0051L/s to 0.0073L/s.
9, method for nanocrystallization of magnesium-based hydrogen storage material as claimed in claim 1, wherein, comprise that adding another high hardness material carries out mixed grinding, form a nano level high hardness material and this nano level magnesium-base hydrogen storage material uniform mixing, and the size of this nano level high hardness material is less than 100nm.
10, method for nanocrystallization of magnesium-based hydrogen storage material as claimed in claim 9, wherein, this high hardness material is V, Ti, Fe, Co, Nb, Ca, Cs, Mn, Ni, Ca, Ce, Y, La, Pd, Hf, K, Rb, Rh, Ru, Zr, Be, Cr, Ge, Si or Li, or above-mentioned two or more mixture arbitrarily, or any two or more alloy.
11, method for nanocrystallization of magnesium-based hydrogen storage material as claimed in claim 9, wherein, the weight ratio of this magnesio compound and this high hardness material is between 100: 5 to 100: 30.
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| CN105132768A (en) * | 2015-08-21 | 2015-12-09 | 苏州莱特复合材料有限公司 | Anti-impact titanium magnesium alloy material and preparing method thereof |
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Inventor after: Yan Peishan Inventor after: Huang Junru Inventor after: Gu Jieren Inventor after: Chen Binhao Inventor after: Zheng Mingshan Inventor after: Cao Fanghai Inventor after: Luo Shengquan Inventor after: Chen Du Inventor before: Yan Peishan Inventor before: Huang Junru Inventor before: Gu Jieren Inventor before: Chen Binhao Inventor before: Zheng Mingshan Inventor before: Cao Fanghai |
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Free format text: CORRECT: INVENTOR; FROM: YAN PEISHAN HUANG JUNRU GU JIEREN CHEN BINHAO ZHENG MINGSHAN CAO FANGHAI TO: YAN PEISHAN HUANG JUNRU GU JIEREN CHEN BINHAO ZHENG MINGSHAN CAO FANGHAI LUO SHENGQUAN CHEN DOU |