CN101117211A - Magnesium hydride nano particle and preparation method and application thereof - Google Patents
Magnesium hydride nano particle and preparation method and application thereof Download PDFInfo
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- CN101117211A CN101117211A CNA2006100891317A CN200610089131A CN101117211A CN 101117211 A CN101117211 A CN 101117211A CN A2006100891317 A CNA2006100891317 A CN A2006100891317A CN 200610089131 A CN200610089131 A CN 200610089131A CN 101117211 A CN101117211 A CN 101117211A
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Abstract
The invention discloses a magnesium hydride nanometer granular material and the preparing method and application, wherein nanometer magnesium powder is prepared through adopting arc heating method and then the magnesium powder is hydrogenated to obtain MgH2 granular product with the grain diameter being 50 nm to 600 nm. The nanometer MgH2 grain possesses high purity and outstanding kinetics property of hydrogen absorption and desorption during being used as hydrogen storage material, thereby possessing extremely important application value and extensive application potential in the hydrogen storage technical field.
Description
Technical field
The present invention relates to the preparation field of metal hydride and magnesium hydride and synthetic method and the application that hydrogen storage technology field, especially granular size are Nano grade.
Background technology
At present, develop the topic that the new energy has become whole world close attention because traditional energy such as coal, oil, Sweet natural gas etc. are exhausted day by day and human that environmental issue is more and more paid attention to.Wherein hydrogen energy source is because the characteristic of its specific mass energy content height and cleanliness without any pollution is to be hopeful one of energy of being used widely in 21 century most.But the utilization of hydrogen energy source relates to and stores this committed step, and therefore how storing hydrogen safely and effectively becomes the problem that needs to be resolved hurrily.The research of hydrogen storage material at present mainly contains systems such as metal hydride, carbon material and alanate, but for the consideration of performance and economic dispatch each side factor, commercial used maximum hydrogen storage material is LaNi
5System, but this system has an inevitable drawback for storing up hydrogen richness very little, only is 1.4wt%, is difficult to satisfy growing social demand.The magnesium metal is then owing to its hydrogen content height (theoretical capacity is 7.6wt%), and the aboundresources low price, therefore very likely substitutes LaNi
5And become a new generation hydrogen storage material.
But Mg simple substance also has certain distance as hydrogen storage material from practicability at present.It is too poor that its matter of utmost importance is that it inhales hydrogen desorption kinetics character, and common magnesium granules needs put hydrogen inhaling under the conditions of 400 degree could inhale slowly after putting hydrogen activation repeatedly more than 250 degree.In addition, though put the hydrogen activation through suction repeatedly, it is complete that common magnesium simple substance still can not be inhaled hydrogen, the MgH of preparation
2Contain certain magnesium simple substance.At present mainly adopt the mechanical ball milling method to make improvements, can obviously reduce its product grain size and increase its specific surface area and defective improves its suction hydrogen desorption kinetics character by ball milling.Yet, since the ductility of metal, the MgH that ball milling obtains
2Though grain size can reach several nanometers, granular size no longer continues to reduce after dropping to about 1 μ m.It is to be noted that here crystal grain is meant single crystal particle, is single-phase in the particle promptly, no crystal boundary.And primary particle is meant a kind of independently particle that contains low porosity, and granule interior can have the interface, such as crystal boundary.Nano particle generally is meant primary particle, is formed by a plurality of crystal grain polymerizations, and its structure can be crystalline state, non-crystalline state and accurate brilliant, it can be single-phase, heterogeneous structure, or polycrystalline structure, when for once particle was monocrystalline, the particle diameter of particulate was just identical with grain-size.And prior art can't prepare the MgH of monocrystalline
2Particle, prepared MgH
2Particle all is a polycrystalline aggregate, and its size is more than micron order.The nano level MgH of present bibliographical information
2The crystal grain that all refers in the particle is nanocrystal, sees (1) Journal of Alloys and Compounds 366 (2004) 269-273, (2) J.Phys.Chem.B2006,110,11697-11703 etc.And MgH
2Particle is the nano level report that yet there are no.Nearest the suction hydrogen desorption kinetics character that studies show that Mg and its granular size have the relation that approaches inverse ratio, and particle is more little, and its suction hydrogen desorption kinetics character is good more.Therefore preparing the higher and granular size of purity is nano level MgH
2Particle has very important theory and practical significance.
Summary of the invention
The purpose of this invention is to provide a kind of nano level MgH that is suitable for as hydrogen storage material and reductive agent
2Particle and preparation method thereof.Described preparation method comprises the steps:
(1) MAG block is being lower than 1bar but makes its evaporation with electric-arc heating in more than or equal to the inert atmosphere of 0.5bar, magnesium vapor breaks away from heating region, and nucleation also is condensed into powder granule.
Normally MAG block is placed in the reaction chamber (as the reaction chamber of plasma arc furnace) of sealing, vacuumizes the back and feed rare gas element, the preferred 0.9bar of air pressure.Described rare gas element comprises all rare gas elementes in the periodic table of chemical element: helium, neon, argon gas, krypton gas, xenon, radon gas.In order to accelerate the velocity of evaporation of magnesium, after playing arc discharge, can extract a part of rare gas element out, feed a certain amount of reactive gas such as hydrogen or nitrogen again, also can directly add reactive gas, condition is that total gas pressure maintains and is lower than 1bar but in the scope more than or equal to 0.5bar, the volume percent that reactive gas accounts for whole system is 0～90%, and preferred version is the shared whole system 40-50% volume percent of reactive gas.
(2) after powder process is finished the magnesium powder is carried out Passivation Treatment.
The purpose of passivation is to avoid the magnesium powder to take out the back vigorous oxidation takes place, common way be with reaction chamber vacuumize the back with speed more slowly to wherein filling air, more than maintenance a few hours.
(3) prepared nano level magnesium powder is put into the hydrogen reaction stove, at 300～500 ℃ and hydrogen reaction, reaction finishes postcooling to room temperature, and obtaining granular size is nano level MgH
2Particle.
The method of above-mentioned synthesizing hydrogenated magnesium can be: after system was vacuumized, the temperature (300-500 ℃) that is heated to setting fed the above hydrogen of 10bar after activating powder 1-3 hour, the reaction more than 2 hours postcooling to room temperature.Activation temperature is preferably 400 ℃, and the time is preferably 1 hour; Be preferably 400 ℃ with the H-H reaction temperature, the reaction times is preferably 4 hours.
The magnesium granules size of the present invention's preparation is a nano level, and its diameter Distribution scope is at 50～500nm, and majority is about 200nm, so specific surface area is big, and defective is many, has more reaction site with H-H reaction.During in addition with H-H reaction, the diffusion length of hydrogen in magnesium granules reduces greatly, inhales hydrogen desorption kinetics character thereby improved it greatly.Therefore compare with common magnesium granules, need not repeatedly to activate to inhale in the hydrogen process in the first time and inhale hydrogen with fast speeds, generating scale size also is nano level MgH
2Particle, its diameter Distribution scope are at 50～600nm, and majority is about 250nm, and its purity is higher, does not comprise unreacted Mg completely.When with this nano level MgH
2When particle is made hydrogen storage material, put behind the hydrogen and can under lower temperature, inhale hydrogen, and demonstrated good cyclicity (referring to Fig. 3) with fast speeds.
Nano level MgH of the present invention
2Particle purity height has very good suction hydrogen desorption kinetics character when being used for hydrogen storage material, very likely become the hydrogen storage material of a new generation, therefore has extremely important using value and application prospects in the hydrogen storage technology field.
Description of drawings
Fig. 1 is the Mg and the MgH of the present invention's preparation
2The X-ray powder diffraction figure of nano particle.
Fig. 2 a is the transmission electron microscope photo of the Mg nano particle of the present invention's preparation.
Fig. 2 b is the MgH of the present invention's preparation
2The transmission electron microscope photo of nano particle.
Fig. 3 is that the present invention prepares MgH
2The absorption of hydrogen curve of nano particle under differing temps.
Embodiment
Embodiment 1, synthetic MgH
2Nano particle
(1) MAG block being put in the hydrogen plasma arc heating furnace, after vacuumizing, is under the Ar atmosphere of 0.8bar in total pressure, applies DC arc plasma and makes magnesium be subjected to thermal evaporation and be condensed to nano particle.
(2) stop to heat and vacuumizing, slowly bubbling air passivation in stove after the system cools, passivation was taken out sample after 48 hours.
(3) prepared Mg particle is put into the hydrogen reaction stove, after system vacuumizes, be heated to 400 ℃, activate 1 hour, the hydrogen reaction of feeding 40bar 4 hours is cooled to room temperature, and promptly getting granular size is nano level magnesium hydride particle.
Embodiment 2, synthetic MgH
2Nano particle
(1) MAG block being put in the hydrogen plasma arc heating furnace, after vacuumizing, is the 40%N of 0.9bar in total pressure
2Under/Ar the mixed atmosphere, apply DC arc plasma and make magnesium be subjected to thermal evaporation and be condensed to nano particle.
(2) stop to heat and vacuumizing, slowly bubbling air passivation in stove after the system cools, passivation was taken out sample after 48 hours.
(3) prepared Mg particle is put into the hydrogen reaction stove, after system vacuumizes, be heated to 350 ℃, activate 2 hours, the hydrogen reaction of feeding 10bar 12 hours is cooled to room temperature, and promptly getting granular size is nano level magnesium hydride particle.
Embodiment 3, synthetic MgH
2Nano particle
(1) MAG block being put in the hydrogen plasma arc heating furnace, after vacuumizing, is the 40%H of 0.5bar in total pressure
2Under/Ar the mixed atmosphere, apply DC arc plasma and make magnesium be subjected to thermal evaporation and be condensed to nano particle.
(2) stop to heat and vacuumizing, slowly bubbling air passivation in stove after the system cools, passivation was taken out sample after 48 hours.
(3) prepared Mg particle is put into the hydrogen reaction stove, after system vacuumizes, be heated to 450 ℃, activate 1 hour, the hydrogen reaction of feeding 40bar 2 hours is cooled to room temperature, and promptly getting granular size is nano level magnesium hydride particle.
Fig. 1 is the product Mg and the MgH of above-mentioned experiment
2XRD (X-ray powder diffraction) figure, can see clearly that prepared magnesium hydride purity is higher, do not contain unreacted Mg completely.
Fig. 2 a and 2b are respectively above-mentioned experimental product Mg and MgH
2The TEM of nano particle (transmission electron microscope) figure can see MgH
2The particle diameter size is 50-600nm, and majority is about 250nm.
Embodiment 4, nanometer MgH
2Particle detects as the suction hydrogen character of hydrogen storage material
(1) with prepared MgH
2Nano particle is put in the volumetric method hydrogen-storing device, vacuumizes, and feeds 1barH
2, be warming up to 400 ℃.
(2) vacuumizing under 400 ℃ condition 1 hour, reduce to temperature required 200 ℃, 250 ℃, 300 ℃ or 350 ℃ of tests then, is the H of 40bar at initial pressure
2Inhale the hydrogen test under the atmosphere, it is inhaled the hydrogen curve and sees Fig. 3.As seen from Figure 3, the nanometer Mg particle is under 300 ℃, and it is complete to inhale hydrogen in the 30min, and hydrogen is 1.97H/M, and under 350 ℃, it is complete that 20min just inhales hydrogen, and hydrogen also is 1.97H/M.Under 250 ℃ and 200 ℃, the nanometer Mg particle also can be to absorb hydrogen than fast speeds, though it is complete to inhale hydrogen in Measuring Time.Under 200 ℃ and 250 ℃, magnesium granules hydrogen in 80min has reached 0.58 and 1.57H/M respectively.What we need emphasize again is, common magnesium granules must be more than 400 ℃, and under the hydrogen high pressure more than the 5MPa, putting the hydrogen circulation through a plurality of suctions later on just can be in the temperature more than 300 ℃, put hydrogen with slow speed suction, demonstrated nanometer MgH thus
2The storage hydrogen character that particle is superior.In addition, if prepared nanometer magnesium hydride particle or the interpolation catalyzer of further ball milling also can demonstrate the storage hydrogen character more superior than the common magnesium of ball milling.
Claims (7)
1. magnesium hydride particulate product, its particle diameter is in 50～600 nanometer range.
2. the preparation method of a magnesium hydride nano particle may further comprise the steps:
(1) MAG block is lower than 1bar at air pressure but makes its evaporation with electric-arc heating in more than or equal to the inert atmosphere of 0.5bar, magnesium vapor breaks away from heating region, and nucleation also is condensed into powder granule;
(2) the magnesium powder is carried out Passivation Treatment;
(3) prepared nano level magnesium powder is put into the hydrogen reaction stove, at 300～500 ℃ and hydrogen reaction, reaction finishes postcooling to room temperature, and obtaining granular size is nano level MgH
2Particle.
3. preparation method as claimed in claim 2, it is characterized in that, extract a part of rare gas element after electric arc plays arc discharge in step (1) out, feed hydrogen or nitrogen again, perhaps directly add hydrogen or nitrogen, the volume percent that makes hydrogen or nitrogen account for whole system is 0～90%, and total gas pressure maintains and is lower than 1bar but in the scope more than or equal to 0.5bar.
4. preparation method as claimed in claim 3 is characterized in that, the volume percent that middle hydrogen of described step (1) or nitrogen account for whole system is 40～50%.
5. as claim 2 or 3 or 4 described preparation methods, it is characterized in that total gas pressure is 0.9bar in the step (1).
6. preparation method as claimed in claim 2, it is characterized in that the concrete grammar of step (3) magnesium powder and hydrogen reaction is:, be heated to 300-500 ℃ of activating powder 1-3 hour earlier with the hydrogen reaction stove evacuation, feed the above hydrogen of 10bar then, reaction more than 2 hours postcooling to room temperature.
7. the magnesium hydride particulate product of particle diameter in 50～600 nanometer range is as the purposes of hydrogen storage material.
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