CN110655036A - Preparation method of yttrium/graphene modified magnesium-nickel hydrogen storage composite material - Google Patents
Preparation method of yttrium/graphene modified magnesium-nickel hydrogen storage composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of yttrium/graphene modified magnesium-nickel hydrogen storage composite material, which comprises the steps of mixing yttrium oxalate solution with graphite oxide, forming oxalic acid by oxalic acid radical ions through hydrolysis, and forming Y+3Uniformly attaching ions on the surface of graphite oxide, freezing the mixed liquid to make oxalic acid and solvent formed by hydrolysis become solid, heating to sublimate the frozen solid oxalic acid and ice to obtain Y+3A graphite oxide composite of+3Uniformly distributed on graphite oxide by dispersing Y+3Reducing the Y into a simple substance to nucleate and grow Y crystal,the magnesium-nickel Y/graphene hydrogen storage composite material is prepared by mixing the Y/graphene composite with magnesium powder and nickel powder. The magnesium-based Y/graphene hydrogen storage composite material prepared by the invention can reduce the binding energy of graphene and hydrogen atoms and improve the hydrogen storage performance of graphene; the nano metal Y is distributed in the magnesium-nickel alloy, so that the hydrogen collection activation energy can be reduced, the hydrogen collection and release rates of the composite material are accelerated, and the hydrogen storage kinetics are improved.
Description
Technical Field
The invention belongs to the field of hydrogen storage material preparation, and particularly relates to a preparation method of a yttrium/graphene modified magnesium-nickel hydrogen storage composite material.
Background
Energy is the basis for human survival and development, and the use of traditional fossil fuels brings serious environmental pollution. And hydrogen is taken as a renewable energy source, has the advantages of no carbon, environmental protection and the like, and is expected to replace the traditional fossil energy source. However, storage of hydrogen gas is a bottleneck in the development of hydrogen energy. Because the liquefaction condition of hydrogen is harsh (the temperature is required to be less than minus 253 ℃), the liquid hydrogen storage cost is high. Therefore, solid-state hydrogen storage has received attention from many scholars. Magnesium alloys are considered to be one of the most promising solid-state hydrogen storage materials due to their advantages of high hydrogen storage capacity (7.6 wt.%), good reversibility, low cost, and high efficiency. Based on this, various magnesium-based hydrogen storage materials are successively proposed and prepared, such as alloying (MgAl, MgNi, MgPd), nanocrystallization (nano MgH) of magnesium2) And composite (Mg/nano Ni particles/graphene), metal organic framework (MOF structure), and the like. The above hydrogen storage material reduces the binding energy of magnesium hydride to some extent, and thus lowers the temperature at the time of hydrogen absorption and desorption. However, the higher activation energy when hydrogen molecules dissolve into hydrogen atoms, the lower reaction rate when magnesium hydride nucleates and grows, and the hydrogen atoms pass through MgH during hydrogen absorption2Lower diffusion rate at layer and MgH2At a high temperature (>Coarsening of magnesium crystal grains caused at the time of dehydrogenation at 300 deg.c, etc., which limits further optimization of hydrogen absorption and desorption temperatures and improvement of hydrogen absorption and desorption kinetic characteristics. Accordingly, in order to solve the above problems, provided herein is a Y/graphene improved magnesium-nickel hydrogen storage material and a method for preparing the same. Because the metallic nickel is cheap and easy to obtain, and the magnesium-based alloy doped with the Ni element not only reduces the stability of magnesium hydride, but also can improve the hydrogen absorbing and releasing conditions and optimize the hydrogen storage cost,it is receiving a great deal of attention. However, the magnesium-nickel alloy has relatively low hydrogen storage efficiency, and the magnesium metal crystal grains are easy to coarsen in the heating hydrogen release process, so that the cycle stability is poor.
Disclosure of Invention
The invention aims to overcome the defects and provide a preparation method of the yttrium/graphene modified magnesium-nickel hydrogen storage composite material, and the obtained Y/graphene modified magnesium-nickel composite material can accelerate the hydrogen collection and hydrogen discharge rate and improve the hydrogen storage kinetics (efficiency). Meanwhile, the growth of magnesium matrix crystal grains caused by overhigh temperature in the hydrogen discharge process can be effectively inhibited, and the hydrogen collection and discharge circulation stability is further maintained.
In order to achieve the above object, the present invention comprises the steps of:
preparing graphite oxide, yttrium oxalate solution and magnesium powder, wherein the concentration of the yttrium oxalate solution is 2.03mol/L, and 10-15g of graphite oxide, 80-90g of magnesium powder and 5-10g of nickel powder are prepared for every 0.01L of yttrium oxalate solution;
adding graphite oxide into an yttrium oxalate solution, and uniformly mixing to obtain a mixed solution A;
step three, freezing the mixed solution A into a solid state, heating the solid state, sublimating the water and the oxalic acid to obtain Y+3/graphite oxide composite prepared by mixing Y+3Heating the graphite oxide composite to reduce the graphite oxide into graphene and Y+3Reducing the graphene into a simple substance Y to obtain a Y/graphene composite;
and step three, mixing the Y/graphene composite with magnesium powder and nickel powder to prepare the magnesium-nickel Y/graphene hydrogen storage composite material.
In the first step, the purity of the graphite oxide is 99%.
And in the second step, ultrasonic vibration mixing is adopted during mixing, and the vibration time is 45 min.
In the third step, the freezing is carried out in a freeze drying box, and the freezing temperature is-10 to-15 ℃.
In the third step, the sublimation of water and oxalic acid is 4.5X 10-3～1.0×10-2The heating temperature is 150-200 ℃ under the Pa vacuum degree.
The temperature is 400-500 ℃ when the graphite oxide is reduced into the graphene.
In the third step, the purity of the magnesium powder and the nickel powder is 99.9 percent, and the granularity is 5-10 mu m.
And in the third step, the Y/graphene composite and magnesium powder are mixed, namely the Y/graphene composite and the magnesium powder are put into a corundum ball milling tank for ball milling.
The diameter of the steel ball in the corundum ball milling tank is 5mm, the rotating speed is 500-1000 r/min, and the ball milling time is 5-15 h.
Compared with the prior art, the invention mixes the yttrium oxalate solution with the graphite oxide, the oxalate ions form oxalic acid through hydrolysis, and Y is+3Uniformly attaching ions on the surface of graphite oxide, freezing the mixed liquid to make oxalic acid and solvent formed by hydrolysis become solid, heating to sublimate the frozen solid oxalic acid and ice to obtain Y+3A graphite oxide composite of+3Uniformly distributed on graphite oxide by dispersing Y+3Reducing the Y into a simple substance, nucleating and growing a Y crystal, and mixing the Y/graphene composite with magnesium powder and nickel powder to prepare the magnesium-nickel Y/graphene hydrogen storage composite material. The magnesium-nickel Y/graphene hydrogen storage composite material prepared by the invention can reduce the binding energy of graphene and hydrogen atoms and improve the hydrogen storage performance of graphene; on the other hand, the nano metal Y is distributed in the magnesium-nickel alloy, so that the hydrogen collection activation energy can be reduced, the hydrogen collection and release rates of the composite material can be accelerated, and the hydrogen storage kinetic efficiency can be improved. The graphene uniformly distributed in the magnesium-nickel alloy can effectively prevent local overhigh temperature and growth of crystal grains in the matrix caused by heating in the hydrogen releasing process, thereby maintaining the hydrogen collecting and releasing cycle stability of the composite material.
Drawings
FIG. 1 is a process scheme of the present invention.
Detailed Description
The invention is further illustrated by the following figures and examples.
Referring to fig. 1, example 1:
preparing graphite oxide, an yttrium oxalate solution and magnesium powder, wherein the concentration of the yttrium oxalate solution is 2.03mol/L, 10g of graphite oxide, 80g of magnesium powder and 5g of nickel powder are prepared in each 0.01L of yttrium oxalate solution, the purity of the graphite oxide is 99%, the purities of the magnesium powder and the nickel powder are both 99.9%, and the particle sizes are both 5 mu m;
adding graphite oxide into an yttrium oxalate solution, and carrying out ultrasonic vibration mixing for 45min to obtain a mixed solution A after uniform mixing;
step three, freezing the mixed solution A into a solid state in a freeze drying oven with the temperature of minus 10 ℃, and then, freezing the mixed solution A into a solid state at the temperature of 4.5 multiplied by 10-3Heating to 150 deg.C under Pa vacuum degree to sublimate water and oxalic acid to obtain Y+3/graphite oxide composite prepared by mixing Y+3Heating the graphite oxide composite to 400 ℃ to reduce the graphite oxide into graphene and Y+3Reducing the graphene into a simple substance Y to obtain a Y/graphene composite;
and step three, loading the Y/graphene complex, magnesium powder and nickel powder into a corundum ball milling tank for ball milling, wherein the diameter of steel balls in the corundum ball milling tank is 5mm, the rotating speed is 500 r/min, the ball milling time is 15h, and uniformly mixing to prepare the magnesium-nickel Y/graphene hydrogen storage composite material.
Example 2:
preparing graphite oxide, an yttrium oxalate solution and magnesium powder, wherein the concentration of the yttrium oxalate solution is 2.03mol/L, 15g of graphite oxide, 90g of magnesium powder and 10g of nickel powder are prepared in each 0.01L of yttrium oxalate solution, the purity of the graphite oxide is 99%, the purities of the magnesium powder and the nickel powder are both 99.9%, and the particle sizes are both 10 mu m;
adding graphite oxide into an yttrium oxalate solution, and carrying out ultrasonic vibration mixing for 45min to obtain a mixed solution A after uniform mixing;
step three, freezing the mixed solution A into a solid state in a freeze drying oven with the temperature of-15 ℃, and then, freezing the mixed solution A into a solid state at the temperature of 1.0 multiplied by 10-2Heating to 200 deg.C under Pa vacuum degree to sublimate water and oxalic acid to obtain Y+3/graphite oxide composite prepared by mixing Y+3Heating the graphite oxide composite to 500 ℃ to reduce the graphite oxide into graphene and Y+3Reducing the graphene into a simple substance Y to obtain a Y/graphene composite;
and step three, loading the Y/graphene complex, magnesium powder and nickel powder into a corundum ball milling tank for ball milling, wherein the diameter of a steel ball in the corundum ball milling tank is 5mm, the rotating speed is 1000 revolutions per minute, the ball milling time is 5 hours, and uniformly mixing to prepare the magnesium-nickel Y/graphene hydrogen storage composite material.
Example 3:
preparing graphite oxide, an yttrium oxalate solution and magnesium powder, wherein the concentration of the yttrium oxalate solution is 2.03mol/L, 8g of graphite oxide, 85g of magnesium powder and 8g of nickel powder are prepared in each 0.01L of yttrium oxalate solution, the purity of the graphite oxide is 99%, the purities of the magnesium powder and the nickel powder are both 99.9%, and the particle sizes are both 7 mu m;
adding graphite oxide into an yttrium oxalate solution, and carrying out ultrasonic vibration mixing for 45min to obtain a mixed solution A after uniform mixing;
step three, freezing the mixed solution A into a solid state in a freeze drying oven with the temperature of-13 ℃, and then, freezing the mixed solution A into a solid state at the temperature of 2.3 multiplied by 10-3Heating to 170 deg.C under Pa vacuum degree to sublimate water and oxalic acid to obtain Y+3/graphite oxide composite prepared by mixing Y+3Heating the graphite oxide composite to 450 ℃ to reduce the graphite oxide into graphene and Y+3Reducing the graphene into a simple substance Y to obtain a Y/graphene composite;
and step three, loading the Y/graphene complex, magnesium powder and nickel powder into a corundum ball milling tank for ball milling, wherein the diameter of a steel ball in the corundum ball milling tank is 5mm, the rotating speed is 8000 revolutions per minute, the ball milling time is 10 hours, and uniformly mixing to prepare the magnesium-nickel Y/graphene hydrogen storage composite material.
Example 5: preparation of Mg5Ni 5Y/graphene hydrogen storage composite material
1) 12g of graphite oxide with a purity of 99% and Y with a concentration of 2.03mol/L and a volume of 0.01L2(C2O4)3·10H2And mixing the O solution in a beaker, and putting the beaker filled with the mixed solution into an ultrasonic vibration instrument for 45 min.
2) And taking the beaker filled with the mixed solution out of the ultrasonic vibration instrument, putting the beaker into a freeze drying oven, and freezing the solution into a solid state at the temperature of minus 10 ℃. Then, at 1.0X 10-2Heating to 150 deg.C under Pa vacuum degree to sublimate ice and oxalic acid simultaneously, leaving Y in the beaker+3And a graphite oxide composite. The sublimation process requires timely venting of the sublimated gas. Finally, drying the Y+3Taking out the graphite oxide composite body, putting the graphite oxide composite body into a tube furnace, heating to 400 ℃, reducing graphite oxide into graphene, and reducing Y+3Reducing the Y into a simple substance. In the obtained composite Y/graphene, the mass fraction of Y is about 50%, and the thickness of graphene is 3-4 layers.
(3) And mixing 90g of magnesium powder, 5g of nickel powder and 5g of the obtained Y/graphene, and then putting the mixture into a corundum ball milling tank for ball milling. The purity of the magnesium powder and the purity of the nickel powder are both 99.9%, the granularity of the magnesium powder and the nickel powder are both 10 microns, the diameter of a stainless steel ball used for ball milling is 5mm, the rotating speed is 500 r/min, and the ball milling time is 5 hours. And finally, successfully preparing the Mg5Ni 5Y/graphene hydrogen storage composite material. In the obtained composite material, the yttrium atom size is 60nm, and the content of the Y/graphene composite is 5%.
Example 5: preparation of Mg10Ni 10Y/graphene hydrogen storage composite material
1) 15g of graphite oxide with a purity of 99% and Y with a concentration of 2.03mol/L and a volume of 0.01L2(C2O4)3·10H2And mixing the O solution in a beaker, and putting the beaker filled with the mixed solution into an ultrasonic vibration instrument for 45 min.
2) Firstly, taking the beaker filled with the mixed solution out of an ultrasonic vibration instrument, putting the beaker into a freeze drying oven, and freezing the solution into a solid state at the temperature of minus 15 ℃. Then, at 4.5X 10-3Heating to 160 deg.C under Pa vacuum degree to sublimate ice and oxalic acid simultaneously, and collecting the residual Y in the beaker+3A graphite oxide composite. The sublimation process requires timely venting of the sublimated gas. Finally, drying the Y+3Taking out the graphite oxide composite body, putting the graphite oxide composite body into a tubular furnace, heating to 500 ℃, reducing graphite oxide into graphene, and reducing Y+3Reducing the Y into a simple substance. In the obtained composite Y/graphene, the mass fraction of Y is about 35%, and the thickness of graphene is 2-3 layers.
(3) And mixing 80g of magnesium powder, 10g of nickel powder and 10g of the obtained Y/graphene, and then putting the mixture into a corundum ball milling tank for ball milling. The purity of the magnesium powder and the purity of the nickel powder are both 99.9 percent, and the particle size is both 5 mu m; the diameter of a stainless steel ball adopted by ball milling is 5mm, the rotating speed is 700 r/min, and the ball milling time is 5 h. Finally obtaining the Mg10Ni 10Y/graphene hydrogen storage composite material. The obtained composite material has an average yttrium atom size of 30nm, and the content of the Y/graphene composite is 10%.
Example 6: preparation of Mg5Ni 15Y/graphene hydrogen storage composite material
1) 14g of graphite oxide having a purity of 99% and Y having a concentration of 2.03mol/L and a volume of 0.01L2(C2O4)3·10H2And mixing the O solution in a beaker, and putting the beaker filled with the mixed solution into an ultrasonic vibration instrument for 45 min.
2) Firstly, taking the beaker filled with the mixed solution out of an ultrasonic vibration instrument, putting the beaker into a freeze drying oven, and freezing the solution into a solid state at the temperature of minus 15 ℃. Then, at 4.5X 10-3Heating to 200 deg.C under Pa vacuum to sublimate ice and oxalic acid simultaneously, and collecting the residual Y in the beaker+3A graphite oxide composite. Finally, drying the Y+3Taking out the graphite oxide composite, putting the graphite oxide composite into a tubular furnace, heating to 500 ℃, reducing the graphite oxide into graphene, and reducing Y+3Reducing the Y into a simple substance. In the obtained composite Y/graphene, the mass fraction of Y is about 25%, and the thickness of graphene is 2-3 layers.
(3) And mixing 80g of magnesium powder, 5g of nickel powder and 15g of the obtained Y/graphene, and then putting the mixture into a corundum ball milling tank for ball milling. The purity of the magnesium powder and the purity of the nickel powder are both 99.9 percent, and the particle size is both 10 mu m; the diameter of the stainless steel ball adopted by the ball milling tank is 5mm, the rotating speed is 1000 r/min, and the ball milling time is 15 h. And finally, successfully preparing the Mg5Ni 15Y/graphene composite material. The obtained composite material has an average yttrium atom size of 20nm, and the content of the Y/graphene composite is 15%.
Claims (9)
1. The preparation method of the yttrium/graphene modified magnesium-nickel hydrogen storage composite material is characterized by comprising the following steps of:
preparing graphite oxide, yttrium oxalate solution and magnesium powder, wherein the concentration of the yttrium oxalate solution is 2.03mol/L, and 10-15g of graphite oxide, 80-90g of magnesium powder and 5-10g of nickel powder are prepared for every 0.01L of yttrium oxalate solution;
adding graphite oxide into an yttrium oxalate solution, and uniformly mixing to obtain a mixed solution A;
step three, freezing the mixed solution A into a solid state, heating the solid state, sublimating the water and the oxalic acid to obtain Y+3/graphite oxide composite prepared by mixing Y+3Heating the graphite oxide composite to reduce the graphite oxide into graphene and Y+3Reducing the graphene into a simple substance Y to obtain a Y/graphene composite;
and step three, mixing the Y/graphene composite with magnesium powder and nickel powder to prepare the magnesium-nickel Y/graphene hydrogen storage composite material.
2. The method for preparing yttrium/graphene modified magnesium-nickel hydrogen storage composite material according to claim 1, wherein in the first step, the purity of graphite oxide is 99%.
3. The method for preparing yttrium/graphene modified magnesium-nickel hydrogen storage composite material according to claim 1, wherein in the second step, ultrasonic vibration is adopted for mixing, and the vibration time is 45 min.
4. The preparation method of the yttrium/graphene modified magnesium-nickel hydrogen storage composite material according to claim 1, wherein in the third step, the freezing is performed in a freeze drying oven, and the freezing temperature is-10 to-15 ℃.
5. The method for preparing yttrium/graphene modified magnesium-nickel hydrogen storage composite material according to claim 1, wherein in the third step, the sublimation of water and oxalic acid is 4.5 x 10-3～1.0×10-2The heating temperature is 150-200 ℃ under the Pa vacuum degree.
6. The method for preparing yttrium/graphene modified magnesium-nickel hydrogen storage composite material as claimed in claim 1, wherein the temperature for reducing graphite oxide into graphene is 400-500 ℃.
7. The method for preparing yttrium/graphene modified magnesium-nickel hydrogen storage composite material according to claim 1, wherein in the third step, the purity of magnesium powder and nickel powder is 99.9%, and the particle size is 5-10 μm.
8. The method for preparing the yttrium/graphene modified magnesium-nickel hydrogen storage composite material as claimed in claim 1, wherein the step of mixing the Y/graphene composite body with magnesium powder is to put the Y/graphene composite body and magnesium powder into a corundum ball mill for ball milling.
9. The method for preparing yttrium/graphene modified magnesium-nickel hydrogen storage composite material as claimed in claim 8, wherein the diameter of steel balls in the corundum ball milling tank is 5mm, the rotation speed is 500-.
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