CN118147466A - Preparation method of Mg-Ni-based hydrogen storage alloy containing rare earth elements - Google Patents
Preparation method of Mg-Ni-based hydrogen storage alloy containing rare earth elements Download PDFInfo
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- CN118147466A CN118147466A CN202410173209.1A CN202410173209A CN118147466A CN 118147466 A CN118147466 A CN 118147466A CN 202410173209 A CN202410173209 A CN 202410173209A CN 118147466 A CN118147466 A CN 118147466A
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 239000001257 hydrogen Substances 0.000 title claims abstract description 104
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 104
- 239000000956 alloy Substances 0.000 title claims abstract description 69
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 67
- 238000003860 storage Methods 0.000 title claims abstract description 62
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 19
- 229910019083 Mg-Ni Inorganic materials 0.000 title claims abstract description 18
- 229910019403 Mg—Ni Inorganic materials 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims description 20
- 239000002184 metal Substances 0.000 claims description 20
- 238000003723 Smelting Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- 239000000126 substance Substances 0.000 claims description 17
- 229910052749 magnesium Inorganic materials 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 5
- 230000006698 induction Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000011232 storage material Substances 0.000 abstract description 8
- 230000004913 activation Effects 0.000 abstract description 2
- 229910000858 La alloy Inorganic materials 0.000 abstract 1
- 239000011777 magnesium Substances 0.000 description 42
- 238000003795 desorption Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 210000001787 dendrite Anatomy 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000013507 mapping Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910019080 Mg-H Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000003797 telogen phase Effects 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
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- Hydrogen, Water And Hydrids (AREA)
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Abstract
The invention discloses a preparation method of a Mg-Ni-based hydrogen storage alloy containing rare earth elements, belonging to the technical field of hydrogen storage alloy materials and preparation thereof. The invention solves the problems of the prior hydrogen storage material such as activation and limited hydrogen storage amount. The rare earth element La is used for modifying the Mg-Ni-based hydrogen storage alloy, and the hydrogen storage performance of the modified Mg-Ni-La hydrogen storage alloy is well improved. Further, based on the Mg-Ni-La alloy, la is replaced by the rare earth element Y, the dynamic performance of the alloy is enhanced by adjusting the contents of the rare earth element Y and La, the hydrogen storage capacity of the alloy is improved, the hydrogen release peak temperature of the replaced hydrogen storage alloy is reduced to 273 ℃, and the hydrogen storage amount is 4.645 wt% under the conditions of 220 ℃ and 5 MPa.
Description
Technical Field
The invention relates to a preparation method of a Mg-Ni-based hydrogen storage alloy containing rare earth elements, belonging to the technical field of hydrogen storage alloy materials and preparation thereof.
Background
Hydrogen has the advantages of rich reserves, high energy value, no pollution to the environment and the like, is regarded as an energy carrier with the most development potential in the twenty-first century, and is the development direction of human energy strategy. In hydrogen energy industrialization application, hydrogen storage and transportation are key links for connecting upstream hydrogen production and downstream hydrogen production, and high-pressure gaseous hydrogen storage, low-temperature liquid hydrogen storage and solid material hydrogen storage are three main hydrogen storage modes. In view of factors such as the volume hydrogen storage density, the hydrogen storage energy consumption, the safety and the like, the hydrogen storage of the metal-based hydrogen storage material is currently recognized as one of the best hydrogen storage methods. Meanwhile, the magnesium-based hydrogen storage material has the advantages of low cost, excellent reversibility, high hydrogen storage capacity, rich element storage capacity and the like, is considered to be one of the most researched and promising hydrogen storage materials, but the Mg-H bond is too stable, the hydrogen release enthalpy change is about 75kJ/mol, and the hydrogen release temperature is too high. And the magnesium-based hydrogen storage material has lower platform pressure and limits the hydrogen storage capacity. Therefore, it is necessary to provide an ideal magnesium-based hydrogen storage material which has large-scale industrial popularization feasibility and can be used for future hydrogen storage and transportation, and how to effectively improve the hydrogen absorption and desorption properties of magnesium-based alloys.
Disclosure of Invention
The invention provides a preparation method of Mg-Ni-based hydrogen storage alloy containing rare earth elements, which aims to solve the problems of activation, limited hydrogen storage amount and the like of the existing hydrogen storage materials.
The technical scheme of the invention is as follows:
the invention aims to provide a preparation method of Mg-Ni-based hydrogen storage alloy containing rare earth elements, which specifically takes a metal simple substance as a raw material, and performs forging forming after vacuum induction melting.
Further defined, the preparation method comprises the steps of:
(1) Weighing Mg, ni, la and Y metal simple substances according to the chemical formula of the hydrogen storage alloy;
(2) Uniformly mixing all the metal simple substances weighed in the step (1), putting the mixture into a smelting crucible, and covering a crucible cover;
(3) Heating the smelting crucible to 400-500 ℃, keeping the temperature for 2-3min, and introducing SF 6 gas to replace air;
(4) And under the condition of keeping the introduction of SF 6 gas, heating to 1000-1050 ℃, preserving heat for 3-5 min, continuously heating to 1100-1150 ℃, preserving heat for 10min, and casting to obtain the hydrogen storage alloy.
Further defined, mg metal element is additionally added in (1) in an amount of 5wt.% based on Mg metal element in the raw material.
Further defined, in (1), an elemental Y metal is additionally added in an amount of 1wt.% based on elemental Y metal in the feedstock.
Further defined, 1wt.% of elemental La metal is additionally added to the feedstock in (1).
Further defined, SF 6 gas purity in (3) and (4) is 99.9%.
Further limited, the rare earth element-containing Mg-Ni-based hydrogen storage alloy prepared by the method has a chemical formula of Mg 3.497Ni0.170LaxYy, wherein x is more than or equal to 0.0280 and less than or equal to 0.0360,0 and y is more than or equal to 0.012.
Further defined, x is 0.032 and y is 0.006.
Still further defined, x is 0.028 and y is 0.012.
Still further defined, x is 0.036 and y is 0.
Further defined, the hydrogen storage alloy stores 4.645wt.% hydrogen at 220 ℃ and 5MPa.
The beneficial effects are that:
According to the invention, the rare earth element La is used for modifying the Mg-Ni-based hydrogen storage alloy, and the hydrogen storage performance of the modified Mg 3.497Ni0.170La0.036 hydrogen storage alloy is well improved. Further, based on Mg 3.497Ni0.170La0.036 alloy, la is replaced by the rare earth element Y, the dynamic performance of the alloy is enhanced by adjusting the contents of the rare earth element Y and La, the hydrogen storage capacity of the alloy is improved, and the hydrogen release peak temperature of the replaced hydrogen storage alloy is reduced to 273 ℃. And the addition of rare earth La and Y elements has great significance for the high-value utilization of high-abundance rare earth elements in China while improving the performance of the hydrogen storage alloy.
Meanwhile, the invention utilizes the vacuum induction smelting process, 99.9 percent of high-purity SF 6 is poured into a smelting furnace, and the Mg-Ni-based hydrogen storage alloy is synthesized in an anaerobic environment.
Drawings
FIG. 1 is a graph showing the first hydrogen absorption kinetics of the hydrogen occluding alloy prepared in examples 1-3 at 220℃and 5 MPa;
FIG. 2 is a graph showing the first hydrogen desorption kinetics of the hydrogen occluding alloy prepared in examples 1 to 3 at 280℃and 0.01 MPa;
FIG. 3 is a graph showing PCT test of hydrogen absorption and desorption of hydrogen storage alloy prepared in examples 1-3 at 260 ℃, 280 ℃, 300 ℃ and 320 ℃;
FIG. 4 is a graph showing DSC test of hydrogen evolution of the hydrogen occluding alloy prepared in example 1 at a heating rate of 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min;
FIG. 5 is a graph showing DSC test of hydrogen evolution of the hydrogen occluding alloy prepared in example 2 at a heating rate of 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min;
FIG. 6 is a graph showing DSC test of hydrogen evolution of the hydrogen occluding alloy prepared in example 3 at a heating rate of 5 ℃/min, 10 ℃/min, 15 ℃/min, 20 ℃/min;
FIG. 7 is an XRD spectrum of the hydrogen occluding alloy prepared in examples 1 to 3;
FIG. 8 is a back-scattering diagram of the hydrogen occluding alloy prepared in example 1;
FIG. 9 is a back-scattering diagram of the hydrogen occluding alloy prepared in example 2;
FIG. 10 is a back-scattering diagram of the hydrogen occluding alloy prepared in example 3;
FIG. 11 is a Mapping graph corresponding to the back-scattering result of the hydrogen occluding alloy prepared in example 2.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
The experimental methods used in the following examples are conventional methods unless otherwise specified. The materials, reagents, methods and apparatus used, without any particular description, are those conventional in the art and are commercially available to those skilled in the art.
Example 1:
the chemical formula of the Mg-Ni-based hydrogen storage alloy prepared in the embodiment is Mg 3.497Ni0.170La0.036.
The method for preparing the Mg-Ni-based hydrogen storage alloy comprises the following steps:
a. according to the atomic ratio of Mg 3.497Ni0.170La0.036, the mass of each element is calculated, and the mass of the simple substances of Mg, ni and La with the purity of 99.9 percent is respectively weighed, and as the metal Mg can be burnt in the smelting process, the mass of 5 percent is additionally added to compensate the burnt part when raw materials are weighed. The specific numerical values are as follows: mg:44.625g, ni:5.028g, la:4.011g, ready for use. Taking Mg, ni and La metal simple substances as raw materials;
b. In order to ensure the accuracy of alloy smelting, a vacuum induction smelting process is applied, firstly, the surfaces of all metal simple substances in the step a are polished, and oxide films on the surfaces are removed; before smelting, the inner wall of the smelting furnace is wiped clean by alcohol cotton. Each weighed alloy sample is preheated and dried, then placed into a smelting crucible in a smelting furnace, and then covered with a crucible cover; heating the smelting crucible to 400-500 ℃, keeping the temperature for 2-3min, and introducing SF 6 gas to replace air; after the air is replaced, continuously introducing SF 6 gas, heating the smelting furnace to 1000-1050 ℃, and keeping the temperature for 3-5min; and continuously heating the smelting crucible furnace to 1100-1150 ℃, keeping the temperature for 10min, and then pouring.
Example 2:
the difference between this embodiment and embodiment 1 is that: using Y instead of 0.5wt.% La, the hydrogen storage alloy has the chemical formula Mg 3.497Ni0.170La0.032Y0.006, and the specific values are weighed as follows: mg:45.0132g, ni:5.1112g, la:3.7875g, Y:0.2525g (wherein Mg, la and Y elements are volatile during smelting, so Mg should be weighed 5% more and La and Y should be weighed 1% more to compensate for the burn-out portion), and the remaining process steps and parameter settings are the same as in example 1 to obtain Mg 3.497Ni0.170La0.032Y0.006 hydrogen storage alloy ingot.
Example 3:
The difference between this embodiment and embodiment 1 is that: the hydrogen storage alloy of which the chemical formula is Mg 3.497Ni0.170La0.028Y0.012 is prepared by replacing 1wt.% of La with Y, and the specific numerical values are weighed as follows: mg:45.058g, ni:5.0194g, la:3.535g, Y:0.505g (wherein the Mg, la and Y elements are volatile in the smelting process, so that the Mg should be weighed 5% more and the La and Y should be weighed 1% more to compensate for the burnt part), and the rest of the process steps and parameter settings are the same as those of example 1, to obtain Mg 3.497Ni0.170La0.028Y0.012 hydrogen storage alloy ingot.
Effect example:
(1) And (3) polishing the surface of the Mg-Ni-based hydrogen storage alloy ingot prepared in the examples 1-3 by using a polisher, removing the surface oxide layer, grinding and crushing the alloy, and sieving with a 200-mesh sieve to obtain hydrogen storage alloy powder. And placing about 0.5g of prepared hydrogen storage alloy powder into a reaction kettle of P-C-T equipment, vacuumizing the reaction kettle to below 0.0001MPa, filling hydrogen with the purity of 99.9%, and making the hydrogen pressure reach 5MPa, and testing the absorption/desorption kinetics of the alloy, wherein the test result is shown in figure 1. From the graph, the dynamic performance of Mg 3.497Ni0.170La0.032Y0.006 prepared in example 2 is optimal under the conditions of 220 ℃ and 5MPa, the first time of hydrogen absorption is 3.35wt.% and the hydrogen storage amount is 4.645wt.%.
(2) The Mg-Ni-based hydrogen storage alloy prepared in examples 1 to 3 was tested for its constant temperature hydrogen release performance at 280 ℃, and the results are shown in fig. 2, where Mg 3.497Ni0.170La0.032Y0.006 was found to have the optimum hydrogen release kinetic performance at 280 ℃ and 0.01MPa, and released 1.834wt.% in 1min, whereas example 3 released 1.431wt.% in 1min, and example 1 released 0.96wt.% in 1 min.
(3) The Mg 3.497Ni0.170La0.036 alloy prepared in example 1 was tested for hydrogen desorption properties at heating rates of 5 ℃/min, 10 ℃/min, 15 ℃/min and 20 ℃/min, and the results are shown in fig. 4, and as can be seen from fig. 4, the peak hydrogen desorption temperatures of the alloy at different heating rates are 336.1 ℃, 352.0 ℃, 365.1 ℃ and 371.2 ℃, respectively.
(4) The Mg 3.497Ni0.170La0.032Y0.006 alloy prepared in example 2 was tested for hydrogen desorption properties at heating rates of 5 ℃/min, 10 ℃/min, 15 ℃/min and 20 ℃/min, and the results are shown in fig. 5. It can be seen from fig. 5 that the peak hydrogen desorption temperatures of the alloy at different heating rates are 273.3 ℃, 288.3 ℃, 298.6 ℃ and 312.3 ℃, respectively.
(5) The Mg 3.497Ni0.170La0.028Y0.012 alloy prepared in example 3 was tested for hydrogen desorption properties at heating rates of 5 ℃/min, 10 ℃/min, 15 ℃/min and 20 ℃/min, and the results are shown in fig. 6, and as can be seen from fig. 6, the peak hydrogen desorption temperatures of the alloy at different heating rates are 324.6 ℃, 339.6 ℃, 349.0 ℃ and 361.9 ℃, respectively.
(6) XRD phase characterization is carried out on the Mg-Ni-based hydrogen storage alloy prepared in the examples 1-3 by adopting an X-ray diffractometer (Bruker D8 advanced X, cu K alpha, 40kV and 40 mA), the result is shown in figure 7, the Mg-Ni-based hydrogen storage alloy prepared in the examples 1-3 is mainly the diffraction peak of Mg, the rest phases are Mg 2Ni,La2Mg17, and the Mg-Ni-based hydrogen storage alloy prepared in the examples 2 and 3 contains the diffraction peak of MgY phase as shown in a graph, a desk and a chair.
(7) As a result of performing a back-scattering analysis on the Mg 3.497Ni0.170La0.036 alloy obtained in example 1, as shown in FIG. 8, it was found that the black portion was Mg phase, the dendrite gray phase was Mg 2 Ni, and the light gray block was La 2Mg17 phase.
(8) The back scattering analysis was performed on Mg 3.497Ni0.170La0.032Y0.006 prepared in example 2, and the result is shown in fig. 9, and fig. 11 is a Mapping graph corresponding to the back scattering result, and it is clear from the graph that the black part is Mg phase, the dendrite gray phase is Mg 2 Ni, the light gray lump is La 2Mg17, the white lump is Y phase, and the scattering result indicates that a small amount of Y element is accumulated.
(9) As a result of back scattering analysis of Mg 3.497Ni0.170La0.028Y0.012 obtained in example 3, as shown in fig. 9, it was revealed that the black portion was Mg phase, the dendrite gray phase was Mg 2 Ni, the light gray lump was La 2Mg17, the white lump was Y phase, and scattering results indicated that more Y element was accumulated, because when La was replaced by the rare earth element Y, when the doping amount of Y element was too large, too much Y made Y compound contained in the alloy not uniformly disperse during solidification, but solidified and crystallized into larger flakes or aggregated at grain boundaries, which was unfavorable for grain refinement of the alloy, and was also responsible for the decrease in hydrogen storage performance of the alloy.
While the invention has been described in terms of preferred embodiments, it is not intended to be limited thereto, but rather to enable any person skilled in the art to make various changes and modifications without departing from the spirit and scope of the present invention, which is therefore to be limited only by the appended claims.
Claims (10)
1. A process for preparing Mg-Ni-base hydrogen-storage alloy containing rare-earth elements features that the metal element is used as raw material, which is then vacuum induction smelted and forged.
2. The method of manufacturing according to claim 1, comprising the steps of:
(1) Weighing Mg, ni, la and Y metal simple substances according to the chemical formula of the hydrogen storage alloy;
(2) Uniformly mixing all the metal simple substances weighed in the step (1), putting the mixture into a smelting crucible, and covering a crucible cover;
(3) Heating the smelting crucible to 400-500 ℃, keeping the temperature at 2-3 min ℃ and introducing SF 6 gas to replace air;
(4) And under the condition of keeping the introduction of SF 6 gas, heating to 1000-1050 ℃, preserving heat for 3-5 min, continuously heating to 1100-1150 ℃, preserving heat for 10min, and pouring to obtain the hydrogen storage alloy.
3. The method according to claim 2, wherein the Mg metal element is added in an amount of 5wt.% based on the Mg metal element in the raw material in (1).
4. The method according to claim 2, wherein 1wt.% of elemental Y metal is additionally added to the feedstock in (1).
5. The preparation method according to claim 2, wherein a simple substance of La metal is additionally added in an amount of 1wt.% based on the simple substance of La metal in the raw material.
6. The method according to claim 1, wherein the rare earth element-containing mg—ni-based hydrogen storage alloy has a chemical formula of Mg 3.497Ni0.170LaxYy, wherein 0.0288.ltoreq.x.ltoreq. 0.0360,0.ltoreq.y.ltoreq.0.012.
7. The method of claim 6, wherein x is 0.032 and y is 0.006.
8. The process of claim 6, wherein x is 0.028 and y is 0.012.
9. The method of claim 6, wherein x is 0.036 and y is 0.
10. The method according to claim 1, wherein the Mg-Ni-based hydrogen storage alloy containing rare earth element obtained by the preparation has a hydrogen storage amount of 4.645wt.% at 220 ℃ and 5 MPa.
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