CN115838882A - Hydrogen compression rare earth hydrogen storage material and preparation method thereof - Google Patents
Hydrogen compression rare earth hydrogen storage material and preparation method thereof Download PDFInfo
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- CN115838882A CN115838882A CN202211567476.4A CN202211567476A CN115838882A CN 115838882 A CN115838882 A CN 115838882A CN 202211567476 A CN202211567476 A CN 202211567476A CN 115838882 A CN115838882 A CN 115838882A
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 111
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 111
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 230000006835 compression Effects 0.000 title claims abstract description 40
- 238000007906 compression Methods 0.000 title claims abstract description 40
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 20
- 239000011232 storage material Substances 0.000 title claims abstract description 20
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000010521 absorption reaction Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 12
- 239000011261 inert gas Substances 0.000 claims description 11
- 229910052746 lanthanum Inorganic materials 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 150000002431 hydrogen Chemical class 0.000 claims description 8
- 238000003723 Smelting Methods 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 150000002739 metals Chemical class 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000002074 melt spinning Methods 0.000 claims 1
- 239000000956 alloy Substances 0.000 abstract description 29
- 229910045601 alloy Inorganic materials 0.000 abstract description 29
- 230000001351 cycling effect Effects 0.000 abstract description 2
- 238000003860 storage Methods 0.000 description 20
- 238000003795 desorption Methods 0.000 description 13
- 230000006698 induction Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 238000010276 construction Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910004247 CaCu Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
Abstract
The invention provides a hydrogen compression rare earth hydrogen storage material, which reduces alloy lag by partially replacing Ni with Fe, improves the compression ratio of the alloy and improves the cycling stability of the alloy; and adjusting the alloy hydrogen absorbing and releasing platform pressure by adjusting the La/Ce ratio; since the price of Ni in the hydrogen compression material is about 50 times of that of Fe, partial Fe replaces Ni to effectively reduce the preparation cost of the alloy.
Description
Technical Field
The invention relates to a rare earth hydrogen storage material, in particular to a preparation method and application of a hydrogen compression material.
Background
With the development of hydrogen fuel cell electric vehicles, research and construction of hydrogen energy infrastructures have attracted general attention of various countries, but the traditional mechanical hydrogen compressor has the defects of large size, heavy weight, high power consumption, high water consumption, low energy efficiency and the like, and related core technologies are firmly mastered in developed capital countries such as European and American days, so that the construction cost of a hydrogen charging station is extremely high.
The metal hydride hydrogen compressor utilizes hydrogen storage alloy (hydrogen compression material) at different temperatures
The platform pressure is different for pressurization. The alloy absorbs low-pressure hydrogen at low temperature and releases high-pressure hydrogen at high temperature, and the whole process is finished.
LaNi 5 Is the most commonly used hydrogen storage alloy having CaCu 5 The hexagonal structure has the advantages of good dynamic performance, excellent hydrogen absorption and desorption performance, large effective hydrogen storage amount, small lag, good poisoning resistance performance and the like. For LaNi 5 The alloy, ce replaces La can adjust the hydrogen absorbing and releasing platform and the circulation stability of the hydrogen storage alloy. However, as the Ce content increases, the hydrogen storage alloy has too large plateau hysteresis, and the compression ratio of the alloy is reduced.
Wherein, the hysteresis coefficient expresses that the hysteresis of the hydrogen absorbing/desorbing process leads to the pressure difference of the alloy hydrogen absorbing/desorbing platform, and the calculation formula is Hf = ln (P hydrogen absorbing/P hydrogen desorbing). The hydrogen compression material absorbs hydrogen at low temperature, releases hydrogen at high temperature, and the pressure rise after temperature rise is reduced due to the overlarge hysteresis coefficient, so that the compression efficiency is reduced.
Disclosure of Invention
Aiming at the large platform lag after Ce is added, the invention can effectively reduce the platform lag and improve the high compression ratio of the material by partially replacing Ni with Fe.
The invention is realized by the following technical scheme:
a hydrogen compression rare earth hydrogen storage material has a structural general formula of La1-xCexNi5-yFey, wherein x = 0.1-0.8, and y = 0.3-1.3.
Preferably, x = 0.7-0.8, y = 0.8-1.1 in the structural general formula, and the hydrogen-absorbing platform pressure of the hydrogen-compressed rare earth hydrogen storage material is 21.92-42.26 atm at 25 ℃; the lag between the hydrogen absorption platform and the hydrogen discharge platform is less than 0.56; the compression ratio is more than 2.8 at the temperature of 25-85 ℃.
Preferably, x = 0.1-0.3, y =0.7 in the general structural formula, and the hydrogen storage material for hydrogen compression rare earth has a hydrogen absorption platform pressure of 2.38-3.98 atm and a hydrogen discharge platform pressure of 4.67-7.33 atm at 25 ℃; the lag between the hydrogen absorption platform and the hydrogen discharge platform is less than 0.35; the compression ratio is 1.84-1.97 at 25-50 ℃.
Another object of the present invention is to provide a method for preparing the hydrogen-compressed rare earth hydrogen storage material, so as to reduce the preparation cost of the alloy.
The method is realized by the following technical scheme:
a manufacturing method of a hydrogen compression rare earth hydrogen storage material comprises the steps of weighing La, ce, ni and Fe according to each atomic proportion of the structural general formula, wherein the La and Ce are excessive by 0.8wt%, heating and melting the metals in a vacuum atmosphere, and then filling inert gas for smelting to obtain the hydrogen compression rare earth hydrogen storage material.
Preferably, the atmosphere is purged with an inert gas before the vacuum atmosphere is formed.
Preferably, the inert gas is argon.
Preferably, the vacuum degree of the vacuum atmosphere is lower than 4Pa.
Preferably, the filling pressure of the inert gas is 0.05-0.07 Mpa.
Preferably, the metal is first preheated, then melted and finally melt spun at a speed of 3 m/s.
Compared with the prior art, the invention has the beneficial effects that: the hydrogen compression rare earth hydrogen storage material reduces alloy lag by partially replacing Ni with Fe, improves the compression ratio of the alloy and improves the cycling stability of the alloy; and adjusting the alloy hydrogen absorbing and releasing platform pressure by adjusting the La/Ce ratio; since the price of Ni in the hydrogen compression material is about 50 times of that of Fe, partial Fe replaces Ni to effectively reduce the preparation cost of the alloy.
Drawings
In order to more clearly illustrate the technical solution in the embodiment of the present invention, the following further describes the seat of the present invention with reference to the drawings of the specification.
FIG. 1 is a PCT plot for example 9 of the present invention;
FIG. 2 is a graph comparing data from the cycle performance test conducted on example 9 of the present invention;
FIG. 3 PCT plot for inventive example 10;
FIG. 4 PCT graph for inventive example 11;
FIG. 5 PCT graph for inventive example 12;
figure 6 PCT profile for inventive example 13.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples, but the scope of the present invention is not limited thereto.
Examples 1 to 6:
in order to illustrate the action of Ce, 4kg of metal La, ce and Ni are weighed according to components, wherein the La and Ce are excessive by 0.8wt%, and the metal La, ce and Ni are placed in a crucible of a medium-frequency induction melting furnace; and cleaning by inert gas, vacuumizing, filling argon protective gas, and smelting under medium-frequency induction to obtain hydrogen compression material examples 1-6.
The alloy after crushing is screened by a 100-mesh screen by adopting a mechanical crushing mode, and the alloy is activated and subjected to performance test by adopting a Sieverts type hydrogen storage material performance test system of AMC company in America. And (2) putting about 2g of sample into a sample rod of a hydrogen storage performance testing system, vacuumizing for 30min at 80 ℃, cooling to 25 ℃, introducing 5MPa of high-purity hydrogen to activate and absorb hydrogen, and vacuumizing for 30min at 80 ℃ after the sample is saturated by absorbing hydrogen to fully dehydrogenate the sample to complete activation for 1 time. In order to ensure that the sample is fully activated, the sample needs to be subjected to 2 hydrogen absorption and desorption processes. After the sample is completely activated, the sample is subjected to a P-C-T (pressure-volume-temperature) curve test, and the hydrogen storage capacity and the platform characteristic of the sample are analyzed.
Table 1 shows the compositions and hydrogen storage performance parameters (25 ℃ C.) for examples 1 to 6. From examples 1 to 6, it is understood that the hydrogen absorption/desorption plateau of the alloy is increased with the addition of Ce, but the hysteresis coefficient is also significantly increased.
TABLE 1 compositions and Hydrogen storage Performance parameters (25 ℃ C.) for examples 1-6
Examples 7 to 9:
in order to discuss the effect of Fe, 4kg of metals La, ce, ni and Fe are weighed according to the components, wherein La and Ce are excessive by 0.8wt% and are placed in a crucible of a medium-frequency induction melting furnace; and cleaning by inert gas, vacuumizing, filling argon protective gas, and smelting under medium-frequency induction to obtain hydrogen compression material examples 7-9. The alloys of examples 7 to 9 were crushed and subjected to a P-C-T (pressure-volume-temperature) curve test to analyze the hydrogen storage capacity and the plateau characteristics thereof.
Table 2 shows the composition and hydrogen storage performance parameters (25 ℃ C.) for examples 7 to 9. It is understood from Table 2 that partial replacement of Ni with Fe effectively reduces the hysteresis of the alloy. Examples 7 to 9 contained more Ce than example 6, and the absorption/desorption plateau hysteresis thereof was more than 1.78. However, since the addition of Fe causes the hydrogen absorption stage to rise and the hydrogen desorption stage to fall, the hysteresis of the hydrogen absorption/desorption stage is greatly reduced to 0.56 or less. It is found that in examples 7 to 9, too much addition of Fe causes a significant decrease in the amount of hydrogen stored, and the hysteresis coefficient also becomes large.
TABLE 2 compositions and Hydrogen storage Performance parameters (25 ℃ C.) for examples 7 to 9
Since example 9 has a good combination property, the hydrogen storage platform characteristics, compression ratio and cycle stability were analyzed by performing a P-C-T (pressure-capacity-temperature) curve test at 85 ℃ and 1000 cycle tests. FIG. 1 is a PCT curve for example 9 at 25 and 85 ℃. As can be seen from FIG. 1, example 9 has a relatively flat hydrogen absorption/desorption plateau with little hysteresis, an effective hydrogen storage capacity of more than 1.20wt, and a compression ratio of 2.83 at 25-85 ℃. FIG. 2 is the 1000 cycle performance of example 9 at 25 ℃. As can be seen from FIG. 2, in example 9, after 1000 cycles, the hysteresis coefficient is still kept low, and the capacity retention rate reaches 92.4%. Thus, example 9 has excellent hydrogen absorption/desorption cycle stability.
Examples 10 to 13:
in addition, the effect of reducing the amount of Fe added was also investigated. The hydrogen storage performance of La1-xCexNi4.3Fe0.7 (x =0.1 to 0.3) was investigated by reducing the amount of Fe added to y = 0.7. Weighing 4kg of metals La, ce, ni and Fe according to the components, wherein the La and Ce are excessive by 0.8wt%, and placing the metals in a crucible of a medium-frequency induction smelting furnace; and cleaning the hydrogen compression material by inert gas, vacuumizing the hydrogen compression material, filling argon protective gas into the hydrogen compression material, and smelting the hydrogen compression material under medium-frequency induction to obtain the hydrogen compression material of the embodiments 10 to 13. After crushing the alloys of examples 10 to 13, P-C-T (pressure-volume-temperature) curve tests were carried out at 25 ℃ and 50 ℃ to analyze the hydrogen storage plateau characteristics and the compression ratio.
FIGS. 2-6 are PCT curves at 25 and 50 ℃ for examples 10-13. As can be seen from FIGS. 2 to 6, examples 10 to 13 had relatively flat hydrogen absorption/desorption platforms with small hysteresis and an effective hydrogen storage amount exceeding 1.30 wt.
Table 3 shows the composition and hydrogen storage performance parameters of examples 10 to 13. As is clear from Table 3, the hydrogen absorption/desorption plateau of the alloy rises as the addition amount of Ce increases, but the hysteresis of the hydrogen absorption/desorption plateau is maintained at 0.31 to 0.35 by the addition of Fe. The compression ratios of examples 10 to 13 were all over 1.84 at 25 to 50 ℃. Comparing examples 7 to 9 with examples 10 to 13, it was found that a smaller Fe addition was more favorable for obtaining an alloy having a low hydrogen absorption/desorption plateau hysteresis and a high compression ratio.
Furthermore, examples 2 and 10, and examples 3 and 12, which contain the same La/Ce ratio, and partially replace Ni with Fe, the alloy shows a decrease in hydrogen absorption/desorption plateau and hydrogen storage capacity, but a significant decrease in hysteresis coefficient, again demonstrating the effect of Fe addition on increasing compression ratio.
Therefore, by partially replacing Ni with Fe, alloy lag is reduced, and the La/Ce ratio is adjusted, so that a series of hydrogen compression materials with wide platforms, high compression ratios and good cycle performance can be prepared.
TABLE 3 compositions and Hydrogen storage Performance parameters for examples 10-13
Claims (9)
1. A hydrogen-compressed rare earth hydrogen storage material is characterized in that: the general formula of the structure is
La 1-x Ce x Ni 5-y Fe y Wherein x =0.1 to 0.8, y =0.3 to 1.3.
2. A hydrogen compressed rare earth hydrogen storage material as claimed in claim 1, wherein: x = 0.7-0.8, y = 0.8-1.1 in the structural general formula, and the hydrogen absorption platform pressure of the hydrogen compression rare earth hydrogen storage material is 21.92-42.26 atm at 25 ℃; the lag between the hydrogen absorption platform and the hydrogen discharge platform is less than 0.56; the compression ratio is more than 2.8 at the temperature of 25-85 ℃.
3. A hydrogen-compressing rare earth hydrogen storage material as claimed in claim 1, wherein: x = 0.1-0.3, y =0.7 in the street general formula, when the hydrogen compression rare earth hydrogen storage material is at 25 ℃, the pressure of a hydrogen absorption platform is 2.38-3.98 atm, and the pressure of a hydrogen discharge platform is 4.67-7.33 atm; the lag between the hydrogen absorption platform and the hydrogen discharge platform is less than 0.35; the compression ratio is 1.84-1.97 at 25-50 ℃.
4. A method of making a hydrogen storage material comprising a rare earth element as claimed in claim 1, wherein: weighing metals La, ce, ni and Fe according to the atomic proportion of the general structural formula, wherein the excess of La and Ce is 0.8wt%, heating and melting the metals in a vacuum atmosphere, and then charging inert gas for smelting to obtain the hydrogen compression rare earth hydrogen storage material.
5. The method of claim 4, wherein the method comprises the steps of: before forming the vacuum atmosphere, atmosphere cleaning is carried out by inert gas.
6. The method for producing a hydrogen-compressed rare earth hydrogen storage material as claimed in claim 4 or 5, wherein: the inert gas is argon.
7. The method of claim 4, wherein the method comprises the steps of: the vacuum degree of the vacuum atmosphere is lower than 4Pa.
8. The method of claim 4, wherein said rare earth material is selected from the group consisting of: the filling pressure of the inert gas is 0.05-0.07 Mpa.
9. The method of claim 4, wherein the method comprises the steps of: firstly, preheating metal, then melting, and finally carrying out melt-spinning melting at the speed of 3 m/s.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1259584A (en) * | 2000-01-20 | 2000-07-12 | 南开大学 | Hydrogen storage alloy/carbon nanometer tube composite hydrogen storage material |
| CN101871060A (en) * | 2010-06-21 | 2010-10-27 | 桂林电子科技大学 | Nickel-hydrogen battery negative electrode hydrogen storage material capable of being used at low temperature and matched electrolytic solution thereof |
| CN102230111A (en) * | 2011-05-31 | 2011-11-02 | 四川宝生实业发展有限公司 | High iron hydrogen storage electrode alloy, preparation method thereof and nickel-hydrogen battery cathode material |
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- 2022-12-07 CN CN202211567476.4A patent/CN115838882A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1259584A (en) * | 2000-01-20 | 2000-07-12 | 南开大学 | Hydrogen storage alloy/carbon nanometer tube composite hydrogen storage material |
| CN101871060A (en) * | 2010-06-21 | 2010-10-27 | 桂林电子科技大学 | Nickel-hydrogen battery negative electrode hydrogen storage material capable of being used at low temperature and matched electrolytic solution thereof |
| CN102230111A (en) * | 2011-05-31 | 2011-11-02 | 四川宝生实业发展有限公司 | High iron hydrogen storage electrode alloy, preparation method thereof and nickel-hydrogen battery cathode material |
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