CN101429606B - Hydrogen storage alloy for first stage of two-stage metal hydride hydrogen compressor - Google Patents
Hydrogen storage alloy for first stage of two-stage metal hydride hydrogen compressor Download PDFInfo
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- CN101429606B CN101429606B CN2007101579685A CN200710157968A CN101429606B CN 101429606 B CN101429606 B CN 101429606B CN 2007101579685 A CN2007101579685 A CN 2007101579685A CN 200710157968 A CN200710157968 A CN 200710157968A CN 101429606 B CN101429606 B CN 101429606B
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 126
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 126
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 123
- 239000000956 alloy Substances 0.000 title claims abstract description 66
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 66
- 238000003860 storage Methods 0.000 title claims abstract description 50
- 229910052987 metal hydride Inorganic materials 0.000 title claims abstract description 32
- 150000004681 metal hydrides Chemical class 0.000 title claims abstract description 32
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 6
- 238000000137 annealing Methods 0.000 claims abstract description 5
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 4
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims description 12
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- 238000010791 quenching Methods 0.000 claims description 4
- 230000000171 quenching effect Effects 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 229910004247 CaCu Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 6
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 5
- 150000002910 rare earth metals Chemical class 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 2
- 229910004269 CaCu5 Inorganic materials 0.000 abstract 1
- 239000010453 quartz Substances 0.000 abstract 1
- 230000006835 compression Effects 0.000 description 15
- 238000007906 compression Methods 0.000 description 15
- 150000004678 hydrides Chemical class 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 230000004913 activation Effects 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000011232 storage material Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000000207 volumetry Methods 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
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Abstract
The invention relates to a rare-earth series hydrogen storage alloy, namely providing a hydrogen storage alloy La1-a-bYaNdbNicMdM'e used in the first stage of a two-stage metal hydride hydrogen compressor, wherein a is more than or equal to 0 and less than or equal to 0.7, b is more than or equal to 0 and less than or equal to 0.7, c is more than or equal to 4.7 and less than or equal to 4.9, d is more than or equal to 0 and less than or equal to 0.2, e is more than or equal to 0 and less than or equal to 0.2, and d+e is more than or equal to 0.1 and less than or equal to 0.3; M and M' are Zr, Mn or Al, and M and M' are same or different. The alloy is a single CaCu5 type hexagonal structure. The alloy production comprises a process of annealing heat treatment, the condition means that a sample is placed into a quartz tube filled with argon at a temperature of 1,273 kelvin and is annealed for 12 hours, and then is rapidly quenched into the water. The rare-earth series hydrogen storage alloy has simple alloy production method and good comprehensive property, and is quite applicable to the first-stage material of the two-stage metal hydride hydrogen compressor.
Description
Technical field
The present invention relates to a kind of rare earth based hydrogen storage alloy, a kind of hydrogen-storage alloy that is applicable to that first stage of two-stage metal hydride hydrogen compressor is used is provided.More precisely, the present invention passes through at LaNi
5Add elements such as Y, Nd, Mn, Al and Zr in the alloy, improve the comprehensive hydrogen storage performance of alloy, thereby make this material can be used as the alloy that first stage of two-stage metal hydride hydrogen compressor is used, belong to the hydrogen-storage alloy field.
Background technology
Energy shortage and the fossil-fuel-fired problem of environmental pollution that causes are serious day by day, and hydrogen is as a kind of reproducible secondary energy of cleaning, and are used widely.But the storage of Hydrogen Energy and transportation are still the key issue of restriction Hydrogen Energy development.The hydrogen source of different purity and pressure is adopted in the different application field, but most occasion adopts compressed hydrogen.Along with the development of lightweight high-pressure hydrogen storage container, compressor is had higher requirement.Traditional compression method is to adopt the reciprocating machine compressor, they not only energy consumption high and also wearing and tearing are arranged, vibration is big, noise is high.In addition, this class compressor does not possess the purification function of hydrogen.And the compression that utilizes metal hydride to carry out hydrogen is a kind of brand-new hydrogen compressed method, and it is the compression of a kind of chemical heat, does not only have the disadvantage of above-mentioned mechanical compressor fully, can also melt hydrogen purification and hydrogen pressure shrinks in one.Its advantage is: environmentally safe, and running is quiet, friction, noiselessness; No drive element; Discharge the purity height of hydrogen; Can reclaim power from low level heat source, utilize used heat current consumption few, trucking costs is low; The multistage compression can produce high pressure.
Metal hydride hydrogen compressor is to utilize the pressure and temp characteristic of hydride to carry out work, hydrogen storage material absorbs hydrogen and forms metal hydride under lesser temps and lower pressure, the temperature of metal hydride is improved in saturated back, the then corresponding raising of its equilibrium pressure, therefore the hydride that is under the high temperature can discharge corresponding highly compressed hydrogen, the principle of work of Here it is metal hydride hydrogen compressor.
High efficiency compressor depends primarily on the characteristic of used hydrogen storage material, generally speaking, wishes to be issued to the high pressure supercharging in the low-temperature heat source heating.Hydrogen compressor to hydrogen storage material require as follows:
The storage hydrogen capacity is big, good reversibility, and promptly alloy has high suction and puts Hydrogen Energy power under desired temperature; Dynamic performance is good, and speed for hydrogen absorbing and releasing is fast, so that obtain big hydrogen flowing quantity as far as possible; Smooth and the wide ranges of pressure platform, this can guarantee to obtain enough hydrogen pressure and big compressed hydrogen amounts of putting under suitable operational temperature; It is little to lag behind, to guarantee that high compression ratio is arranged (low temperature is inhaled the ratio of releasing hydrogen balance pressure under hydrogen balance pressure and the high temperature down), because the size that lags behind directly influences the compression ratio of system; Compression ratio height, high compression ratio mean can obtain higher putting hydrogen pressure or can reduce service temperature specified putting under the hydrogen pressure under certain service temperature under the lower temperature.
In order to produce ultra-high voltage hydrogen, adopt the twin-stage metal hydride hydrogen compressor usually, utilize the lower pressure stage alloy to produce higher transition hydrogen pressure exactly, behind the importing high pressure stage absorption hydrogen,, thereby produce ultra-high voltage hydrogen by water or oily as heating medium.
Choosing suitable hydride material is one of key that realizes the metal hydride compressor efficiency operation.Present most of hydrogen compressor all adopts AB with hydrogen storage material
5System and AB system, also useful V are hydride.V series hydrogen storage alloy compression ratio height, but anti-poisoning capability is poor, need be operated in the high-purity hydrogen.AB
5Be that alloy has excellent comprehensive performances, especially its smooth pressure platform characteristic and good activation performance have stronger anti-poisoning ability simultaneously, can doublely do purifying and squeezed material.Therefore we adopt LaNi
5Carry out the mode of alloying and seek the hydrogen-storage alloy that suitable first stage of two-stage metal hydride hydrogen compressor is used.
Summary of the invention
The purpose of this invention is to provide the hydrogen-storage alloy La that a kind of first stage of two-stage metal hydride hydrogen compressor is used
1-a-bY
aNd
bNi
cM
dM '
e, this alloy has higher storage hydrogen capacity, easily activation, advantage such as dynamic performance is good.
The invention provides the hydrogen-storage alloy that a kind of first stage of two-stage metal hydride hydrogen compressor is used, it is characterized in that: described alloy composition is La
1-a-bY
aNd
bNi
cM
dM '
e, 0≤a≤0.7,0≤b≤0.7,4.7≤c≤4.9,0≤d≤0.2,0≤e≤0.2 wherein, M and M ' they are Zr, Mn or Al, M and M ' are identical or different.
The hydrogen-storage alloy that first stage of two-stage metal hydride hydrogen compressor provided by the invention is used, wherein 0.1≤d+e≤0.3.
The hydrogen-storage alloy that first stage of two-stage metal hydride hydrogen compressor provided by the invention is used, wherein a=0 or b=0.
The hydrogen-storage alloy that first stage of two-stage metal hydride hydrogen compressor provided by the invention is used, wherein when a=0, M is different with M '.
The hydrogen-storage alloy that first stage of two-stage metal hydride hydrogen compressor provided by the invention is used, wherein when b=0, M is identical with M '.
The hydrogen-storage alloy that first stage of two-stage metal hydride hydrogen compressor provided by the invention is used, described alloy are single CaCu
5The type hexagonal crystallographic texture.
The hydrogen storage preparation method that the present invention also provides a kind of first stage of two-stage metal hydride hydrogen compressor to use, raw metal melting in non-consumable arc furnace is made 10～50g alloy cast ingot 3～4 times, the alloy sample that obtains is packed into and is annealed under 1223～1423K in the silica tube that is full of argon gas, annealing time is 8～15h, in the entry of quenching rapidly afterwards.
Rare earth based hydrogen storage alloy of the present invention melting preparation by the following method: preparation hydrogen-storage alloy La
1-a-bY
aNd
bNi
cM
dM '
eThe button ingot, the following La99% of the purity of raw metal, Y99%, Nd99%, Ni99.5%, Mn99.7%, Al99.5% and Zr99.5% (weight percent).Carry out proportioning raw materials by chemical formula, in non-consumable arc furnace, be smelted into the 30g alloy cast ingot then.For anti-oxidation is all carried out under argon shield atmosphere.In order to guarantee the homogeneity of alloy, alloy melt back 3 to 4 times.Because the fusing point of Mn is lower, volatilize easily during melting, so add certain weight when joining sample in proportion.The alloy sample for preparing is packed into and is annealed under 1273K in the silica tube that is full of argon gas, and annealing time is 12h, in the entry of quenching rapidly afterwards.
The activation of alloy and hydrogen storage performance test experiments all carry out on the PCT tester of development voluntarily.Suction is put hydrogen PCT curve and is all adopted volumetry.Used hydrogen purity is 99.999%, the fluctuating temperature≤1K of reactor, and the precision of pressure transmitter is 0.1%FS.Take by weighing 1g left and right sides sample and put into the sample chamber, be heated to 353K and vacuumize 30 minutes to remove sample surfaces impurity, cool to room temperature and the hydrogen that feeds 4MPa make itself and example reaction then.Inhale repeatedly and put hydrogen and guarantee under differing temps, to carry out respectively after sample fully activates the hydrogen storage performance test for 10 times.
Alloy hydrogen absorption and desorption platform lag coefficient
The calculation formula of reaction enthalpy change and reaction entropy variate adopts Van ' t Hoff formula:
(wherein, Δ H and Δ S are respectively standard enthalpy change amount and standard entropy variable).
The present invention has adopted multi-element alloyed.By the method for polynary replacement, can obtain needed decomposition pressure according to actual needs, obtain needed performance.On the other hand, rare earth of the present invention is AB
5The design of type hydrogen-storage alloy composition the time has partly adopted B side element to exceed stoichiometric ratio, and this helps inhaling, and to put the hydrogen platform smooth, reduces to lag behind and improve the resistance to chalking energy.
Description of drawings
La of the present invention
1-a-bY
aNd
bNi
cM
dM '
eHydrogen-storage alloy not only has higher storage hydrogen capacity, and easily activation, and dynamic performance is fine, and the thermal source that hydride need only 95 ℃ just can obtain higher compression ratio.This is typical waste heat supply temperatures for most of industrial plants, therefore is highly suitable for the first stage of two-stage metal hydride hydrogen compressor hydrogen-storage alloy.
Fig. 1 is La of the present invention
1-a-bY
aNd
bNi
cM
dM '
eThe XRD diffracting spectrum of alloy;
Fig. 2 is La of the present invention
1-a-bY
aNd
bNi
cM
dM '
eThe suction hydrogen kinetic curve of alloy;
Fig. 3 is La of the present invention
0.8Y
0.2Ni
4.8Mn
0.2The PCT curve of alloy;
Fig. 4 is La of the present invention
0.6Y
0.4Ni
4.8Mn
0.2The PCT curve of alloy;
Fig. 5 is La of the present invention
0.6Y
0.4Ni
4.8Al
0.2The PCT curve of alloy;
Fig. 6 is La of the present invention
0.5Y
0.5Ni
4.8Mn
0.2The PCT curve of alloy;
Embodiment
Fig. 7 is La of the present invention
0.6Nd
0.4Ni
4.8Mn
0.2Zr
0.1The PCT curve of alloy.
Preparation and test hydrogen-storage alloy La
0.8Y
0.2Ni
4.8Mn
0.2Preparation method, heat-treat condition and activation method are as mentioned above.
Test result: the hydride hydrogen storage amount that forms under 293K is 5.96, inhaling hydrogen balance pressure is 189KPa, and putting hydrogen balance pressure is 117KPa, and lag coefficient is 581.26J/mol, it is very fast to inhale hydrogen kinetics speed, reaches 90% needs 79s of maximum hydrogen when initially hydrogen pressure is for 4MPa.Activation easily.Suction is put the hydrogen enthalpy change and is respectively-28.52KJ/Mol and 30.81KJ/Mol.Suction when 368K is put hydrogen balance pressure and is respectively 2193KPa and 1645KPa, and compression ratio is 8.7.
Be with the difference of embodiment 1: preparation and test hydrogen-storage alloy La
0.6Y
0.4Ni
4.8Mn
0.2
Test result: the hydride hydrogen storage amount that forms under 293K is 5.92, inhaling hydrogen balance pressure is 386.3KPa, putting hydrogen balance pressure is 261.2KPa, lag coefficient is 953.28J/Mol, it is very fast to inhale hydrogen kinetics speed, and the 90% needed time that reaches maximum hydrogen when initially hydrogen pressure is for 4MPa is 85s.Activation easily.Suction is put the hydrogen enthalpy change and is respectively-27.4KJ/Mol and 28.1KJ/Mol.Suction when 368K is put hydrogen balance pressure and is respectively 2892KPa and 1980KPa, and compression ratio is 7.6.
Be with the difference of embodiment 1: preparation and test hydrogen-storage alloy La
0.6Y
0.4Ni
4.8Al
0.2
Test result: the hydride hydrogen storage amount that forms under 293K is 5.87, inhaling hydrogen balance pressure is 410.9KPa, and putting hydrogen balance pressure is 311KPa, and lag coefficient is 678.57J/Mol, it is very fast to inhale hydrogen kinetics speed, reaches 90% needs 100s of maximum hydrogen when initially hydrogen pressure is for 4MPa.Activation easily.Suction is put the hydrogen enthalpy change and is respectively-26.7KJ/Mol and 27.7KJ/Mol.Suction when 368K is put hydrogen balance pressure and is respectively 3587KPa and 2061KPa, and compression ratio is 5.1.
Be with the difference of embodiment 1: preparation and test hydrogen-storage alloy La
0.5Y
0.5Ni
4.8Mn
0.2
Test result: the hydride hydrogen storage amount that forms under 293K is 5.67, inhaling hydrogen balance pressure is 527KPa, and putting hydrogen balance pressure is 326KPa, and lag coefficient is 594.49J/Mol, it is very fast to inhale hydrogen kinetics speed, reaches 90% needs 92s of maximum hydrogen when initially hydrogen pressure is for 4MPa.Activation easily.Suction is put the hydrogen enthalpy change and is respectively-27.45KJ/Mol and 30.81KJ/Mol.Suction when 368K is put hydrogen balance pressure and is respectively 5142KPa and 3925KPa, and compression ratio is 7.5.
Difference from Example 1 is: preparation and test hydrogen-storage alloy La
0.6Nd
0.4Ni
4.8Mn
0.2Zr
0.1
Test result: the hydride storage hydrogen capacity that forms under 313K is 5.3, lag coefficient is 408.7J/Mol, inhaling hydrogen balance pressure when 303K is 156KPa, putting hydrogen balance pressure is 106.5KPa, it is very fast to inhale hydrogen kinetics speed, reach 90% needs 26s of maximum hydrogen when initial hydrogen pressure is for 4MPa under 313K, inhale the hydrogen discharge reaction enthalpy and be respectively-30.91KJ/Mol and 32.42KJ/Mol.Suction under 368K is put hydrogen balance pressure and is respectively 1415KPa and 1091KPa, and compression ratio is 7.0.
Claims (9)
1. hydrogen-storage alloy that first stage of two-stage metal hydride hydrogen compressor is used, it is characterized in that: described alloy composition is La
1-a-bY
aNd
bNi
cM
dM '
e, 0≤a≤0.7,0≤b≤0.7,4.7≤c≤4.9,0≤d≤0.2,0≤e≤0.2 wherein, M and M ' they are Zr, Mn or Al, M and M ' are identical or different.
2. the hydrogen-storage alloy of using according to the described first stage of two-stage metal hydride hydrogen compressor of claim 1 is characterized in that: 0.1≤d+e≤0.3.
3. the hydrogen-storage alloy of using according to the described first stage of two-stage metal hydride hydrogen compressor of claim 1 is characterized in that: a=0 or b=0.
4. the hydrogen-storage alloy of using according to the described first stage of two-stage metal hydride hydrogen compressor of claim 1, it is characterized in that: during a=0, M is different with M '.
5. the hydrogen-storage alloy of using according to the described first stage of two-stage metal hydride hydrogen compressor of claim 1, it is characterized in that: during b=0, M is identical with M '.
6. the hydrogen-storage alloy of using according to the described first stage of two-stage metal hydride hydrogen compressor of claim 1, it is characterized in that: described alloy is single CaCu
5The type hexagonal crystallographic texture.
7. hydrogen storage preparation method that the described first stage of two-stage metal hydride hydrogen compressor of claim 1 is used, it is characterized in that: raw metal melting in non-consumable arc furnace is made 10～50g alloy cast ingot 3～4 times, the alloy sample that obtains is packed into and is annealed under 1223～1423K in the silica tube that is full of argon gas, annealing time is 8～15h, in the entry of quenching rapidly afterwards.
8. the hydrogen storage preparation method of using according to the described first stage of two-stage metal hydride hydrogen compressor of claim 7, it is characterized in that: the 30g alloy cast ingot is made in raw metal melting in non-consumable arc furnace, the alloy sample that obtains is packed into and is annealed under 1273K in the silica tube that is full of argon gas, annealing time is 12h, in the entry of quenching rapidly afterwards.
9. the hydrogen storage preparation method of using according to claim 7 or 8 described first stage of two-stage metal hydride hydrogen compressor, it is characterized in that: the weight percent of the purity of described raw metal is La99%, Y99%, Nd99%, Ni99.5%, Mn99.7%, Al99.5% and Zr99.5%.
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| CN1651587A (en) * | 2005-02-02 | 2005-08-10 | 华南理工大学 | REMg3 type hydrogen storage alloy and its preparation method |
| CN1712550A (en) * | 2004-06-23 | 2005-12-28 | 中国科学院金属研究所 | Hydrogen-storage alloy of metal oxide for air-conditioner |
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| CN1712550A (en) * | 2004-06-23 | 2005-12-28 | 中国科学院金属研究所 | Hydrogen-storage alloy of metal oxide for air-conditioner |
| CN1651587A (en) * | 2005-02-02 | 2005-08-10 | 华南理工大学 | REMg3 type hydrogen storage alloy and its preparation method |
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