CN1175120C - New-type hydrogen-storing RE electrode alloy and its heat treatment process - Google Patents
New-type hydrogen-storing RE electrode alloy and its heat treatment process Download PDFInfo
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- CN1175120C CN1175120C CNB011452501A CN01145250A CN1175120C CN 1175120 C CN1175120 C CN 1175120C CN B011452501 A CNB011452501 A CN B011452501A CN 01145250 A CN01145250 A CN 01145250A CN 1175120 C CN1175120 C CN 1175120C
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- 239000000956 alloy Substances 0.000 title claims abstract description 61
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 59
- 238000010438 heat treatment Methods 0.000 title claims abstract description 6
- 238000000034 method Methods 0.000 title abstract description 6
- 238000000137 annealing Methods 0.000 claims abstract description 7
- 229910052796 boron Inorganic materials 0.000 claims abstract description 6
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 6
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 4
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 3
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 3
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 3
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 3
- 229910052802 copper Inorganic materials 0.000 claims abstract description 3
- 229910052742 iron Inorganic materials 0.000 claims abstract description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 3
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 3
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 3
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 3
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 3
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 238000003723 Smelting Methods 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 9
- 150000002910 rare earth metals Chemical class 0.000 abstract description 9
- 229910052749 magnesium Inorganic materials 0.000 abstract description 3
- 229910052790 beryllium Inorganic materials 0.000 abstract 1
- 229910052793 cadmium Inorganic materials 0.000 abstract 1
- 229910052735 hafnium Inorganic materials 0.000 abstract 1
- 229910052758 niobium Inorganic materials 0.000 abstract 1
- 229910052763 palladium Inorganic materials 0.000 abstract 1
- 229910052698 phosphorus Inorganic materials 0.000 abstract 1
- 229910052697 platinum Inorganic materials 0.000 abstract 1
- 229910052707 ruthenium Inorganic materials 0.000 abstract 1
- 229910052706 scandium Inorganic materials 0.000 abstract 1
- 238000005204 segregation Methods 0.000 abstract 1
- 229910052712 strontium Inorganic materials 0.000 abstract 1
- 229910052715 tantalum Inorganic materials 0.000 abstract 1
- 229910052721 tungsten Inorganic materials 0.000 abstract 1
- 238000003860 storage Methods 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 238000011068 loading method Methods 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 230000005518 electrochemistry Effects 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 229910000905 alloy phase Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052987 metal hydride Inorganic materials 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- 229910000967 As alloy Inorganic materials 0.000 description 1
- 229910019080 Mg-H Inorganic materials 0.000 description 1
- 229910003307 Ni-Cd Inorganic materials 0.000 description 1
- 229910002640 NiOOH Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910010380 TiNi Inorganic materials 0.000 description 1
- RZJQYRCNDBMIAG-UHFFFAOYSA-N [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] Chemical class [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] RZJQYRCNDBMIAG-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000004087 circulation Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 229910001068 laves phase Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
Classifications
-
- 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
- Y02E60/10—Energy storage using batteries
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention discloses novel hydrogen-storing RE electrode alloy and a heat treatment method thereof. A molecular formula of the novel hydrogen-storing RE electrode alloy is A<1-y>B<y>C<x>, wherein A is composed of one or two or more than two kinds of components of La, mixed rare earth Ml rich in the La, Ce, mixed rare earth Mm rich in the Ce, Pr and Nd, B is composed of one or two or more than two kinds of components of Mg, Ca, Be, Sr and Ba C is composed of one or two or more than two kinds of components of Mn, Fe, Mo, Co, Al, Si, Ga, S, Pt, Sc, Ti, V, Cr, Cu, Zn, Zr, Nb, Ru, Pd, Cd, W, Hf, Ta, B and P and y and x meet the following requirements of 0.01 <=y<=0.8 and 2.0<=x<=4.0. The heat treatment method of the present invention comprises the steps that firstly, the hydrogen-storing electrode alloy is heated up to certain temperature under high vacuum environment; then, heat is preserved for numbers of hours for annealing treatment. Because an internal structure of the electrode alloy which is treated by using the heat method is more uniform, and some segregation phases are eliminated simultaneously, the electrochemical performance of discharge capacity, cycle life, etc. of an alloy electrode is obviously improved.
Description
Technical field
The present invention relates to secondary cell, especially relate to a kind of nickel-metal hydrides (Ni-MH) secondary battery cathode material New-type hydrogen-storing RE electrode alloy and preparation method thereof.
Background technology
In recent years; along with popularizing of household electrical appliance such as mobile telephone, portable computer and pick up camera; demand to chargeable battery increases day by day, and simultaneously because requirement on environmental protection, countries in the world all have high-energy-density, long lifetime and pollution-free green battery being devoted to research.Because nickel-metal hydrides (Ni-MH) secondary cell, with respect to the Ni-Cd secondary cell, advantages such as having the capacity height, have extended cycle life, memory-less effect, anti-over-charging are crossed the strong and non-environmental-pollution of exoergic power and become the focus of lot of domestic and foreign scholar's research.
The anodal general nickel electrode that adopts of nickle-metal hydride secondary battery, negative material then is selected from hydrogen-storage alloy.Theoretically, the hydrogen-storage alloy that can be used as the Ni-MH secondary battery cathode material comprises rare earth based AB
5Type alloy, AB
2Type Laves phase alloy, Magnuminium and vanadium radical sosoloid alloy.Wherein, people are to rare earth based AB
5The research of type alloy is the most ripe, and it has high-energy-density density, high charge-discharge speed, and overcharging resisting, cross and put, memory-less effect, good comprehensive performances such as low pollution have now realized industrialization production.But, rare earth based AB
5Type hydrogen-occlussion alloy electrode finite capacity is about about 280~320mAh/g, and the shortcoming of their ubiquity battery lack of homogeneitys.Here except that cell integrated design, negative pole technology and the influence of other associated materials, unstable properties also was one of reason during storage alloy material for hydrogen was produced in enormous quantities.In addition, from the requirement in Ni/MH battery practical application market, battery need reach 1C, 100%DOD, and cycle life improves the erosion resistance of alloy material in alkaline electrolyte and is still an important topic more than 500 time.Moreover, battery in the 1C charging later stage, press too high and when 1C discharges average voltage on the low side, this also is a big problem.
At present in the world the research of high-performance hydrogen-storage electrode metal is mainly concentrated on AB
2Type Laves hydrogen storage alloy phase, magnesium base hydrogen-storing alloy and vanadium radical sosoloid alloy.AB
2Type Laves hydrogen storage alloy phase exists alloy P-C-T curve platform gradient bigger, and the electrode surface reaction resistance is higher, causes the high-rate discharge ability of electrode relatively poor relatively bigger with the inclination of battery discharge voltage platform.In addition, AB
2Also there are problems such as the initial stage activation is difficult, the prices of raw and semifnished materials are higher relatively in type Laves hydrogen storage alloy phase.
The V radical sosoloid alloy is not owing to itself possess electrode activity, thereby its electrochemical applications seldom studied, though studies show that recently by after separating out the good TiNi grade in an imperial examination two-phase of electro catalytic activity on the crystal boundary of V based solid solution, can obtain high electrochemistry capacitance, but its cyclical stability is very poor, remain further to be studied to improve, and the price of V is higher.
Magnesium base hydrogen-storing alloy is a much-talked-about topic in the research of Ni/MH battery, but the chemical impellent of Mg-H reaction is very low, and the hydride of formation is too stable, is difficult to carry out more much practical applications.Alloy loading capacity decline simultaneously is very fast, and the corrosion in alkaline electrolyte is still a great problem, and also need effort for a long time make a breakthrough.
New-type hydrogen-storing RE electrode alloy has higher electrochemical discharge capacity.Kohno has studied La
5Mg
2Ni
23The electrochemical discharge capacity of type hydrogen-occlussion alloy electrode can reach 400mAh/g, has surmounted rare earth based AB greatly
5The loading capacity of type hydrogen-occlussion alloy electrode.And its alloy electrode has good cyclical stability, good high magnification characteristic and advantage such as activation capacity and low price and has demonstrated powerful application prospect in electrolytic solution.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of New-type hydrogen-storing RE electrode alloy.
1) New-type hydrogen-storing RE electrode alloy places vacuum magnetic suspension smelting furnace or arc melting, and the molecular formula of said alloy is A
1-yB
yC
xWherein A is one or both or the two or more composition among La, Ce, Pr, the Nd, B is one or both compositions among Mg, the Ca, C is one or both or the two or more composition among Mn, Fe, Mo, Co, Al, Si, Ga, S, Ti, V, Cr, Cu, Zn, Zr, B, the Sn, 0.01≤y≤0.8,2.0≤x≤4.0.
2) melted as cast condition hydrogen-storing alloy as electrode is placed on is evacuated to 10 in the vacuum annealing furnace
-2-10
-5Pascal;
3) hydrogen-storing alloy as electrode is heated to 650-1300 ℃ and be incubated 1-48 hour;
4) the hydrogen-storing alloy as electrode furnace cooling after the insulation is handled.
The A that adopts preparation method of the present invention to handle
1-yB
yC
xAfter hydrogen-storing alloy as electrode, the especially 850-950 ℃ * 8h thermal treatment, the loading capacity of alloy electrode is greatly improved, and simultaneously, the cyclical stability of alloy electrode also is improved, thereby has improved A
1-yB
yC
xThe comprehensive electrochemical of hydrogen-storing alloy as electrode.A of the present invention
1-yB
yC
xThe heat treating method of hydrogen-storing alloy as electrode will (comprise rare earth based AB for improving other hydrogen-storing alloy as electrode
5Type alloy, AB
2Type alloy, Magnuminium and vanadium radical sosoloid alloy) comprehensive electrochemical provide the reference frame of usefulness.
Description of drawings
Accompanying drawing is the loading capacity of cast alloy electrode of the alloy electrode handled according to embodiment and unprocessed mistake and the relation curve between the cycle index.
Embodiment
Novel rare-earth is A
1-yB
yC
xThe Heating temperature of the annealing furnace among the preparation method of hydrogen-storing alloy as electrode is 950 ℃, and soaking time is 8h.
Embodiment
According to novel rare-earth is A
1-yB
yC
xThe design mix of hydrogen-storing alloy as electrode adopts vacuum magnetic suspension stove or arc melting alloy, is designated as alloy X.Wherein, the purity of alloy constituent element is all more than 90%.Get alloy part X and enclose respectively in the vitreosil Glass tubing, the vacuum tightness in the quartz glass tube is 10
-5Pascal.Respectively pipe is put into annealing furnace then and carry out heat tracing.Heating condition is 950 ℃ * 8h, treat that soaking time arrives after, turn off annealing furnace, the alloy furnace cooling.The test of chemical property is to carry out in an open type three-electrode system, and it comprises a working electrode (being hydrogen-occlussion alloy electrode), a sintering Ni (OH)
2/ NiOOH supporting electrode and a Hg/HgO reference electrode.Electrolytic solution adopts the 6N KOH aqueous solution, and probe temperature remains on 303K.All test electrodes all are to form by uniform mixing 100mg hydrogen-storage alloy powder (300 order) and 300mg carbonyl nickel powder and the electrode slice that is pressed into diameter 10mm, thickness 1mm under the pressure of 20Mpa.Electrode adopts the electric current of 400mA/g to charge and discharge, and wherein the duration of charging is 5 hours, and the discharge stopping potential is-0.5V (with respect to the Hg/HgO reference electrode).
Comparing embodiment
The alloy X of melting does not do any processing among the selected part embodiment, makes electrode and carries out the test of electrochemistry cycle life according to the described method of embodiment.
From figure as can be seen, the high electrochemistry capacitance of alloy X under as-cast condition only has 357mAh/g, and after carrying out 950 ℃ * 8h thermal treatment, its high electrochemistry capacitance becomes 396mAh/g, improved 39mAh/g, and after 250 circulations, its capacity still is higher than the loading capacity of cast alloy.
Claims (2)
1. the preparation method of a New-type hydrogen-storing RE electrode alloy is characterized in that, it comprises the following steps:
1) New-type hydrogen-storing RE electrode alloy places vacuum magnetic suspension smelting furnace or arc melting, and the molecular formula of said alloy is A
1-yB
yC
xWherein A is one or both or the two or more composition among La, Ce, Pr, the Nd, B is one or both compositions among Mg, the Ca, C is one or both or the two or more composition among Mn, Fe, Mo, Co, Al, Si, Ga, S, Ti, V, Cr, Cu, Zn, Zr, B, the Sn, 0.01≤y≤0.8,2.0≤x≤4.0.
2) melted as cast condition hydrogen-storing alloy as electrode is placed on is evacuated to 10 in the vacuum annealing furnace
-2-10
-5Pascal;
3) hydrogen-storing alloy as electrode is heated to 650-1300 ℃ and be incubated 1-48 hour;
4) the hydrogen-storing alloy as electrode furnace cooling after the insulation is handled.
2. the preparation method of a kind of New-type hydrogen-storing RE electrode alloy according to claim 2 is characterized in that, the Heating temperature of said annealing furnace is 850-950 ℃, and soaking time is 8h.
Priority Applications (1)
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CNB011452501A CN1175120C (en) | 2001-12-26 | 2001-12-26 | New-type hydrogen-storing RE electrode alloy and its heat treatment process |
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Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB011452501A CN1175120C (en) | 2001-12-26 | 2001-12-26 | New-type hydrogen-storing RE electrode alloy and its heat treatment process |
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Publication Number | Publication Date |
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CN1375571A CN1375571A (en) | 2002-10-23 |
CN1175120C true CN1175120C (en) | 2004-11-10 |
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CNB011452501A Expired - Fee Related CN1175120C (en) | 2001-12-26 | 2001-12-26 | New-type hydrogen-storing RE electrode alloy and its heat treatment process |
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Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100399607C (en) * | 2004-03-23 | 2008-07-02 | 株式会社东芝 | Nonaqueous electrolyte secondary battery |
CN102517487B (en) * | 2011-12-13 | 2013-11-06 | 浙江大学 | Hydrogen-storage alloy producing high-pressure hydrogen |
CN105970069B (en) * | 2016-05-16 | 2018-10-02 | 昆明贵金属研究所 | More pivot equimolars are than noble metal high-entropy alloy |
CN114107739B (en) * | 2021-11-10 | 2022-05-10 | 浙江大学 | Solid rare earth hydrogen storage alloy with low hysteresis and high pulverization resistance and preparation and application thereof |
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2001
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