CN101740770A - RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery and storage battery thereof - Google Patents

RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery and storage battery thereof Download PDF

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CN101740770A
CN101740770A CN200910266237A CN200910266237A CN101740770A CN 101740770 A CN101740770 A CN 101740770A CN 200910266237 A CN200910266237 A CN 200910266237A CN 200910266237 A CN200910266237 A CN 200910266237A CN 101740770 A CN101740770 A CN 101740770A
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alloy
storage battery
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temperature
hydrogen storage
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闫慧忠
熊玮
孔繁清
李宝犬
李金�
王利
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Ruike Rare Earth Metallurgy and Functional Materials National Engineering Research Center Co Ltd
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Ruike Rare Earth Metallurgy and Functional Materials National Engineering Research Center Co Ltd
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Abstract

The invention relates to an RE-Fe-B serial hydrogen storage alloy for a low-temperature storage battery and a storage battery thereof, wherein the preparation raw materials of the RE-Fe-B serial hydrogen storage alloy for the low-temperature storage battery comprise RE (rare earth) and a simple substance of a substituted element thereof, Fe and the simple substance of the substituted element thereof, B and the simple substance of the substituted element thereof, an RE-Fe alloy, a B-Fe alloy, a B-Ni alloy, an RE-Fe-B alloy, an LaNi5 type alloy and other intermediate alloys containing composition elements in alloy compositions, and the RE-Fe-B serial hydrogen storage alloy is prepared by selecting two or more raw materials according to a chemical composition formula of the alloy. The cathode active material of the storage battery is the RE-Fe-B serial hydrogen storage alloy for the low-temperature storage battery. The RE-Fe-B serial hydrogen storage alloy has the advantages that the alloy has good activation performance, and the electrochemical capacity after activation for 1-3 times is larger than 300mAh/g; a hydrogen storage alloy electrode has good low-temperature discharge performance, and the discharge capacity at the temperature of 40 DEG C below zero is 50 percent larger than the rated capacity; and the hydrogen storage alloy electrode has excellent rate discharge capability and good dynamic performance, the charge efficiency of 3C(0.9A/g)-10C(3A/g) reaches more than 90 percent, and the discharge time of 30C(10A/g) is longer than 10 seconds.

Description

RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery and storage battery thereof
Technical field:
The present invention relates to a kind of RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery and storage battery thereof, belong to battery and battery and use the hydrogen-storage alloy field.
Background technology:
Alkalescence ni-mh (MH-Ni) but secondary cell has advantages such as high-energy-density fast charging and discharging, pollution-free and long-life, be widely used in portable radio communication equipment and household electrical appliance.The high-power Ni hydrogen battery also is the main power supply of hybrid electric vehicle (HEV) and electric motor car new-energy automobiles such as (EV).
It is AB that the negative electrode active material of present Ni-MH battery generally adopts rare earth 5(LaNi 5) the type hydrogen-storage alloy, its serviceability temperature generally in-20～50 ℃ of scopes, is mainly used under 0～40 ℃ of condition.In fields such as cold district (40 ℃) and military affairs, Aero-Space, Ni-MH battery can't satisfy instructions for use, and especially the Ni-MH power cell that uses of HEV and EV must guarantee the cold start-up of automobile under low temperature environment.
The cryogenic property of Ni-MH battery with just/negative material, barrier film, electrolyte and battery design all have certain relation, but depend primarily on the low temperature performance of metal-hydride negative alloy.Chinese patent " cathode hydrogen-stored material and the battery thereof that can be used for the low temperature nickel hydrogen battery " (200510123747.7) and " a kind of hydrogen storage alloy for low temperature Ni-MH power cell " (200810027969.2) all disclose a kind of hydrogen-storage alloy that is used for the use of low temperature (being low to moderate-40 ℃) Ni-MH battery, but the hydrogen-storage alloy of being invented is still traditional LaNi 5The improvement of type hydrogen-storage alloy, and the not mentioned combination properties such as activity function, cycle life that comprise.
Patent of invention " RE-Fe-B base hydrogen storage alloy " (200810176872.8), " La 15Fe 77B 8Type hydrogen storage alloy and uses thereof " point out that RE-Fe-B is that hydrogen storage material can replace the LaNi in the nickel-hydrogen secondary cell in (200810176873.2) 5The type hydrogen-storing alloy as electrode significantly reduces the cost of Ni-MH battery, but does not relate to low temperature performance.
Summary of the invention:
The objective of the invention is according to RE-Fe-B is that the chemical constitution formula of alloy provides a kind of RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery and storage battery thereof.The present invention is by the partly or entirely alternative and suitable preparation condition of some element to RE, Fe, B element in the RE-Fe-B series alloy, and making RE-Fe-B is that alloy becomes the good hydrogen-storage alloy of low temperature performance.Contain the B element in the composition of the RE-Fe-B series hydrogen storage alloy of being invented, and have rich iron second phase of high catalytic activity, can significantly improve low temperature (40 ℃) electrochemical properties.The RE-Fe-B series hydrogen storage alloy of being invented can be used to prepare low temperature nickel hydrogen battery and metal hydride air battery.
The chemical constitution formula of RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery of the present invention is: RE 8Fe 27B 24, RE 8Fe 28B 24(RE 2Fe 7B 6), RE 15Fe 77B 8Or RE 17Fe 76B 7In a kind of, wherein: RE is one or more in rare-earth elements of lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu), scandium (Sc) and the yttrium (Y), and RE can be formed one or more all or part of replacements in the magnesium (Mg), calcium (Ca), zirconium (Zr), titanium (Ti), vanadium (V) element of hydride with hydrogen in the periodic table of chemical element; Fe (iron) can be by one or more all or part of replacements among the transition metal nickel (Ni) in the periodic table of chemical element, manganese (Mn), aluminium (Al), cobalt (Co), copper (Cu), zirconium (Zr), titanium (Ti), vanadium (V), zinc (Zn), chromium (Cr), tungsten (W) and nontransition metal element gallium (Ga), tin (Sn), plumbous (Pb); B (boron) can be by one or more all or part of replacements in metallic elements of ferrum (Fe), nickel (Ni), manganese (Mn), aluminium (Al), cobalt (Co), copper (Cu), zirconium (Zr), titanium (Ti), vanadium (V), zinc (Zn), chromium (Cr), tungsten (W), gallium (Ga), tin (Sn), plumbous (Pb) and nonmetalloid silicon (Si), sulphur (S), carbon (C), the phosphorus (P).
The preparation raw material of described RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery are simple substance, RE-Fe alloy, B-Fe alloy, B-Ni alloy, RE-Fe-B alloy, the LaNi of simple substance, B and substitute element thereof of simple substance, Fe and the substitute element thereof of RE (rare earth) in the alloy composition and substitute element thereof 5Type alloy and other contain the intermediate alloy of component, select wherein the chemical constitution formula preparation of two or more raw material according to alloy.
Each atoms of elements ratio can be adjusted in ± 10% scope during described RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery was formed.
High melt casting or high melt-quick quenching technique are adopted in the preparation of described RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery; wherein; the THICKNESS CONTROL of fast quenching alloy sheet is below 1.0mm, and preparation process need be carried out under inert gas shielding or under vacuum environment.
The alloy of ingot of described RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery and fast quenching alloy sheet are in the environment of 10-2-10-6Pa in vacuum degree, the heat treatment of perhaps annealing in the environment of inert gas shielding.Anneal heat treated temperature between 600-1050 ℃, be incubated 2-24 hour, the hydrogen-storage alloy after the insulation is with the stove cool to room temperature.
Described RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery adopts one or more methods in airflow milling, ball milling, sledge mill, the high temperature atomization method to unite and uses the powder that is prepared into 30-150 μ m.
The present invention provides also that to contain described low-temperature storage battery be the nickel-hydrogen secondary cell and metal hydride air (MH-Air) battery of metal-hydride negative alloy with RE-Fe-B, and such battery comprises positive pole, barrier film, negative pole and electrolyte, and they are packaged in the battery case.The negative electrode active material of nickel-hydrogen secondary cell and metal hydride air battery is described RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery.
The main distinction of the present invention and prior art: the low temperature of the present invention RE-Fe-B series hydrogen storage alloy that uses for nickel-hydrogen battery has good cryogenic discharging characteristic and heavy-current discharge characteristic.
The effect of invention:
Low-temperature storage battery of the present invention has good activity function with the RE-Fe-B alloys for hydrogen-bearing electrode, and 1-3 activation back electrochemistry capacitance is greater than 300mAh/g; This hydrogen-occlussion alloy electrode has good low temperature performance, and-40 ℃ discharge capacity is greater than 50% of rated capacity; This hydrogen-occlussion alloy electrode multiplying power discharging ability excellence has good dynamic performance, and the charge efficiency of 3C (0.9A/g)-10C (3A/g) reaches more than 90%, and 30C (10A/g) discharge time is greater than 10s; This hydrogen bearing alloy is owing to distinctive The Nomenclature Composition and Structure of Complexes has excellent corrosion resisting performance, thereby has the favorable charge-discharge cyclical stability, charge and discharge circulation life 〉=500 time; The manufacturing of this hydrogen bearing alloy can be used as cheap raw material such as Fe and can not use as Co etc. and be worth higher raw material, therefore has lower cost, and cost is than traditional LaNi 5The type alloy reduces more than 10%.Adopt hydrogen-storage alloy of the present invention can make nickel-hydrogen secondary cell and the metal hydride air battery that satisfies instructions for use under the low temperature.
Embodiment:
Embodiment 1.
Is RE in the alloy according to institute's invention low-temperature storage battery with RE-Fe-B 8Fe 27B 24Chemical constitution formula, RE is a rare earth element, partly substitutes Fe, B element with Ni, Mn, Al, Cu element, prepared alloy composition such as table 1 are listed.Stoichiometric proportion according to alloy composition, consider La, Mn, B wherein, the melting scaling loss of Al element simultaneously, calculate the also raw material of each component of weighing (the B element adds with the form of B-Fe alloy or B-Ni alloy, and purity is all greater than 99.0%) conduct preparation alloy.Adopt Medium frequency induction melting-rapid quenching technique that load weighted raw material are made alloy sheet under the Ar gas shiled.The preparation method of test electrode is, alloy becomes 200-300 purpose powder through Mechanical Crushing, alloyed powder mixes with the mass ratio of carbonyl nickel powder with 1: 4, under 16MPa pressure, make the MH electrode slice of φ 15mm, this electrode slice is placed between two nickel foam, sandwich nickel strap simultaneously, under 16MPa pressure, make the metal-hydride negative (MH electrode) that is used to test once more, guarantee tight contact the between electrode slice and the nickel screen by spot welding around the electrode slice as lug.
Negative pole in open type two electrode systems of test chemical property is the MH electrode, the sintering Ni (OH) of anodal employing capacity surplus 2/ NiOOH electrode, electrolyte are 6molL -1KOH solution, the battery that assembles is shelved 24h, use the LAND cell tester and measure the chemical property (activation number of times, peak capacity, high-rate discharge capacity HRD, low temperature performance, cyclical stability etc.) of alloy electrode with galvanostatic method, the ambient temperature of conventionally test is 298K, density of charging current 70mAg -1, charging interval 6h, discharge current density 70mAg -1, the discharge stopping potential is 1.0V, charge and discharge intermittent time 10min.The capability retention that charge and discharge cycles is 500 times all reaches more than 80%.The test result of other performance sees Table 1.
Table 1RE 8Fe 27B 24The electrochemical properties of alloy electrode
Figure G2009102662373D00031
Annotate: a is the cycle-index that electrode activation needs; B is a maximum discharge capacity; C is discharge current density I dMultiplying power discharging ability during for 10C (3A/g); D is the respectively discharge capacity 0 ℃ ,-30 ℃ ,-40 ℃ time the and the ratio of rated capacity of ambient temperature.
Embodiment 2.
Is RE in the alloy according to institute's invention low-temperature storage battery with RE-Fe-B 8Fe 28B 24Chemical constitution formula, RE is a rare earth element, partly substitutes Fe, B element with Ni, Mn, Al, Cu element, prepared alloy composition such as table 2 are listed.Stoichiometric proportion according to alloy composition, consider La, Mn, B wherein, the melting scaling loss of Al element simultaneously, calculate the also raw material of each component of weighing (the B element adds with the form of B-Fe alloy or B-Ni alloy, and purity is all greater than 99.0%) conduct preparation alloy.Adopt Medium frequency induction melting-rapid quenching technique that load weighted raw material are made alloy sheet under the Ar gas shiled.The preparation of test electrode and method of testing are with embodiment 1.The capability retention that charge and discharge cycles is 500 times all reaches more than 80%.The test result of other performance sees Table 2.
Table 2RE 8Fe 28B 24The electrochemical properties of alloy electrode
Figure G2009102662373D00041
Embodiment 3.
Is RE in the alloy according to institute's invention low-temperature storage battery with RE-Fe-B 15Fe 77B 8Chemical constitution formula, RE is a rare earth element, partly substitutes Fe, B element with Ni, Mn, Al, Cu element, prepared alloy composition such as table 3 are listed.Stoichiometric proportion according to alloy composition, consider La, Mn, B wherein, the melting scaling loss of Al element simultaneously, calculate the also raw material of each component of weighing (the B element adds with the form of B-Fe alloy or B-Ni alloy, and purity is all greater than 99.0%) conduct preparation alloy.Adopt Medium frequency induction melting-rapid quenching technique that load weighted raw material are made alloy sheet under the Ar gas shiled.Is 10 with prepared alloy in vacuum degree -2Heat-treat in the environment of Pa, heat-treat condition is 950 ℃ of insulations 3 hours, and 600 ℃ of insulations 3 hours, the hydrogen bearing alloy after the insulation was with the stove cool to room temperature then.The preparation of test electrode and method of testing are with embodiment 1.The capability retention that charge and discharge cycles is 500 times all reaches more than 80%.The test result of other performance sees Table 3.
Table 3RE 15Fe 77B 8The electrochemical properties of alloy electrode
Figure G2009102662373D00042
Embodiment 4.
Is RE in the alloy according to institute's invention low-temperature storage battery with RE-Fe-B 17Fe 76B 7Chemical constitution formula, RE is a rare earth element, partly substitutes Fe, B element with Ni, Mn, Al, Cu element, prepared alloy composition such as table 4 are listed.Stoichiometric proportion according to alloy composition, consider La, Mn, B wherein, the melting scaling loss of Al element simultaneously, calculate the also raw material of each component of weighing (the B element adds with the form of B-Fe alloy or B-Ni alloy, and purity is all greater than 99.0%) conduct preparation alloy.Adopt Medium frequency induction melting-rapid quenching technique that load weighted raw material are made alloy sheet under the Ar gas shiled.The preparation of test electrode and method of testing are with embodiment 1.The capability retention that charge and discharge cycles is 500 times all reaches more than 80%.The test result of other performance sees Table 4.
Table 4RF 17Fe 76B 7The electrochemical properties of alloy electrode

Claims (7)

1. RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery, its chemical constitution formula is: RE 8Fe 27B 24, RE 8Fe 28B 24(RE 2Fe 7B 6), RE 15Fe 77B 8Or RE 17Fe 76B 7In a kind of, wherein: RE is one or more in rare-earth elements of lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu), scandium (Sc) and the yttrium (Y), and RE can be formed one or more all or part of replacements in the magnesium (Mg), calcium (Ca), zirconium (Zr), titanium (Ti), vanadium (V) element of hydride with hydrogen in the periodic table of chemical element; Fe (iron) can be by one or more all or part of replacements among the transition metal nickel (Ni) in the periodic table of chemical element, manganese (Mn), aluminium (Al), cobalt (Co), copper (Cu), zirconium (Zr), titanium (Ti), vanadium (V), zinc (Zn), chromium (Cr), tungsten (W) and nontransition metal element gallium (Ga), tin (Sn), plumbous (Pb); B (boron) can be by metallic elements of ferrum (Fe), nickel (Ni), manganese (Mn), aluminium (Al), cobalt (Co), copper (Cu), zirconium (Zr), titanium (Ti), vanadium (V), zinc (Zn), chromium (Cr), tungsten (W), gallium (Ga), tin (Sn), plumbous (Pb) and nonmetalloid silicon (Si), sulphur (S), carbon (C), one or more all or part of replacements in the phosphorus (P) is characterized in that: the preparation raw material of described RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery are the RE (rare earth) in the alloy composition and the simple substance of substitute element thereof, the simple substance of Fe and substitute element thereof, the simple substance of B and substitute element thereof, the RE-Fe alloy, the B-Fe alloy, the B-Ni alloy, the RE-Fe-B alloy, LaNi 5Type alloy and other contain the intermediate alloy of component, select wherein the chemical constitution formula preparation of two or more raw material according to alloy.
2. RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery according to claim 1 is characterized in that: each atoms of elements ratio can be adjusted in ± 10% scope during described RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery was formed.
3. RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery according to claim 1; it is characterized in that: high melt casting or high melt-quick quenching technique are adopted in the preparation of described RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery; wherein; the THICKNESS CONTROL of fast quenching alloy sheet is below 1.0mm, and preparation process need be carried out under inert gas shielding or under vacuum environment.
4. RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery according to claim 1 is characterized in that: the alloy of ingot of described RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery and fast quenching alloy sheet are 10 in vacuum degree -2-10 6In the environment of Pa, the heat treatment of perhaps annealing in the environment of inert gas shielding is annealed heat treated temperature between 600-1050 ℃, is incubated 2-24 hour, and the hydrogen-storage alloy after the insulation is with the stove cool to room temperature.
5. RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery according to claim 1 is characterized in that: described RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery adopts one or more methods in airflow milling, ball milling, sledge mill, the high temperature atomization method to unite and uses the powder that is prepared into 30-150 μ m.
6. storage battery, it is characterized in that: the negative electrode active material of storage battery is described RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery.
7. storage battery according to claim 6 is characterized in that: storage battery is nickel-hydrogen secondary cell or metal hydride air (MH-Air) battery.
CN200910266237A 2009-07-08 2009-12-23 RE-Fe-B serial hydrogen storage alloy for low-temperature storage battery and storage battery thereof Pending CN101740770A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102952988A (en) * 2011-08-16 2013-03-06 中国科学院金属研究所 High activity and high hydrogen-induced disproportionation resisting hydrogen storage isotope Sc-Cr-Mn alloy
CN105215372A (en) * 2015-10-21 2016-01-06 龙岩紫荆创新研究院 A kind of preparation of 3D printing NdFeB magnetic powder
CN109585790A (en) * 2018-11-30 2019-04-05 华南理工大学 A kind of preparation method of AB5 base hydrogen-storing alloy, nickel-hydrogen cell electrode, secondary cell and its hydrogen-storage alloy
CN111411262A (en) * 2020-04-14 2020-07-14 包头稀土研究院 A5B19 type gadolinium-containing hydrogen storage alloy, negative electrode and preparation method
CN111471895A (en) * 2020-04-14 2020-07-31 包头稀土研究院 Hydrogen storage alloy containing gadolinium and nickel, cathode, battery and preparation method
CN111471894A (en) * 2020-04-14 2020-07-31 包头稀土研究院 Doped A5B19 type samarium-containing hydrogen storage alloy, battery and preparation method

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102230111B (en) * 2011-05-31 2015-12-09 四川宝生实业发展有限公司 High ferro hydrogen-storing alloy as electrode and nickel-hydrogen battery negative pole material
CN102952988A (en) * 2011-08-16 2013-03-06 中国科学院金属研究所 High activity and high hydrogen-induced disproportionation resisting hydrogen storage isotope Sc-Cr-Mn alloy
CN102952988B (en) * 2011-08-16 2014-10-15 中国科学院金属研究所 High activity and high hydrogen-induced disproportionation resisting hydrogen storage isotope Sc-Cr-Mn alloy
CN105215372A (en) * 2015-10-21 2016-01-06 龙岩紫荆创新研究院 A kind of preparation of 3D printing NdFeB magnetic powder
CN109585790A (en) * 2018-11-30 2019-04-05 华南理工大学 A kind of preparation method of AB5 base hydrogen-storing alloy, nickel-hydrogen cell electrode, secondary cell and its hydrogen-storage alloy
CN109585790B (en) * 2018-11-30 2022-03-29 华南理工大学 AB 5-based hydrogen storage alloy, electrode for nickel-metal hydride battery, secondary battery and preparation method of hydrogen storage alloy
US11929488B2 (en) 2018-11-30 2024-03-12 South China University Of Technology AB5-based hydrogen storage alloy, electrode for Ni-MH battery, secondary battery, and preparation method of hydrogen storage alloy
CN111411262A (en) * 2020-04-14 2020-07-14 包头稀土研究院 A5B19 type gadolinium-containing hydrogen storage alloy, negative electrode and preparation method
CN111471895A (en) * 2020-04-14 2020-07-31 包头稀土研究院 Hydrogen storage alloy containing gadolinium and nickel, cathode, battery and preparation method
CN111471894A (en) * 2020-04-14 2020-07-31 包头稀土研究院 Doped A5B19 type samarium-containing hydrogen storage alloy, battery and preparation method
CN111471894B (en) * 2020-04-14 2021-09-10 包头稀土研究院 Doped A5B19 type samarium-containing hydrogen storage alloy, battery and preparation method

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Application publication date: 20100616