CN102403489A - Cathode hydrogen-storing alloy for long-longevity and low-self-discharging type power cell - Google Patents

Cathode hydrogen-storing alloy for long-longevity and low-self-discharging type power cell Download PDF

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CN102403489A
CN102403489A CN2010102860837A CN201010286083A CN102403489A CN 102403489 A CN102403489 A CN 102403489A CN 2010102860837 A CN2010102860837 A CN 2010102860837A CN 201010286083 A CN201010286083 A CN 201010286083A CN 102403489 A CN102403489 A CN 102403489A
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alloy
hydrogen bearing
bearing alloy
hydrogen
self
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简旭宇
尉海军
朱磊
王�忠
蒋利军
刘晓鹏
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Beijing General Research Institute for Non Ferrous Metals
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Beijing General Research Institute for Non Ferrous Metals
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Abstract

The present invention discloses a hydrogen-storing alloy for a cathode of a power cell with low self-discharge, good high magnification performance and long longevity, wherein the alloy composition is NdaPrbMgcLnd(NixAlyAz), wherein Ln is at least one element selected from Zr, Ti, Sm and Ca, and A is at least one element selected from Mn, V, Cr, Zn, Cu, Si and B. a, b, c and d satisfy the following conditions: a>=0.5, b>0, 0<c<=0.2, d>0, and a+b+c+d=1; and x, y and z satisfy the following conditions: 0.01<=y<=0.25, 0<=z<=0.05, and 3.0<=x+y+z<=3.5. The alloy is prepared to the hydrogen-storing alloy for the cathode of the power cell after thermo alkaline surface treatment.

Description

A kind of long-life low self-discharge type electrokinetic cell is used the negative pole hydrogen bearing alloy
Technical field
The present invention relates to a kind of long-life low self-discharge type Ni-MH power cell negative pole and use hydrogen bearing alloy.Adopt hydrogen bearing alloy of the present invention will improve the self-discharge performance of Ni-MH power cell greatly, guarantee that simultaneously it has long useful life and high rate capability preferably.
Background technology
Ni-MH battery is a kind of secondary cell of good comprehensive properties, and it is widely used, and comprises PHEV, camera, mobile phone, electric tool etc.In recent years, make great efforts down at everybody, hydrogen bearing alloy is greatly improved at aspect of performances such as specific capacity, cycle life, low temperature.But the self discharge of Ni-MH battery is bigger, has brought inconvenience for user's use, has received researcher's concern.Japan correlative study personnel make self-discharge performance obtain certain improvement, and are mainly used in the communication battery through battery prescriptions such as adjustment positive pole, electrolyte, barrier films.And the high rate capability research of using to electrokinetic cell good, the low self-discharge type hydrogen storage alloy is less relatively.
At present, still there is the bigger problem of self discharge in Ni-MH power cell in application process.After the full electricity of battery was shelved a period of time, the user often found that battery owing to the self discharge reason, the electric weight deficiency occurs, can't use.
Summary of the invention
The present invention is intended to solve the difficult problem of the high self discharge of Ni-MH power cell; Provide a kind of long-life low self-discharge type electrokinetic cell to use the negative pole hydrogen bearing alloy; The power battery cathode that adopts hydrogen bearing alloy of the present invention is after shelving a period of time; Still have higher carrying capacity, can better guarantee the consistency of battery and good cycle life.
For realizing above-mentioned purpose, the present invention takes following technical scheme:
The disclosed hydrogen bearing alloy of the present invention has Nd aPr bMg cLn d(Ni xAl yAz )General formula, wherein Ln is at least a element of from Zr, Ti, Sm and Ca, selecting, A is at least a element of from Mn, V, Cr, Zn, Cu, Si and B, selecting, a in the formula>=0.5, b＞0,0＜c≤0.2, d＞0, and a+b+c+d=1; 0.01≤y≤0.25,0≤z≤0.05,3.0≤x+y+z≤3.5.
With broken average grain diameter 50～70 μ m alloyed powders that obtain of the alloy that obtains; And, make alloy surface form rich nickel dam with its thermokalite surface treatment of carrying out certain hour, it is active to improve its surface catalysis; Under the prerequisite that guarantees the alloy ratio capacity, improve its high-rate performance.
In the described hydrogen bearing alloy that uses for nickel-hydrogen battery, when the mol ratio c of Mg surpassed 0.2, alloy structure was inhomogeneous, and corrosion resistance is relatively poor, inhaled to be prone to efflorescence, the obvious variation of the cycle life of alloy when putting hydrogen; On the other hand, when the ratio content of Mg element more after a little while, the hydrogen bearing alloy hydrogen storage capacity obviously reduces, and self discharge is more serious.
In said hydrogen bearing alloy; The Al element has very important effect, and optimum Al constituent content scope should satisfy 0.01～0.25, when the Al constituent content less than 0.01 the time; This hydrogen bearing alloy is easy to receive the corrosion of Ni-MH battery electrolyte; Not only Ni-MH battery cycle life can descend greatly, and the inner electrolyte of Ni-MH battery can cause the Ni-MH battery internal resistance to increase because the oxidation hydrogen bearing alloy becomes fewer and feweri.On the other hand, when the Al constituent content greater than 0.25 the time, the maximum storage hydrogen quantity of hydrogen bearing alloy can descend, therefore should be according to Al constituent content in the practical application request appropriate regulation hydrogen bearing alloy, preferred Al constituent content scope is 0.05≤y≤0.2.
In said alloy, Ln is at least a element of from Zr, Ti, Sm, Ca, selecting, and can effectively improve alloy pressure variation when hydrogen is put in suction and cause hysteresis, and when preventing that it is used for nickel-hydrogen battery negative pole, discharge voltage descends.The hydrogen hysteresis effect is put in the suction of adopting a spot of Zr, Ti, Sm, Ca can improve alloy; These several kinds of atoms of elements radiuses are less, and interatomic adhesion is strengthened, and unit cell volume reduces; The hydrogen balance pressure drop is low; Improve the hysteresis effect of alloy, can suppress the efflorescence of alloy simultaneously, improve the life-span of alloy.
In said alloy, add the Pr of trace, can make alloy under the prerequisite that guarantees the low self-discharge performance, the life-span of further improving alloy.
In addition, the invention still further relates to the thermokalite surface treatment of this alloy, treatment fluid is one or more in potassium hydroxide, NaOH and the lithium hydroxide, and proportionaling alkali-forming concentration is 5～8M, and the treatment fluid temperature remains on 60～75 degrees centigrade.Through the alloy fragmentation that obtains is obtained average grain diameter 50～70 μ m alloyed powders; And it is carried out the thermokalite surface treatment; Remove the Mg of the excessive segregation of alloy surface, and make alloy surface form rich nickel dam, it is active to improve its surface catalysis; Under the prerequisite that guarantees the alloy ratio capacity, improve its high-rate performance.
A kind of long-life low self-discharge type Ni-MH power cell negative pole is with the preparation method of hydrogen bearing alloy, and this method comprises the steps:
(1), be raw material with the simple substance of Nd, Pr, Mg, Ln, Ni, Al and A respectively; Wherein Ln is at least a element of from Zr, Ti, Sm and Ca, selecting; A is at least a element of from Mn, V, Cr, Zn, Cu, Si and B, selecting, and forms and stoichiometric proportion takes by weighing required raw material according to the chemical formula of above-mentioned hydrogen bearing alloy; Be smelted into the ingot casting of hydrogen bearing alloy;
(2), the hydrogen bearing alloy ingot casting with melting in the step (1) carries out heat treatment in 5 hours～7 hours with 950 ℃～980 ℃ in argon gas atmosphere;
(3), in inert atmosphere, the hydrogen bearing alloy ingot after the heat treatment is carried out mechanical disintegration, after its screening, obtain average grain diameter 50～70 μ m alloyed powders;
(4), 60～80 degrees centigrade of temperature of preparation, concentration is the aqueous slkali of 5～8M, the surface treatment that the alloyed powder that step (3) is obtained carries out is last, uses the washed with de-ionized water alloyed powder, promptly obtains hydrogen bearing alloy of the present invention.
Advantage of the present invention is:
Hydrogen bearing alloy of the present invention is to be suitable for low self-discharge; High rate capability is good; The hydrogen bearing alloy that long-life power battery cathode is used; The power battery cathode that adopts hydrogen bearing alloy of the present invention still has higher carrying capacity after shelving a period of time, can better guarantee the consistency of battery and good cycle life.
Description of drawings
Fig. 1 is 100 cycle life curves of the embodiment of the invention 1.
Fig. 2 is 100 cycle life curves of the embodiment of the invention 2.
Embodiment
Embodiment one
Employing high frequency magnetic levitation melting stove will be by neodymium metal, the metal praseodymium, and magnesium metal, metal zirconium, metallic nickel and metallic aluminium are smelted into the ingot casting of regulation alloy, and it consists of Nd 0.5Pr 0.3Mg 0.15Zr 0.05(Ni 3.25Al 0.1), and through inducing binding plasma spectrum analysis (ICP) to measure.At first, with this hydrogen bearing alloy ingot casting, in argon gas atmosphere, carry out heat treatment in 5 hours with 950 ℃, make alloy structure even, in inert atmosphere, alloy pig is carried out mechanical disintegration, after its screening, obtaining average grain diameter is 65 μ m.Secondly, 60～80 degrees centigrade of preparation temperature, concentration is the aqueous slkali of 5～8M, the surface treatment that this alloyed powder is carried out.At last, use the washed with de-ionized water alloyed powder.
Accurately take by weighing above hydrogen-storage alloy powder of 200mg and 800mg carbonyl nickel powder, after evenly mixing, in the mould of packing into, the sequin that under 580MPa pressure, is cold-pressed into Φ 16mm * 1mm is as alloy electrode plate to be measured.Electrode slice is weighed in deburring, and calculates the actual mass of hydrogen-storage alloy in the electrode slice according to the proportional meter of alloyed powder and nickel powder.Then, electrode slice is with nickel foam parcel and compression moulding, and is spot-welded together with nickel strap again, as alloy electrode to be measured.
The electrochemical property test of alloy electrode carries out in open type H type glass three electrode test systems, and auxiliary electrode is the sintered type nickel hydroxide electrode (Ni (OH) of electrochemistry capacitance far above alloy electrode to be measured 2/ NiOOH), reference electrode is homemade mercury-mercury oxide (Hg/HgO) electrode, and electrolyte is the 6mol/LKOH+15g/L LiOH aqueous solution, and probe temperature remains on 30 ℃ through water bath with thermostatic control.
The electrochemical property test of alloy electrode (comprising high-rate performance, cyclical stability) all adopts the constant current charge-discharge mode to carry out; Tester is a Wuhan gold promise LAND series battery test macro, and test process is by real-time monitoring of computer and automatic the collection and record data.
Alloy electrode adopts 60mAg -1Constant current charge 500min leaves standstill 15min, then 60mAg -1Constant-current discharge, stopping potential is 0.6V, leaves standstill 15min, successively circulation.Under this discharges and recharges system, reach the stable maximum discharge capacity of alloy after, adopt 450mAg -1Constant current charge 65min leaves standstill 10min, uses 450mAg then -1Constant-current discharge, stopping potential is 0.6V, leaves standstill 10min, successively circulation.Under this discharges and recharges system, with promptly the circulate capability retention (S of 100 all after dates of the discharge capacity in the 100th cycle and the very big ratio of discharge capacity 100, %) characterize the cyclical stability of alloy.
Under the activation system that alloy electrode is provided in the above, reach the stable maximum discharge capacity of alloy after, rice is used 60mAg -1Constant current charge 500min leaves standstill 15min, adopts 1200mAg -1Constant-current discharge, stopping potential is 0.6V, calculates the ratio of its discharge capacity and maximum discharge capacity, is designated as heavy-current discharge efficient, and threshold voltage in the discharge is compared, and characterizes the alloy high-rate performance.
The self-discharge performance of alloy electrode adopts following A A type battery to estimate, and adopts the current charges 16 hours of 0.1C, left standstill 0.5 hour, then with the current discharge of 0.2C to 1.0V, remember that its capacity is C 1Electric current with same is full of battery, shelves 3 months at 40 degrees centigrade, leaves standstill after 0.5 hour to discharge with 0.2C, remembers that its capacity is C 2, therefore, the self-discharge rate of this battery is (C 1-C 2)/C 1The self-discharge rate of * 100%. embodiment and Comparative Examples is seen shown in the table 1.
When making this embodiment hydrogen bearing alloy nickel-hydrogen battery negative pole; With above-mentioned hydrogen bearing alloy 100 serves as to calculate benchmark, adds 0.4% Sodium Polyacrylate, 0.1% CMC, 2.5% polytetrafluoroethylene (60%), after slurry is mixed; Evenly spreading upon thickness is on the punched steel plate collector of 60 μ m; After drying, on roller mill, suppress, the cathode pole piece that uses for nickel-hydrogen battery is processed in section then.
In addition, nickel-hydrogen battery positive pole material adopts the ball-type nickel hydroxide of the Co contain 2.5% Zn and 1.0%, adds 0.2% hydroxypropyl cellulose (50%) then, is modulated into slurry, and it is 600g/m that this slurry is filled in surface density 2, porosity is 95%, and thickness is on the nickel foam of 2mm, and the compacting of dry back cuts into the anode pole piece that uses for nickel-hydrogen battery.
In the present embodiment process, barrier film adopts sulfonated membrane, and electrolyte uses the mixed liquor of 15: 2: 1 KOH, NaOH and LiOH, and concentration is 30%, has made AA type cylinder Ni-MH battery.
Embodiment two
Employing high frequency magnetic levitation melting stove will be by neodymium metal, the metal praseodymium, and magnesium metal, metal zirconium, metallic nickel, metallic aluminium and manganese metal are smelted into the ingot casting of regulation alloy, and it consists of Nd 0.8Pr 0.05Mg 0.1Zr 0.05(Ni 3.15Al 0.1Mn 0.05), and through inducing binding plasma spectrum analysis (ICP) to measure.At first, with this hydrogen bearing alloy ingot casting, in argon gas atmosphere, carry out heat treatment in 5 hours with 950 ℃, make alloy structure even, in inert atmosphere, alloy pig is carried out mechanical disintegration, after its screening, obtaining average grain diameter is 65 μ m.Secondly, 65～80 degrees centigrade of preparation temperature, concentration is the aqueous slkali of 5～8M, the surface treatment that this alloyed powder is carried out.At last, use the washed with de-ionized water alloyed powder.After this, the electrode making is identical with embodiment 1 with method of testing.
Embodiment three
Employing high frequency magnetic levitation melting stove will be by neodymium metal, the metal praseodymium, and magnesium metal, Titanium, metallic nickel, metallic aluminium and manganese metal are smelted into the ingot casting of regulation alloy, and it consists of Nd 0.8Pr 0.05Mg 0.1Ti 0.05(Ni 3.15Al 0.1Mn 0.05), and through inducing binding plasma spectrum analysis (ICP) to measure.At first, with this hydrogen bearing alloy ingot casting, in argon gas atmosphere, carry out heat treatment in 5 hours with 950 ℃, make alloy structure even, in inert atmosphere, alloy pig is carried out mechanical disintegration, after its screening, obtaining average grain diameter is 65 μ m.Secondly, 65～80 degrees centigrade of preparation temperature, concentration is the aqueous slkali of 5～8M, the surface treatment that this alloyed powder is carried out.At last, use the washed with de-ionized water alloyed powder.After this, the electrode making is identical with embodiment 1 with method of testing.
Embodiment four
Employing high frequency magnetic levitation melting stove will be by neodymium metal, the metal praseodymium, and magnesium metal, samarium metal, metallic nickel, metallic aluminium and manganese metal are smelted into the ingot casting of regulation alloy, and it consists of Nd 0.8Pr 0.05Mg 0.1Sm 0.05(Ni 3.15Al 0.1Mn 0.05), and through inducing binding plasma spectrum analysis (ICP) to measure.At first, with this hydrogen bearing alloy ingot casting, in argon gas atmosphere, carry out heat treatment in 5 hours with 950 ℃, make alloy structure even, in inert atmosphere, alloy pig is carried out mechanical disintegration, after its screening, obtaining average grain diameter is 65 μ m.Secondly, 65～80 degrees centigrade of preparation temperature, concentration is the aqueous slkali of 5～8M, the surface treatment that this alloyed powder is carried out.At last, use the washed with de-ionized water alloyed powder.After this, the electrode making is identical with embodiment 1 with method of testing.
Embodiment five
Employing high frequency magnetic levitation melting stove will be by neodymium metal, the metal praseodymium, and magnesium metal, calcium metal, metallic nickel, metallic aluminium and manganese metal are smelted into the ingot casting of regulation alloy, and it consists of Nd 0.8Pr 0.05Mg 0.1Ca 0.05(Ni 3.15Al 0.1Mn 0.05), and through inducing binding plasma spectrum analysis (ICP) to measure.At first, with this hydrogen bearing alloy ingot casting, in argon gas atmosphere, carry out heat treatment in 5 hours with 950 ℃, make alloy structure even, in inert atmosphere, alloy pig is carried out mechanical disintegration, after its screening, obtaining average grain diameter is 65 μ m.Secondly, 65～80 degrees centigrade of preparation temperature, concentration is the aqueous slkali of 5～8M, the surface treatment that this alloyed powder is carried out.At last, use the washed with de-ionized water alloyed powder.After this, the electrode making is identical with embodiment 1 with method of testing.
Comparative Examples
Employing high frequency magnetic levitation melting stove will be by lanthanoid metal, neodymium metal, and metallic nickel, metallic cobalt, manganese metal and metallic aluminium are smelted into the ingot casting of regulation alloy, and it consists of La 0.65Nd 0.35Ni 3.55Co 0.75Mn 0.4Al 0.3, and through inducing binding plasma spectrum analysis (ICP) to measure.With this hydrogen bearing alloy ingot casting, in argon gas atmosphere, carry out heat treatment in 5 hours with 950 ℃, make alloy structure even, in inert atmosphere, alloy pig is carried out mechanical disintegration, after its screening, obtaining average grain diameter is 65 μ m.After this, the electrode making is identical with embodiment 1 with method of testing.
Table 1 is the data contrast of the embodiment of the invention and Comparative Examples.As shown in table 1, the high-rate performance of the battery of employing hydrogen bearing alloy of the present invention all is higher than the high-rate performance of the battery that adopts the Comparative Examples hydrogen bearing alloy; 100 cycle lives of the battery of employing hydrogen bearing alloy of the present invention also all are higher than 100 cycle lives of the battery that adopts the Comparative Examples hydrogen bearing alloy; The self-discharge performance of the battery of employing hydrogen bearing alloy of the present invention all is lower than the self-discharge performance of the battery that adopts the Comparative Examples hydrogen bearing alloy.
Table 1 embodiment performance comparison
Figure BSA00000276626300061

Claims (3)

1. a long-life low self-discharge type electrokinetic cell is used the negative pole hydrogen bearing alloy, and it is characterized in that: this hydrogen bearing alloy composition is Nd aPr bMg cLn d(Ni xAl yA z), wherein Ln is at least a element of from Zr, Ti, Sm and Ca, selecting, A is at least a element of from Mn, V, Cr, Zn, Cu, Si and B, selecting; A, b, c, d satisfy following condition: a>=0.5, b＞0,0＜c≤0.2; D＞0, a+b+c+d=1; X, y, z satisfy following condition: 0.01≤y≤0.25,0≤z≤0.05,3.0≤x+y+z≤3.5.
2. long-life low self-discharge type electrokinetic cell according to claim 1 is used the negative pole hydrogen bearing alloy, and it is characterized in that: this hydrogen bearing alloy is the alloyed powder of average grain diameter 50～70 μ m.
3. long-life low self-discharge type electrokinetic cell according to claim 2 is used the negative pole hydrogen bearing alloy, it is characterized in that: the alloyed powder surface of this hydrogen bearing alloy is the alkali lye processing of 5～8M through 60～75 degrees centigrade with alkali concn.
CN2010102860837A 2010-09-17 2010-09-17 Cathode hydrogen-storing alloy for long-longevity and low-self-discharging type power cell Pending CN102403489A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103107314A (en) * 2011-11-11 2013-05-15 北京有色金属研究总院 Hydrogen storage alloy for cathode of long-service life low-self-discharge power battery and preparation process of hydrogen storage alloy

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CN1525586A (en) * 2003-02-28 2004-09-01 三洋电机株式会社 Hydrogen absorbing alloy, electrode thereof and nickel-metal hydride battery
CN1649191A (en) * 2004-01-26 2005-08-03 三洋电机株式会社 Hydrogen-absorbing alloy for alkaline storage battery, method of manufacturing the same, and alkaline storage battery
CN1988221A (en) * 2005-12-22 2007-06-27 三洋电机株式会社 Hydrogen storage alloy and alkaline secondary battery using the same
CN101823692A (en) * 2010-04-20 2010-09-08 浙江大学 Reversible hydrogen adsorption and desorption method using piperidine as media and device

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
CN1525586A (en) * 2003-02-28 2004-09-01 三洋电机株式会社 Hydrogen absorbing alloy, electrode thereof and nickel-metal hydride battery
CN1649191A (en) * 2004-01-26 2005-08-03 三洋电机株式会社 Hydrogen-absorbing alloy for alkaline storage battery, method of manufacturing the same, and alkaline storage battery
CN1988221A (en) * 2005-12-22 2007-06-27 三洋电机株式会社 Hydrogen storage alloy and alkaline secondary battery using the same
CN101823692A (en) * 2010-04-20 2010-09-08 浙江大学 Reversible hydrogen adsorption and desorption method using piperidine as media and device

Cited By (1)

* Cited by examiner, † Cited by third party
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