CN110405219A - The preparation method and high power hydrogen-bearing alloy powder of high power hydrogen-bearing alloy powder - Google Patents
The preparation method and high power hydrogen-bearing alloy powder of high power hydrogen-bearing alloy powder Download PDFInfo
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- CN110405219A CN110405219A CN201910691559.6A CN201910691559A CN110405219A CN 110405219 A CN110405219 A CN 110405219A CN 201910691559 A CN201910691559 A CN 201910691559A CN 110405219 A CN110405219 A CN 110405219A
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- B22F9/00—Making metallic powder or suspensions thereof
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
- C01B3/0031—Intermetallic compounds; Metal alloys; Treatment thereof
- C01B3/0047—Intermetallic compounds; Metal alloys; Treatment thereof containing a rare earth metal; Treatment thereof
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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/049—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by pulverising at particular temperature
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- 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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
Abstract
The invention discloses a kind of preparation methods of high power hydrogen-bearing alloy powder, and belong to hydrogen bearing alloy electric conductivity technical field, comprising the following steps: S1: hydrogen bearing alloy carries out Mechanical Crushing in oxygen-free environment, obtain the first powder；S2: the first powder is subjected to second-time breakage in oxygen-free environment of the temperature lower than 5 DEG C, obtains the second powder, the partial size of the second powder is less than 5 μm；The electric conductivity and dynamic performance of hydrogen bearing alloy can be improved in the preparation method, so as to improve the high rate performance, power-performance, low temperature discharge capacity of battery cathode.
Description
Technical field
The invention belongs to hydrogen bearing alloy electric conductivity technical fields, and in particular to a kind of preparation of high power hydrogen-bearing alloy powder
Method and high power hydrogen-bearing alloy powder.
Background technique
In the past few years, nickel-metal hydride battery is although impact by lithium ion battery, lead-acid battery, supercapacitor,
Electrochemistry that nickel-metal hydride battery still relies on the security performance of itself, low temperature excellent, environmentally protective, higher specific power are military
Device and electric car field achieve more successful application.The chemical property of nickel-metal hydride battery mainly by cathode, (close by hydrogen storage
Gold) it determines.Influencing AB5 type hydrogen storage alloy chemical property at present mainly has lower three reasons: 1, ion is in electrolyte and electricity
Transfer rate in extremely；2, electrode surface electrochemical reaction speed and electro catalytic activity；3, the diffusion speed of Hydrogen Proton in the electrodes
Rate.
It is decrystallized and lose to guiding discharge capacity that traditional ball-milling technology will lead to hydrogen bearing alloy, and ball milling part
The high temperature of generation can make hydrogen bearing alloy surface oxidation, influence hydrogen bearing alloy electric charge transfer rate.Most of all, ball milling refinement storage
The ability of hydrogen alloy is limited, and hydrogen bearing alloy cannot be refined to micro-nano rank.
Summary of the invention
In order to solve the above problem existing for traditional ball-milling technology, the present invention provides a kind of high power hydrogen-bearing alloy powders
Preparation method, which crushes hydrogen bearing alloy in the oxygen-free environment of low temperature, and the grain of smashed particle
Less than 5 μm, the hydrogen bearing alloy specific surface area after refinement increases diameter, can increase the site that can be more electrochemically reacted,
The Charge-transfer resistance on hydrogen bearing alloy surface can be effectively reduced, particle surface is not oxidized, improves the transfer rate of particle.
The technical scheme adopted by the invention is as follows: a kind of preparation method of high power hydrogen-bearing alloy powder, including following step
It is rapid:
S1: hydrogen bearing alloy carries out Mechanical Crushing in oxygen-free environment, obtains the first powder；
S2: by the first powder in temperature lower than second-time breakage is carried out in 5 DEG C of oxygen-free environment, obtaining the second powder, and second
The partial size of powder is less than 5 μm.
The working principle of the invention/have the beneficial effect that first, carrying out Mechanical Crushing is in order to enable second broken more preferable
Ground carries out, be in the oxygen-free environment of oxygen-free environment and temperature lower than 5 DEG C so that the fine grained surface obtained after being crushed not
It is oxidized；The partial size of the second, the second powder is the specific surface area in order to increase hydrogen bearing alloy less than 5 μm, and increasing more can be into
The site of row electrochemical reaction effectively reduces the Charge-transfer resistance on hydrogen bearing alloy surface, is reducing the same of Charge-transfer resistance
When, since hydrogen storage alloy particle becomes smaller, the diffusion path of Hydrogen Proton is caused to shorten, effectively improves hydrogen bearing alloy Hydrogen Proton diffusion speed
Rate.In summary two o'clock, which can be improved the electric conductivity and dynamic performance of hydrogen bearing alloy, so as to improve electricity
High rate performance, power-performance, the low temperature discharge capacity of pond cathode.
It further limits, the partial size of first powder is 10~100 μm.
The working principle of the invention/have the beneficial effect that partial size has good dispersibility for 10~100 μm of the first powder
Can, it can be scattered in organic solvent and form uniform disperse system.
It further limiting, the oxygen-free environment in step S2 is that the organic solvent by oxygen content less than 0.5PPm is formed, the
One powder is scattered in organic solvent of the oxygen content less than 0.5PPm, is dried to obtain the after broken after washing removal contaminant filter
Two powder.
The dispersion of the first powder of the working principle of the invention/have the beneficial effect that, starvation avoid the second powder surface
It is oxidized.
It further limits, temperature is by ice water mixing water-bath, liquid nitrogen or cryogenic box to oxygen-free environment lower than 5 DEG C in step S2
Carry out cooling realization.
The working principle of the invention/have the beneficial effect that the speed for containing oxidation reaction, further decreases the second powder surface
Degree of oxidation.
It further limits, the organic solvent is ethyl alcohol, isopropanol or N-Methyl pyrrolidone.
The working principle of the invention/have the beneficial effect that is cheap, and volatile performance is good.
It further limits, the sonioation method or high-energy ball milling method that second-time breakage uses in step S2.
The working principle of the invention/have the beneficial effect that sonioation method or high-energy ball milling method crushing performance are good, can make
The partial size of the second powder is obtained less than 5 μm.
It further limits, the hydrogen bearing alloy is pressed by purity in 99.99% or more lanthanum or cerium, nickel, cobalt, manganese and aluminium
1.0:3.7:0.75:0.35:0.3 molar ratio mixing after be mixed to get in vacuum environment.
It further limits, electromagnetic levitation type blender is used in mixed process.
Further limit, the Mechanical Crushing in step S1 using alligator, cone crusher or ball milling machine into
Row is broken.
A kind of high power hydrogen-bearing alloy powder that the preparation method of high power hydrogen-bearing alloy powder is prepared.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram of G-200, G-400, U-1 and U-2；G-200, G-400, U-1 and U-2 respectively represent grain
The hydrogen bearing alloy of about 200 mesh of diameter, partial size are about the hydrogen bearing alloy of 400 mesh, and the hydrogen bearing alloy that partial size is about 10 microns, partial size is about
For 1 micron of hydrogen bearing alloy.
Fig. 2 is the SEM shape appearance figure of G-200, and amplification factor is 1000 times；
Fig. 3 is the SEM shape appearance figure of G-400, and amplification factor is 1000 times；
Fig. 4 is the SEM shape appearance figure of U-1, and amplification factor is 1000 times；
Fig. 5 is the SEM shape appearance figure of U-2, and amplification factor is 1000 times；
Fig. 6 is the discharge curve of the current density with 3000mAg-1 of G-200, G-400, U-1 and U-2；
Fig. 7 is the discharge capacity figure of G-200, G-400, U-1 and U-2 at -40 DEG C；
Fig. 8 is the discharge capacity figure of G-200, G-400, U-1 and U-2 at -20 DEG C；
Fig. 9 is the discharge capacity figure of G-200, G-400, U-1 and U-2 at 0 DEG C；
Figure 10 is G-200, G-400, U-1 and U-2 in the discharge capacity of different temperatures and electric discharge mean voltage relational graph；
Figure 11 is the power curve of G-200, G-400, U-1 and U-2 and the relational graph of discharge voltage；
Figure 12 is G-200, G-400, U-1 and U-2 in -40 DEG C of power graph.
Specific embodiment
With reference to the accompanying drawing and specific embodiment the present invention is further elaborated.
The embodiment of the present invention is described below in detail, examples of the embodiments are shown in the accompanying drawings, wherein from beginning to end
Same or similar label indicates same or similar element or element with the same or similar functions.Below with reference to attached
The embodiment of figure description is exemplary, it is intended to is used to explain the present invention, and is not considered as limiting the invention.
In the description of the present invention, it is to be understood that, term " first ", " second " are used for description purposes only, and cannot
It is interpreted as indication or suggestion relative importance or implicitly indicates the quantity of indicated technical characteristic.Define as a result, " the
One ", the feature of " second " can explicitly or implicitly include one or more of the features.In the description of the present invention,
The meaning of " plurality " is two or more, unless otherwise specifically defined.
In the present invention unless specifically defined or limited otherwise, term " installation ", " connected ", " connection ", " fixation " etc.
Term shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can be machine
Tool connection, is also possible to be electrically connected；It can be directly connected, two members can also be can be indirectly connected through an intermediary
Connection inside part.For the ordinary skill in the art, above-mentioned term can be understood in this hair as the case may be
Concrete meaning in bright.
Embodiment 1
1.0:3.7:0.75 is pressed in 99.99% or more lanthanum or cerium, nickel, cobalt, manganese and aluminum metal element using purity:
The fixed molar ratio of 0.35:0.3 carries out melting in vacuum arc melting furnace, and fusion process is protected using argon gas, and uses magnetcisuspension
Floating stirring turns over melting 4 times to guarantee that structural constituent is uniform；Hydrogen bearing alloy after melting is crushed by alligator, bevel-type
Machine or ball milling crusher machine cross 200 mesh filter screens and obtain 10~100 μm of the first powder.
The first powder of 1g is dissolved in the beaker of 100ml ethyl alcohol, isopropanol or N-Methyl pyrrolidone solution, is first existed
1 hour is reacted under the conditions of 1000r/min in high speed disperser, then in the Ultrasonic cell smash or height of power 600W
Energy ball milling device is crushed 2 hours, and reaction process whole process low temperature ice-water bath, liquid nitrogen or cryogenic box are to prevent temperature is excessively high from leading to hydrogen storage
Alloy surface generates oxide, and temperature is lower than 5 DEG C.Hydrogen bearing alloy after collecting reaction uses distilled water and ethanol washing to neutrality
And impurity is removed, the hydrogen bearing alloy after washing is obtained into the second powder, the second powder after 80 DEG C of vacuum ovens static 2 hours
The partial size at end measures the X-ray diffractogram of the hydrogen bearing alloy of different-grain diameter and SEM shape appearance figure, X in the second powder and penetrates less than 5 μm
Ray diffraction diagram is as shown in Figure 1, SEM shape appearance figure is as shown in Figure 2-5, in which: G-200, G-400, U-1 and U-2 respectively represent partial size
The hydrogen bearing alloy of about 200 mesh, partial size are about the hydrogen bearing alloy of 400 mesh, and partial size is the hydrogen bearing alloy for being about 10 microns, and partial size is about
1 micron of hydrogen bearing alloy；By Fig. 1-5 it is found that the crystal structure of the hydrogen bearing alloy by ultrasonic wave refinement is obvious there is no occurring
Change and the miscellaneous peak of oxide does not occur.
It takes the second powder of 100mg and 300mg nickel powder to be blended in 65MPa pressure and depresses to disk (10 microns of partial size).It will bear
Pole and reference electrode, to half-cell is formed in electrode intrusion 6mol/LKOH electrolyte, use half electricity of blue electrical testing system testing
Pond.Electro-active with current density 10 charge and discharges of progress of 0.2C under normal temperature conditions first, electric discharge is 0.6V by voltage, then right
Half-cell carries out the high-multiplying power discharge test of 10C, and electric discharge is 0.6V by voltage, as shown in fig. 6, with the partial size of hydrogen bearing alloy
It is smaller, it is bigger to participate in discharge current density of the electrode at 10C；U-2 participates in electrode and discharges under the discharge current density under 10C
Capacity is that 239.92mAhg-1 is much higher than untreated hydrogen bearing alloy 38.17mAhg-1.
It takes the second powder of 100mg and 300mg nickel powder to be blended in 65MPa pressure and depresses to disk (10 microns of partial size).It will bear
Pole and reference electrode, to half-cell is formed in electrode intrusion 6mol/LKOH electrolyte, use half electricity of blue electrical testing system testing
Pond.Electro-active with current density 20 charge and discharges of progress of 0.2C under normal temperature conditions first, electric discharge is 1V by voltage, then will
Battery is put into static in cryogenic box, and quiescent time is half an hour.In 0 DEG C, -20 DEG C and -40 DEG C condition discharge capacity point
Not as shown in Fig. 9, Fig. 8 and Fig. 7；Held by Fig. 9, Fig. 8 and Fig. 7 it is found that discharging under the conditions of 0 DEG C, -20 DEG C and -40 DEG C
Amount is obviously improved；As shown in Figure 10, under the conditions of -40 DEG C of low-temperature test, compared to untreated hydrogen bearing alloy, warp
The hydrogen bearing alloy discharge capacity of micronization processes is promoted to 204.69mAhg-1 from 49.58mAhg-1, electric discharge mean voltage from
0.814V is promoted to 1.128V.
It takes the second powder of 100mg and 300mg nickel powder to be blended in 65MPa pressure and depresses to disk (10 microns of partial size).It will bear
Pole and reference electrode, to half-cell is formed in electrode intrusion 6mol/LKOH electrolyte, use half electricity of blue electrical testing system testing
Pond.Electro-active with current density 10 charge and discharges of progress of 0.2C under normal temperature conditions first, electric discharge is 1V by voltage, in room temperature
Under the conditions of 20 DEG C, activated battery is subjected to power test, is discharged 5 seconds under the current density of 1C to 16C, is discharged every time
Static 2 minutes afterwards, the relational graph of power curve and discharge voltage is obtained, as shown in Figure 11, the hydrogen bearing alloy peak work after refinement
Rate increases as partial size reduces, and the peak power of U-2 is that 5040.24Wkg-1 is significantly larger than untreated hydrogen bearing alloy
3757.44Wkg-1。
Before carrying out low-temperature test, half-cell is put into static 4 hours in low temperature baking oven, carries out power test later
Hydrogen bearing alloy peak power after refining under the conditions of -40 DEG C is that 1038.59Wkg-1 and untreated hydrogen bearing alloy are
688.91Wkg-1, as shown in figure 12.
The present invention is not limited to above-mentioned optional embodiment, anyone can show that other are various under the inspiration of the present invention
The product of form, however, make any variation in its shape or structure, it is all to fall into the claims in the present invention confining spectrum
Technical solution, be within the scope of the present invention.
Claims (10)
1. a kind of preparation method of high power hydrogen-bearing alloy powder, which comprises the following steps:
S1: hydrogen bearing alloy carries out Mechanical Crushing in oxygen-free environment, obtains the first powder；
S2: the first powder is subjected to second-time breakage in oxygen-free environment of the temperature lower than 5 DEG C, obtains the second powder, the second powder
Partial size less than 5 μm.
2. the preparation method of high power hydrogen-bearing alloy powder according to claim 1, which is characterized in that first powder
Partial size be 10~100 μm.
3. the preparation method of high power hydrogen-bearing alloy powder according to claim 1, which is characterized in that the nothing in step S2
Oxygen environment is that the organic solvent by oxygen content less than 0.5PPm is formed, and the first powder is scattered in oxygen content less than 0.5PPm's
In organic solvent, the second powder is dried to obtain after removal contaminant filter is washed after broken.
4. the preparation method of high power hydrogen-bearing alloy powder according to claim 1 or 3, which is characterized in that in step S2
Temperature is to carry out cooling realization to oxygen-free environment by ice water mixing water-bath, liquid nitrogen or cryogenic box lower than 5 DEG C.
5. the preparation method of high power hydrogen-bearing alloy powder according to claim 3, which is characterized in that the organic solvent
For ethyl alcohol, isopropanol or N-Methyl pyrrolidone.
6. the preparation method of high power hydrogen-bearing alloy powder according to claim 1-3, which is characterized in that step
The sonioation method or high-energy ball milling method that second-time breakage uses in S2.
7. the preparation method of high power hydrogen-bearing alloy powder according to claim 1 or 2, which is characterized in that the hydrogen storage
Alloy is pressed the molar ratio of 1.0:3.7:0.75:0.35:0.3 by purity in 99.99% or more lanthanum or cerium, nickel, cobalt, manganese and aluminium
It is mixed to get in vacuum environment after mixing.
8. the preparation method of high power hydrogen-bearing alloy powder according to claim 7, which is characterized in that adopted in mixed process
With electromagnetic levitation type blender.
9. the preparation method of high power hydrogen-bearing alloy powder according to claim 1 or 2, which is characterized in that in step S1
Mechanical Crushing be crushed using alligator, cone crusher or ball milling machine.
10. the Gao Gong that go the preparation method of the described in any item high power hydrogen-bearing alloy powders of 1-9 to be prepared according to right
Rate hydrogen-bearing alloy powder.
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| CN110842192A (en) * | 2019-11-13 | 2020-02-28 | 四川大学 | Nitrogen-doped porous carbon-coated hydrogen storage alloy powder and preparation method thereof |
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| CN113735057A (en) * | 2021-08-31 | 2021-12-03 | 苏州睿分电子科技有限公司 | Activation-free hydrogen storage material and preparation method and device thereof |
| CN114122420A (en) * | 2021-03-24 | 2022-03-01 | 包头稀土研究院 | Method for manufacturing anode of direct sodium borohydride fuel cell |
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| CN110993932A (en) * | 2019-12-24 | 2020-04-10 | 惠州时代电池有限公司 | High-temperature high-cycle negative electrode active material, preparation method thereof and nickel-metal hydride battery |
| CN110993932B (en) * | 2019-12-24 | 2021-05-04 | 惠州时代电池有限公司 | High-temperature high-cycle negative electrode active material, preparation method thereof and nickel-metal hydride battery |
| CN114122420A (en) * | 2021-03-24 | 2022-03-01 | 包头稀土研究院 | Method for manufacturing anode of direct sodium borohydride fuel cell |
| CN114122420B (en) * | 2021-03-24 | 2023-12-12 | 包头稀土研究院 | Method for manufacturing anode of direct sodium borohydride fuel cell |
| CN113735057A (en) * | 2021-08-31 | 2021-12-03 | 苏州睿分电子科技有限公司 | Activation-free hydrogen storage material and preparation method and device thereof |
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