CN108054369A - A kind of preparation method of hydrogen bearing alloy and graphene composite material - Google Patents
A kind of preparation method of hydrogen bearing alloy and graphene composite material Download PDFInfo
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- CN108054369A CN108054369A CN201711344582.5A CN201711344582A CN108054369A CN 108054369 A CN108054369 A CN 108054369A CN 201711344582 A CN201711344582 A CN 201711344582A CN 108054369 A CN108054369 A CN 108054369A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M4/364—Composites as mixtures
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- 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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Abstract
The preparation method of a kind of hydrogen bearing alloy and graphene composite material belongs to cell negative electrode material manufacturing technology field.It is characterised in that it includes following steps：To NiCl2·6H2KBH is added in the solution of O4, obtain Ni B alloys；Ni B alloys are added in after graphite oxide colloid is heated, 200 DEG C ~ 350 DEG C is raised the temperature to, is cooled to room temperature isolated nanoscale Ni B alloys；PH is adjusted as alkalescence, restores again reaction；It is made annealing treatment, finally obtains HSAs/RGO composite materials using legal system from top to bottom.HSAs/3D RGO composite materials prepared by the present invention have the advantages that discharge capacity is high, high-rate discharge ability is good, stability test is high and electronic and ionic transmission speed is fast.
Description
Technical field
The preparation method of a kind of hydrogen bearing alloy and graphene composite material belongs to cell negative electrode material manufacturing technology field.
Background technology
At present, the negative material of Ni-MH battery is mainly rare-earth-based ABxThe advantages of type hydrogen storage alloy, such alloy material is
Cheap, raw material is easy to get, prepares the advantages that simple, activity function is good, long lifespan, but its drawback is that its battery chemistries is held
It measures low, is so difficult to meet the needs of Current electronic product.People have carried out substantial amounts of research for hydrogen storage material in recent years
And achieve certain achievement.
The preparation method of current cathode hydrogen bearing alloy class material mainly has Mechanical Method, additive method, surface preparation.These
Method still has several drawbacks for the performance and promotion discharge performance aspect of hydrogen storage, such as Mechanical Method easily breaks alloy crystal form
Bad, galvanoplastic can not accurately control the thickness of coating.Three-dimensional grapheme material has large specific surface area, electrical and thermal conductivity performance
Well, the advantages that stability is high, and the Ni-B alloys adulterated have the function of good hydrogen storage, therefore the two is combined, Ji Nengti
The electric conductivity of high cathode, and there is good hydrogen storage, it is fully able to meet the needs of contemporary electric equipment products.
The content of the invention
The technical problem to be solved by the present invention is to：It is high to overcome the deficiencies of the prior art and provide a kind of discharge capacity, Xun Huan is steady
The preparation method of qualitative good hydrogen bearing alloy and graphene composite material.
The technical solution adopted by the present invention to solve the technical problems is：The system of the hydrogen bearing alloy and graphene composite material
Preparation Method, which is characterized in that comprise the following steps：
1）To NiCl under ice-water bath2·6H2KBH is added in the multicomponent alcoholics compound solution of O4, stirring and dissolving obtain Ni-B conjunction
Gold；
2）Graphite oxide colloid is heated to 42 DEG C ~ 48 DEG C under inert gas shielding, then by step 1）The Ni-B alloys of preparation
It is gradually added into, until raising the temperature to 200 DEG C ~ 350 DEG C after whole liquid blackening, after keeping the temperature 1 ~ 2h, stops heating, be down to room
Obtained material is separated, washed, dried by Wen Hou, obtains nanoscale Ni-B alloys；
3）To step 2）In the nanoscale Ni-B alloys of preparation add in ammonium hydroxide adjust solution pH for alkalescence, add reducing agent into
Row reduction reaction；
4）Nanoscale Ni-B alloys after reduction reaction are made annealing treatment under argon gas and hydrogen atmosphere, annealing temperature 500
DEG C ~ 900 DEG C, the time is 6h ~ 8h；
5）HSAs/RGO composite materials are obtained using legal system from top to bottom.
The present invention provides a kind of hydrogen bearing alloy（HSAs）With 3D graphene composite materials（3D RGO）Preparation method.This hair
It is bright that Ni-B alloys are prepared by polyol process, with reference to the grapheme material with two-dimentional porous structure, finally by simply certainly
It is upper and laxative remedy prepares hydrogen bearing alloy and graphene composite material.HSAs/3D RGO composite materials prepared by the present invention have electric discharge
The advantages of capacity is high, high-rate discharge ability is good, stability test is high and electronic and ionic transmission speed is fast.
Involved reaction equation is as follows during Ni-B alloys are synthesized：
BH4 -+H2O=B+OH-+2.5H2（1）
BH4 -+2H2O=BO2 -+4H2（2）
BH4 -+2H2O+2M2+=2M+BO2 -+2H2+4H+（3）
The mechanism of the reaction is exactly BH4 -First combined with water generates B, then again with（3）The W metal of reaction generation is tied at high temperature
Symphysis is into crystalline state nanoscale Ni-B alloys.
Preferably, step 1）Described in multicomponent alcoholics compound be tetraethylene glycol.Preferred tetraethylene glycol can be protected as solvent
Card nickel chloride is more evenly distributed, and the rate of above-mentioned synthesis Ni-B alloys is faster.
Preferably, step 1）Described in Ni-B alloys be Ni2B、Ni3B、NiB、Ni2B2One or both of type alloy
Above mixture.Various forms of Ni-B alloys can be obtained according to the ratio of Ni, B of addition, when selection tetraethylene glycol conduct
During solvent, Ni can be obtained3B and Ni2B2In mass ratio 13 ~ 17：The alloy mixture of 7 ~ 12 forms, in the form of such ratio
Under collocation, the discharge capacity of obtained product is farsighted higher than remaining combination or individual alloy form.
Preferably, step 4）Described in annealing in hydrogen and argon gas by volume 1：0.7 ~ 1.3 mixed gas
Middle progress.
Preferably, step 4）In annealing be temperature be 600 DEG C ~ 700 DEG C, the time be 6.5h ~ 7h.
Under preferred annealing conditions the part group in graphene can be made to obtain better, further reduction, so that
The interaction for obtaining hydrogen bearing alloy and grapheme material (HSAs/ RGO) is even closer.
Preferably, step 3）In reducing agent be hydrazine hydrate or KBH4.Preferred reducing agent can be protected sufficiently after use
Demonstrate,prove reduction efficiency and reduction rate.
Preferably, step 3）Described in add in ammonium hydroxide adjust solution pH be 9 ~ 11.PH is adjusted to preferred scope
After can graphene preferably be disperseed.
Preferably, step 2）Described in the temperature that heats graphite oxide colloid under inert gas shielding be 45 DEG C ~ 46
℃。
The graphene oxide may be employed Hummers methods and prepare graphene oxide；Hummer methods prepare oxidation stone
Black alkene has two-dimentional porous structure, simple, safety, the hydrogen storage property higher of products obtained therefrom good to the adaptability of the present invention.
Compared with prior art, possessed advantageous effect of the invention is：Hydrogen bearing alloy made from the method for the present invention with
Graphene composite material (HSAs/RGO), since graphene has unique porous structure, electrical and thermal conductivity performance is good, accelerates electricity
The transmission speed of son and ion substantially increases the chemical reaction rate of electrode surface, while its porous structure is more conducive to
The diffusion of hydrogen.Nanoscale Ni-B alloys have larger specific surface area, and hydrogen storage property is also more superior, the such knot of the two
Conjunction mode so that the negative material discharge capacity of Ni-MH battery is high, good cycling stability.
Description of the drawings
Fig. 1 is the Ni-B alloy SEM images in the embodiment of the present invention 2.
Fig. 2 is the P-C-T curves of the embodiment of the present invention 1.
Fig. 3 is the discharge current of the embodiment of the present invention 3 and discharge capacity relation curve.
Specific embodiment
With reference to specific embodiment, the present invention will be further described, and wherein embodiment 1 is most preferred embodiment.
Embodiment 1
1）To NiCl under ice-water bath2·6H2KBH is added dropwise in the tetraethylene glycol solution of O4, while stirring and dissolving obtains Ni3B with
Ni2B2In mass ratio 15：The Ni-B alloys of 8 forms；
2）Graphite oxide colloid is heated to 45 DEG C under protection of argon gas, then by step 1）The Ni-B alloys of preparation are gradually added into,
280 DEG C are raised the temperature to after to whole liquid blackening, after keeping the temperature 1.5h, stops heating, is cooled to room temperature, by obtained material
It carries out centrifugal treating and is repeatedly washed with absolute ethyl alcohol, dry three hours, obtain nanoscale Ni-B alloys at 60 DEG C；
3）To step 2）The pH that ammonium hydroxide adjusting solution is added in the nanoscale Ni-B alloys of preparation is 10, adds hydrazine hydrate reduction
Agent carries out reduction reaction；
4）Nanoscale Ni-B alloys after reduction reaction are in hydrogen and argon gas by volume 1：It is made annealing treatment under 1 atmosphere,
Annealing temperature is 650 DEG C, and the time is 6. 7h；
5）HSAs/RGO composite materials are obtained using legal system from top to bottom；Maximum storage hydrogen quantity is 1.85wt%.
Embodiment 2
1）To NiCl under ice-water bath2·6H2KBH is added dropwise in the tetraethylene glycol solution of O4, while stirring and dissolving obtains Ni3B with
Ni2B2In mass ratio 13：The Ni-B alloys of 12 forms；
2）Graphite oxide colloid is heated to 45 DEG C under inert gas shielding, then by step 1）The Ni-B alloys of preparation gradually add
Enter, until raising the temperature to 250 DEG C after whole liquid blackening, after keeping the temperature 1.8h, stop heating, be cooled to room temperature, by gained
Substance carries out centrifugal treating and is repeatedly washed with absolute ethyl alcohol, and dry three hours, obtain nanoscale Ni-B alloys at 60 DEG C；
3）To step 2）The pH that ammonium hydroxide adjusting solution is added in the nanoscale Ni-B alloys of preparation is 10, adds hydrazine hydrate reduction
Agent carries out reduction reaction；
4）Nanoscale Ni-B alloys after reduction reaction are made annealing treatment under argon gas and hydrogen atmosphere, annealing temperature 600
DEG C, time 7h；Hydrogen is 1 by volume with argon gas：1.1；
5）HSAs/RGO composite materials are obtained using legal system from top to bottom；Maximum storage hydrogen quantity is 1.85wt%.
Embodiment 3
1）To NiCl under ice-water bath2·6H2KBH is added dropwise in the tetraethylene glycol solution of O4, while stirring and dissolving obtains Ni3B with
Ni2B2In mass ratio 17：The Ni-B alloys of 7 forms；
2）Graphite oxide colloid is heated to 46 DEG C under inert gas shielding, then by step 1）The Ni-B alloys of preparation gradually add
Enter, until raising the temperature to 300 DEG C after whole liquid blackening, after keeping the temperature 1.2h, stop heating, be cooled to room temperature, by gained
Substance carries out centrifugal treating and is repeatedly washed with absolute ethyl alcohol, and dry three hours, obtain nanoscale Ni-B alloys at 60 DEG C；
3）To step 2）The pH that ammonium hydroxide adjusting solution is added in the nanoscale Ni-B alloys of preparation is 11, adds KBH4Reducing agent
Carry out reduction reaction；
4）Nanoscale Ni-B alloys after reduction reaction are made annealing treatment under argon gas and hydrogen atmosphere, annealing temperature 700
DEG C, time 6.5h；Hydrogen is 1 by volume with argon gas：0.8；
5）HSAs/RGO composite materials are obtained using legal system from top to bottom；Maximum storage hydrogen quantity is 1.83wt%.
Embodiment 4
1）To NiCl under ice-water bath2·6H2KBH is added dropwise in the glycerite of O4, while stirring and dissolving obtains Ni3B is pressed with NiB
Mass ratio 15：The Ni-B alloys of 8 forms；
2）Graphite oxide colloid is heated to 42 DEG C under inert gas shielding, then by step 1）The Ni-B alloys of preparation gradually add
Enter, until raising the temperature to 200 DEG C after whole liquid blackening, after keeping the temperature 2h, stop heating, be cooled to room temperature, by gains
Matter carries out centrifugal treating and is repeatedly washed with absolute ethyl alcohol, and dry three hours, obtain nanoscale Ni-B alloys at 60 DEG C；
3）To step 2）The pH that ammonium hydroxide adjusting solution is added in the nanoscale Ni-B alloys of preparation is 9, adds hydrazine hydrate reduction
Agent carries out reduction reaction；
4）Nanoscale Ni-B alloys after reduction reaction are made annealing treatment under argon gas and hydrogen atmosphere, annealing temperature 900
DEG C, time 6h；Hydrogen and argon gas by volume 1：0.7；
5）HSAs/RGO composite materials are obtained using legal system from top to bottom；Maximum storage hydrogen quantity is 1.58wt%.
Embodiment 5
1）To NiCl under ice-water bath2·6H2KBH is added dropwise in the propylene glycol solution of O4, while stirring and dissolving obtain NiB with
Ni2B2In mass ratio 13：The Ni-B alloys of 2 forms；
2）Graphite oxide colloid is heated to 48 DEG C under inert gas shielding, then by step 1）The Ni-B alloys of preparation gradually add
Enter, until raising the temperature to 350 DEG C after whole liquid blackening, after keeping the temperature 1h, stop heating, be cooled to room temperature, by gains
Matter carries out centrifugal treating and is repeatedly washed with absolute ethyl alcohol, and dry three hours, obtain nanoscale Ni-B alloys at 60 DEG C；
3）To step 2）The pH that ammonium hydroxide adjusting solution is added in the nanoscale Ni-B alloys of preparation is 12, adds hydrazine hydrate reduction
Agent carries out reduction reaction；
4）Nanoscale Ni-B alloys after reduction reaction are made annealing treatment under argon gas and hydrogen atmosphere, annealing temperature 500
DEG C, time 8h；Hydrogen and argon gas by volume 1：1.3；
5）HSAs/RGO composite materials are obtained using legal system from top to bottom；Maximum storage hydrogen quantity is 1.65wt%.
Embodiment 6
1）To NiCl under ice-water bath2·6H2KBH is added dropwise in the ethylene glycol solution of O4, while stirring and dissolving obtains Ni3B forms
Ni-B alloys；
2）Under inert gas shielding by graphite oxide colloid be heated to 45 DEG C ~, then by step 1）The Ni-B alloys of preparation are gradual
It adds in, until raising the temperature to 280 DEG C after whole liquid blackening, after keeping the temperature 1 ~ 2h, stops heating, be cooled to room temperature, by institute
It obtains substance to carry out centrifugal treating and repeatedly washed with absolute ethyl alcohol, dry three hours, obtain nanoscale Ni-B alloys at 60 DEG C；
3）To step 2）The pH that ammonium hydroxide adjusting solution is added in the nanoscale Ni-B alloys of preparation is 8, adds hydrazine hydrate reduction
Agent carries out reduction reaction；
4）Nanoscale Ni-B alloys after reduction reaction are made annealing treatment under argon gas and hydrogen atmosphere, annealing temperature 700
DEG C, time 6.5h；Hydrogen and argon gas by volume 1：2；
5）HSAs/RGO composite materials are obtained using legal system from top to bottom；Maximum storage hydrogen quantity is 1.56wt%.
Electro-chemical test in above-mentioned six embodiments carries out in opening three-electrode system, and cathode is electrode to be measured,
Just extremely Ni (OH)2/ NiOOH, mercuric oxide electrode are reference electrode, and 30wt%KOH solution is electrolyte, and temperature is 25 DEG C, is surveyed
Performance is as shown in table 1.
1 performance comparison table of table
。
The above described is only a preferred embodiment of the present invention, being not that the invention has other forms of limitations, appoint
What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc.
Imitate embodiment.But it is every without departing from technical solution of the present invention content, technical spirit according to the invention is to above example institute
Any simple modification, equivalent variations and the remodeling made still fall within the protection domain of technical solution of the present invention.
Claims (8)
1. the preparation method of a kind of hydrogen bearing alloy and graphene composite material, which is characterized in that comprise the following steps：
1）To NiCl under ice-water bath2·6H2KBH is added in the multicomponent alcoholics compound solution of O4, stirring and dissolving obtain Ni-B conjunction
Gold；
2）Graphite oxide colloid is heated to 42 DEG C ~ 48 DEG C under inert gas shielding, then by step 1）The Ni-B alloys of preparation
It is gradually added into, until raising the temperature to 200 DEG C ~ 350 DEG C after whole liquid blackening, after keeping the temperature 1 ~ 2h, stops heating, be down to room
Obtained material is separated, washed, dried by Wen Hou, obtains nanoscale Ni-B alloys；
3）To step 2）In the nanoscale Ni-B alloys of preparation add in ammonium hydroxide adjust solution pH for alkalescence, add reducing agent into
Row reduction reaction；
4）Nanoscale Ni-B alloys after reduction reaction are made annealing treatment under argon gas and hydrogen atmosphere, annealing temperature 500
DEG C ~ 900 DEG C, the time is 6h ~ 8h；
5）HSAs/RGO composite materials are obtained using legal system from top to bottom.
2. the preparation method of a kind of hydrogen bearing alloy according to claim 1 and graphene composite material, it is characterised in that：Step
Rapid 1）Described in multicomponent alcoholics compound be tetraethylene glycol.
3. the preparation method of a kind of hydrogen bearing alloy according to claim 1 and graphene composite material, it is characterised in that：Step
Rapid 1）Described in Ni-B alloys be Ni2B、Ni3B、NiB、Ni2B2Mixture more than one or both of type alloy.
4. the preparation method of a kind of hydrogen bearing alloy according to claim 1 and graphene composite material, it is characterised in that：Step
Rapid 4）Described in annealing in hydrogen and argon gas by volume 1：It is carried out in 0.7 ~ 1.3 mixed gas.
5. the preparation method of a kind of hydrogen bearing alloy according to claim 1 and graphene composite material, it is characterised in that：Step
Rapid 4）In annealing be temperature be 600 DEG C ~ 700 DEG C, the time be 6.5h ~ 7h.
6. the preparation method of a kind of hydrogen bearing alloy according to claim 1 and graphene composite material, it is characterised in that：Step
Rapid 3）In reducing agent be hydrazine hydrate or KBH4。
7. the preparation method of a kind of hydrogen bearing alloy according to claim 1 and graphene composite material, it is characterised in that：Step
Rapid 3）Described in add in ammonium hydroxide adjust solution pH be 9 ~ 11.
8. the preparation method of a kind of hydrogen bearing alloy according to claim 1 and graphene composite material, it is characterised in that：Step
Rapid 2）Described in the temperature that heats graphite oxide colloid under inert gas shielding be 45 DEG C ~ 46 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116706168A (en) * | 2023-07-03 | 2023-09-05 | 徐州工程学院 | Nickel/nickel boron/hexagonal boron nitride composite material and preparation method and application thereof |
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| CN116706168A (en) * | 2023-07-03 | 2023-09-05 | 徐州工程学院 | Nickel/nickel boron/hexagonal boron nitride composite material and preparation method and application thereof |
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Application publication date: 20180518 |