CN104835958B - A kind of preparation method and application of nickel sulfide hydrogen storage material - Google Patents
A kind of preparation method and application of nickel sulfide hydrogen storage material Download PDFInfo
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- CN104835958B CN104835958B CN201410120691.9A CN201410120691A CN104835958B CN 104835958 B CN104835958 B CN 104835958B CN 201410120691 A CN201410120691 A CN 201410120691A CN 104835958 B CN104835958 B CN 104835958B
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- Prior art keywords
- hydrogen storage
- storage material
- nickel
- powder
- nickel sulfide
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Classifications
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/24—Alkaline accumulators
- H01M10/30—Nickel accumulators
-
- 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
- H01M4/24—Electrodes for alkaline accumulators
- H01M4/242—Hydrogen storage electrodes
-
- 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
- H01M4/24—Electrodes for alkaline accumulators
- H01M4/26—Processes of manufacture
- H01M4/30—Pressing
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- 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
Abstract
The invention provides a kind of preparation method and application of nickel sulfide hydrogen storage material, wherein, preparing the method for nickel sulfide hydrogen storage material includes：By nickel powder and sulphur powder in molar ratio 0.5 2：1 ratio mixing, to obtain mixed-powder；Under an argon atmosphere, the mixed-powder is subjected to ball milling 5~80 hours, to obtain nickel sulfide hydrogen storage material.In addition, when nickel powder and sulphur powder in molar ratio 1：During 1 ratio mixing, obtained nickel sulfide hydrogen storage material has preferable cryogenic property.Using this method of the present invention, the nickel sulfide hydrogen storage material with preferable cryogenic property can be fast and effeciently prepared, and this method technique is simple, it is easy to control, there is no particular/special requirement to equipment, it is safe, it is easy to accomplish large-scale production.
Description
Technical field
The present invention relates to battery material field, in particular it relates to a kind of preparation method and application of nickel sulfide hydrogen storage material,
More particularly, to method, nickel sulfide hydrogen storage material, the method and electricity for preparing GND for preparing nickel sulfide hydrogen storage material
Pond.
Background technology
With the development of battery technology, to the cryogenic property of battery also more and more higher, accordingly, the low temperature properties of battery material
Also can increasingly it be taken seriously.In recent years, hydrogen storage battery material such as NiX, CoX of a series of new（X represents S, C, P）Into people
Sight, wherein the nickel sulfide hydrogen storage material with very big potentiality arouses attention.Vulcanization prepared by hydro-thermal method or solvent-thermal method
Nickel hydrogen storage material method is complicated, and cost is high, the nickel sulfide hydrogen storage material prepared with these methods as hydrogen storage material advantage simultaneously
It is unobvious.
Thus, the research on nickel sulfide hydrogen storage material is still to be improved.
The content of the invention
It is contemplated that at least solving one of technical problem in correlation technique to a certain extent.Therefore, the present invention
One purpose is to propose a kind of hydrogen storage material with higher electric conductivity, good high rate performance and cryogenic property.
In one aspect of the invention, the invention provides a kind of method for preparing nickel sulfide hydrogen storage material.According to this hair
Bright embodiment, this method includes：By nickel powder and sulphur powder 0.5-2 in molar ratio：1 ratio mixing, to obtain mixed-powder；
Under an argon atmosphere, the mixed-powder is subjected to ball milling 5~80 hours, to obtain nickel sulfide hydrogen storage material.Invention human hair
It is existing, using this method of the present invention, nickel sulfide hydrogen storage material can be fast and effeciently prepared, and this method technique is simple,
It is easily controllable, there is no particular/special requirement to equipment, it is safe, it is easy to accomplish large-scale production.In addition, the nickel sulfide prepared
Hydrogen storage material is suitable for manufacturing the battery used under low temperature environment, and the battery cryogenic property prepared is protruded, and disclosure satisfy that
Demand of some particular surroundings to battery performance.
Embodiments in accordance with the present invention, by nickel powder and sulphur powder in molar ratio 1：1 ratio mixing.Thus, the vulcanization of acquisition
Preferably, battery cryogenic property prepared therefrom is protruded the performance of nickel hydrogen storage material.
Embodiments in accordance with the present invention, carry out the ball milling under conditions of 450 revs/min.Thus, the nickel sulfide of acquisition
The particle diameter of hydrogen storage material reaches optimum value, can effectively improve its hydrogen discharging performance.
In another aspect of this invention, the invention provides a kind of nickel sulfide hydrogen storage material.Embodiments in accordance with the present invention,
The nickel sulfide hydrogen storage material is prepared by foregoing method.Inventor's discovery, nickel sulfide hydrogen storage material of the invention
Material, can be effective for preparing battery with higher electric conductivity, and the battery prepared has good high rate performance
And cryogenic property, especially cryogenic property are more prominent, it is suitable for using at low ambient temperatures.
In another aspect of the invention, the invention provides a kind of method for preparing GND.According to the reality of the present invention
Example is applied, this method includes：By foregoing nickel sulfide hydrogen storage material and nickel powder according to mass ratio 1：1 mixing, to obtain sulphur
Change the mixture of nickel hydrogen storage material and nickel powder；The mixture of the nickel sulfide hydrogen storage material and nickel powder is pressed in nickel foam
Piece, to obtain GND.Using this method of the present invention, GND, and the party can be fast and effeciently prepared
Method is simple to operate, convenient and swift, and great feasibility is provided for industrialization.In addition, will be prepared using this method of the present invention
The GND of acquisition is assembled into battery, and resulting battery has higher electric conductivity, good high rate performance and low temperature
Performance, disclosure satisfy that demand of some particular surroundings to battery performance.
In another aspect of the invention, the invention provides a kind of battery.Embodiments in accordance with the present invention, the battery bag contains
Foregoing nickel sulfide hydrogen storage material.Inventor has found that the battery of the invention has good high rate performance and low temperature properties
Can, it disclosure satisfy that demand of some particular surroundings to battery performance.In addition, the preparation technology of the battery of the present invention is simple, safety
Property it is high, provide great feasibility for industrialization.
Brief description of the drawings
Fig. 1 is shown according to one embodiment of present invention, prepares the schematic flow sheet of the method for nickel sulfide hydrogen storage material；
Fig. 2 is shown according to one embodiment of present invention, prepares the schematic flow sheet of the method for GND；
Fig. 3 shows according to one embodiment of present invention, button cell S1 ', button cell S4 ' and button cell S5 '
Cycle performance testing result；And
Fig. 4 shows that according to one embodiment of present invention button cell S1 ' and button cell D1 ' cycle performance are examined
Survey result.
Embodiment
Embodiments of the invention are described below in detail.The embodiments described below is exemplary, is only used for explaining this hair
It is bright, and be not considered as limiting the invention.Unreceipted particular technique or condition in embodiment, according to text in the art
Offer described technology or condition or carried out according to product description.Agents useful for same or the unreceipted production firm person of instrument,
For can be by the conventional products of acquisition purchased in market.
In one aspect of the invention, the invention provides a kind of method for preparing nickel sulfide hydrogen storage material.According to this hair
Bright embodiment, reference picture 1, this method comprises the following steps：
S100：By nickel powder and sulphur powder 0.5-2 in molar ratio：1 ratio mixing, to obtain mixed-powder.Thereby, it is possible to
Mixed with most suitable ratio, the electric conductivity of the nickel sulfide hydrogen storage material prepared is protruded, be adapted to manufacture low temperature bar
The battery used under part.
Embodiments in accordance with the present invention, by nickel powder and sulphur powder in molar ratio 1：During 1 ratio mixing, thus, the sulphur of acquisition
The performance for changing nickel hydrogen storage material preferably, is especially protruded by the battery cryogenic property of its preparation.
S200：Under an argon atmosphere, the mixed-powder is subjected to ball milling 5~80 hours, to obtain nickel sulfide hydrogen storage
Material.Thus, raising is conducive to prepare the efficiency of nickel sulfide hydrogen storage material.
Embodiments in accordance with the present invention, carry out the ball milling under conditions of 450 revs/min.Thus, the nickel sulfide of acquisition
The particle diameter of hydrogen storage material reaches optimum value, can effectively improve its hydrogen discharging performance.
It should be noted that ball-milling technology has an impact to particle size, particle size has an impact to hydrogen discharging performance.Ball
Time consuming is longer, and rotational speed of ball-mill is bigger, and particle size is smaller, and hydrogen discharging temperature is lower, and hydrogen discharging rate is faster.But particle is excessively refined
On the one hand can make alloy surface tension force increase and it is inter-adhesive, on the other hand alloy powder activity can be made to increase and aoxidize.It is long
Time ball milling, not only without facilitation, can be also negatively affected to synthetic reaction.The mixed-powder is existed in the present invention
Under conditions of 450 revs/min, ball milling is carried out 5~80 hours, enable to the particle diameter of nickel sulfide hydrogen storage material to reach optimum value,
Effectively improve its hydrogen discharging performance.
Inventor has found, using this method of the present invention, can fast and effeciently prepare nickel sulfide hydrogen storage material, and
This method technique is simple, it is easy to control, and does not have particular/special requirement to equipment, safe, it is easy to accomplish large-scale production.In addition,
The nickel sulfide hydrogen storage material prepared, is suitable for manufacturing the battery used under low temperature environment, the battery low temperature properties prepared
Can be prominent, it disclosure satisfy that demand of some particular surroundings to battery performance.
In one embodiment of the invention, it is used as battery using the nickel sulfide hydrogen storage material prepared by the above method to bear
Under the battery of pole active material, normal temperature condition, when cycle-index reaches 100 times, hold with the electric discharge for being not less than 300mAh/g
Under amount, subzero 20 degrees celsius, when cycle-index reaches 100 times, still with the discharge capacity for being not less than 270mAh/g.
In another aspect of this invention, the invention provides a kind of nickel sulfide hydrogen storage material.Embodiments in accordance with the present invention,
The nickel sulfide hydrogen storage material is prepared by foregoing method.Inventor's discovery, nickel sulfide hydrogen storage material of the invention
Material, with higher electric conductivity, the battery comprising the nickel sulfide hydrogen storage material has good high rate performance and cryogenic property,
Especially cryogenic property is more prominent, disclosure satisfy that demand of some particular surroundings to battery performance.
In another aspect of the invention, the invention provides a kind of method for preparing GND.According to the reality of the present invention
Apply example, reference picture 2, this method comprises the following steps：
S300：By foregoing nickel sulfide hydrogen storage material and nickel powder according to mass ratio 1：1 mixing, to obtain nickel sulfide
The mixture of hydrogen storage material and nickel powder.
S400：The mixture of the nickel sulfide hydrogen storage material and nickel powder is subjected to tabletting in nickel foam, to obtain electricity
Pond negative pole.
Using this method of the present invention, GND can be fast and effeciently prepared, and this method is simple to operate, side
Just it is quick, provide great feasibility for industrialization.In addition, being born comprising the battery that this method using the present invention is prepared
The battery of pole, with higher electric conductivity, good high rate performance and cryogenic property, disclosure satisfy that some particular surroundings to electricity
The demand of pond performance.
In another aspect of the invention, the invention provides a kind of battery.Embodiments in accordance with the present invention, the battery bag contains
Foregoing nickel sulfide hydrogen storage material.Embodiments in accordance with the present invention, the type of the battery is not particularly limited.According to this hair
Bright one embodiment, is made GND, using hydroxide using foregoing method by the nickel sulfide hydrogen storage material
Nickel is positive electrode active materials, and button is prepared into as electrolyte, and barrier film using the mixed solution of sodium hydroxide and potassium hydroxide
Battery.Inventor has found that the battery of the invention has good high rate performance and cryogenic property, disclosure satisfy that some Special Rings
Demand of the border to battery performance.In addition, the preparation technology of the battery of the present invention is simple, and it is safe, provide pole for industrialization
Big feasibility.
Embodiments of the invention are described below in detail.The embodiments described below is exemplary, is only used for explaining this hair
It is bright, and be not considered as limiting the invention.
Embodiment 1
According to mol ratio it is 1 by nickel powder and sulphur powder：1 ratio is added in ball grinder, argon gas 5 is filled with into ball grinder small
Shi Hou, ball milling 10 hours under the conditions of 450rpm obtain nickel sulfide hydrogen storage material S1.
Embodiment 2
According to mol ratio it is 1 by nickel powder and sulphur powder：1 ratio is added in ball grinder, argon gas 6 is filled with into ball grinder small
Shi Hou, ball milling 5 hours under the conditions of 450rpm obtain nickel sulfide hydrogen storage material S2.
Embodiment 3
According to mol ratio it is 1 by nickel powder and sulphur powder：1 ratio is added in ball grinder, argon gas 5 is filled with into ball grinder small
Shi Hou, ball milling 80 hours under the conditions of 450rpm obtain nickel sulfide hydrogen storage material S3.Wherein, it is to prevent material in mechanical milling process
Overheat shuts down rest, it is necessary to be spaced 10 hours.
Embodiment 4
According to mol ratio it is 0.5 by nickel powder and sulphur powder：1 ratio is added in ball grinder, and argon gas 5 is filled with into ball grinder
After hour, ball milling 10 hours under the conditions of 450rpm obtain nickel sulfide hydrogen storage material S4.
Embodiment 5
According to mol ratio it is 2 by nickel powder and sulphur powder：1 ratio is added in ball grinder, argon gas 5 is filled with into ball grinder small
Shi Hou, ball milling 10 hours under the conditions of 450rpm obtain nickel sulfide hydrogen storage material S5.
Comparative example 1
According to mol ratio it is 1 by cobalt powder and carbon dust：1 ratio is added in ball grinder, argon gas 5 is filled with into ball grinder small
Shi Hou, ball milling 10 hours under the conditions of 450rpm obtain cobalt carbide hydrogen storage material D1.
Embodiment 6
By the nickel sulfide hydrogen storage material S1 prepared in embodiment, nickel sulfide hydrogen storage material S4, nickel sulfide hydrogen storage material
The cobalt carbide hydrogen storage material D1 prepared in S5 and comparative example is respectively with nickel powder according to mass ratio 1：1 mixing, then by institute
Obtained mixture carries out tabletting in nickel foam respectively, so as to obtain GND S1, GND S4, GND S5 with
And GND D1.
Test 1
Respectively with the GND S1 prepared in embodiment, GND S4, GND S5 and GND
D1 is negative pole, uses nickel hydroxide for positive electrode active materials, electrolysis is used as using the mixed solution of sodium hydroxide and potassium hydroxide
Liquid, and barrier film are prepared into button cell S1 ', button cell S4 ', button cell S5 ' and button cell D1 '.
In the button cell S1 ', button cell S4 ' and button cell that under room temperature condition, are prepared in testing example
S5 ' cycle performance, wherein, discharge cut-off voltage is 1.1V, and charge cutoff voltage is 4.2V.Result of the test is as shown in Figure 3.
It is can be seen that from Fig. 3 result in the case of cycle-index identical, button cell S4 '（0.5：1）With button electricity
Pond S5 '（2：1）Discharge capacity and button cell S1 '（1：1）Cycle performance it is good.But, button cell S1 '（1：1）
Cycle performance it is optimal, i.e. button cell S1 ' have preferable cycle performance.
Test 2
Button cell D1 ', button cell S1 ' cycle performance are tested under subzero 20 degrees Celsius, comparing, wherein, electric discharge
Blanking voltage is 1.1V, and charge cutoff voltage is 4.2V.Result of the test is as shown in Figure 4.
It can be seen from Fig. 4 result in the case of cycle-index identical, button cell D1 '（CoC）Discharge capacity
Substantially less than button cell S1 '（NiS）, showing the battery of the present invention has good cycle performance and cryogenic property.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means to combine specific features, structure, material or the spy that the embodiment or example are described
Point is contained at least one embodiment of the present invention or example.In this manual, to the schematic representation of above-mentioned term not
Identical embodiment or example must be directed to.Moreover, specific features, structure, material or the feature of description can be with office
Combined in an appropriate manner in one or more embodiments or example.In addition, in the case of not conflicting, the skill of this area
Art personnel can be tied the not be the same as Example or the feature of example and non-be the same as Example or example described in this specification
Close and combine.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changed, replacing and modification.
Claims (3)
1. a kind of method for preparing GND, it is characterised in that including：
By nickel powder and sulphur powder 0.5-2 in molar ratio：1 ratio mixing, to obtain mixed-powder；
Under an argon atmosphere, the mixed-powder is subjected to ball milling 5~80 hours, to obtain nickel sulfide hydrogen storage material；
By the nickel sulfide hydrogen storage material and nickel powder according to mass ratio 1：1 mixing, to obtain nickel sulfide hydrogen storage material and nickel powder
Mixture；
The mixture of the nickel sulfide hydrogen storage material and nickel powder is subjected to tabletting in nickel foam, to obtain GND.
2. according to the method described in claim 1, it is characterised in that be 1 in molar ratio by the nickel powder and the sulphur powder：1
Ratio is mixed.
3. method according to claim 1 or 2, it is characterised in that the ball milling is carried out under conditions of 450 revs/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410120691.9A CN104835958B (en) | 2014-03-27 | 2014-03-27 | A kind of preparation method and application of nickel sulfide hydrogen storage material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410120691.9A CN104835958B (en) | 2014-03-27 | 2014-03-27 | A kind of preparation method and application of nickel sulfide hydrogen storage material |
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| Publication Number | Publication Date |
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| CN104835958A CN104835958A (en) | 2015-08-12 |
| CN104835958B true CN104835958B (en) | 2017-10-10 |
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| CN107799769B (en) * | 2017-02-20 | 2019-11-15 | 湖南大学 | A kind of nanometer of curing nickel material and its preparation method and application |
| CN109252188B (en) * | 2018-09-30 | 2021-05-07 | 河北工业大学 | Preparation method of nickel sulfide nano film |
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| CN1073969C (en) * | 1999-07-15 | 2001-10-31 | 北京矿冶研究总院 | Synthesis method of high-purity nickel disulfide powder |
| US8361654B2 (en) * | 2007-08-24 | 2013-01-29 | Nat'l Institute of Advanced Industrial Science . . . | Process for producing metal sulfide |
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