CN110078137A - Vulcanize nickel electrode material and the preparation method and application thereof - Google Patents
Vulcanize nickel electrode material and the preparation method and application thereof Download PDFInfo
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- C01G53/00—Compounds of nickel
- C01G53/11—Sulfides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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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
- Y02E60/13—Energy storage using capacitors
Abstract
The present invention provides a kind of vulcanization nickel electrode material and the preparation method and application thereof, preparation method includes: that deionized water and organic solvent are mixed and made into reaction dissolvent, is then dissolved in reaction dissolvent nickel salt with containing sulfur feedstock, forms mixed solution after stirring；Mixed solution is heated, cooled down, filtered and is washed, black pie material is obtained；Ultrasonic etching processing is carried out to black pie material, refilters, wash and dries, obtain black powdered material；Black powdered material is sintered at high temperature, then obtains vulcanization nickel electrode material after ground crushing.Gained vulcanizes nickel electrode material and is made of the particle that partial size is 3~8 μm, particle is 3D flower-like structure, with unique nanometer sheet intersection construction and rough surface, more reactivity sites can be provided, shorten the diffusion length of electrolyte ion, has excellent fake capacitance characteristic, specific capacity and cyclical stability can be effectively improved in supercapacitor by being applied.
Description
Technical field
The present invention relates to electrode material for super capacitor preparation technical field, in particular to a kind of vulcanization nickel electrode material and
Preparation method and application.
Background technique
Supercapacitor has many advantages, such as that charge-discharge velocity is fast, has extended cycle life and cheap, is at present by pass
The research hotspot of note.The study found that the energy density of supercapacitor depends primarily on its electrode material.Wherein, transition metal
Sulfide material has more higher than the carbon material being widely used at present theoretical than electricity due to its fake capacitance energy storage mechanism
Hold；Meanwhile there is electric conductivity more stronger than transition metal oxide and hydroxide electrode material and structural stability.Moreover,
The production technology of transient metal sulfide is relatively simple, and it is a kind of environmentally friendly material that raw material resources are abundant.To sum up,
Transient metal sulfide material is a kind of high-performance super capacitor electrode material with development potentiality.
The common method for preparing transient metal sulfide material includes hydro-thermal method and solvent-thermal method, and hydro-thermal method includes presoma
Preparation process and subsequent sulfidation, preparation step is cumbersome, the production cycle is long.Solvent-thermal method can provide more compared with hydro-thermal method
Wide range of reaction temperature and more solvent selections, but its uncertain high temperature and high pressure environment brings for the controllable preparation of material
Challenge.Other preparation methods include high temperature gas phase, high temperature process heat, electrochemistry formated etc., these method equipment are expensive, product
Purity is not high, is difficult to realize industrialized production.
Therefore, solvent and raw material self character are given full play to, develop easy to operate, process is short, it is at low cost, realize it is controllable
The synthetic method of preparation has great impetus to the development of electrode material for super capacitor.
Summary of the invention
The present invention provides a kind of vulcanization nickel electrode materials and the preparation method and application thereof, and its purpose is to realize one
It walks controlledly synthesis in solvent-thermal method and vulcanizes nickel material, and the vulcanization nickel material specific capacitance with higher and stable circulation made
Property.
To achieve the goals above, the present invention provides following scheme:
(1) deionized water and organic solvent are mixed according to the ratio that volume ratio is 0.5~2:1, obtains reaction dissolvent；It will
Nickel salt is dissolved in gained reaction dissolvent with containing the ratio that sulfur feedstock is 0.5~1:1 in molar ratio, and mixed solution is formed after stirring；
Wherein, nickel ion concentration is 0.08~0.12mol/L；
(2) mixed solution obtained by step (1) is reacted into 12~14h at 180~200 DEG C, then through cooling, filter and wash
It washs, obtains black pie material；
(3) ultrasonic etching processing is carried out to black pie material obtained by step (2), is then filtered, washed and dried drying, is obtained
To black powdered material；
(4) black powdered material obtained by step (3) is placed at 200~300 DEG C normal pressure-sintered 3~6h in argon atmosphere,
Vulcanization nickel electrode material is obtained after ground crushing again.
Preferably, the organic solvent is ethylene glycol, ethylenediamine, n,N-Dimethylformamide and n,N-dimethylacetamide
One or more of.
Preferably, the nickel salt is one or more of nickel nitrate, nickel sulfate, nickel acetate and nickel chloride.
Preferably, it is described containing sulfur feedstock be one of thiocarbamide, Sodium Sulphate Nine Hydroxide, thioacetamide and carbon disulfide or
It is several.
Preferably, the mixing speed of stirring described in step (1) is 200~400r/min, and mixing time is 1~2h.
Preferably, the ultrasound etching is specially to immerse black pie material in etching agent, is 20~25kHz in frequency
0.5~1h of lower ultrasonic disperse；Wherein, the concentration of etching agent is 0.1~0.2mol/L.
Preferably, the etching agent is one or more of potassium hydroxide, hydrochloric acid, phosphoric acid and acetic acid.
Preferably, dry described in step (3) to include the steps that pre-freeze and freeze-drying, wherein the time of freeze-drying
For 30~48h.
The inventive concept total as one, the present invention also provides a kind of vulcanizations being prepared by above-mentioned any one method
Nickel electrode material, the vulcanization nickel electrode material are made of the particle that partial size is 3~8 μm, and the particle is 3D flower-like structure.
The inventive concept total as one, the present invention also provides one kind electricity of the nickel sulfide as made from above-mentioned any one method
The application of pole material or above-mentioned vulcanization nickel electrode material in supercapacitor.
The present invention carries out ultrasonic etching processing to the material of a step solvent-thermal method controllable preparation, before keeping material structure
Put the specific surface area that can significantly increase material.High temperature sintering is carried out to the material after ultrasonic etching processing again, water can be improved
Thermal method prepares the bad problem of material crystalline.Ultrasound etching with high temperature sintering step is easily operated, the time is short, integrated operation stream
Journey is still relatively simple.
Above scheme of the invention have it is following the utility model has the advantages that
For the problems such as conventional hydrothermal method preparation process needs template/activating agent, reaction time is long, energy consumption is high, the present invention
The solvent-thermal method of offer gives full play to the physicochemical properties of organic solvent, big using its viscosity, can be combined into metal ion
The characteristics such as complex realize the controlledly synthesis for vulcanizing nickel material in a step solvent-thermal method.Solvent-thermal method provided by the invention is not
It needs to pre-process, temperature is low in synthesis process, short preparation period, reduces energy consumption and reaction cost, and controllability and reproducibility
It is good, it is suitble to large-scale production.
Vulcanization nickel electrode material preparation method provided by the invention is sintered further promotion to vulcanization nickel material
The crystallinity of material, while ultrasound etching on the flower-shaped vulcanization nickel material of 3D prepares rough surface, can significantly increase material
Specific surface area, improve electrolyte and be impregnated with rate.
Vulcanization nickel electrode material produced by the present invention is 3D flower-like structure, with unique nanometer sheet intersection construction and slightly
Rough surface can provide more reactivity sites, shorten the diffusion length of electrolyte ion, and it is special to have excellent fake capacitance
Property, to have higher specific capacitance and better cyclical stability and longer cycle life.It is made in the embodiment of the present invention
The vulcanization nickel electrode material obtained, conservation rate is higher than 80% after 2000 circles are recycled under 2A/g current density；In the voltage of 0~0.5V
Specific capacitance of discharging in range, under 1A/g current density is up to 1308F/g.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph for the flower-shape Ni S material that the embodiment of the present invention 1 is prepared.
Fig. 2 is the XRD spectrum for the flower-shape Ni S material that the embodiment of the present invention 1 is prepared.
Fig. 3 is CV curve of the flower-shape Ni S material that is prepared of the embodiment of the present invention 1 under different scanning rates.
Fig. 4 is charging and discharging curve of the flower-shape Ni S material that is prepared of the embodiment of the present invention 1 under different current densities.
Fig. 5 is specific discharge capacity of the flower-shape Ni S material that is prepared of the embodiment of the present invention 1 under different current densities.
Fig. 6 is cycle performance of the flower-shape Ni S material that is prepared of the embodiment of the present invention 1 under 2A/g current density.
Specific embodiment
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with specific implementation
Example is described in detail.
Embodiment 1
(1) 40mL deionized water and 20mLN are measured, 20min is mixed in dinethylformamide (DMF), and reaction is made
Solvent；Weigh 4.8mmol Ni (NO3)2.6H2O is dispersed therein, according to nickel in solution and sulphur molar ratio after magnetic agitation 30min
7.2mmol CH is added in 0.67:14N2S continues to stir 30min, obtains mixed solution, mixing speed 200r/min.
(2) mixed solution obtained by step (1) is transferred in the polytetrafluoroethyllining lining autoclave of 100mL volume,
180 DEG C of baking oven inside holding 12h are placed in fully reacting.Power supply is closed after reaction, after reaction kettle cooled to room temperature
It takes out.
(3) it is successively filtered with deionized water and dehydrated alcohol, washing reaction product, obtains black pie material.
(4) it disperses gained black pie material in step (3) in the KOH solution that concentration is 0.2mol/L, in 20kHz
Ultrasonic disperse 1h under frequency.It then successively filtered, washed with deionized water and dehydrated alcohol, obtained material is placed in culture dish
In, it is 0.2:1 that a small amount of deionized water to solid-to-liquid ratio, which is added, is placed in dispersion 10min under ultrasound condition and obtains uniform suspension.It will be equal
Even suspension pre-freeze in refrigerator-freezer is placed on the dry 30h of freeze drying equipment for 24 hours, obtains black powder.
(5) gained black powdered material in step (4) is placed in 300 DEG C of high-temperature atmosphere sintering furnaces and is protected in argon atmosphere
Under normal pressure-sintered 4h, obtained after grinding vulcanization nickel electrode material.
In the present embodiment using go from water and DMF volume ratio for 2:1 mixed solution as reaction dissolvent, nickel and sulphur molar ratio
For the nickel sulfide that the solvent-thermal method of 0.67:1 is prepared into, vulcanize nickel electrode material by KOH etching and gained after high temperature sintering
Scanning electron microscope is as shown in Figure 1, from Fig. a kind as can be seen that the NiS that the present embodiment preparation method synthesizes is in 3D flower-like structure, the flower
Shape structure is assembled by shaggy nanometer sheet intersection, and grain diameter is 3~5 μm, even particle distribution.
X-ray diffraction test (XRD) is carried out to material, test results are shown in figure 2, and the XRD diffraction maximum of material is sharp
And it is corresponding with the standard card of NiS, without other miscellaneous peaks, illustrate that synthetic material is pure phase NiS, and stronger diffraction maximum confirms
Its good crystallinity.
The 3D flower-shape Ni S material that the present embodiment is prepared into is assembled into three electrode electrolyser test systems, in different electric currents
Charging and discharging curve under density is as shown in Figure 4.As can be seen from Figure 4 the material is in the voltage range of 0~0.5V, 1A/g electricity
Specific capacitance of discharging under current density is up to 1308F/g.Under different current densities, the present embodiment prepares the specific discharge capacity of material such as
Shown in Fig. 5.As shown in figure, as current density increases, specific capacitance value is decayed, when current density increases to from 1A/g
When 10A/g, capacity retention 33.64%.Its cycle performance under 2A/g current density is as shown in Figure 6.As shown in figure,
Conservation rate is still up to 82.22% after 2000 circle of circulation under 2A/g current density, has excellent cyclical stability.
Embodiment 2
(1) it measures 30mL deionized water and 30min is mixed in 30mL ethylene glycol, reaction dissolvent is made；Weigh 5.4mmol
NiCl2 .6H2O is dispersed therein, and 7.2mmol is added according to nickel in solution and sulphur molar ratio 0.75:1 after magnetic agitation 60min
CH4N2S continues to stir 60min, obtains mixed solution, mixing speed 300r/min.
(2) mixed solution made from step (1) is transferred to the polytetrafluoroethyllining lining autoclave of 100mL volume
In, 180 DEG C of baking oven inside holding 14h are placed in fully reacting.Power supply is closed after reaction, to reaction kettle cooled to room temperature
After take out.
(3) it is successively filtered with deionized water and dehydrated alcohol, washing reaction product, obtains black pie material.
(4) it disperses black pie material in step (3) in the HCl solution that concentration is 0.1mol/L, in 25kHz frequency
Lower ultrasound 0.5h.It is then successively centrifuged, washed with deionized water and dehydrated alcohol, obtained material is placed in culture dish, is added
Entering a small amount of deionized water to solid-to-liquid ratio is 0.15:1, is placed in dispersion 10min under ultrasound condition and obtains uniform suspension.It will uniformly hang
Turbid pre-freeze in refrigerator-freezer is placed on the dry 36h of freeze drying equipment for 24 hours and obtains black powder.
(5) gained black powdered material in step (4) is placed in 200 DEG C of high-temperature atmosphere sintering furnaces and is protected in argon atmosphere
Under normal pressure-sintered 3h, flower-shape Ni S fake capacitance material is obtained after grinding.
In the present embodiment using water and ethylene glycol volume ratio for 1:1 mixed solution as reaction dissolvent, nickel and sulphur molar ratio
For the nickel sulfide that the solvent-thermal method of 0.75:1 is prepared into, is etched by HCl and gained NiS is shaggy receives after high temperature sintering
Rice piece intersects the flower-like structure assembled, and material particle size is 5~8 μm, and particle is uniformly dispersed.Nanometer sheet compared with Example 1
Thickness increases, and electric discharge specific capacitance performance is affected, and specific capacitance of discharging under 1A/g current density is 868F/g, 2A/g current density
Conservation rate is higher than 80% after lower 2000 circle of circulation.
Embodiment 3
(1) it measures 20mL deionized water and 40min is mixed in 40mL n,N-dimethylacetamide (DMAC), be made anti-
Answer solvent；Weigh 7.2mmol NiCl2 .6H2O is dispersed therein, according to nickel in solution and sulphur molar ratio after magnetic agitation 30min
7.2mmol CH is added in 1:14N2S continues to stir 40min, obtains mixed solution, mixing speed 400r/min.
(2) mixed solution made from step (1) is transferred to the polytetrafluoroethyllining lining autoclave of 100mL volume
In, 200 DEG C of baking oven inside holding 12h are placed in fully reacting.Power supply is closed after reaction, to reaction kettle cooled to room temperature
After take out.
(3) it is successively centrifuged with deionized water and dehydrated alcohol, washing reaction product, obtains black pie material.
(4) it disperses black pie material in step (3) in acetic acid (HAc) solution that concentration is 0.2mol/L,
Ultrasound 1h under 20kHz frequency.Deionized water and dehydrated alcohol successively centrifuge washing are then used, obtained material is placed in culture dish
In, it is 0.15:1 that a small amount of deionized water to solid-to-liquid ratio, which is added, is placed in dispersion 10min under ultrasound condition and obtains uniform suspension.It will
Uniform suspension pre-freeze in refrigerator-freezer is placed on the dry 48h of freeze drying equipment for 24 hours, obtains black powder.
(5) gained dusty material in step (4) is placed in 300 DEG C of high-temperature atmosphere sintering furnaces under argon atmosphere protection often
Pressure sintering 6h, obtains vulcanization nickel electrode material after grinding.
In the present embodiment using deionized water and DMAC volume ratio for 1:2 mixed solution as reaction dissolvent, nickel rubs with sulphur
, than the nickel sulfide that the solvent-thermal method for 1:1 is prepared into, it is shaggy for etching by HAc with resulting materials after high temperature sintering for you
Nanometer sheet intersects the flower-like structure of composition, and material particle size is 3~5 μm, and particle is uniformly dispersed.Nanometer the piece number compared with Example 1
Measure less, electric discharge specific capacitance performance is affected, and specific capacitance of discharging under 1A/g current density is 674F/g, under 2A/g current density
Conservation rate is higher than 80% after 2000 circle of circulation.
Comparative example
(1) 60mL deionized water is measured as reaction dissolvent, weighs 4.8mmol Ni (NO3)2 .6H2O is dispersed therein, magnetic
7.2mmolCH is added according to nickel in solution and sulphur molar ratio 0.67:1 after power stirring 30min4N2S continues stirring 30min and obtains
One solution.
(2) mixed solution made from step (1) is transferred to the polytetrafluoroethyllining lining autoclave of 100mL volume
In, 180 DEG C of baking oven inside holding 12h are placed in fully reacting.Power supply is closed after reaction, to reaction kettle cooled to room temperature
After take out.
(3) deionized water and dehydrated alcohol successively filtering and washing reaction product are used, obtained material is placed in culture dish,
It is 0.2:1 that a small amount of deionized water to solid-to-liquid ratio, which is added, is placed in dispersion 10min under ultrasound condition and obtains uniform suspension.In refrigerator-freezer
It is nickel sulfide that middle pre-freeze, which is placed on the dry 36h of freeze drying equipment for 24 hours and obtains black powder,.
Using deionized water as reaction dissolvent in the present embodiment, products therefrom be bulky grain bulk material, no etching agent plus
Material surface is smooth in the case where entering, and lesser specific surface area limits the infiltration of electrolyte.Compared with Example 1, material
Crystallinity is poor, reunion is serious, impurity content is high.And specific capacitance is low, specific capacitance of discharging under 1A/g current density is 354F/g, remote low
Conservation rate is lower than 70% after 2000 circle of circulation under embodiment 1,2A/g current density.
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, it can also make several improvements and retouch, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of preparation method for vulcanizing nickel electrode material, which comprises the steps of:
(1) deionized water and organic solvent are mixed according to the ratio that volume ratio is 0.5~2:1, obtains reaction dissolvent；By nickel salt
It is dissolved in gained reaction dissolvent with containing the ratio that sulfur feedstock is 0.5~1:1 in molar ratio, forms mixed solution after stirring；Wherein,
Nickel ion concentration is 0.08~0.12mol/L；
(2) mixed solution obtained by step (1) is reacted at 180~200 DEG C 12~14h, then through cooling, filtering and washing, obtained
To black pie material；
(3) ultrasonic etching processing is carried out to black pie material obtained by step (2), is then filtered, washed and dried drying, is obtained black
Toner powder material；
(4) black powdered material obtained by step (3) is placed at 200~300 DEG C normal pressure-sintered 3~6h in argon atmosphere, then passed through
Vulcanization nickel electrode material is obtained after grinding.
2. vulcanizing the preparation method of nickel electrode material according to claim 1, which is characterized in that the organic solvent is second two
One or more of alcohol, ethylenediamine, N,N-dimethylformamide and DMAC N,N' dimethyl acetamide.
3. according to claim 1 vulcanize nickel electrode material preparation method, which is characterized in that the nickel salt be nickel nitrate,
One or more of nickel sulfate, nickel acetate and nickel chloride.
4. vulcanizing the preparation method of nickel electrode material according to claim 1, which is characterized in that the sulfur feedstock that contains is sulphur
One or more of urea, Sodium Sulphate Nine Hydroxide, thioacetamide and carbon disulfide.
5. vulcanizing the preparation method of nickel electrode material according to claim 1, which is characterized in that stirred described in step (1)
Mixing speed be 200~400r/min, mixing time be 1~2h.
6. vulcanizing the preparation method of nickel electrode material according to claim 1, which is characterized in that the ultrasound, which etches, is specially
Black pie material is immersed in etching agent, 0.5~1h of ultrasonic disperse in the case where frequency is 20~25kHz；Wherein, etching agent is dense
Degree is 0.1~0.2mol/L.
7. vulcanizing the preparation method of nickel electrode material according to claim 6, which is characterized in that the etching agent is hydroxide
One or more of potassium, hydrochloric acid, phosphoric acid and acetic acid.
8. vulcanizing the preparation method of nickel electrode material according to claim 1, which is characterized in that dry described in step (3)
Include the steps that pre-freeze and freeze-drying, wherein the time of freeze-drying is 30~48h.
9. a kind of vulcanization nickel electrode material being prepared by claim 1~8 any one the method, which is characterized in that
The vulcanization nickel electrode material is made of the particle that partial size is 3~8 μm, and the particle is 3D flower-like structure.
10. one kind vulcanizes nickel electrode material as made from claim 1~8 any one the method or such as claim 9 institute
Application of the vulcanization nickel electrode material stated in supercapacitor.
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| CN110683588A (en) * | 2019-09-06 | 2020-01-14 | 中南大学 | Self-supporting CoMoS4Super capacitor electrode material, preparation method and application |
| CN114452986A (en) * | 2020-11-09 | 2022-05-10 | 湖南大学 | Grass-shaped carbon nitride/flower-shaped nickel sulfide composite material and preparation method and application thereof |
| CN114890481A (en) * | 2022-04-22 | 2022-08-12 | 四川智立方博导科技有限责任公司 | Two-dimensional nickel oxysulfide nano-sheet material, preparation method and application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110683588A (en) * | 2019-09-06 | 2020-01-14 | 中南大学 | Self-supporting CoMoS4Super capacitor electrode material, preparation method and application |
| CN114452986A (en) * | 2020-11-09 | 2022-05-10 | 湖南大学 | Grass-shaped carbon nitride/flower-shaped nickel sulfide composite material and preparation method and application thereof |
| CN114890481A (en) * | 2022-04-22 | 2022-08-12 | 四川智立方博导科技有限责任公司 | Two-dimensional nickel oxysulfide nano-sheet material, preparation method and application |
| CN114890481B (en) * | 2022-04-22 | 2023-12-12 | 四川智立方博导科技有限责任公司 | Two-dimensional nickel oxysulfide nano-sheet material, preparation method and application |
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Application publication date: 20190802 |