CN107086131A - Water system Asymmetric Supercapacitor based on NiS/N rGO Yu N rGO - Google Patents
Water system Asymmetric Supercapacitor based on NiS/N rGO Yu N rGO Download PDFInfo
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- CN107086131A CN107086131A CN201710273098.1A CN201710273098A CN107086131A CN 107086131 A CN107086131 A CN 107086131A CN 201710273098 A CN201710273098 A CN 201710273098A CN 107086131 A CN107086131 A CN 107086131A
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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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- 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
- Y02E60/13—Energy storage using capacitors
Abstract
Water system Asymmetric Supercapacitor of the invention based on NiS/N rGO Yu N rGO, specifically includes positive electrode, negative material, barrier film and electrolyte.Described NiS/N rGO（NiS/ nitrogen-doped graphenes）Positive electrode, the N rGO of composite（Nitrogen-doped graphene）Negative material is made using solvent thermal process, and electrolyte is alkali water-soluble electrolyte solution.The operating voltage range of NiS/N rGO//N rGO water system Asymmetric Supercapacitors prepared by the present invention is up to 1.6V, and with excellent energy density and power density, and preparation technology is simple, easy to operate, is adapted to large-scale production, with good application prospect.
Description
Technical field
Water system Asymmetric Supercapacitor of the invention based on NiS/N-rGO and N-rGO is used as positive pole using NiS/N-rGO
Material, N-rGO is assembled to be made as negative material, particularly belongs to electrochemical energy storage technical field.
Background technology
Energy density and power density are two key parameters of the chemical property for assessing ultracapacitor.Although mostly
The energy density of number commercialization ultracapacitor (is less than 10 W h kg-1) be far above traditional sucrose capacitor, but still less than lithium from
The energy density of sub- battery and fuel cell.
On the one hand, the energy density of ultracapacitor is directly proportional to the specific capacitance of electrode, by the specific capacitance for improving material
It is an effective raising energy density method, this can be realized by improving the specific capacitance of positive electrode and negative material.
On the other hand, the energy density of ultracapacitor is directly proportional to actual operating voltage square.Therefore, operating voltage window is widened
The energy density of electrochemical capacitance can be effectively improved.An effective way for widening operating voltage window is exactly to develop asymmetric super electricity
Container.
Asymmetric Supercapacitor is by two different electrode materials, a positive electrode (fake capacitance) and a negative electrode
(electric double layer capacitance electrode) is constituted, and has complementary voltage window in a system, can be by the operating voltage of two electrodes
Combine, increase voltage window, so as to improve energy density.Although the voltage window of organic bath can reach 3V,
It is that organic bath has the shortcomings of cost is high, toxicity is big, complex process, operating condition are harsh.Comparatively speaking, water system electrolyte
There is low, nontoxic cost, safety, technique simply and without specific use condition.Therefore, suitable electrode material is selected
As the prerequisite for building high-performance water system Asymmetric Supercapacitor.Publication No. CN103606467A and
CN103887076A Chinese patent all discloses a kind of preparation method of water system Asymmetric Supercapacitor, and above-mentioned patent is made
Negative material is all traditional absorbent charcoal material.However, due to the limitation of carbon material feature itself, such as high porosity causes
Bulk density is not high, and specific capacitance is not linearly increasing with specific surface area, and flourishing micropore canals can not be all electrolysed
Liquid ion is utilized, and carbon material still hardly possible has breakthrough raising in specific capacitance.In addition, being compared with secondary cell, porous carbon
Ultracapacitor unit mass/volume capacity is still too small so that the energy density of the ultracapacitor assembled with carbon material by
To limitation.Publication No. CN 105355461A Chinese patent discloses a kind of based on MoS2The asymmetric super capacitor of anode
Device and preparation method thereof.With MoS in the patent2It is used as anode, Co (OH)2The Asymmetric Supercapacitor for cathode assembling, but
MoS2Low conductance is inferior position, it is difficult to obtain high specific capacitance and energy density, and highest energy density is only 19.7 W h kg-1。
Graphene is individual layer sp2Hydbridized carbon atoms are arranged in cellular hexaplanar crystal, with very high intrinsic current-carrying
Transport factor (200000 cm2v-1s-1), good heat conductivity (5000W m-1 k-1), high specific surface area (2630 m2 g-1) and excellent mechanical strength, it is the outstanding candidate material of advanced electrode material required by ultracapacitor.
Research finds that the transient metal sulfide with excellent physical and chemical performance also has higher specific capacitance, makes
It turns into the electrode material for super capacitor with development prospect.This has mainly due to the metal ion among metal sulfide
There is multiple valence state, the mode for being capable of metalloid oxide carries out redox reaction.Wherein NiS is with its excellent electrochemistry
Can, low cost the features such as the candidate materials as electrode material for super capacitor.
Up to the present, and nobody reported and uses NiS/N-rGO（NiS/ nitrogen-doped graphene composites）As just
Pole material, N-rGO（Nitrogen-doped graphene）Water system Asymmetric Supercapacitor is assembled as negative material.Research is found, is passed through
Adulterate other atoms to carbon material, thus it is possible to vary the characteristic of the electron donor-acceptor of electronics carbon material, correspondingly contributes counterfeit electricity
Hold.In addition, preparing composite using N-rGO as matrix material load NiS, the flexible layer structure of N-rGO nanometer sheets is not only
Support can be provided for the NiS of load, can simultaneously serve as the matrix of high conductivity, stronger combination is produced between particles,
The interface of big electrode/electrolyte can be provided for charge transfer reaction with significantly more efficient, thus improve material specific capacitance and
Energy density.
The content of the invention
It is an object of the invention to overcome the shortcomings of that prior art is present there is provided a kind of technique simple possible based on NiS/N-
The water system Asymmetric Supercapacitor of rGO composites and N-rGO.
Water system Asymmetric Supercapacitor of the invention based on NiS/N-rGO and N-rGO is used as positive pole using NiS/N-rGO
Material, N-rGO is as negative material, and specific preparation process is as follows：
(1) positive electrode of NiS/N-rGO composites is prepared
Using solvent thermal process, according to 10 ~ 15：8~14：1 mass ratio, respectively adds nickel salts, sulphur source, graphene oxide
Enter into DMF, be transferred to after dissolving the mixed solution to be formed that is uniformly dispersed in reactor, at 180-220 DEG C
12-36h is reacted, is cleaned 2-3 times through absolute ethyl alcohol, deionized water by centrifuging the product collected, then it is dry through 80 DEG C of vacuum
Dry 12 h, obtains the positive electrode of NiS/N-rGO composites.
(2) N-rGO negative materials are prepared
Using solvent thermal process, graphene oxide is dispersed in DMF, concentration is configured to for 1 ~ 2.5 mg/
The DMF solution of mL graphene oxide, is transferred in reactor thereafter, and 12- is reacted at 180-200 DEG C
N-rGO negative materials are made through separation and drying process in 36h, products therefrom.
(3) electrode is prepared
Above-mentioned positive electrode or negative material are mixed in proportion with acetylene black, bonding agent respectively, N- methyl pyrroles are added
Even application is put into drying box thereafter, dried at 60 DEG C in the clean nickel foam in surface after pyrrolidone formation slurry
12h, obtains negative or positive electrode；Wherein, the mass ratio of described positive electrode or negative material, acetylene black and bonding agent is 8:1:
1。
(4) capacitor is prepared
Alkali water-soluble electrolyte solution using concentration as 3-6 mol/L enters above-mentioned positive pole, negative pole and barrier film as electrolyte
Row assembling, obtains the water system Asymmetric Supercapacitor based on NiS/N-rGO and N-rGO.
Described alkali water-soluble electrolyte solution is NaOH or the KOH aqueous solution.
Described nickel salts are one kind in nickel chloride, nickel acetate or nickel acetylacetonate.
Described sulphur source is Cys, CS2Or one kind in thiocarbamide.
Described bonding agent is Kynoar.
Beneficial effects of the present invention：
1. in N-rGO of the present invention, the introducing of nitrogen-atoms can correspondingly contribute fake capacitance, improve the specific capacitance of material, and prepare
Process is easy.
2. N-rGO is prepared composite by the present invention, is conducive to improving NiS conduction
Property, so that the specific capacitance of overall electrode is improved, the NiS/N-rGO//N-rGO water systems Asymmetric Supercapacitor work electricity of preparation
Press window up to 1.6V, energy density is up to 32.4W h kg-1。
Brief description of the drawings
Fig. 1：The charge-discharge curves figure of water system Asymmetric Supercapacitor of the invention based on NiS/N-rGO//N-rGO；
Fig. 2：The energy-power density map of water system Asymmetric Supercapacitor of the invention based on NiS/N-rGO//N-rGO.
Embodiment
Make further details of elaboration to the present invention with reference to specific embodiment.But these embodiments are merely to illustrate this
Invention rather than limitation the scope of the present invention.
Embodiment 1
（1）The preparation of NiS/N-rGO composites：It is 10 by mass ratio：8：1 nickel chloride, thiocarbamide, graphene oxide are added to
In DMF, dissolving, which is uniformly dispersed to be formed after mixed solution, to be transferred in reactor, and 12-36h is reacted at 180-220 DEG C, passes through centrifugation
The product separated and collected is cleaned 2-3 times through absolute ethyl alcohol, deionized water, then through 80 DEG C of 12 h of vacuum drying, obtains NiS/N-rGO
Composite.
（2）N-rGO preparation：Add graphene oxide into DMF, ultrasonic disperse formation concentration is the molten of 1 mg/mL
Liquid, is transferred them in reactor, 220oC reacts 12 h, is dried to obtain N-rGO.
（3）The preparation of NiS/N-rGO composite positive poles：By NiS/N-rGO composites and acetylene black, bonding agent according to
8:1:1 mass ratio is well mixed, and 1-METHYLPYRROLIDONE formation slurry is added, by its even application in clean nickel foam
On, it is transferred in drying box and dries 12h under the conditions of 60 DEG C.
（4）The preparation of N-rGO negative poles：N-rGO is with acetylene black, bonding agent according to 8:1:1 mass ratio is well mixed, and is added
1-METHYLPYRROLIDONE formation slurry, by its even application in clean nickel foam, is transferred in drying box under the conditions of 60 DEG C
Dry 12h.
（5）Using 6 mol/L sodium hydroxide solution as electrolyte, positive electrode, negative material and barrier film are assembled
NiS/N-rGO//N-rGO Asymmetric Supercapacitors.The operating voltage of the Asymmetric Supercapacitor is up to 1.6 V, specific capacitance
Up to 91.3 F g-1, energy density is up to 32.4 W h kg-1。
Embodiment 2
（1）The preparation of NiS/N-rGO composites：It is 12 to 8 nickel acetate, carbon disulfide, the graphene oxide than 1 by mass ratio
Sequentially add in DMF, dissolving, which is uniformly dispersed to be formed after mixed solution, to be transferred in reactor, 180oC reacts 24 h.Reaction
Room temperature is naturally cooled to after end.Cleaned several times with absolute ethyl alcohol and deionized water, 80oC is dried in vacuo 12 h and obtains NiS/
N-rGO composites.
（2）N-rGO preparation：Add graphene oxide into DMF, ultrasonic disperse formation concentration is the molten of 1.5 mg/mL
Liquid, is transferred them in reactor, 220oC reacts 12 h, is dried to obtain N-rGO.
（3）The preparation of NiS/N-rGO composite positive poles：By NiS/N-rGO composites and acetylene black, bonding agent according to
8:1:1 mass ratio is well mixed, and 1-METHYLPYRROLIDONE formation slurry is added, by its even application in clean nickel foam
On, it is transferred in drying box and dries 12h under the conditions of 60 DEG C.
（4）The preparation of N-rGO negative poles：N-rGO is with acetylene black, bonding agent according to 8:1:1 mass ratio is well mixed, and is added
1-METHYLPYRROLIDONE formation slurry, by its even application in clean nickel foam, is transferred in drying box under the conditions of 60 DEG C
Dry 12h.
（5）Using 6 mol/L potassium hydroxide solution as electrolyte, positive electrode, negative material and barrier film are assembled
NiS/N-rGO//N-rGO Asymmetric Supercapacitors.The operating voltage of the Asymmetric Supercapacitor is up to 1.6 V, specific capacitance
Up to 77.5 F g-1, energy density is up to 27.6 W h kg-1。
Embodiment 3
（1）The preparation of NiS/N-rGO composites：It is 15 to 14 nickel acetylacetonate, Cys, the oxygen than 1 by mass ratio
Graphite alkene is sequentially added in DMF solution, and dissolving, which is uniformly dispersed to be formed after mixed solution, to be transferred in reactor, 200oC is anti-
Answer 12 h.Reaction naturally cools to room temperature after terminating.Cleaned several times with absolute ethyl alcohol and deionized water, 80oC is dried in vacuo
12 h obtain NiS/N-rGO composites.
（2）N-rGO preparation：Add graphene oxide into DMF, ultrasonic disperse formation concentration is the molten of 2.5 mg/mL
Liquid, is transferred them in reactor, 220oC reacts 12 h, is dried to obtain N-rGO.
（3）The preparation of NiS/N-rGO composite positive poles：By NiS/N-rGO composites and acetylene black, bonding agent according to
8:1:1 mass ratio is well mixed, and 1-METHYLPYRROLIDONE formation slurry is added, by its even application in clean nickel foam
On, it is transferred in drying box and dries 12h under the conditions of 60 DEG C.
（4）The preparation of N-rGO negative poles：N-rGO is with acetylene black, bonding agent according to 8:1:1 mass ratio is well mixed, and is added
1-METHYLPYRROLIDONE formation slurry, by its even application in clean nickel foam, is transferred in drying box under the conditions of 60 DEG C
Dry 12h.
（5）Using 6 mol/L sodium hydroxide solution as electrolyte, positive electrode, negative material and barrier film are assembled
NiS/N-rGO//N-rGO Asymmetric Supercapacitors.The operating voltage of the Asymmetric Supercapacitor is up to 1.6 V, specific capacitance
Up to 83.4 F g-1, energy density is up to 29.7 W h kg-1。
Claims (5)
1. the water system Asymmetric Supercapacitor based on NiS/N-rGO and N-rGO, it is characterised in that：Described capacitor is used
NiS/N-rGO is as positive electrode, and N-rGO is as negative material, and specific preparation process is as follows：
(1) positive electrode of NiS/N-rGO composites is prepared
Using solvent thermal process, according to 10 ~ 15：8~14：1 mass ratio, respectively adds nickel salts, sulphur source, graphene oxide
Enter into DMF, be transferred to after dissolving the mixed solution to be formed that is uniformly dispersed in reactor, at 180-220 DEG C
12-36h is reacted, is cleaned 2-3 times through absolute ethyl alcohol, deionized water by centrifuging the product collected, then it is dry through 80 DEG C of vacuum
Dry 12 h, obtains the positive electrode of NiS/N-rGO composites；
(2) N-rGO negative materials are prepared
Using solvent thermal process, graphene oxide is dispersed in DMF, concentration is configured to for 1 ~ 2.5 mg/
The DMF solution of mL graphene oxide, is transferred in reactor thereafter, and 12- is reacted at 180-200 DEG C
N-rGO negative materials are made through separation and drying process in 36h, products therefrom；
(3) electrode is prepared
Above-mentioned positive electrode or negative material are mixed in proportion with acetylene black, bonding agent respectively, N- methyl pyrroles are added
Even application is put into drying box thereafter, dried at 60 DEG C in the clean nickel foam in surface after pyrrolidone formation slurry
12h, obtains negative or positive electrode；Wherein, the mass ratio of described positive electrode or negative material, acetylene black and bonding agent is 8:1:
1；
(4) capacitor is prepared
Alkali water-soluble electrolyte solution using concentration as 3-6 mol/L enters above-mentioned positive pole, negative pole and barrier film as electrolyte
Row assembling, obtains the water system Asymmetric Supercapacitor based on NiS/N-rGO and N-rGO.
2. the water system Asymmetric Supercapacitor according to claim 1 based on NiS/N-rGO and N-rGO, its feature exists
In：Described alkali water-soluble electrolyte solution is NaOH or the KOH aqueous solution.
3. the water system Asymmetric Supercapacitor according to claim 1 based on NiS/N-rGO and N-rGO, its feature exists
In：Described nickel salts are one kind in nickel chloride, nickel acetate or nickel acetylacetonate.
4. the water system Asymmetric Supercapacitor according to claim 1 based on NiS/N-rGO and N-rGO, its feature exists
In：Described sulphur source is Cys, CS2Or one kind in thiocarbamide.
5. the water system Asymmetric Supercapacitor according to claim 1 based on NiS/N-rGO and N-rGO, its feature exists
In：Described bonding agent is Kynoar.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109616334A (en) * | 2018-12-11 | 2019-04-12 | 中国科学院兰州化学物理研究所 | The preparation method of carbon-clad metal oxidate nano point load graphene composite material |
| CN109686585A (en) * | 2018-12-21 | 2019-04-26 | 山东大学 | A kind of water system Asymmetric Supercapacitor and preparation method thereof based on NiCo-LDH/rGO and rGO |
| CN109847784A (en) * | 2019-02-21 | 2019-06-07 | 青岛科技大学 | A kind of Cu1.81S/Ni1.03S/NG/NF composite material and preparation method |
| CN110164707A (en) * | 2019-05-09 | 2019-08-23 | 齐齐哈尔大学 | The preparation method of the compound Ni/Cu sulfide electrode of self assembly graphene in nickel foam |
| CN110808170A (en) * | 2019-09-27 | 2020-02-18 | 西安交通大学 | Water system asymmetric supercapacitor based on porous carbon nitride/graphene/nickel disulfide and carbon nitride/graphene and preparation method thereof |
| US11437199B1 (en) | 2022-04-08 | 2022-09-06 | King Fahd University Of Petroleum And Minerals | Layered dual hydroxide (LDH) composite |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109616334A (en) * | 2018-12-11 | 2019-04-12 | 中国科学院兰州化学物理研究所 | The preparation method of carbon-clad metal oxidate nano point load graphene composite material |
| CN109686585A (en) * | 2018-12-21 | 2019-04-26 | 山东大学 | A kind of water system Asymmetric Supercapacitor and preparation method thereof based on NiCo-LDH/rGO and rGO |
| CN109847784A (en) * | 2019-02-21 | 2019-06-07 | 青岛科技大学 | A kind of Cu1.81S/Ni1.03S/NG/NF composite material and preparation method |
| CN109847784B (en) * | 2019-02-21 | 2021-11-09 | 青岛科技大学 | Cu1.81S/Ni1.03S/NG/NF composite material and preparation method thereof |
| CN110164707A (en) * | 2019-05-09 | 2019-08-23 | 齐齐哈尔大学 | The preparation method of the compound Ni/Cu sulfide electrode of self assembly graphene in nickel foam |
| CN110164707B (en) * | 2019-05-09 | 2021-05-18 | 齐齐哈尔大学 | Preparation method of self-assembled graphene composite Ni/Cu sulfide electrode on foamed nickel |
| CN110808170A (en) * | 2019-09-27 | 2020-02-18 | 西安交通大学 | Water system asymmetric supercapacitor based on porous carbon nitride/graphene/nickel disulfide and carbon nitride/graphene and preparation method thereof |
| CN110808170B (en) * | 2019-09-27 | 2020-10-27 | 西安交通大学 | High-energy super capacitor with porous carbon nitride interlayer material configuration and preparation method thereof |
| US11437199B1 (en) | 2022-04-08 | 2022-09-06 | King Fahd University Of Petroleum And Minerals | Layered dual hydroxide (LDH) composite |
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