CN109637825A - A kind of nanometer nickel sulfide piece/carbon quantum dot composite material and preparation method and application - Google Patents
A kind of nanometer nickel sulfide piece/carbon quantum dot composite material and preparation method and application Download PDFInfo
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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
The invention belongs to electrode material for super capacitor technical field, a kind of nanometer nickel sulfide piece/carbon quantum dot composite material and preparation method and application are disclosed.The composite material be by carbon quantum dot ultrasonic disperse in aqueous solution, soluble nickel salt and hexa is added, obtain carbon quantum dot/nickel hydroxide mixture precursor solution, precursor solution is grown on foam nickel surface at 90~120 DEG C, carbon quantum dot/nickel hydroxide mixture and sodium sulfide solution are mixed again, after 100~140 DEG C of hydro-thermal reactions, washed, dry it is obtained.The features such as preparation process of the present invention is simple, process stabilizing, easily operated, at low cost, pollution-free.Nanometer nickel sulfide piece/carbon quantum dot composite material has unique cellular nano chip architecture, not only contribute to effective infiltration of electrolyte, electrolyte and active material can be made to come into full contact with simultaneously, to improve the chemical property of material, can be used as electrode material for super capacitor.
Description
Technical field
The invention belongs to electrode material for super capacitor technical fields, more particularly, to a kind of nanometer nickel sulfide piece/carbon
Quantum dot composite material and its preparation and application.
Background technique
Supercapacitor is as the energy storage device extensive concern by many researchers in recent years with superior prospect.It is super
The common carbon-based double layer capacity material of electrode material-in grade capacitor, due to its relatively low specific capacity make its application development by
It is difficult to meet demand growing, to electrical energy storage to limitation.Under normal circumstances, containing the oxidation of transition metal
Object or vulcanization have higher specific capacity.Wherein, nickel sulfide is because have cheap, easily prepared, hypotoxicity and specific capacitance
Height is used as electrode material extensive in high-performance super capacitor, lithium ion battery and solar battery in that advantage
Research.However, nickel sulfide is since electric conductivity is lower and then keeps its electron mobility poor, it is difficult to bear higher current density etc.
Reason, as high-performance super capacitor electrode material, chemical property is ideal not enough.Currently, in order to effectively improve
The electric conductivity of electrode material, nickel sulfide and the carbon material (such as carbon nanotube and graphene etc.) with satisfactory electrical conductivity is compound
Preparing composite material is another effective way for improving electrode material chemical property.As a kind of novel carbon material, carbon
The features such as quantum dot has class graphene-structured, and size is enriched in several nanometers, surface functional group, and specific surface area is larger, these
Property makes it have special performance and application.So far, nickel sulfide/carbon quantum is prepared using a kind of simple and easy method
Point composite material, the correlative study report for inquiring into its chemical property are very limited.
Summary of the invention
In order to solve above-mentioned the shortcomings of the prior art and disadvantage, the object of the present invention is to provide a kind of nickel sulfides
Nanometer sheet/carbon quantum dot composite material, the composite material have superior high rate performance and cycle performance.
Another object of the present invention is the provision of the preparation method of above-mentioned nanometer nickel sulfide piece/carbon quantum dot composite material.
Still a further object of the present invention is the provision of the application of above-mentioned nanometer nickel sulfide piece/carbon quantum dot composite material.
The purpose of the present invention is realized by following technical proposals:
A kind of nanometer nickel sulfide piece/carbon quantum dot composite material, the composite material is that sulphur is prepared in foam nickel base
Change nickel nano film, by carbon quantum dot ultrasonic disperse in aqueous solution, soluble nickel salt and hexa is added, obtains carbon amounts
Sub- point/nickel hydroxide mixture precursor solution, using hydro-thermal method by carbon quantum dot/nickel hydroxide mixture presoma 90~
120 DEG C are grown on foam nickel surface, then carbon quantum dot/nickel hydroxide mixture and sodium sulfide solution are mixed, 100~
Under the conditions of 140 DEG C after hydro-thermal reaction, washed, dry it is obtained.
Preferably, the molar ratio of the carbon quantum dot, water, nickel salt and hexa is (2~3): 2:5:10；It is described
Soluble nickel salt be nickel chloride, nickel nitrate, nickel sulfate or nickel acetylacetonate, the carbon quantum dot/nickel hydroxide mixture and
The proportionate relationship value range molar ratio of sodium sulfide solution is 1:(1~3).
Nanometer nickel sulfide piece/carbon quantum dot composite material preparation method, comprising the following specific steps
S1., nickel foam is successively used to acetone, hydrochloric acid, distilled water and EtOH Sonicate, it is spare that drying obtains foam nickel base；
S2. carbon quantum dot ultrasonic disperse in aqueous solution, soluble nickel salt and hexa is dissolved in wherein, obtained
To carbon quantum dot/nickel hydroxide mixture precursor solution；
S3. carbon quantum dot/nickel hydroxide mixture precursor solution is transferred to ptfe autoclave, and by foam
Nickel immerses in mixed solution, and reaction kettle is sealed to and is placed on air dry oven, after reacting under the conditions of 90~120 DEG C, will steep
Foam nickel is washed with water and is dried after taking out, and obtains carbon quantum dot/nickel hydroxide compound that nickel foam supports；
S4. carbon quantum dot/nickel hydroxide the compound and sodium sulfide solution supported using the resulting nickel foam of step S2 is mixed
It closes, is then transferred into ptfe autoclave, after reacting under the conditions of 100~140 DEG C, stop reaction and Temperature fall
Afterwards, the sample in reaction kettle is taken out, with a large amount of washing and drying, obtains nanometer nickel sulfide piece/carbon quantum dot composite material.
Preferably, the time ultrasonic described in step S1 is 10~60 minutes.
Preferably, the molar ratio of carbon quantum dot described in step S2, water, nickel salt and hexa is (2~3): 2:
5:10；The soluble nickel salt is nickel chloride, nickel nitrate, nickel sulfate or nickel acetylacetonate.
Preferably, the time of reaction described in step S3 is 8~16h.
Preferably, the time of reaction described in step S4 is 3~8h.
Preferably, the concentration of sodium sulfide solution described in step S4 is 0.5~3mol/L.
Preferably, the molar ratio of carbon quantum dot described in step S4/nickel hydroxide compound and sodium sulfide solution is 1:
(1~3).
The nanometer nickel sulfide piece/application of the carbon quantum dot composite material in supercapacitor field.
Compared with prior art, the invention has the following advantages:
1. the present invention prepares nanometer nickel sulfide piece/carbon quantum dot composite material nanometer chip architecture in foam nickel base,
Carbon quantum dot with cellular nano chip architecture/nickel sulfide mixture, added carbon quantum dot are conducive to improve nickel sulfide
The electric conductivity and stability of material, and then improve the high rate performance and cycle performance of material.This is attributed to unique honeycomb and receives
Rice chip architecture not only contributes to effective infiltration of electrolyte, while electrolyte and active material can be made to come into full contact with, to improve
The chemical property of material.
2. the present invention is simple to the control of reaction condition during the preparation process, equipment is easily operated, and production cost is low, no dirt
The features such as dye, reaction temperature and time are easier to control, it is easy to accomplish industrialized production.
3. nanometer nickel sulfide piece/carbon quantum dot composite material prepared by the present invention has three-dimensional honeycomb nanometer chip architecture, receive
Connection is taken between rice piece and provides transportation route for electronics, is effectively raised the transmission rate of electronics or ion, is put with reducing high current
Capacity attenuation when electric, the addition of carbon quantum dot further improve stability of material and electric conductivity, make material high rate performance
With cycle performance to being obviously improved.
Detailed description of the invention
Fig. 1 is the material SEM photograph of Examples 1 and 2 preparation, wherein (a), (b) and (c) is nanometer nickel sulfide piece/carbon amounts
Son point composite material, (d), (e) and (f) is nanometer nickel sulfide sheet material.
Fig. 2 is nanometer nickel sulfide piece/carbon quantum dot composite material TEM photo prepared by embodiment 2.
Fig. 3 is nanometer nickel sulfide piece/carbon quantum dot composite material X-ray powder diffraction figure of Examples 1 and 2 preparation.
Fig. 4 is nanometer nickel sulfide piece/carbon quantum dot composite material x-ray photoelectron spectroscopy prepared by embodiment 2 and 4
Figure.
Fig. 5 is nanometer nickel sulfide piece/carbon quantum dot composite material high rate performance curve prepared by embodiment 2 and 3.
Fig. 6 is nanometer nickel sulfide piece/carbon quantum dot composite material AC impedance performance curve prepared by embodiment 2 and 5.
Fig. 7 is nanometer nickel sulfide piece/carbon quantum dot composite material cycle performance test chart prepared by embodiment 2.
Specific embodiment
The contents of the present invention are further illustrated combined with specific embodiments below, but should not be construed as limiting the invention.
Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.Except non-specifically
Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagents, method and apparatus.
Embodiment 1
1. at room temperature, by nickel foam (size: 1*4cm2) it is put into beaker, successively with acetone, the hydrochloric acid of 0.5mol/L, steaming
Distilled water, dehydrated alcohol ultrasound 20min, weigh spare after drying；
It is sufficiently stirred 2. the nickel nitrate of 5mmol is added in 35mL deionized water with 10mmol hexa
10min obtains mixed solution；
3. by nickel foam (size: 1*4cm2) ultrasound 30min after step 2 gained mixed solution is immersed, magneton is taken out, so
Above-mentioned mixed solution and nickel foam are transferred in ptfe autoclave afterwards；Reaction kettle seals and is placed on forced air drying
Case, reaction condition are 100 DEG C, and the reaction time is 10 hours；
4. after stopping reaction and Temperature fall, the sample in reaction kettle is taken out, with a large amount of washing, take 30mL's
The sodium sulfide solution and nickel foam of 0.1mol/L is transferred in ptfe autoclave；120 DEG C are reacted 10 hours；
5. after stopping reaction and Temperature fall, take out gained nickel foam samples with water in step 4 and rinse, then through distilled water and
Dehydrated alcohol is washed, and sample is placed in baking oven in 60 DEG C of dryings, nanometer nickel sulfide piece is made.
Embodiment 2
1. under room temperature, by nickel foam (size: 1*4cm2) be put into beaker, successively with acetone, 0.5mol/L hydrochloric acid,
Distilled water, dehydrated alcohol ultrasound weigh spare after twenty minutes, after drying；
2. the nickel nitrate 10mmol hexa of 5mmol to be added to the 1mg/mL carbon quantum dot mixed solution of 35mL
In be sufficiently stirred 10 minutes, obtain carbon quantum dot/nickel hydroxide mixture precursor solution；
3. by nickel foam (size: 1*4cm2) immerse step 2 gained carbon quantum dot/nickel hydroxide mixture precursor solution
Ultrasound 30 minutes afterwards, magneton is taken out, then above-mentioned mixed solution and nickel foam are transferred in ptfe autoclave；Instead
It answers kettle to seal and is placed on air dry oven, reacted 10 hours at 100 DEG C；
4. after stopping reaction and Temperature fall, the sample in reaction kettle is taken out, with a large amount of washing, take 30mL's
The sodium sulfide solution and nickel foam of 0.1mol/L is transferred in ptfe autoclave, is reacted 3 hours at 120 DEG C；
5. after stopping reaction and Temperature fall, take out gained nickel foam samples with water in step 4 and rinse, then through distilled water and
Dehydrated alcohol is washed, and sample is placed in baking oven drying at 60 DEG C, nanometer nickel sulfide piece/carbon quantum dot composite material is made.
Fig. 1 is the material SEM photograph of Examples 1 and 2 preparation, wherein (a), (b) and (c) is nanometer nickel sulfide piece/carbon amounts
Son point composite material, (d), (e) and (f) is nanometer nickel sulfide sheet material.From figure 1 it appears that the nanometer nickel sulfide of preparation
Piece and nanometer nickel sulfide piece/carbon quantum dot are a nanometer chip architecture, but nanometer nickel sulfide piece/carbon quantum dot is than nanometer nickel sulfide piece
Structure is more fine and close.Apparent honey-comb shape array formula structure, structure is presented in nanometer nickel sulfide piece/carbon quantum dot composite material, material
More smooth at cellular nanometer sheet surface, without breakage, and honey-comb shape array formula structure, portion is presented in nanometer nickel sulfide sheet material
Separation structure collapses, and constituting cellular nanometer sheet surface has breakage.Fig. 2 be embodiment 2 in synthesize nanometer nickel sulfide piece/
TEM (a) and HRTEM (b) figure of carbon quantum dot composite material.As can be seen that Fig. 2 (a) in Leaves'Shape nanometer sheet surface compared with
Smooth, without breakage, while nanometer nickel sulfide piece/carbon quantum dot composite material prepared in Fig. 2 (b) has highly crystalline special
Property, and feature interplanar distance 0.194nm, 0.280nm and 0.408nm respectively correspond heazlewoodite (Ni3S2) in crystal structure
(311), (210) and (101) crystal face, prepared nanometer nickel sulfide piece/carbon quantum dot nanometer sheet have highly crystalline characteristic, and
Feature interplanar distance meets heazlewoodite (Ni3S2) crystal structure.Fig. 3 is nickel sulfide/carbon quantum dot of Examples 1 and 2 preparation
The X-ray powder diffraction figure of nanosheet composite material.As seen from the figure, higher crystallization property is all presented in two samples, and similar
Peak type, the characteristics of peak with standard spectrogram nickel sulfide (Ni3S2, JCPDSNo.44-1418) it is consistent.
Embodiment 3
1. under room temperature, by nickel foam (size: 1*4cm2) be put into beaker, successively with acetone, 0.5mol/L hydrochloric acid,
Distilled water, dehydrated alcohol ultrasound weigh spare after twenty minutes, after drying；
2. the nickel chloride of 5mmol is mixed with the 1.5mg/mL carbon quantum dot that 10mmol hexa is added to 35mL
It is sufficiently stirred in solution 10 minutes, obtains carbon quantum dot/nickel hydroxide mixture precursor solution；
3. by nickel foam (size: 1*4cm2) immerse step 2 gained carbon quantum dot/nickel hydroxide mixture precursor solution
Ultrasound 30 minutes afterwards, magneton is taken out, then above-mentioned mixed solution and nickel foam are transferred in ptfe autoclave；Instead
It answers kettle to seal and is placed on air dry oven, reacted 8 hours at 120 DEG C；
4. after stopping reaction and Temperature fall, the sample in reaction kettle is taken out, with a large amount of washing, take 30mL's
The sodium sulfide solution and nickel foam of 0.2mol/L is transferred in ptfe autoclave, is reacted 8 hours at 100 DEG C；
5. after stopping reaction and Temperature fall, takes out a large amount of water of gained nickel foam sample in step 4 and rinse, distillation washing,
Dehydrated alcohol is washed, and sample is finally placed in baking oven drying at 60 DEG C, nanometer nickel sulfide piece/carbon quantum dot composite wood is made
Material.
Fig. 3 is the x-ray powder of embodiment 2 with nanometer nickel sulfide piece/carbon quantum dot composite material obtained in embodiment 3
Diffraction pattern.As can be seen that nanometer nickel sulfide piece/carbon quantum dot composite material obtained all has heazlewoodite (Ni3S2) knot
Structure.Fig. 5 is nickel sulfide/carbon quantum dot nanosheet composite material high rate performance curve prepared by embodiment 2 and 3.As seen from the figure,
Current density from 2A/g to 15A/g, nickel sulfide/foam nickel electrode specific discharge capacity be followed successively by 156mAh/g, 133mAh/g,
122mAh/g,120mAh/g,111mAh/g；Nickel sulfide/carbon quantum dot/foam nickel electrode specific discharge capacity is followed successively by simultaneously
154mAh/g,142mAh/g,133mAh/g,131mAh/g,117mAh/g.In addition, nickel sulfide/carbon quantum dot/foam nickel electrode
Specific capacity has been respectively increased 7.3%, 5.4% and 14.4% under each flux density.
Embodiment 4
1. under room temperature, by nickel foam (size: 1*4cm2) be put into beaker, successively with acetone, 0.5mol/L hydrochloric acid,
Distilled water, dehydrated alcohol ultrasound weigh spare after twenty minutes, after drying；
2. the nickelous carbonate of 5mmol is mixed with the 1mg/mL carbon quantum dot that 10mmol hexa is added to 35mL molten
It is sufficiently stirred in liquid 10 minutes, obtains carbon quantum dot/nickel hydroxide mixture precursor solution；
3. by nickel foam (size: 1*4cm2) immerse step 2 gained carbon quantum dot/nickel hydroxide mixture precursor solution
Ultrasound 30 minutes afterwards, magneton is taken out, then above-mentioned mixed solution and nickel foam are transferred in ptfe autoclave；Instead
It answers kettle to seal and is placed on air dry oven, reacted 16 hours at 90 DEG C；
4. after stopping reaction and Temperature fall, the sample in reaction kettle is taken out, with a large amount of washing, take 30mL's
The sodium sulfide solution and nickel foam of 0.15mol/L is transferred in ptfe autoclave, is reacted 5 hours at 100 DEG C；
5. after stopping reaction and Temperature fall, takes out a large amount of water of gained nickel foam sample in step 4 and rinse, distillation washing,
Dehydrated alcohol is washed, and sample is finally placed in baking oven drying at 60 DEG C, nanometer nickel sulfide piece/carbon quantum dot composite wood is made
Material.
Fig. 4 is the xps energy spectrum figure of embodiment 2 with nickel sulfide/carbon quantum dot material obtained in embodiment 4.As Fig. 4 can
Know, includes nickel, three kinds of elements of sulphur and carbon, Ni in sample3S2Middle nickel is the mixing of divalent and trivalent.
Embodiment 5
It is working electrode, calomel by preparation gained nickel foam supports carbon quantum dot/vulcanization nickel composite in above-described embodiment 2
Electrode is electrolyte as normal electrode, 6mol/L potassium hydroxide aqueous solution, and platinized platinum is working electrode, using three electrode test sides
Method carries out sample electrochemical property test.Fig. 5 is nickel sulfide/foam nickel electrode and nickel sulfide/carbon quantum dot/foam nickel electrode
Specific capacitance under the conditions of different charge and discharge.Current density be can be seen that from 2A/g to 15A/g, nickel sulfide/foam nickel electrode
Specific discharge capacity is followed successively by 156mAh/g, 133mAh/g, 122mAh/g, 120mAh/g, 111mAh/g；Nickel sulfide/carbon amounts simultaneously
The specific discharge capacity of sub- point/foam nickel electrode is followed successively by 154mAh/g, 142mAh/g, 133mAh/g, 131mAh/g, 117mAh/
g.In addition, 7.3%, 5.4% and has been respectively increased in nickel sulfide/carbon quantum dot/foam nickel electrode specific capacity under each flux density
14.4%.Fig. 6 is nanometer nickel sulfide piece/carbon quantum dot composite material AC impedance performance curve prepared by embodiment 2 and 5.
It will be appreciated from fig. 6 that nickel sulfide/carbon quantum dot/foam nickel electrode shows lesser impedance compared with nickel sulfide/foam nickel electrode.Figure
The 7 nanometer nickel sulfide piece/carbon quantum dot composite material cycle performance test charts prepared for embodiment 2.As seen from the figure, vulcanize
For nickel carbon quantum dot/foam nickel electrode when current density is 10A/g, capacity still maintains initial appearance after 3000 circulations
The 80% of amount.It follows that the addition of carbon quantum dot greatly improves nanometer nickel sulfide piece/carbon quantum dot composite material times
Rate performance and cycle performance.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination and simplify,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of nanometer nickel sulfide piece/carbon quantum dot composite material, which is characterized in that the composite material is in foam nickel base
On prepare nanometer nickel sulfide piece, by carbon quantum dot ultrasonic disperse in aqueous solution, soluble nickel salt and hexa is added,
Carbon quantum dot/nickel hydroxide mixture precursor solution is obtained, using hydro-thermal method by carbon quantum dot/nickel hydroxide mixture forerunner
Liquid solution is grown on foam nickel surface at 90~120 DEG C, then carbon quantum dot/nickel hydroxide mixture and sodium sulfide solution are mixed
Close, under the conditions of 100~140 DEG C after hydro-thermal reaction, washed, dry it is obtained.
2. nanometer nickel sulfide piece/carbon quantum dot composite material according to claim 1, which is characterized in that the carbon quantum
Point, water, nickel salt and hexa molar ratio be (2~3): 2:5:10；The soluble nickel salt is nickel chloride, nitric acid
Nickel, nickel sulfate or nickel acetylacetonate；The molar ratio of the carbon quantum dot/nickel hydroxide mixture and sodium sulfide solution is 1:(1
~3).
3. the preparation method of nanometer nickel sulfide piece/carbon quantum dot composite material according to claim 1 or 2, feature exist
In, comprising the following specific steps
S1., nickel foam is successively used to acetone, hydrochloric acid, distilled water and EtOH Sonicate, it is spare that drying obtains foam nickel base；
S2. carbon quantum dot ultrasonic disperse in aqueous solution, soluble nickel salt and hexa is dissolved in wherein, carbon is obtained
Quantum dot/nickel hydroxide mixture precursor solution；
S3. carbon quantum dot/nickel hydroxide mixture precursor solution is transferred to ptfe autoclave, and nickel foam is soaked
Enter in mixed solution, reaction kettle is sealed to and is placed on air dry oven, after being reacted under the conditions of 90~120 DEG C, by nickel foam
It washes with water and dries after taking-up, obtain carbon quantum dot/nickel hydroxide compound that nickel foam supports；
S4. carbon quantum dot/nickel hydroxide the compound and sodium sulfide solution supported using the resulting nickel foam of step S2 is mixed, so
After be transferred in ptfe autoclave, under the conditions of 100~140 DEG C react after, stop reaction and Temperature fall after, will be anti-
It answers the sample in kettle to take out, with a large amount of washing and drying, obtains nanometer nickel sulfide piece/carbon quantum dot composite material.
4. the preparation method of nanometer nickel sulfide piece/carbon quantum dot composite material according to claim 3, which is characterized in that
The ultrasonic time described in step S1 is 10~60min.
5. nanometer nickel sulfide piece/carbon quantum dot composite material and preparation method thereof according to claim 3, which is characterized in that step
Suddenly the molar ratio of carbon quantum dot described in S2, water, nickel salt and hexa is (2~3): 2:5:10.
6. nanometer nickel sulfide piece/carbon quantum dot composite material and preparation method thereof according to claim 3, which is characterized in that step
Nickel salt described in rapid S2 is nickel chloride, nickel nitrate, nickel sulfate or nickel acetylacetonate.
7. nanometer nickel sulfide piece/carbon quantum dot composite material and preparation method thereof according to claim 3, which is characterized in that step
The time of reaction described in rapid S3 is 8~16h；The time of reaction described in step S4 is 3~8h.
8. the preparation method of nanometer nickel sulfide piece/carbon quantum dot composite material according to claim 3, which is characterized in that
The concentration of sodium sulfide solution described in step S4 is 0.5~3mol/L.
9. the preparation method of nanometer nickel sulfide piece/carbon quantum dot composite material according to claim 3, which is characterized in that
The molar ratio of carbon quantum dot described in step S4/nickel hydroxide compound and sodium sulfide solution is 1:(1~3).
10. nanometer nickel sulfide piece/carbon quantum dot composite material according to claim 1 or 2 is in supercapacitor field
Application.
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| CN111180215A (en) * | 2019-12-03 | 2020-05-19 | 哈尔滨工程大学 | Sodium ion capacitor electrode material of nickel sulfide nanosheet composite carbonized yellow quay |
| CN112133569A (en) * | 2020-09-17 | 2020-12-25 | 吉林化工学院 | Carbon-modified three-dimensional tree-like Ni3S2Electrode material for super capacitor |
| CN113036097A (en) * | 2021-02-04 | 2021-06-25 | 淮阴工学院 | Sulfur vacancy nitrogen doped carbon coated nickel sulfide composite electrode material and preparation method thereof |
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| US11123717B2 (en) * | 2019-05-30 | 2021-09-21 | Korea University Research And Business Foundation | Catalyst for oxygen reduction reaction and oxygen evolution reaction and method for manufacturing of the same |
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| CN111017904A (en) * | 2019-12-26 | 2020-04-17 | 大连理工大学 | Carbon quantum dot-CoFe Prussian blue nano composite material and preparation method and application thereof |
| CN111017904B (en) * | 2019-12-26 | 2021-09-24 | 大连理工大学 | Carbon quantum dot-CoFe Prussian blue nano composite material and preparation method and application thereof |
| CN112133569A (en) * | 2020-09-17 | 2020-12-25 | 吉林化工学院 | Carbon-modified three-dimensional tree-like Ni3S2Electrode material for super capacitor |
| CN113036097A (en) * | 2021-02-04 | 2021-06-25 | 淮阴工学院 | Sulfur vacancy nitrogen doped carbon coated nickel sulfide composite electrode material and preparation method thereof |
| CN113036097B (en) * | 2021-02-04 | 2022-05-17 | 淮阴工学院 | Sulfur vacancy nitrogen doped carbon coated nickel sulfide composite electrode material and preparation method thereof |
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