CN110189922A - Honeycomb nano-chip arrays cobalt acid nickel/rGO/ nickel foam and preparation method - Google Patents
Honeycomb nano-chip arrays cobalt acid nickel/rGO/ nickel foam and preparation method 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
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- H—ELECTRICITY
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- 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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- H—ELECTRICITY
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- 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
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- H—ELECTRICITY
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- 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
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- 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
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- H—ELECTRICITY
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- 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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Abstract
A kind of honeycomb nano-chip arrays cobalt acid nickel/rGO/ nickel foam and preparation method, belong to multilevel structure nano-catalyst material technical field.Honeycomb nano-chip arrays cobalt acid nickel/rGO/ nickel foam be by the ultra-fine cobalt acid nickel nano particle single layer Alignment of 10.8nm at ultra-thin cobalt acid nickel nano film (110 × 11nm) vertical interlaced be grown on the honeycomb nano-chip arrays structure that the foam nickel surface of graphene modified constitutes.By the way that citric acid is added into graphene suspension and obtains graphene/nickel foam matrix using hydro-thermal process, then liquid-phase coprecipitation and calcination process appropriate is helped to prepare honeycomb nano-chip arrays cobalt acid nickel/rGO/ nickel foam by citric acid.The advantage is that preparation method is easy to operate, mild condition is environmentally protective.Obtained material shows very excellent super capacitor performance and cyclical stability directly as electrode of super capacitor.
Description
Technical field
The invention belongs to multilevel structure nano-catalyst material technical fields, in particular, provide a kind of honeycomb nanometer sheet
Array cobalt acid nickel/rGO/ nickel foam and preparation method.
Background technique
The rapid growth of the increasingly consumption and energy demand of conventional fossil fuel, accelerates research of the people to new energy
With exploitation.The advantages that supercapacitor is because of its no pollution to the environment, high power density, quick charge and discharge process is by researcher
Extensive concern.Electrode material is the key factor for influencing its performance, currently, used anode catalyst such as RuO2Etc. expensive
The application of metal is limited to its expensive cost and itself toxicity.Therefore, finding, there is good catalytic activity and high circulation to stablize
The base metal elctro-catalyst of property has become an important research direction of supercapacitor.
Cobalt acid nickel (NiCo2O4) be a kind of spinel structure transition metal oxide, since there are Co in its structure3+/
Co2+And Ni3+/Ni2+Two kinds of oxidation-reduction pairs thus have chemical property more higher than single nickel oxide, cobalt oxide.So
And the cyclical stability difference of single composite oxides cobalt acid nickel limits its application.By cobalt acid nickel with have high-specific surface area,
The compound chemical property for effectively improving material of the graphene of high conductivity and good mechanical stability.
In traditional electrode preparation process, electrode material often influences electro-chemical activity because coating unevenly, meanwhile, it is added
Bonding agent inevitably reduce the efficiency of electrode.Currently, the research tendency of super capacitor material is directly in afflux
Growth activity material in body nickel foam constructs 3-D nano, structure electrode.Compared with traditional electrode, these adhesive-free electrodes are not
Only there is the simple and convenient advantage without being further processed, while the chemical property of supercapacitor can also be significantly improved.
Currently used graphene/nickel foam the method for preparing mostly uses vapour deposition process (CVD), but CVD method the high requirements on the equipment, and
It is cumbersome, it is unfavorable for economizing on resources.However, so far there is not yet related honeycomb nano-chip arrays cobalt acid nickel/rGO/ bubble
The report of foam nickel material and its preparation method and application.
Summary of the invention
The purpose of the present invention is to provide a kind of honeycomb nano-chip arrays cobalt acid nickel/rGO/ nickel foam and preparation method,
It is easy to operate, the use of the reaction condition and organic reagent of high temperature and pressure is avoided, the material of preparation can be directly as super capacitor
Device electrode has high activity and excellent cyclical stability.
Honeycomb nano-chip arrays cobalt acid nickel/rGO/ nickel foam of the invention is the ultra-fine cobalt acid nickel nanoparticle by 10.8nm
Sub- single layer Alignment at ultra-thin cobalt acid nickel nano film (110 × 11nm) vertical interlaced be grown on the nickel foam of graphene modified
The honeycomb nano-chip arrays structure that surface is constituted.By the way that citric acid is added into graphene suspension and is obtained using hydro-thermal process
To graphene/nickel foam matrix, then liquid-phase coprecipitation and calcination process appropriate is helped to prepare honeycomb by citric acid
Nano-chip arrays cobalt acid nickel/rGO/ nickel foam.
Honeycomb nano-chip arrays cobalt acid nickel/rGO/ foam nickel material of the present invention the preparation method comprises the following steps:
(1) graphite oxide gel is add to deionized water ultrasonic disperse 15-25min and obtains graphite oxide suspension,
After citric acid continuation ultrasound 10min is added, pour into the autoclave of polytetrafluoroethylene (PTFE) (Teflon) lining；It then will be by pre- place
Nickel foam (2 3cm × 5cm) after reason is totally submerged in graphite oxide suspension, hydro-thermal reaction 5- at 110 DEG C -130 DEG C
7h, cooled to room temperature, products therefrom is washed repeatedly with deionized water after reaction, is freeze-dried 2-3h, is obtained stone
Black alkene/nickel foam matrix (GO/NF)；
(2) GO/NF that step (1) obtains is placed in the four-hole boiling flask for filling 100-150mL deionized water, 5- is added
NaOH lye is added dropwise under lasting stirring condition with the speed of 0.5-2ml/min in 30mg citric acid, and control pH value of solution=10 ±
0.1, stablize 5-10min, solvable nickel salt, solvable cobalt salt are dissolved in deionized water and form mixing salt solution, while with 0.5-
Mixing salt solution and lye is added dropwise in the speed of 2ml/min, stablizes solution ph in pH=10 ± 0.1；Salting liquid drop to be mixed
It adds complete, gained is transferred in Teflon reaction kettle containing the slurries of GO/NF, in 80-100 DEG C of crystallization 5-7h, reaction terminates
Cooled to room temperature afterwards washs products therefrom with deionized water repeatedly, be freeze-dried 2-3h, obtain cobalt acid nickel precursor/
RGO/ foam nickel material；
The product that step (2) obtains is placed in nitrogen atmosphere, 200~400 DEG C of roasting 2-3h, heating rate be 2 DEG C/
Min, nitrogen flow rate 100mL/min prepare honeycomb nano-chip arrays cobalt acid nickel/rGO/ nickel foam hybrid, are denoted as NiCo2O4/
rGO/NF。
The concentration of step (1) the graphite oxide suspension is 0.5,1,3mg/mL, preferably 1mg/mL；Graphite oxide and lemon
The mass ratio of lemon acid is 2:1, ultrasonic power 300W.
The molar ratio of nickel ion and cobalt ions is 1:2 in the mixing salt solution that step (2) is prepared；Nickel ion and cobalt ions
Mole the sum of range be 5-20mmol, preferably 10mmol.
The above-mentioned honeycomb nano-chip arrays cobalt acid nickel/rGO/ foam nickel material being prepared, structure are that graphene is equal
Even to be wrapped in foam nickel surface, then vertical interlaced grows ultra-thin mesoporous nickel cobalt nanometer in graphene/foam nickel base
Piece, cobalt acid nickel nano film are spinelle cubic phase, and size is 110 × 11nm, and nanometer sheet is the cobalt acid by diameter for 10.8nm
Nickel nanoparticle single layer Alignment forms.
The beneficial effects of the present invention are:
1, the present invention is used using loose porous nickel foam as substrate by the way that citric acid is added into graphene suspension
Hydro-thermal process obtains graphene/nickel foam matrix, and graphene oxide is uniformly wrapped on foam nickel skeleton, easy to operate, avoids
The use of high temperature and pressure operation and organic reagent, it is environmentally protective.Liquid-phase coprecipitation and subsequent is further helped by citric acid
Calcination processing prepares honeycomb nano-chip arrays cobalt acid nickel/rGO/ nickel foam hybrid, can be directly as electrode of super capacitor
Materials'use avoids the cumbersome process for preparing electrode slice, increases active surface, improves active material utilization.
2, foam nickel material provided by the invention, initial feed graphene oxide has biggish specific surface area and surface is rich
There is oxygen-containing functional group, is conducive to the nucleation of nickel ion, cobalt ions.Meanwhile the nickel foam as collector is directly and active material
Contact, reduces electrode resistance.Electrochemical results show that honeycomb nano-chip arrays cobalt acid nickel/rGO/ foam nickel material has
Very excellent high specific capacitance and cyclical stability.
3, preparation method of the invention is easy to operate, easily controllable, low in cost.
Detailed description of the invention
Fig. 1 is the NiCo that embodiment 1 is prepared2O4The SEM of/rGO/NF schemes.
Fig. 2 is the NiCo that embodiment 1 is prepared2O4The local SEM of/rGO/NF schemes.
Fig. 3 is the NiCo that embodiment 1 is prepared2O4/ rGO/NF 5Ag in 2M KOH electrolyte-1Recycle 5000 perseverances
Current charge-discharge electrograph；
Specific embodiment
Current following most preferred embodiment illustrates the present invention, but does not limit the scope of the invention.
Embodiment 1:
(1) pretreatment of nickel foam: the salt for being successively 2M with acetone, concentration by the nickel foam that 2 sizes are 3cm × 5cm
Acid solution, deionized water and each supersound washing 15min of dehydrated alcohol, then 80 DEG C of vacuum drying 2h；
(2) the graphite oxide colloidal sol for weighing 60mg is dissolved in the deionized water of 60mL, and ultrasonic disperse 20min obtains oxidation stone
Black alkene suspension is added 30mg citric acid and continues ultrasound 10min；
(3) suspension obtained by step (2) preparation of graphene/nickel foam (GO/NF) matrix: is poured into polytetrafluoroethylene (PTFE)
(Teflon) in the autoclave of lining, the nickel foam obtained by pretreatment is completely submerged in graphene oxide suspension,
120 DEG C of hydro-thermal reaction 5h, to reaction kettle cooled to room temperature, by products therefrom deionized water repeated flushing, freeze-drying
3h obtains the nickel foam of graphene uniform package, is denoted as GO/NF.
(4) GO/NF that (3) obtain 10 1cm × 3cm are cut into be placed in the four-hole boiling flask for filling 120mL deionized water,
10mg citric acid is added, under lasting stirring condition, 0.13MNaOH solution is slowly added dropwise, controls pH value of solution=10 ± 0.1, surely
10min is determined, by the Ni (NO of 0.9694g3)2·6H2Co (the NO of O (3.33mmol) and 1.94g3)2·6H2O (6.67mmol) is molten
In the deionized water of 100mL, ultrasonic 5min is configured to mixing salt solution, while mixing salt solution and lye is slowly added dropwise, and makes
Solution ph is stablized 10 ± 0.1；Salting liquid to be mixed is added dropwise, and gained is transferred to Teflon containing the slurries of GO/NF
In reaction kettle, in 90 DEG C of crystallization 6h, cooled to room temperature, products therefrom is washed repeatedly with deionized water after reaction,
It is freeze-dried 3h, obtains cobalt acid nickel precursor/rGO/ nickel foam.
(5) by above-mentioned precursor, (heating rate is 2 DEG C/min) is forged in the case where nitrogen flow rate is the atmosphere of 100mL/min 300 DEG C
2h is burnt, product honeycomb nano-chip arrays cobalt acid nickel/rGO/ foam nickel material is obtained, is denoted as NiCo2O4/rGO/NF-1.Its SEM
Figure is shown in Fig. 1.
(6) to NiCo2O4/ rGO/NF-1 is characterized, by SEM (Fig. 1) it is found that product is by the super of diameter about 10.8nm
Thin NiCo2O4The nanometer sheet vertical interlaced that thickness made of nano particle single layer Alignment is about 11nm, length is about 110nm
It is grown in graphene/nickel foam matrix and constitutes.
Honeycomb nano-chip arrays NiCo2O4The electrochemical Characterization of/rGO/NF
(1) using traditional three-electrode system to NiCo2O4/ rGO/NF electrode carries out electrochemical property test, clip 1cm
The NiCo of × 1cm2O4/ rGO/NF is 0.5mg/cm as working electrode, the load capacity of active material2.Saturated calomel electrode
(SCE) it is used as reference electrode, platinized platinum is used as to electrode, and electrolyte solution is 2M KOH solution.
(4) the honeycomb nano-chip arrays NiCo that embodiment 1 is prepared2O4The perseverance electricity of/rGO/NF electrode in 2MKOH
Flow charging and discharging curve.In 5Ag-1High current density under, after 5000 constant current charge-discharges, specific capacitance is still initial electricity
78% held reaches 1828Fg-1.This shows the honeycomb nano-chip arrays NiCo that embodiment 1 is prepared2O4/ rGO/NF electrode
With excellent cyclical stability.
Embodiment 2:
The present embodiment is in addition to following characteristics with embodiment 1: the graphite oxide colloidal sol for weighing 30mg is dissolved in the deionization of 60mL
In water, ultrasonic disperse 20min obtains graphene oxide suspension, and 15mg citric acid is added and continues ultrasound 10min, subsequent step and
Embodiment 1 is identical, obtains catalyst n iCo2O4/rGO/NF-2。
Embodiment 3:
The present embodiment is in addition to following characteristics with embodiment 1: the graphite oxide colloidal sol for weighing 180mg is dissolved in the deionization of 60mL
In water, ultrasonic disperse 20min obtains graphene oxide suspension, and 90mg citric acid is added and continues ultrasound 10min, subsequent step and
Embodiment 1 is identical, obtains catalyst n iCo2O4/rGO/NF-3。
Embodiment 4:
The present embodiment is in addition to following characteristics with embodiment 1: obtained GO/NF being placed in and fills the four of 120mL deionized water
In mouth flask, 5mg citric acid is added, under lasting stirring condition, 0.13MNaOH solution is slowly added dropwise, controls pH value of solution=10
± 0.1, stablize 10min, by the Ni (NO of 0.9694g3)2·6H2Co (the NO of O (3.33mmol) and 1.94g3)2·6H2O
(6.67mmol) is dissolved in the deionized water of 100mL, and ultrasonic 5min is configured to mixing salt solution, while salt-mixture is slowly added dropwise
Solution and lye stablize solution ph 10 or so；Salting liquid to be mixed is added dropwise, the slurries by gained containing GO/NF
It is transferred in Teflon reaction kettle, in 90 DEG C of crystallization 6h, cooled to room temperature after reaction, by products therefrom deionization
Water washs repeatedly, is freeze-dried 3h, obtains cobalt acid nickel precursor/rGO/ nickel foam hybrid.
Above-mentioned precursor is calcined into 2h in 300 DEG C of (heating rate is 2 DEG C/min) nitrogen atmospheres, product honeycomb is obtained and receives
Rice chip arrays cobalt acid nickel/rGO/ foam nickel material, is denoted as NiCo2O4/rGO/NF-4。
Embodiment 5:
The present embodiment is in addition to following characteristics with embodiment 1: obtained GO/NF being placed in and fills the four of 120mL deionized water
In mouth flask, 15mg citric acid is added, under lasting stirring condition, 0.13MNaOH solution is slowly added dropwise, controls pH value of solution=10
± 0.1, stablize 10min, by the Ni (NO of 0.9694g3)2·6H2Co (the NO of O (3.33mmol) and 1.94g3)2·6H2O
(6.67mmol) is dissolved in the deionized water of 100mL, and ultrasonic 5min is configured to mixing salt solution, while salt-mixture is slowly added dropwise
Solution and lye stablize solution ph 10 or so；Salting liquid to be mixed is added dropwise, the slurries by gained containing GO/NF
It is transferred in Teflon reaction kettle, in 90 DEG C of crystallization 6h, cooled to room temperature after reaction, by products therefrom deionization
Water washs repeatedly, is freeze-dried 3h, obtains cobalt acid nickel precursor/rGO/ foam nickel material.
Above-mentioned precursor is calcined into 2h in 300 DEG C of (heating rate is 2 DEG C/min) nitrogen atmospheres, product honeycomb is obtained and receives
Rice chip arrays cobalt acid nickel/rGO/ foam nickel material, is denoted as NiCo2O4/rGO/NF-5。
Embodiment 6:
The present embodiment is in addition to following characteristics with embodiment 1: by above-mentioned precursor in 200 DEG C of (heating rate is 2 DEG C/min) nitrogen
2h is calcined in gas atmosphere, product honeycomb nano-chip arrays cobalt acid nickel/rGO/ foam nickel material is obtained, is denoted as NiCo2O4/rGO/
NF-6。
Embodiment 7:
The present embodiment is in addition to following characteristics with embodiment 1: by above-mentioned precursor in 400 DEG C of (heating rate is 2 DEG C/min) nitrogen
2h is calcined in gas atmosphere, product honeycomb nano-chip arrays cobalt acid nickel/rGO/ foam nickel material is obtained, is denoted as NiCo2O4/rGO/
NF-7。
Claims (6)
1. a kind of honeycomb nano-chip arrays cobalt acid nickel/rGO/ nickel foam, which is characterized in that be the ultra-fine cobalt acid nickel by 10.8nm
Nano particle single layer Alignment at ultra-thin cobalt acid nickel nano film (110 × 11nm) vertical interlaced be grown on graphene modified
The honeycomb nano-chip arrays structure that foam nickel surface is constituted；By the way that citric acid is added into graphene suspension and uses hydro-thermal
Processing obtains graphene/nickel foam matrix, then helps liquid-phase coprecipitation and calcination process appropriate to prepare by citric acid
Honeycomb nano-chip arrays cobalt acid nickel/rGO/ nickel foam.
2. a kind of preparation method of honeycomb nano-chip arrays cobalt acid nickel/rGO/ nickel foam, which is characterized in that including following
Step:
(1) ultrasonic disperse 15-25min in deionized water is added in graphite oxide gel and obtains graphite oxide suspension, lemon is added
Lemon acid continues ultrasound 10min, and pours into the autoclave of polytetrafluoroethylene (PTFE) Teflon lining；Then it will pass through pretreated foam
Nickel is totally submerged in graphite oxide suspension, 110-130 DEG C of hydro-thermal reaction 5-7h, after reaction cooled to room temperature,
Products therefrom is washed repeatedly with deionized water, 2-3h is freeze-dried, obtains graphene/nickel foam matrix GO/NF；
(2) GO/NF that step (1) obtains is placed in the four-hole boiling flask for filling 100-150mL deionized water, 5-30mg lemon is added
Lemon acid is added dropwise NaOH lye with the speed of 0.5-2ml/min, controls pH value of solution=10 ± 0.1, surely under lasting stirring condition
Determine 5-10min, Nickelous nitrate hexahydrate, cabaltous nitrate hexahydrate are dissolved in deionized water and form mixing salt solution, while with 0.5-
Mixing salt solution and lye is added dropwise in the speed of 2mL/min, stablizes solution ph 10 ± 0.1；Salting liquid to be mixed drips
Finish, gained is transferred in Teflon reaction kettle containing the slurries of GO/NF, the crystallization 5-7h at 80-100 DEG C, after reaction
Cooled to room temperature washs products therefrom with deionized water repeatedly, is freeze-dried 2-3h, obtains cobalt acid nickel precursor/rGO/
Nickel foam；
(3) product for obtaining step (2) is in nitrogen atmosphere, nitrogen flow rate 100mL/min, is warming up to 200- with 2 DEG C/min
400 DEG C of calcining 2-3h obtain honeycomb nano-chip arrays cobalt acid nickel/rGO/ nickel foam, are denoted as NiCo2O4/rGO/NF。
3. preparation method according to claim 2, it is characterised in that: the concentration of step (1) the graphite oxide suspension
Range is 0.5-3mg/mL；The mass ratio of graphite oxide and citric acid is 2:1, ultrasonic power 300W.
4. preparation method according to claim 2, it is characterised in that: nickel ion in the mixing salt solution that step (2) is prepared
Molar ratio with cobalt ions is 1:2；The sum of mole range of nickel ion and cobalt ions is 5~20mmol.
5. preparation method according to claim 2, it is characterised in that: the NaOH concentration of lye that step (2) is prepared is 0.2-
0.3mol/L。
6. preparation method according to claim 2, it is characterised in that: the mass range of citric acid is 5- in step (2)
30mg。
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| WO2023207813A1 (en) * | 2022-04-29 | 2023-11-02 | 一汽奔腾轿车有限公司 | Preparation method for multi-stage nanosheet array nico2o4/rgo/nf and application as electrode |
| CN115385606A (en) * | 2022-09-22 | 2022-11-25 | 浙江智峰科技有限公司 | Light fireproof nano building material and preparation method thereof |
| CN115385606B (en) * | 2022-09-22 | 2023-06-02 | 浙江智峰科技有限公司 | Light fireproof nano building material and preparation method thereof |
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