CN106910647B - Compound cobalt acid nickel nano-wire array material of graphene aerogel and preparation method thereof - Google Patents
Compound cobalt acid nickel nano-wire array material of graphene aerogel and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to compound cobalt acid nickel nano-wire array materials of a kind of graphene aerogel and preparation method thereof.Its technical solution is：By graphene oxide solution, hydro-thermal reaction, drying obtain graphene aerogel in reaction kettle.By Nickel dichloride hexahydrate: cobalt chloride hexahydrate: the molar ratio of urea is 1: 2:（7~10）With a concentration of 0.016 ~ 0.1mol/L of Nickel dichloride hexahydrate, Nickel dichloride hexahydrate, cobalt chloride hexahydrate and urea are dissolved in deionized water, stirs, obtains mixed solution.By graphene aerogel: the mass ratio of the Nickel dichloride hexahydrate in mixed solution is 1:（2~4）Graphene aerogel is put into mixed solution, hydro-thermal reaction, it is dry, obtain presoma.Presoma is kept the temperature into 1.5 ~ 3h at 300 ~ 400 DEG C, the compound cobalt acid nickel nano-wire array material of graphene aerogel is made.Present invention process is simple, environmental-friendly and can realize industrialized production, and prepared product specific capacity is high, good rate capability and cyclical stability are excellent.
Description
Technical field
The invention belongs to cobalt acid nickel nano-wire array technical field of composite materials.It is multiple more particularly to a kind of graphene aerogel
Close cobalt acid nickel nano-wire array material and preparation method thereof.
Background technology
Ultracapacitor is a kind of new type of energy storage device between traditional capacitor and accumulator, it is considered to be is most had
Reproducible, the clean energy conversion and storage device of development prospect, with higher than energy, operating temperature range is wide, uses
The advantages that long lifespan, good cycle, power density are big and environmentally protective, be widely used in electronic product, electric vehicle industry,
The fields such as aerospace and redundant electrical power.Currently, the research of electrode material for super capacitor includes mainly carbon material, metal oxygen
Compound and conducting polymer, wherein metal oxide is of much attention with its high specific capacity.
Cobalt acid nickel derives from a wealth of sources, is cheap and environmentally friendly, as a kind of transiting metal oxidation of polyhybird valence state
Object has than NiO and Co3O4Higher conductivity and electrochemical reaction activity, the suitable electrode material that exactly we find.
However the low native electronic conductivity of cobalt acid nickel inherently has still seriously affected the performance of its performance, especially high rate performance and cycle is steady
Qualitative energy, and then limit application of the cobalt acid nickel in electrochemical energy storage.Although having developed cobalt acid nickel and carbon fiber at present
Or the method for modifying that graphene is compound, though the chemical property of cobalt acid nickel is promoted to a certain extent, it is carbon fiber loaded easy
The reunion of cobalt acid nickel is formed to reduce active specific surface, and graphene sheet layer is easy to stack during the reaction to form sheet,
These problems, which remain unchanged, limits the performance performance of cobalt acid nickel material, it is difficult to meet the property higher and higher to electrode material for super capacitor
It can require.
Invention content
The present invention is directed to overcome the deficiencies in the prior art, and it is an object of the present invention to provide one kind is simple for process, easy to operate, environment is friendly
Preparation method that is good and can realizing the compound cobalt acid nickel nano-wire array material of the graphene aerogel of industrialized production；Use this method
The compound cobalt acid nickel nano-wire array material specific capacity of the graphene aerogel of preparation is high, good rate capability and cyclical stability are excellent
It is different.
To achieve the above object, the present invention adopts the following technical scheme that：
(1) by a concentration of 2~2.5kg/m3Graphene oxide solution be placed in reaction kettle, in 145~155 DEG C of conditions
Graphene aerogel is made in 2~3h of lower hydro-thermal reaction, natural cooling, freeze-drying.
(2) Nickel dichloride hexahydrate: cobalt chloride hexahydrate is pressed: the molar ratio of urea is 1: 2: (7~10) dispensing, then press six water
Close nickel chloride a concentration of 0.016~0.1mol/L, by the Nickel dichloride hexahydrate, cobalt chloride hexahydrate and urea be dissolved in from
In sub- water, stirring, ultrasonic disperse obtains mixed solution.
(3) graphene aerogel is pressed: the mass ratio of the Nickel dichloride hexahydrate in the mixed solution is 1: (2~4),
The graphene aerogel is put into the mixed solution, the hydro-thermal reaction 20~for 24 hours under the conditions of 90~95 DEG C is naturally cold
But, it washs, freeze-drying obtains presoma.
(4) presoma is placed in tube-type atmosphere furnace, is warming up to 300~400 DEG C with 1~2 DEG C/min rates, heat preservation
1.5~3h, it is cooling, the compound cobalt acid nickel nano-wire array material of graphene aerogel is made.
The cobalt acid nickel nano wire of the compound cobalt acid nickel nano-wire array material of graphene aerogel and three-dimensional macropore airsetting
Graphene in glue is combined, and forms compact arranged nano-wire array, the cobalt acid nickel nano wire of load is porous structure, is formed
Aeroge macropore and the compound cobalt acid nickel nano-wire array material of the mesoporous nested graphene aerogel of nano wire.
The Nickel dichloride hexahydrate, cobalt chloride hexahydrate and urea are that analysis is pure.
The washing is first to be washed 3~5 times with ethyl alcohol, then be washed with deionized water 3~5 times, then 8 are impregnated with deionized water~
12 hours, then be washed with deionized water 3~5 times.
Due to the adoption of the above technical scheme, the present invention having the beneficial effect that compared with the existing technology：
(1) present invention first through simple hydro-thermal reaction i.e. obtain graphene aerogel, then by the graphene aerogel with
Prefabricated mixed solution hydro-thermal reaction, the then compound cobalt acid nickel nano-wire array material of thermally treated obtained graphene aerogel,
Therefore it is simple for process.
(2) present invention is discharged without toxic gas during the reaction, and the waste liquid environmental pollution being discharged after reaction
It is small, it is environmentally protective.Cobalt source and the nickel source for preparing cobalt acid nickel are cheap, and equipment needed for production process is simple, and production cost is low.
(3) the cobalt acid nickel nano wire in the compound cobalt acid nickel nano-wire array material of graphene aerogel prepared by the present invention is tight
Solid matter is listed on graphene sheet layer, and specific surface area is high；Three-dimensional grapheme aeroge forms space structure, can be effectively reduced electrification
The reunion of graphene sheet layer stacks during, and high electric conductivity can significantly improve the conduction of electronics in addition, promotes cobalt acid nickel
Specific capacity, multiplying power and cycle performance.
(4) the cobalt acid nickel nano wire and three of the compound cobalt acid nickel nano-wire array material of graphene aerogel prepared by the present invention
Graphene in dimension macropore aeroge is combined, and forms compact arranged nano-wire array, the cobalt acid nickel nano wire of load is more
Pore structure forms aeroge macropore and the compound cobalt acid nickel nano-wire array material of the mesoporous nested graphene aerogel of nano wire.
Three-dimensional macropore therein can accelerate the infiltration of electrolyte with mesoporous nested porous structure, increase active material and connect with electrolyte
Tactile active surface area, while ion transmission channel is shortened, to further promote specific capacity, multiplying power and the cycle of cobalt acid nickel
Performance.
(5) the compound cobalt acid nickel nano-wire array material of graphene aerogel for preparing of the present invention is after testing：Graphene airsetting
The aperture of glue is 50~200 μm, and cobalt acid nickel nano wire is evenly distributed on graphene sheet layer；The cobalt acid nickel nano wire of made product
For porous structure, aperture is 3~15nm；Specific surface area is 50~90m2/g。
The compound cobalt acid nickel nano-wire array material of graphene aerogel prepared by the present invention is through electrochemical property test：It is made
Product is 1A g in current density-1Under the conditions of specific capacity be 1990~2200F g-1；It is 100A g in current density-1Condition
Under specific capacity be 970~1000F g-1；It is 80A g in current density-1Under the conditions of specific capacity be 1100~1200F g-1,
Capability value conservation rate is up to 80~88% after 10000 cyclic processes.
Therefore, the present invention has the characteristics that simple for process, easy to operate, environmental-friendly and can realize industrialized production, institute
The compound cobalt acid nickel nano-wire array material specific capacity of the graphene aerogel of preparation is high, good rate capability and cyclical stability are excellent
It is different.
Description of the drawings
Fig. 1 is a kind of SEM figures of the compound cobalt acid nickel nano-wire array material of graphene aerogel prepared by the present invention；
Fig. 2 is the XRD diagram of the compound cobalt acid nickel nano-wire array material of graphene aerogel shown in Fig. 1；
Fig. 3 is the TEM figures of the compound cobalt acid nickel nano-wire array material of graphene aerogel shown in Fig. 1.
Specific implementation mode
The present invention is described further below in conjunction with the drawings and specific embodiments, not to the claims in the present invention model
The limitation enclosed.
In present embodiment：
The cobalt acid nickel nano wire of the compound cobalt acid nickel nano-wire array material of graphene aerogel and three-dimensional macropore airsetting
Graphene in glue is combined, and forms compact arranged nano-wire array, the cobalt acid nickel nano wire of load is porous structure, is formed
Aeroge macropore and the compound cobalt acid nickel nano-wire array material of the mesoporous nested graphene aerogel of nano wire.
The Nickel dichloride hexahydrate, cobalt chloride hexahydrate and urea are that analysis is pure.
The washing is first to be washed 3~5 times with ethyl alcohol, then be washed with deionized water 3~5 times, then 8 are impregnated with deionized water~
12 hours, then be washed with deionized water 3~5 times.
It is repeated no more in embodiment.
Embodiment 1
A kind of compound cobalt acid nickel nano-wire array material of graphene aerogel and preparation method thereof.It is prepared described in the present embodiment
Method comprises the concrete steps that：
(1) by a concentration of 2~2.5kg/m3Graphene oxide solution be placed in reaction kettle, in 145~155 DEG C of conditions
Graphene aerogel is made in 2~3h of lower hydro-thermal reaction, natural cooling, freeze-drying.
(2) Nickel dichloride hexahydrate: cobalt chloride hexahydrate is pressed: the molar ratio of urea is 1: 2: (7~8) dispensing, then press six water
A concentration of 0.016~the 0.04mol/L for closing nickel chloride, the Nickel dichloride hexahydrate, cobalt chloride hexahydrate and urea are dissolved in
In ionized water, stirring, ultrasonic disperse obtains mixed solution.
(3) graphene aerogel is pressed: the mass ratio of the Nickel dichloride hexahydrate in the mixed solution is 1: (2~3),
The graphene aerogel is put into the mixed solution, the hydro-thermal reaction 20~for 24 hours under the conditions of 90~95 DEG C is naturally cold
But, it washs, freeze-drying obtains presoma.
(4) presoma is placed in tube-type atmosphere furnace, is warming up to 300~330 DEG C with 1~2 DEG C/min rates, heat preservation
2.5~3h, it is cooling, the compound cobalt acid nickel nano-wire array material of graphene aerogel is made.
Fig. 1 is a kind of SEM figures of the compound cobalt acid nickel nano-wire array material of graphene aerogel manufactured in the present embodiment；Figure
2 be the XRD diagram of the compound cobalt acid nickel nano-wire array material of graphene aerogel shown in Fig. 1；Fig. 3 is graphene airsetting shown in Fig. 1
The TEM of the compound cobalt acid nickel nano-wire array material of glue schemes.As seen from Figure 1, the cobalt acid nickel nano-wire array in product according to
Attached thin graphene grows and is cross-linked, and graphene sheet layer forms the space structure of three-dimensional interconnection, the hole of graphene aerogel
Diameter is 130~200 μm, and cobalt acid nickel nano wire is evenly distributed on graphene sheet layer；As seen from Figure 2, product is pure phase
NiCo2O4Material (PDF#20-0781)；As seen from Figure 3, the cobalt acid nickel nano wire of product is porous structure, and aperture is
10~15nm.It is tested through BET, specific surface area 50-70m2/g。
The compound cobalt acid nickel nano-wire array material of graphene aerogel manufactured in the present embodiment is through electrochemical property test：?
Current density is 1A g-1Under the conditions of specific capacity be 1990~2080F g-1；It is 100A g in current density-1Under the conditions of ratio
Capacity is 970~985F g-1；It is 80A g in current density-1Under the conditions of specific capacity be 1100~1150F g-1, pass through
Capability value conservation rate is up to 84~88% after 10000 cyclic processes.
Embodiment 2
A kind of compound cobalt acid nickel nano-wire array material of graphene aerogel and preparation method thereof.It is prepared described in the present embodiment
Method comprises the concrete steps that：
(1) by a concentration of 2~2.5kg/m3Graphene oxide solution be placed in reaction kettle, in 145~155 DEG C of conditions
Graphene aerogel is made in 2~3h of lower hydro-thermal reaction, natural cooling, freeze-drying.
(2) Nickel dichloride hexahydrate: cobalt chloride hexahydrate is pressed: the molar ratio of urea is 1: 2: (8~9) dispensing, then press six water
Close nickel chloride a concentration of 0.04~0.07mol/L, by the Nickel dichloride hexahydrate, cobalt chloride hexahydrate and urea be dissolved in from
In sub- water, stirring, ultrasonic disperse obtains mixed solution.
(3) graphene aerogel is pressed: the mass ratio of the Nickel dichloride hexahydrate in the mixed solution is 1: (2.5~
3.5), the graphene aerogel is put into the mixed solution, the hydro-thermal reaction 20~for 24 hours under the conditions of 90~95 DEG C, from
It is so cooling, it washs, freeze-drying obtains presoma.
(4) presoma is placed in tube-type atmosphere furnace, is warming up to 330~370 DEG C with 1~2 DEG C/min rates, heat preservation
2~2.5h, it is cooling, the compound cobalt acid nickel nano-wire array material of graphene aerogel is made.
The compound cobalt acid nickel nano-wire array material of graphene aerogel manufactured in the present embodiment is after testing：Graphene aerogel
Aperture be 90~160 μm, cobalt acid nickel nano wire is evenly distributed on graphene sheet layer；The cobalt acid nickel nano wire of made product is
Porous structure, aperture are 7~12nm；Specific surface area is 60~80m2/g。
The compound cobalt acid nickel nano-wire array material of graphene aerogel manufactured in the present embodiment is through electrochemical property test：?
Current density is 1A g-1Under the conditions of specific capacity be 2050~2140F g-1；It is 100A g in current density-1Under the conditions of ratio
Capacity is 980~995F g-1；It is 80A g in current density-1Under the conditions of specific capacity be 1130~1180F g-1, pass through
Capability value conservation rate is up to 82~86% after 10000 cyclic processes.
Embodiment 3
A kind of compound cobalt acid nickel nano-wire array material of graphene aerogel and preparation method thereof.It is prepared described in the present embodiment
Method comprises the concrete steps that：
(1) by a concentration of 2~2.5kg/m3Graphene oxide solution be placed in reaction kettle, in 145~155 DEG C of conditions
Graphene aerogel is made in 2~3h of lower hydro-thermal reaction, natural cooling, freeze-drying.
(2) Nickel dichloride hexahydrate: cobalt chloride hexahydrate is pressed: the molar ratio of urea is 1: 2: (9~10) dispensing, then press six water
Close nickel chloride a concentration of 0.07~0.1mol/L, by the Nickel dichloride hexahydrate, cobalt chloride hexahydrate and urea be dissolved in from
In sub- water, stirring, ultrasonic disperse obtains mixed solution.
(3) graphene aerogel is pressed: the mass ratio of the Nickel dichloride hexahydrate in the mixed solution is 1: (3~4),
The graphene aerogel is put into the mixed solution, the hydro-thermal reaction 20~for 24 hours under the conditions of 90~95 DEG C is naturally cold
But, it washs, freeze-drying obtains presoma.
(4) presoma is placed in tube-type atmosphere furnace, is warming up to 370~400 DEG C with 1~2 DEG C/min rates, heat preservation
1.5~2h, it is cooling, the compound cobalt acid nickel nano-wire array material of graphene aerogel is made.
The compound cobalt acid nickel nano-wire array material of graphene aerogel manufactured in the present embodiment is after testing：Graphene aerogel
Aperture be 50~120 μm, cobalt acid nickel nano wire is evenly distributed on graphene sheet layer；The cobalt acid nickel nano wire of made product is
Porous structure, aperture are 3~8nm；Specific surface area is 70~90m2/g。
The compound cobalt acid nickel nano-wire array material of graphene aerogel manufactured in the present embodiment is through electrochemical property test：?
Current density is 1A g-1Under the conditions of specific capacity be 2110~2200F g-1；It is 100A g in current density-1Under the conditions of ratio
Capacity is 985~1000F g-1；It is 80A g in current density-1Under the conditions of specific capacity be 1150~1200F g-1, pass through
Capability value conservation rate is up to 80~84% after 10000 cyclic processes.
Present embodiment having the beneficial effect that compared with the existing technology：
(1) present embodiment first obtains graphene aerogel through simple hydro-thermal reaction, then by the graphene
Aeroge and prefabricated mixed solution hydro-thermal reaction, the then compound cobalt acid nickel nanometer linear array of thermally treated acquisition graphene aerogel
Row material, thus it is simple for process.
(2) present embodiment is discharged without toxic gas during the reaction, and the waste liquid pair being discharged after reaction
Environmental pollution is small, environmentally protective.Cobalt source and the nickel source for preparing cobalt acid nickel are cheap, and equipment needed for production process is simple, production
It is at low cost.
(3) the cobalt acid nickel in the compound cobalt acid nickel nano-wire array material of graphene aerogel prepared by present embodiment
Nano wire is arranged closely on graphene sheet layer, and specific surface area is high；Three-dimensional grapheme aeroge forms space structure, can be effectively
The reunion for reducing graphene sheet layer in electrochemical process stacks, and high electric conductivity can significantly improve the conduction of electronics in addition, carry
Rise specific capacity, multiplying power and the cycle performance of cobalt acid nickel.
(4) the cobalt acid nickel of the compound cobalt acid nickel nano-wire array material of graphene aerogel prepared by present embodiment is received
Rice noodles are combined with the graphene in three-dimensional macropore aeroge, form compact arranged nano-wire array, the cobalt acid nickel of load is received
Rice noodles are porous structure, form aeroge macropore and the compound cobalt acid nickel nanometer linear array of the mesoporous nested graphene aerogel of nano wire
Row material.Three-dimensional macropore therein can accelerate the infiltration of electrolyte with mesoporous nested porous structure, increase active material and
The active surface area of electrolyte contacts, while shortening ion transmission channel, to further promoted cobalt acid nickel specific capacity, times
Rate and cycle performance.
(5) present embodiment prepare the compound cobalt acid nickel nano-wire array material of graphene aerogel after testing：Stone
The aperture of black alkene aeroge is 50~200 μm, and cobalt acid nickel nano wire is evenly distributed on graphene sheet layer；The cobalt acid of made product
Nickel nano wire is porous structure, and aperture is 3~15nm；Specific surface area is 50~90m2/g。
The compound cobalt acid nickel nano-wire array material of graphene aerogel prepared by present embodiment is through chemical property
Test：Made product is 1A g in current density-1Under the conditions of specific capacity be 1990~2200F g-1；It is in current density
100A g-1Under the conditions of specific capacity be 970~1000F g-1；It is 80A g in current density-1Under the conditions of specific capacity be 1100
~1200F g-1, capability value conservation rate is up to 80~88% after 10000 cyclic processes.
Therefore, present embodiment has simple for process, easy to operate, environmental-friendly and can realize industrialized production
Feature, the compound cobalt acid nickel nano-wire array material specific capacity height of prepared graphene aerogel, good rate capability and cycle are steady
It is qualitative excellent.
Claims (4)
1. a kind of preparation method of the compound cobalt acid nickel nano-wire array material of graphene aerogel, it is characterised in that the preparation side
The step of method is：
(1) by a concentration of 2~2.5kg/m3Graphene oxide solution be placed in reaction kettle, water under the conditions of 145~155 DEG C
Graphene aerogel is made in 2~3h of thermal response, natural cooling, freeze-drying；
(2) Nickel dichloride hexahydrate: cobalt chloride hexahydrate is pressed: the molar ratio of urea is 1: 2: (7~10) dispensing, then by six hydration chlorine
A concentration of 0.016~the 0.1mol/L for changing nickel, is dissolved in deionized water by the Nickel dichloride hexahydrate, cobalt chloride hexahydrate and urea
In, stirring, ultrasonic disperse obtains mixed solution；
(3) graphene aerogel is pressed: the mass ratio of the Nickel dichloride hexahydrate in the mixed solution is 1: (2~4), by institute
It states graphene aerogel to be put into the mixed solution, the hydro-thermal reaction 20~for 24 hours under the conditions of 90~95 DEG C, natural cooling is washed
It washs, is freeze-dried, obtains presoma；
(4) presoma is placed in tube-type atmosphere furnace, is warming up to 300~400 DEG C with 1~2 DEG C/min rates, heat preservation 1.5
~3h, it is cooling, the compound cobalt acid nickel nano-wire array material of graphene aerogel is made；
In the cobalt acid nickel nano wire of the compound cobalt acid nickel nano-wire array material of graphene aerogel and three-dimensional macropore aeroge
Graphene be combined, form compact arranged nano-wire array, the cobalt acid nickel nano wire of load is porous structure, forms airsetting
Glue macropore and the compound cobalt acid nickel nano-wire array material of the mesoporous nested graphene aerogel of nano wire.
2. the preparation method of the compound cobalt acid nickel nano-wire array material of graphene aerogel according to claim 1, special
Sign is that the Nickel dichloride hexahydrate, cobalt chloride hexahydrate and urea are that analysis is pure.
3. the preparation method of the compound cobalt acid nickel nano-wire array material of graphene aerogel according to claim 1, special
Sign is that the washing is first to be washed 3~5 times with ethyl alcohol, then be washed with deionized water 3~5 times, then impregnates 8~12 with deionized water
Hour, then be washed with deionized water 3~5 times.
4. a kind of compound cobalt acid nickel nano-wire array material of graphene aerogel, it is characterised in that the graphene aerogel is compound
Cobalt acid nickel nano-wire array material is received according to the compound cobalt acid nickel of any one of the claims 1 to 3 item graphene aerogel
The compound cobalt acid nickel nano-wire array material of graphene aerogel prepared by the preparation method of nanowire arrays material.
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| CN108380238A (en) * | 2018-02-07 | 2018-08-10 | 大连工业大学 | A kind of cobalt acid Raney nickel and preparation method thereof for sodium borohydride hydrolysis |
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| CN111613453B (en) * | 2020-05-29 | 2022-02-08 | 大连交通大学 | Preparation method of porous nickel cobaltate/graphene nano composite electrode material |
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| CN104882298A (en) * | 2015-04-30 | 2015-09-02 | 江苏大学 | Method for preparing NiCo2O4/graphene supercapacitor material with microwave method |
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