CN105374574B - A kind of preparation method and applications of cobalt hydroxide/graphene flexible electrode material - Google Patents
A kind of preparation method and applications of cobalt hydroxide/graphene flexible electrode material Download PDFInfo
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- CN105374574B CN105374574B CN201510990677.9A CN201510990677A CN105374574B CN 105374574 B CN105374574 B CN 105374574B CN 201510990677 A CN201510990677 A CN 201510990677A CN 105374574 B CN105374574 B CN 105374574B
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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
A kind of preparation method and applications of cobalt hydroxide/graphene flexible electrode material, the present invention relates to a kind of preparation method and applications of flexible electrode material, the conducting membrane material specific capacitance prepared the present invention is to solve existing method is low and the problem of poor mechanical property.Method is：Prepare bacteria cellulose slurry；Cobalt hydroxide/graphene composite material is prepared, bacteria cellulose slurry is filtered by vacuum and is formed a film, cobalt hydroxide/graphene composite material dispersion liquid is then added in and continues to filter drying, cobalt hydroxide/graphene flexible electrode material is made, applied to ultracapacitor.Electrode active material specific capacitance of the present invention is high, flexible electrode good mechanical performance, is prepared into ultracapacitor with good capacitive character.The invention belongs to technical field of nano material.
Description
Technical field
The present invention relates to a kind of preparation method and applications of cobalt hydroxide/graphene flexible electrode material.
Background technology
Ultracapacitor combines the advantage of battery and conventional dielectric capacitor, and energy density and power density are filled up
Blank between battery and conventional dielectric capacitor.
Ultracapacitor can be divided into electrochemical capacitor in double electrode layer and fake capacitance capacitor by mechanism.Wherein by increasing electricity
The surface area of pole material and the thickness for reducing electric double layer can improve the specific capacity of capacitor.Grapheme material chemical stabilization is led
Electric rate is high, and theoretical specific surface area is high.Relative to double layer capacitor, pseudocapacitors can provide higher by faraday's reaction
Capacitance.Transition group metallic oxide or hydroxide can generate good fake capacitance, provide higher capacitance.Have
Preferably high rate performance and cyclical stability relatively.Cobalt hydroxide has layer structure and larger interlamellar spacing, possesses high reason
By specific capacity, high specific surface area and quick ion be inserted into extrusion rate, become a kind of outstanding electrode material.But it often makes
Standby material specific capacity out is very low.
With the development of flexible, flexible electronic device, flexible electrode material of the exploitation with bending stability has become
The important directions of energy storage area research at present.Relative to metal oxide and its hydroxide, in the electrode production process of early stage,
Addition binding agent is generally required, contact of the part electrolyte with active material is hindered, increases the internal resistance of electrode, increase ion
With the fast transfer of electronics.
Invention content
The present invention is to solve existing method prepare conducting membrane material specific capacitance is low and cycle performance and mechanical property
Can be poor the problem of, provides a kind of preparation method and applications of cobalt hydroxide/graphene flexible electrode material.
A kind of preparation method of cobalt hydroxide/graphene flexible electrode material of the present invention, carries out according to the following steps：
First, bacteria cellulose is impregnated supersound washing in deionized water to deacidify, is then uniformly dispersed in deionized water,
The stirring of refiner high speed is then transferred to, obtains substrate bacteria cellulose slurry；
2nd, it by graphene oxide, is scattered in distilled water, obtains graphene oxide dispersion；Cobalt salt is dissolved in distilled water
In, it is then added in graphene oxide dispersion, ultrasonic disperse is uniform, then adds in ammonium hydroxide, is transferred to reaction after mixing
In kettle, heating obtains cobalt hydroxide graphene composite material；
3rd, bacteria cellulose slurry is filtered by vacuum and formed a film, then added in cobalt hydroxide graphene composite material and continue to take out
Filter film forming, then be placed in vacuum drying chamber and be dried, cobalt hydroxide/graphene flexible electrode material is made；
The quality of cobalt hydroxide and bacteria cellulose after vacuum filtration wherein in cobalt hydroxide/graphene flexible electrode material
Than for (0.1~6)：1；The ratio of graphene oxide and cobalt salt is 1mg in step 2:(0.001mmol~0.3mmol)；Oxidation
The mass volume ratio of graphene and ammonium hydroxide is 1mg：(0.001~0.1) mL；The wherein described ammonium hydroxide is the ammonium hydroxide of 25wt%.
Beneficial effects of the present invention：
(1) bacteria cellulose is resourceful, environmental-friendly, has hyperfine reticular structure and extraordinary mechanical property.
Numerous studies have shown that the carbon materials such as bacteria cellulose and graphene have extraordinary binding force.Utilize its feature, load
Cobalt hydroxide graphene composite material, make materials serve act synergistically, remain flexible material excellent mechanical property and
The high specific capacitance of cobalt hydroxide.Bacteria cellulose contains a large amount of hydroxyl simultaneously, in the application of aqueous ultracapacitor, has
Good hydrophily, reduces impedance.Bacteria cellulose is resourceful, of low cost, and cobalt hydroxide specific capacitance is high, graphene tool
There is excellent electric conductivity to also improve good electric double layer capacitance simultaneously.Using the synergistic effect of material, it is prepared for high specific capacitance
And the flexible material of mechanical property, specific capacitance can reach 847F/g, applied to ultracapacitor；
(2) preparation process is simple, and the prices of raw materials are cheap；
(3) directly it is used as electrode of super capacitor with good capacitive character.
Description of the drawings
The stereoscan photograph of the cobalt hydroxide that Fig. 1 and Fig. 2 is obtained by embodiment 1/graphene flexible electrode material；
The working electrode prepared with cobalt hydroxide/graphene flexible electrode material that Fig. 3 is obtained by embodiment 1 is in 6M hydrogen
The cyclic voltammetry curve under different scanning speed in potassium oxide electrolyte；Wherein a is 20mV/s, and b 50mV/s, c are
100mV/s；
The stereoscan photograph of the cobalt hydroxide that Fig. 4 is obtained by embodiment 2/graphene flexible electrode material；
The working electrode prepared with cobalt hydroxide/graphene flexible electrode material that Fig. 5 is obtained by embodiment 2 is in 6M hydrogen
The cyclic voltammetry curve under different scanning speed in potassium oxide electrolyte；Wherein a is 20mV/s, and b 50mV/s, c are
100mV/s。
Specific embodiment
Specific embodiment one：A kind of preparation method of cobalt hydroxide of present embodiment/graphene flexible electrode material, is pressed
Following steps carry out：
First, bacteria cellulose is impregnated supersound washing in deionized water to deacidify, is then uniformly dispersed in deionized water,
The stirring of refiner high speed is then transferred to, obtains substrate bacteria cellulose slurry；
2nd, it by graphene oxide, is scattered in distilled water, obtains graphene oxide dispersion；Cobalt salt is dissolved in distilled water
In, it is then added in graphene oxide dispersion, ultrasonic disperse is uniform, then adds in ammonium hydroxide, is transferred to reaction after mixing
In kettle, heating obtains cobalt hydroxide graphene composite material；
3rd, bacteria cellulose slurry is filtered by vacuum and formed a film, then added in cobalt hydroxide graphene composite material and continue to take out
Filter film forming, then be placed in vacuum drying chamber and be dried, cobalt hydroxide/graphene flexible electrode material is made；
The quality of cobalt hydroxide and bacteria cellulose after vacuum filtration wherein in cobalt hydroxide/graphene flexible electrode material
Than for (0.1~6)：1；The ratio of graphene oxide and cobalt salt is 1mg in step 2:(0.001mmol~0.3mmol)；Oxidation
The mass volume ratio of graphene and ammonium hydroxide is 1mg：(0.001~0.1) mL；The wherein described ammonium hydroxide is the ammonium hydroxide of 25wt%.
The advantageous effect of present embodiment：
(1) bacteria cellulose is resourceful, environmental-friendly, has hyperfine reticular structure and extraordinary mechanical property.
Numerous studies have shown that the carbon materials such as bacteria cellulose and graphene have extraordinary binding force.Utilize its feature, load
Cobalt hydroxide graphene composite material, make materials serve act synergistically, remain flexible material excellent mechanical property and
The high specific capacitance of cobalt hydroxide.Bacteria cellulose contains a large amount of hydroxyl simultaneously, in the application of aqueous ultracapacitor, has
Good hydrophily, reduces impedance.Bacteria cellulose is resourceful, of low cost, and cobalt hydroxide specific capacitance is high, graphene tool
There is excellent electric conductivity to also improve good electric double layer capacitance simultaneously.Using the synergistic effect of material, it is prepared for high specific capacitance
And the flexible material of mechanical property, specific capacitance can reach 847F/g, applied to ultracapacitor；
(2) preparation process is simple, and the prices of raw materials are cheap；
(3) directly it is used as electrode of super capacitor with good capacitive character.
Specific embodiment two：The present embodiment is different from the first embodiment in that：The power of described ultrasound is
1000w, frequency are 30KHz.It is other same as the specific embodiment one.
Specific embodiment three：The present embodiment is different from the first and the second embodiment in that：It is super described in step 1
The condition of sound washing is 1~10h of ultrasonic time.It is other the same as one or two specific embodiments.
Specific embodiment four：Unlike one of present embodiment and specific embodiment one to three：Described in step 1
High-speed stirred speed be 8000~15000r/min, 3~30min of mixing time.Other and specific embodiment one to three
One of it is identical.
Specific embodiment five：Unlike one of present embodiment and specific embodiment one to four：Described in step 2
Cobalt salt be cobalt acetate, cobalt chloride, cobaltous sulfate or cobalt nitrate.It is other identical with one of specific embodiment one to four.
Specific embodiment six：Unlike one of present embodiment and specific embodiment one to five：Described in step 2
Reaction kettle be liner tetrafluoro high-temperature high-pressure reaction kettle.It is other identical with one of specific embodiment one to five.
Specific embodiment seven：Unlike one of present embodiment and specific embodiment one to six：Add in step 2
The temperature of heat is 90~200 DEG C, and the reaction time is 2h~15h.It is other identical with one of specific embodiment one to six.
Specific embodiment eight：The application of present embodiment cobalt hydroxide/graphene flexible electrode material refers to be applied to
In ultracapacitor.
Specific embodiment nine：Present embodiment is unlike specific embodiment eight：The flexible electrode material conduct
Positive electrode is applied in ultracapacitor.It is other identical with specific embodiment eight.
Beneficial effects of the present invention are verified by following embodiment：
Embodiment 1：A kind of preparation method of cobalt hydroxide of the present embodiment/graphene flexible electrode material, according to the following steps
It carries out：
First, 5g bacteria celluloses are impregnated into supersound washing 3h in deionized water, then uniformly dispersed in deionized water,
The stirring of refiner high speed is then transferred to, obtains substrate bacteria cellulose slurry；
2nd, it by 30mg graphene oxides, is scattered in distilled water, obtains graphene oxide dispersion；By 0.4mmol sulfuric acid
Cobalt is dissolved in distilled water, is then added in graphene oxide dispersion, ultrasonic 30min, then adds in the ammonia of 0.1mL25wt%
Water is transferred to after stirring 30min in liner tetrafluoro high-temperature high-pressure reaction kettle, is heated to 150 DEG C of reaction 4h, is obtained cobalt hydroxide stone
Black alkene composite material；
3rd, bacteria cellulose slurry is filtered by vacuum and formed a film, then added in cobalt hydroxide graphene composite material and continue to take out
Filter film forming, then be placed in vacuum drying chamber and be dried, cobalt hydroxide/graphene flexible electrode material is made；
The quality of bacteria cellulose substrate after being dried in vacuo in cobalt hydroxide/graphene flexible electrode material is 0.15g.
Cobalt hydroxide obtained/graphene flexible electrode material is cut into 1cm × 2cm rectangles, is directly used as super
Capacitor working pole, platinized platinum are used as to electrode, using mercury/mercuric oxide electrode as reference electrode, test the electricity of flexible electrode material
Hold characteristic.Test sample is labeled as COGO-BC-1.
The flexible electrode material obtained to the present embodiment is tested.As seen from Figure 1 cobalt hydroxide nano material with
Graphene uniform disperses, and can clearly find out that sheet is presented in cobalt hydroxide nano material by Fig. 2.Difference is shown in Fig. 3
The scanning potential window for sweeping the cobalt hydroxide graphene composite material of speed is 0.2~0.75V.With apparent redox peaks.
With the increase of sweep speed, response current increases, it is shown that preferable high rate performance.The flexible electrode that the present embodiment is obtained
For material in 2mV/s, specific capacitance can reach 847F/g.
Embodiment 2：A kind of preparation method of cobalt hydroxide of the present embodiment/graphene flexible electrode material, according to the following steps
It carries out：
First, 4g bacteria celluloses are impregnated into supersound washing 3h in deionized water, then uniformly dispersed in deionized water,
The stirring of refiner high speed is then transferred to, obtains substrate bacteria cellulose slurry；
2nd, it by 40mg graphene oxides, is scattered in distilled water, obtains graphene oxide dispersion；By 0.35mmol sulphur
Sour cobalt is dissolved in distilled water, is then added in graphene oxide dispersion, ultrasonic 30min, then adds in 0.18mL25wt%'s
Ammonium hydroxide is transferred to after stirring 30min in liner tetrafluoro high-temperature high-pressure reaction kettle, is heated to 170 DEG C of reaction 3h, is obtained cobalt hydroxide
Graphene composite material；
3rd, bacteria cellulose slurry is filtered by vacuum and formed a film, then added in cobalt hydroxide graphene composite material and continue to take out
Filter film forming, then be placed in vacuum drying chamber and be dried, cobalt hydroxide/graphene flexible electrode material is made；
The quality of bacteria cellulose substrate after being dried in vacuo in cobalt hydroxide/graphene flexible electrode material is 0.12g.
Cobalt hydroxide obtained/graphene flexible electrode material is cut into 1cm × 1.5cm rectangles, is directly used as surpassing
Grade capacitor working pole, platinized platinum are used as to electrode, using mercury/mercuric oxide electrode as reference electrode, test flexible electrode material electricity
The capacitance characteristic of pole material.Test sample is labeled as COGO-BC-2.
As seen from Figure 4 piece attitude cobalt hydroxide nano material composition flower dress, and with the more uniform dispersion of graphene；
Shown in Fig. 5 the scanning potential windows of the different cobalt hydroxide graphene composite materials for sweeping speed for 0.2~
0.75V.With apparent redox peaks.With the increase of sweep speed, response current increases, it is shown that preferable forthright again
Energy.
Examples 1 to 2 cobalt hydroxide specific capacitance is high, and it is good that there is graphene excellent electric conductivity to also improve simultaneously
Electric double layer capacitance.Using the synergistic effect of material, the flexible electrode material for being prepared for high specific capacitance and mechanical property is applied to surpass
There is good capacitive character in grade capacitor；Preparation process is simple, and the prices of raw materials are cheap.
Claims (7)
1. a kind of preparation method of cobalt hydroxide/graphene flexible electrode material, it is characterised in that this method according to the following steps into
Row：
First, bacteria cellulose is impregnated supersound washing in deionized water to deacidify, is then uniformly dispersed in deionized water, then turn
The stirring of refiner high speed is moved on to, obtains substrate bacteria cellulose slurry；
2nd, it by graphene oxide, is scattered in distilled water, obtains graphene oxide dispersion；Cobalt salt is dissolved in distilled water, then
It being added in graphene oxide dispersion, ultrasonic disperse is uniform, then adds in ammonium hydroxide, is transferred in reaction kettle after mixing,
Heating, obtains cobalt hydroxide graphene composite material；The temperature wherein heated is 90 ~ 200 DEG C, and the reaction time is 2h ~ 15h；
3rd, by bacteria cellulose slurry be filtered by vacuum form a film, then add in cobalt hydroxide graphene composite material continue filter into
Film, then be placed in vacuum drying chamber and be dried, cobalt hydroxide/graphene flexible electrode material is made；
Cobalt salt wherein described in step 2 is cobalt acetate, cobalt chloride, cobaltous sulfate or cobalt nitrate；Cobalt hydroxide/graphene flexible electrical
The mass ratio of cobalt hydroxide and bacteria cellulose after vacuum filtration is in the material of pole（0.1~6）：1；Graphene oxide in step 2
Ratio with cobalt salt is 1mg:(0.001mmol~0.3 mmol)；The mass volume ratio of graphene oxide and ammonium hydroxide is 1mg：
(0.001~0.1)mL；The wherein described ammonium hydroxide is the ammonium hydroxide of 25wt%.
2. a kind of preparation method of cobalt hydroxide/graphene flexible electrode material according to claim 1, it is characterised in that
The ultrasonic power is 1000w, and frequency is 30KHz.
3. a kind of preparation method of cobalt hydroxide/graphene flexible electrode material according to claim 1, it is characterised in that
The condition of supersound washing described in step 1 is 1 ~ 10h of ultrasonic time.
4. a kind of preparation method of cobalt hydroxide/graphene flexible electrode material according to claim 1, it is characterised in that
The speed of high-speed stirred described in step 1 is 8000 ~ 15000r/min, 3 ~ 30min of mixing time.
5. a kind of preparation method of cobalt hydroxide/graphene flexible electrode material according to claim 1, it is characterised in that
Reaction kettle described in step 2 is anticorrosion high temperature high voltage resistant reaction kettle.
6. the application of the cobalt hydroxide that preparation method as described in claim 1 obtains/graphene flexible electrode material, feature
It is that the flexible electrode material is applied in ultracapacitor.
7. the application of a kind of cobalt hydroxide/graphene flexible electrode material according to claim 6, it is characterised in that this is soft
Property electrode material as positive electrode be applied to ultracapacitor.
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| CN106920932B (en) * | 2017-03-10 | 2019-12-03 | 上海应用技术大学 | A kind of leaf of bamboo shape Co (OH)2/ graphene combination electrode material and preparation method thereof |
| CN109772179B (en) * | 2018-12-14 | 2021-09-21 | 华南理工大学 | Method for preparing film by utilizing electrodeposition cobalt hydroxide nanosheet |
| CN112185714B (en) * | 2020-10-12 | 2022-01-04 | 广西大学 | Cellulose nanofibril/carbon nanotube/cobaltosic oxide/cobalt-nickel double hydroxide flexible electrode and preparation method thereof |
| CN113394028A (en) * | 2021-06-17 | 2021-09-14 | 辽宁工程技术大学 | Preparation of Co by gas phase diffusion3O4Method for compounding supercapacitor material with graphene |
| CN114743800B (en) * | 2022-04-25 | 2023-07-21 | 武夷学院 | Preparation method of polyacrylic acid/graphene-based flexible electrode material |
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| CN101867046A (en) * | 2010-04-15 | 2010-10-20 | 上海交通大学 | Composite anode material of graphene nanoflakes and cobalt hydroxide for lithium ion battery and preparation method thereof |
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