CN105428091B - A kind of preparation method and applications of bacteria cellulose graphene paper load nickel hydroxide flexible electrode material - Google Patents
A kind of preparation method and applications of bacteria cellulose graphene paper load nickel hydroxide flexible electrode material Download PDFInfo
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- CN105428091B CN105428091B CN201510990854.3A CN201510990854A CN105428091B CN 105428091 B CN105428091 B CN 105428091B CN 201510990854 A CN201510990854 A CN 201510990854A CN 105428091 B CN105428091 B CN 105428091B
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Abstract
A kind of preparation method and applications of bacteria cellulose graphene paper load nickel hydroxide flexible electrode, the present invention relates to a kind of preparation method and applications of flexible electrode material, the present invention is to solve existing method prepare conducting membrane material specific capacitance is low and the problem of high rate performance and poor mechanical property, method is:Prepare bacteria cellulose slurry;Bacteria cellulose graphene paper is prepared, prepares the reaction solution containing nickel salt, bacteria cellulose graphene paper is immersed in the reaction solution containing nickel salt, bacteria cellulose graphene paper load nickel hydroxide flexible electrode is made, applied to ultracapacitor.Electrode active material of the present invention has high specific capacitance, high magnification, and flexible electrode good mechanical performance, being prepared into ultracapacitor has good capacitive character.The invention belongs to technical field of nano material.
Description
Technical field
The present invention relates to a kind of bacteria cellulose graphene paper load nickel hydroxide flexible electrode material preparation method and
It is applied.
Background technology
Graphene assigns its higher theoretical specific surface area and ultrafast electron transfer because of its unique two-dimensional layered structure
Rate, allows its electrode material as ultracapacitor.Ultracapacitor is close with of a relatively high power density and energy
Degree, compensate for the low deficiency low with cell power density of traditional capacitor energy density, is a kind of new type of energy storage device.Super electricity
The performance of container depends primarily upon its electrode material.As the demand to high-performance super capacitor flexibility is increasingly urgent, flexible, tool
The electronic device for having Bending Stability has become the important directions of current energy storage area research.The metal oxide or hydrogen-oxygen of early stage
In the preparation process of compound electrode material, addition binding agent etc. is generally required, hinders fully connecing for electrolyte and active material
Touch, add internal resistance of electrode etc..
The content of the invention
The present invention is to solve existing method prepare conducting membrane material specific capacitance is low and high rate performance and mechanical property
Can be poor the problem of, there is provided a kind of bacteria cellulose graphene paper loads the preparation method of nickel hydroxide flexible electrode material and its answers
With.
A kind of preparation method of bacteria cellulose graphene paper load nickel hydroxide flexible electrode material of the present invention, by as follows
Step carries out:
First, bacteria cellulose is soaked into supersound washing in deionized water, disperses in deionized water, to be then transferred into even
Pulp grinder high speed stirs, and obtains bacteria cellulose slurry;By acidifying graphite alkene ultrasonic disperse in deionized water, acidifying stone is obtained
Black alkene dispersion liquid;
2nd, bacteria cellulose slurry is filtered by vacuum and formed a film, then added acidifying graphite alkene dispersion liquid and continue to filter film forming,
It is placed in vacuum drying chamber and is dried again, bacteria cellulose graphene paper is made;
3rd, nickel salt and ammonium salt are dissolved in distilled water, bacteria cellulose graphene paper is immersed in nickel salt solution, added
Ammonium hydroxide, is transferred in reaction kettle after mixing, heating, and bacteria cellulose graphene paper load nickel hydroxide flexible electrode is made
Material;
The mass ratio of bacteria cellulose and acidifying graphite alkene is (3~30) wherein in bacteria cellulose graphene paper:1;Step
The molar ratio of nickel salt and ammonium salt is (0.2~10) in rapid three:1;The ratio of nickel salt and ammonium hydroxide is 1mmol:(0.5~5ml).
Beneficial effects of the present invention:
(1) bacteria cellulose cost is low, and aboundresources is environmental-friendly, has hyperfine net structure and excellent mechanics
Performance, and study and have shown that the carbon material such as bacteria cellulose and graphene has extraordinary combination power.Using its feature,
Preparing bacteria cellulose graphene paper makes materials serve act synergistically, and remains the excellent mechanical property and stone of flexible material
The excellent electric conductivity of black alkene.
Transition group metallic oxide and hydroxide can produce good fake capacitance.The oxide and its hydroxide of nickel
It is that one kind is cheap, height ratio capacity, effective electrode material.But the shortcomings of its electric conductivity is not high limits its application, and graphene
The advantages of can by chance compensate its defect, therefore, nickel hydroxide and graphene it is compound after, performance obtains larger improvement and carries
It is high.
Bacteria cellulose aboundresources, of low cost, nickel hydroxide specific capacitance is high, and graphene has excellent electric conductivity.
Using the synergistic effect of material, high specific capacitance and the flexible material of mechanical property are prepared for, applied to ultracapacitor;
(2) by the way of hydrothermal growth, the material of preparation has high high rate performance;
(3) preparation process is simple, and the prices of raw materials are cheap;
(4) being directly used as electrode of super capacitor has good capacitive character.
Brief description of the drawings
The bacteria cellulose graphene paper stereoscan photograph that Fig. 1 is obtained by embodiment 1;
The scanning electron microscope for the bacteria cellulose graphene paper load nickel hydroxide flexible electrode that Fig. 2 is obtained by embodiment 1
Photo;
The work prepared with bacteria cellulose graphene paper load nickel hydroxide flexible electrode that Fig. 3 is obtained by embodiment 1
Make the cyclic voltammetry curve under different scanning speed of the electrode in 6M potassium hydroxide electrolytes;Wherein a is 30mV/s, and b is
100mV/s, c 200mV/s;
The work prepared with bacteria cellulose graphene paper load nickel hydroxide flexible electrode that Fig. 4 is obtained by embodiment 2
Make the cyclic voltammetry curve under different scanning speed of the electrode in 6M potassium hydroxide electrolytes;Wherein a is 30mV/s, and b is
80mV/s, c 150mV/s.
Embodiment
Embodiment one:A kind of bacteria cellulose graphene paper load nickel hydroxide flexible electrode material of present embodiment
The preparation method of material, carries out as follows:
First, bacteria cellulose is soaked into supersound washing in deionized water, disperses in deionized water, to be then transferred into even
Pulp grinder high speed stirs, and obtains bacteria cellulose slurry;By acidifying graphite alkene ultrasonic disperse in deionized water, acidifying stone is obtained
Black alkene dispersion liquid;
2nd, bacteria cellulose slurry is filtered by vacuum and formed a film, then added acidifying graphite alkene dispersion liquid and continue to filter film forming,
It is placed in vacuum drying chamber and is dried again, bacteria cellulose graphene paper is made;
3rd, nickel salt and ammonium salt are dissolved in distilled water, obtain mixed solution;Bacteria cellulose graphene paper is immersed in mixed
Close in solution, add ammonium hydroxide, be transferred to after mixing in reaction kettle, heat, bacteria cellulose graphene paper load hydrogen is made
Nickel oxide flexible electrode material;
The mass ratio of bacteria cellulose and acidifying graphite alkene is (3~30) wherein in bacteria cellulose graphene paper:1;Step
The molar ratio of nickel salt and ammonium salt is (0.2~10) in rapid three:1;The ratio of nickel salt and ammonium hydroxide is 1mmol:(0.5~5ml).
Beneficial effects of the present invention:
(1) bacteria cellulose cost is low, and aboundresources is environmental-friendly, has hyperfine net structure and excellent mechanics
Performance, and study and have shown that the carbon material such as bacteria cellulose and graphene has extraordinary combination power.Using its feature,
Preparing bacteria cellulose graphene paper makes materials serve act synergistically, and remains the excellent mechanical property and stone of flexible material
The excellent electric conductivity of black alkene.
Transition group metallic oxide and hydroxide can produce good fake capacitance.The oxide and its hydroxide of nickel
It is that one kind is cheap, height ratio capacity, effective electrode material.But the shortcomings of its electric conductivity is not high limits its application, and graphene
The advantages of can by chance compensate its defect, therefore, nickel hydroxide and graphene it is compound after, performance obtains larger improvement and carries
It is high.
Bacteria cellulose aboundresources, of low cost, nickel hydroxide specific capacitance is high, and graphene has excellent electric conductivity.
Using the synergistic effect of material, high specific capacitance and the flexible material of mechanical property are prepared for, applied to ultracapacitor;
(2) by the way of hydrothermal growth, the material of preparation has high high rate performance;
(3) preparation process is simple, and the prices of raw materials are cheap;
(4) being directly used as electrode of super capacitor has good capacitive character.
Embodiment two:The present embodiment is different from the first embodiment in that:The ultrasonic power is
1000w, frequency are 30KHz.It is other identical with embodiment one.
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.
Embodiment four:Unlike one of present embodiment and embodiment one to three:Described in step 1
The speed of high-speed stirred be 8000~15000r/min, 3~30min of mixing time.Other and embodiment one to three
One of it is identical.
Embodiment five:Unlike one of present embodiment and embodiment one to four:Described in step 2
Nickel salt be nickel chloride, nickel sulfate or nickel nitrate;Ammonium salt is ammonium nitrate or ammonium fluoride.It is other with embodiment one to four it
One is identical.
Embodiment six:Unlike one of present embodiment and embodiment one to five:Described in step 2
Reaction kettle be anticorrosion high temperature high voltage resistant reaction kettle.It is other identical with one of embodiment one to five.
Embodiment seven:Unlike one of present embodiment and embodiment one to six:Institute in step 3
The ammonium hydroxide stated is the ammonium hydroxide that mass percentage is 25%.It is other identical with one of embodiment one to six.
Embodiment eight:Unlike one of present embodiment and embodiment one to seven:Add in step 3
The temperature of heat is 70~150 DEG C, and the reaction time is 3h~16h.It is other identical with one of embodiment one to seven.
Embodiment nine:Unlike one of present embodiment and embodiment one to eight:Described in step 3
Bacteria cellulose graphene paper media area and the ratio of nickel chloride be 1cm2:(0.1-10)mmol.Other and specific implementation
Mode is to one of eight identical.
Embodiment ten:Unlike one of present embodiment and embodiment one to nine:Described in step 3
Bacteria cellulose graphene paper media area and the ratio of nickel sulfate be 1cm2:(0.1-10)mmol.Other and specific implementation
One of mode one to nine is identical.
Embodiment 11:Unlike one of present embodiment and embodiment one to ten:Step 3 institute
The bacteria cellulose graphene paper media area and the ratio of nickel nitrate stated are 1cm2:(0.1-10)mmol.Other and specific reality
It is identical to apply one of mode one to ten.
Embodiment 12:Present embodiment bacteria cellulose graphene paper loads nickel hydroxide flexible electrode material
Application refer to be applied to ultracapacitor in.
Embodiment 13:Present embodiment is unlike embodiment 12:The flexible electrode material
It is applied to as positive electrode in ultracapacitor.It is other identical with embodiment 12.
Beneficial effects of the present invention are verified by following embodiments:
Embodiment 1:A kind of preparation of bacteria cellulose graphene paper load nickel hydroxide flexible electrode material of the present embodiment
Method, carries out as follows:
First, 4g bacteria celluloses are soaked into supersound washing in deionized water, disperses in deionized water, to be then transferred into
10min is stirred with the speed of 12000r/min in refiner, obtains bacteria cellulose slurry;By 8mg acidifying graphites alkene ultrasound point
Dissipate in deionized water, obtain acidifying graphite alkene dispersion liquid;
2nd, bacteria cellulose slurry is filtered by vacuum and formed a film, then added acidifying graphite alkene dispersion liquid and continue to filter film forming,
It is placed in vacuum drying chamber and is dried again, bacteria cellulose graphene paper is made;
3rd, 10mmol nickel sulfates are weighed and 4mmol ammonium nitrate is dissolved in 20ml distilled water, obtain mixed solution;By 8cm2
Bacteria cellulose graphene paper is immersed in mixed solution, is added the ammonium hydroxide of 15mL25wt%, is transferred to liner after mixing
In tetrafluoro high-temperature high-pressure reaction kettle, 10h is heated at 100 DEG C, it is flexible to obtain bacteria cellulose graphene paper load nickel hydroxide
Electrode material;
Obtained bacteria cellulose graphene paper load nickel hydroxide flexible electrode is cut into 1cm × 2cm rectangles, directly
Connect and be used as ultracapacitor working electrode, platinized platinum is used as to electrode, using mercury/mercuric oxide electrode as reference electrode, tests flexible electrical
The capacitance characteristic of pole material.Test sample is labeled as BCGO-NI-1.
The flexible electrode material for inventing obtained is tested.Fig. 1 is bacteria cellulose graphene paper scanning electron microscopic picture,
Graphene uniform is distributed on bacteria cellulose as seen from the figure;As seen from Figure 2 in bacteria cellulose graphene paper
Nickel hydroxide nano material in even load, by stratiform nickel hydroxide regular array into cellular;Show that difference sweeps speed in Fig. 3
The scanning potential window of nickel hydroxide be 0.1~0.5V.With obvious redox peaks.With the increase of sweep speed,
Response current increase, the total number can reach 200mV/s, it is shown that preferable high rate performance.
Embodiment 2:A kind of preparation of bacteria cellulose graphene paper load nickel hydroxide flexible electrode material of the present embodiment
Method, carries out as follows:
First, 5g bacteria celluloses are soaked into supersound washing in deionized water, disperses in deionized water, to be then transferred into
10min is stirred with the speed of 12000r/min in refiner, obtains bacteria cellulose slurry;By 15mg acidifying graphites alkene ultrasound point
Dissipate in deionized water, obtain acidifying graphite alkene dispersion liquid;
2nd, bacteria cellulose slurry is filtered by vacuum and formed a film, then added acidifying graphite alkene dispersion liquid and continue to filter film forming,
It is placed in vacuum drying chamber and is dried again, bacteria cellulose graphene paper is made;
3rd, 12mmol nickel sulfates are weighed and 6mmol ammonium nitrate is dissolved in 20ml distilled water, obtain mixed solution;By 8cm2
Bacteria cellulose graphene paper is immersed in mixed solution, adds the ammonium hydroxide of 8mL25wt%, is transferred to liner four after mixing
In fluorine high-temperature high-pressure reaction kettle, 6h is heated at 95 DEG C, obtains bacteria cellulose graphene paper load nickel hydroxide flexible electrode
Material;
Obtained bacteria cellulose graphene paper load nickel hydroxide flexible electrode is cut into 1cm × 2cm rectangles, directly
Connect and be used as ultracapacitor working electrode, platinized platinum is used as to electrode, using mercury/mercuric oxide electrode as reference electrode, tests flexible electrical
The capacitance characteristic of pole material electrodes material.Test sample is labeled as BCGO-NI-2.The scanning of nickel hydroxide as seen from Figure 4
Potential window is 0.1~0.5V.Cyclic voltammetry curve has obvious redox peaks.With the increase of sweep speed, response
Electric current increase, sweep speed can reach 150mV/s, and the deviation of very little occurs for oxidation peak and reduction peak value, it is shown that
Good high rate performance.
1~2 nickel hydroxide specific capacitance of embodiment is high, and graphene is had excellent electric conductivity, loaded with bacteria cellulose
Graphene be bottom, grow nickel hydroxide, not only maintained high specific capacitance, but also add high rate performance so that material can carry
For heavy-current discharge, meanwhile, base material has excellent mechanical property;Flexible electrode material has applied to ultracapacitor
Good capacitive character.
Claims (9)
- A kind of 1. preparation method of bacteria cellulose graphene paper load nickel hydroxide flexible electrode material, it is characterised in that the party Method carries out as follows:First, bacteria cellulose is soaked into supersound washing in deionized water, disperses in deionized water, to be then transferred into refiner High speed stirs, and obtains bacteria cellulose slurry;By acidifying graphite alkene ultrasonic disperse in deionized water, acidifying graphite alkene is obtained Dispersion liquid;2nd, bacteria cellulose slurry is filtered by vacuum and formed a film, then added acidifying graphite alkene dispersion liquid and continue to filter film forming, then put It is dried in vacuum drying chamber, bacteria cellulose graphene paper is made;3rd, nickel salt and ammonium salt are dissolved in distilled water, bacteria cellulose graphene paper is immersed in nickel salt solution, add ammonia Water, is transferred in reaction kettle after mixing, heating, and bacteria cellulose graphene paper load nickel hydroxide flexible electrode material is made Material;The mass ratio of bacteria cellulose and acidifying graphite alkene is (3~30) wherein in bacteria cellulose graphene paper:1;Step 3 The molar ratio of middle nickel salt and ammonium salt is (0.2~10):1;The ratio of nickel salt and ammonium hydroxide is 1mmol:(0.5~5ml);Step 2 institute The nickel salt stated is nickel chloride, nickel sulfate, nickel acetate or nickel nitrate;Ammonium salt is ammonium nitrate or ammonium fluoride.
- A kind of 2. preparation of bacteria cellulose graphene paper load nickel hydroxide flexible electrode material according to claim 1 Method, it is characterised in that the ultrasonic frequency is 1000w for ultrasonic power, and frequency is 30KHz.
- A kind of 3. preparation of bacteria cellulose graphene paper load nickel hydroxide flexible electrode material according to claim 1 Method, it is characterised in that the condition of the supersound washing described in step 1 is 1~10h of ultrasonic time.
- A kind of 4. preparation of bacteria cellulose graphene paper load nickel hydroxide flexible electrode material according to claim 1 Method, it is characterised in that the speed of the high-speed stirred described in step 1 is 8000~15000r/min, 3~30min of mixing time.
- A kind of 5. preparation of bacteria cellulose graphene paper load nickel hydroxide flexible electrode material according to claim 1 Method, it is characterised in that the reaction kettle described in step 3 is anticorrosion high temperature high voltage resistant reaction kettle.
- A kind of 6. preparation of bacteria cellulose graphene paper load nickel hydroxide flexible electrode material according to claim 1 Method, it is characterised in that the temperature heated in step 3 is 70~150 DEG C, and the reaction time is 3h~16h.
- A kind of 7. preparation of bacteria cellulose graphene paper load nickel hydroxide flexible electrode material according to claim 1 Method, it is characterised in that the ammonium hydroxide described in step 3 is the ammonium hydroxide that mass percentage is 25%.
- 8. the bacteria cellulose graphene paper load nickel hydroxide flexible electrode material that preparation method as claimed in claim 1 obtains The application of material, it is characterised in that the flexible electrode material is applied in ultracapacitor.
- 9. a kind of bacteria cellulose graphene paper load nickel hydroxide flexible electrode material according to claim 8 is answered With, it is characterised in that the flexible electrode material is applied to ultracapacitor as positive electrode.
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CN108294741B (en) * | 2017-01-12 | 2023-01-20 | 国家纳米科学中心 | Miniature flexible bioelectrode array and preparation method thereof |
CN108538647A (en) * | 2018-05-07 | 2018-09-14 | 中国科学技术大学 | The preparation method of membrane electrode |
CN109243838B (en) * | 2018-09-25 | 2022-08-30 | 浙江衡远新能源科技有限公司 | Nickel-cobalt double hydroxide electrode material and preparation method thereof |
CN110212156B (en) * | 2019-05-31 | 2020-12-04 | 南方科技大学 | Flexible electrode, preparation method and flexible lithium ion battery |
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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CN105175761B (en) * | 2015-09-08 | 2018-06-22 | 哈尔滨工业大学 | A kind of preparation method and applications of bacteria cellulose/polyaniline/graphene film material |
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