CN105428091A - Preparation method for bacterial cellulose graphene paper loaded nickel hydroxide flexible electrode material and application thereof - Google Patents
Preparation method for bacterial cellulose graphene paper loaded nickel hydroxide flexible electrode material and application thereof Download PDFInfo
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- CN105428091A CN105428091A CN201510990854.3A CN201510990854A CN105428091A CN 105428091 A CN105428091 A CN 105428091A CN 201510990854 A CN201510990854 A CN 201510990854A CN 105428091 A CN105428091 A CN 105428091A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 69
- 239000007772 electrode material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 title abstract description 14
- 229920002749 Bacterial cellulose Polymers 0.000 title abstract 7
- 239000005016 bacterial cellulose Substances 0.000 title abstract 7
- 150000002815 nickel Chemical class 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 3
- 229920002678 cellulose Polymers 0.000 claims description 75
- 239000001913 cellulose Substances 0.000 claims description 75
- 241000894006 Bacteria Species 0.000 claims description 73
- -1 hydrogen nickel oxide Chemical class 0.000 claims description 48
- 229910052739 hydrogen Inorganic materials 0.000 claims description 28
- 239000001257 hydrogen Substances 0.000 claims description 28
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 229910002804 graphite Inorganic materials 0.000 claims description 18
- 239000010439 graphite Substances 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 239000006185 dispersion Substances 0.000 claims description 15
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- 150000003863 ammonium salts Chemical class 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 5
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000003828 vacuum filtration Methods 0.000 claims description 5
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical group OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims 1
- 229940078494 nickel acetate Drugs 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 18
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000004513 sizing Methods 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 4
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229940101209 mercuric oxide Drugs 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910000474 mercury oxide Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 239000011149 active material Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/10—Multiple hybrid or EDL capacitors, e.g. arrays or modules
- H01G11/12—Stacked hybrid or EDL capacitors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/38—Carbon pastes or blends; Binders or additives therein
-
- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention relates to a preparation method for a bacterial cellulose graphene paper loaded nickel hydroxide flexible electrode and an application thereof, and relates to a preparation method for a flexible electrode material and an application thereof, aiming to solve the problem that a conducing film material prepared by an existing method has low specific capacitance and poor rate capability and mechanical property. The preparation method comprises the steps of preparing a bacterial cellulose sizing agent; and preparing bacterial cellulose graphene paper, preparing a reaction solution containing nickel salt, and soaking the bacterial cellulose graphene paper in the reaction solution containing the nickel salt to prepare the bacterial cellulose graphene paper loaded nickel hydroxide flexible electrode. The bacterial cellulose graphene paper loaded nickel hydroxide flexible electrode is applied to a supercapacitor. The electrode active material has high specific capacitance, high multiplying power, and good flexible electrode mechanical property, and the supercapacitor prepared by the electrode active material has good capacitive performance. The preparation method belongs to the technical field of nano materials.
Description
Technical field
The present invention relates to a kind of preparation method and application thereof of bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material.
Background technology
Graphene gives its higher theoretical specific surface area and ultrafast electron mobility because of the two-dimensional layered structure of its uniqueness, makes it can as the electrode material of ultracapacitor.Ultracapacitor has relatively high power density and energy density, and compensate for the deficiency that traditional capacitor energy density is low and cell power density is low, is a kind of novel energy-storing device.The performance of ultracapacitor depends primarily on its electrode material.Along with the important directions that demand is day by day urgent, flexible, electronic device that is that have Bending Stability has become current energy storage area research to high-performance super capacitor flexibility.In the preparation process of early stage metal oxide or hydroxide electrode material, often need to add binding agent etc., hinder fully contacting of electrolyte and active material, add the internal resistance etc. of electrode.
Summary of the invention
The present invention is the problem that will solve conducting membrane material specific capacitance prepared by existing method low and high rate performance and poor mechanical property, provides a kind of preparation method and application thereof of bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material.
The preparation method of a kind of bacteria cellulose graphene paper of the present invention load hydrogen nickel oxide flexible electrode material, carries out as follows:
One, bacteria cellulose is immersed in deionized water for ultrasonic washing, dispersion in deionized water, is then transferred to refiner high speed and is stirred, obtain bacteria cellulose slurry; By acidifying graphite alkene ultrasonic disperse in deionized water, acidifying graphite alkene dispersion liquid is obtained;
Two, by bacteria cellulose slurry vacuum filtration film forming, then add acidifying graphite alkene dispersion liquid and continue suction filtration film forming, then be placed in vacuum drying chamber and carry out drying, make bacteria cellulose graphene paper;
Three, be dissolved in distilled water by nickel salt and ammonium salt, be immersed in nickel salt solution, add ammoniacal liquor by bacteria cellulose graphene paper, transfer in reactor after mixing, heating, makes bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material;
Wherein in bacteria cellulose graphene paper, the mass ratio of bacteria cellulose and acidifying graphite alkene is (3 ~ 30): 1; In step 3, the mol ratio of nickel salt and ammonium salt is (0.2 ~ 10): 1; The ratio of nickel salt and ammoniacal liquor is 1mmol:(0.5 ~ 5ml).
Beneficial effect of the present invention:
(1) bacteria cellulose cost is low, aboundresources, environmental friendliness, has the mechanical property of hyperfine network structure and excellence, and research has shown that the material with carbon element such as bacteria cellulose and Graphene has extraordinary adhesion.Utilize its feature, prepare bacteria cellulose graphene paper and make materials serve synergy, remain the mechanical property of the excellence of flexible material and the electric conductivity of Graphene excellence.
Transition group metallic oxide and hydroxide can produce good fake capacitance.The oxide of nickel and hydroxide thereof are a kind of cheap, height ratio capacity, effective electrode material.But the shortcomings such as its conductivity is not high limit its application, and the advantage of Graphene by chance can compensate its defect, therefore, after nickel hydroxide and Graphene compound, performance obtains larger improving.
Bacteria cellulose aboundresources, with low cost, nickel hydroxide ratio capacitance is high, and Graphene has excellent conductivity.Utilize the synergy of material, prepared the flexible material of high specific capacitance and mechanical property, be applied to ultracapacitor;
(2) adopt the mode of hydrothermal growth, the material of preparation has high high rate performance;
(3) preparation technology is simple, and the prices of raw and semifnished materials are cheap;
(4) be directly used as electrode of super capacitor and there is good capacitive character.
Accompanying drawing explanation
The bacteria cellulose graphene paper stereoscan photograph that Fig. 1 obtains for embodiment 1;
The stereoscan photograph of the bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode that Fig. 2 obtains for embodiment 1;
Cyclic voltammetry curve under the different scanning speed of the work electrode prepared with bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode that Fig. 3 obtains for embodiment 1 in 6M potassium hydroxide electrolyte; Wherein a is 30mV/s, b be 100mV/s, c is 200mV/s;
Cyclic voltammetry curve under the different scanning speed of the work electrode prepared with bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode that Fig. 4 obtains for embodiment 2 in 6M potassium hydroxide electrolyte; Wherein a is 30mV/s, b be 80mV/s, c is 150mV/s.
Embodiment
Embodiment one: the preparation method of a kind of bacteria cellulose graphene paper of present embodiment load hydrogen nickel oxide flexible electrode material, carry out as follows:
One, bacteria cellulose is immersed in deionized water for ultrasonic washing, dispersion in deionized water, is then transferred to refiner high speed and is stirred, obtain bacteria cellulose slurry; By acidifying graphite alkene ultrasonic disperse in deionized water, acidifying graphite alkene dispersion liquid is obtained;
Two, by bacteria cellulose slurry vacuum filtration film forming, then add acidifying graphite alkene dispersion liquid and continue suction filtration film forming, then be placed in vacuum drying chamber and carry out drying, make bacteria cellulose graphene paper;
Three, nickel salt and ammonium salt are dissolved in distilled water, obtain mixed solution; Be immersed in mixed solution by bacteria cellulose graphene paper, add ammoniacal liquor, transfer in reactor after mixing, heating, makes bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material;
Wherein in bacteria cellulose graphene paper, the mass ratio of bacteria cellulose and acidifying graphite alkene is (3 ~ 30): 1; In step 3, the mol ratio of nickel salt and ammonium salt is (0.2 ~ 10): 1; The ratio of nickel salt and ammoniacal liquor is 1mmol:(0.5 ~ 5ml).
Beneficial effect of the present invention:
(1) bacteria cellulose cost is low, aboundresources, environmental friendliness, has the mechanical property of hyperfine network structure and excellence, and research has shown that the material with carbon element such as bacteria cellulose and Graphene has extraordinary adhesion.Utilize its feature, prepare bacteria cellulose graphene paper and make materials serve synergy, remain the mechanical property of the excellence of flexible material and the electric conductivity of Graphene excellence.
Transition group metallic oxide and hydroxide can produce good fake capacitance.The oxide of nickel and hydroxide thereof are a kind of cheap, height ratio capacity, effective electrode material.But the shortcomings such as its conductivity is not high limit its application, and the advantage of Graphene by chance can compensate its defect, therefore, after nickel hydroxide and Graphene compound, performance obtains larger improving.
Bacteria cellulose aboundresources, with low cost, nickel hydroxide ratio capacitance is high, and Graphene has excellent conductivity.Utilize the synergy of material, prepared the flexible material of high specific capacitance and mechanical property, be applied to ultracapacitor;
(2) adopt the mode of hydrothermal growth, the material of preparation has high high rate performance;
(3) preparation technology is simple, and the prices of raw and semifnished materials are cheap;
(4) be directly used as electrode of super capacitor and there is good capacitive character.
Embodiment two: present embodiment and embodiment one unlike: described ultrasonic power is 1000w, and frequency is 30KHz.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two unlike: the condition of the supersound washing described in step one is ultrasonic time 1 ~ 10h.Other is identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three unlike: the speed of the high-speed stirred described in step one is 8000 ~ 15000r/min, mixing time 3 ~ 30min.Other is identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four unlike: the nickel salt described in step 2 is nickel chloride, nickelous sulfate or nickel nitrate; Ammonium salt is ammonium nitrate or ammonium fluoride.Other is identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five unlike: the reactor described in step 2 is anticorrosion high temperature high voltage resistant reactor.Other is identical with one of embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six unlike: the ammoniacal liquor described in step 3 to be mass percentage be 25% ammoniacal liquor.Other is identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven unlike: the temperature heated in step 3 is 70 ~ 150 DEG C, and the reaction time is 3h ~ 16h.Other is identical with one of embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight unlike: the bacteria cellulose graphene paper media area described in step 3 and the ratio of nickel chloride are 1cm
2: (0.1-10) mmol.Other is identical with one of embodiment to eight.
Embodiment ten: one of present embodiment and embodiment one to nine unlike: the bacteria cellulose graphene paper media area described in step 3 and the ratio of nickelous sulfate are 1cm
2: (0.1-10) mmol.Other is identical with one of embodiment one to nine.
Embodiment 11: one of present embodiment and embodiment one to ten unlike: the bacteria cellulose graphene paper media area described in step 3 and the ratio of nickel nitrate are 1cm
2: (0.1-10) mmol.Other is identical with one of embodiment one to ten.
Embodiment 12: the application of present embodiment bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material refers to and is applied in ultracapacitor.
Embodiment 13: present embodiment and embodiment 12 unlike: this flexible electrode material is applied in ultracapacitor as positive electrode.Other is identical with embodiment 12.
Beneficial effect of the present invention is verified by following examples:
Embodiment 1: the preparation method of a kind of bacteria cellulose graphene paper of the present embodiment load hydrogen nickel oxide flexible electrode material, carry out as follows:
One, 4g bacteria cellulose is immersed in deionized water for ultrasonic washing, dispersion in deionized water, is then transferred in refiner and is stirred 10min with the speed of 12000r/min, obtain bacteria cellulose slurry; By 8mg acidifying graphite alkene ultrasonic disperse in deionized water, acidifying graphite alkene dispersion liquid is obtained;
Two, by bacteria cellulose slurry vacuum filtration film forming, then add acidifying graphite alkene dispersion liquid and continue suction filtration film forming, then be placed in vacuum drying chamber and carry out drying, make bacteria cellulose graphene paper;
Three, take 10mmol nickelous sulfate and 4mmol ammonium nitrate is dissolved in 20ml distilled water, obtain mixed solution; By 8cm
2bacteria cellulose graphene paper is immersed in mixed solution, add the ammoniacal liquor of 15mL25wt%, transfer to after mixing in liner tetrafluoro high-temperature high-pressure reaction kettle, at 100 DEG C, heat 10h, obtain bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material;
Obtained bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode is cut into 1cm × 2cm rectangle, directly be used as ultracapacitor work electrode, platinized platinum, as to electrode, with mercury/mercuric oxide electrode for reference electrode, tests the capacitance characteristic of flexible electrode material.Test specimens product are labeled as BCGO-NI-1.
Test inventing the flexible electrode material obtained.Fig. 1 is bacteria cellulose graphene paper scanning electron microscopic picture, and graphene uniform is distributed on bacteria cellulose as seen from the figure; Nickel hydroxide nano material in uniform load in bacteria cellulose graphene paper, becomes cellular by stratiform nickel hydroxide regular array as seen from Figure 2; Demonstrating the scanning potential window of nickel hydroxide that difference sweeps speed in Fig. 3 is 0.1 ~ 0.5V.There is obvious redox peak.Along with the increase of sweep speed, response current increases, and the total number can reach 200mV/s, shows good high rate performance.
Embodiment 2: the preparation method of a kind of bacteria cellulose graphene paper of the present embodiment load hydrogen nickel oxide flexible electrode material, carry out as follows:
One, 5g bacteria cellulose is immersed in deionized water for ultrasonic washing, dispersion in deionized water, is then transferred in refiner and is stirred 10min with the speed of 12000r/min, obtain bacteria cellulose slurry; By 15mg acidifying graphite alkene ultrasonic disperse in deionized water, acidifying graphite alkene dispersion liquid is obtained;
Two, by bacteria cellulose slurry vacuum filtration film forming, then add acidifying graphite alkene dispersion liquid and continue suction filtration film forming, then be placed in vacuum drying chamber and carry out drying, make bacteria cellulose graphene paper;
Three, take 12mmol nickelous sulfate and 6mmol ammonium nitrate is dissolved in 20ml distilled water, obtain mixed solution; By 8cm
2bacteria cellulose graphene paper is immersed in mixed solution, adds the ammoniacal liquor of 8mL25wt%, transfers in liner tetrafluoro high-temperature high-pressure reaction kettle, at 95 DEG C, heat 6h after mixing, and obtains bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material;
Obtained bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode is cut into 1cm × 2cm rectangle, directly be used as ultracapacitor work electrode, platinized platinum, as to electrode, with mercury/mercuric oxide electrode for reference electrode, tests the capacitance characteristic of flexible electrode material electrode material.Test specimens product are labeled as BCGO-NI-2.The scanning potential window of nickel hydroxide is 0.1 ~ 0.5V as seen from Figure 4.Cyclic voltammetry curve has obvious redox peak.Along with the increase of sweep speed, response current increases, and sweep speed can reach 150mV/s, and very little departing from occurs for oxidation peak and reduction peak value, shows good high rate performance.
Embodiment 1 ~ 2 nickel hydroxide specific capacitance is high, Graphene has excellent conductivity, with the Graphene of bacteria cellulose load the end of for, growth nickel hydroxide, both maintain high ratio capacitance, turn increased high rate performance, and make material to provide heavy-current discharge, meanwhile, base material has excellent mechanical property; Flexible electrode material is applied to ultracapacitor and has good capacitive character.
Claims (10)
1. a preparation method for bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material, is characterized in that the method is carried out as follows:
One, bacteria cellulose is immersed in deionized water for ultrasonic washing, dispersion in deionized water, is then transferred to refiner high speed and is stirred, obtain bacteria cellulose slurry; By acidifying graphite alkene ultrasonic disperse in deionized water, acidifying graphite alkene dispersion liquid is obtained;
Two, by bacteria cellulose slurry vacuum filtration film forming, then add acidifying graphite alkene dispersion liquid and continue suction filtration film forming, then be placed in vacuum drying chamber and carry out drying, make bacteria cellulose graphene paper;
Three, be dissolved in distilled water by nickel salt and ammonium salt, be immersed in nickel salt solution, add ammoniacal liquor by bacteria cellulose graphene paper, transfer in reactor after mixing, heating, makes bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material;
Wherein in bacteria cellulose graphene paper, the mass ratio of bacteria cellulose and acidifying graphite alkene is (3 ~ 30): 1; In step 3, the mol ratio of nickel salt and ammonium salt is (0.2 ~ 10): 1; The ratio of nickel salt and ammoniacal liquor is 1mmol:(0.5 ~ 5ml).
2. the preparation method of a kind of bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material according to claim 1, it is characterized in that described ultrasonic frequency be ultrasonic power is 1000w, frequency is 30KHz.
3. the preparation method of a kind of bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material according to claim 1, is characterized in that the condition of the supersound washing described in step one is ultrasonic time 1 ~ 10h.
4. the preparation method of a kind of bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material according to claim 1, is characterized in that the speed of the high-speed stirred described in step one is 8000 ~ 15000r/min, mixing time 3 ~ 30min.
5. the preparation method of a kind of bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material according to claim 1, is characterized in that the nickel salt described in step 2 is nickel chloride, nickelous sulfate, nickel acetate or nickel nitrate; Ammonium salt is ammonium nitrate or ammonium fluoride.
6. the preparation method of a kind of bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material according to claim 1, is characterized in that the reactor described in step 3 is anticorrosion high temperature high voltage resistant reactor.
7. the preparation method of a kind of bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material according to claim 1, it is characterized in that the temperature heated in step 3 is 70 ~ 150 DEG C, the reaction time is 3h ~ 16h.
8. the preparation method of a kind of bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material according to claim 1, is characterized in that the ammoniacal liquor described in step 3 to be mass percentage is the ammoniacal liquor of 25%.
9. the application of bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material that obtains of preparation method as claimed in claim 1, is characterized in that this flexible electrode material is applied in ultracapacitor.
10. the application of a kind of bacteria cellulose graphene paper load hydrogen nickel oxide flexible electrode material according to claim 9, is characterized in that this flexible electrode material is applied to ultracapacitor as positive electrode.
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Cited By (5)
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CN108538647A (en) * | 2018-05-07 | 2018-09-14 | 中国科学技术大学 | The preparation method of membrane electrode |
CN109243838A (en) * | 2018-09-25 | 2019-01-18 | 浙江衡远新能源科技有限公司 | A kind of nickel cobalt double-hydroxide electrode material and preparation method thereof |
CN110212156A (en) * | 2019-05-31 | 2019-09-06 | 南方科技大学 | Flexible electrode and preparation method and flexible lithium ion battery |
CN114743800A (en) * | 2022-04-25 | 2022-07-12 | 武夷学院 | Preparation method of polyacrylic acid/graphene-based flexible electrode material |
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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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