CN106449182A - Preparation method of polyaniline/graphene/tin dioxide composite material - Google Patents
Preparation method of polyaniline/graphene/tin dioxide composite material Download PDFInfo
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- CN106449182A CN106449182A CN201611068285.8A CN201611068285A CN106449182A CN 106449182 A CN106449182 A CN 106449182A CN 201611068285 A CN201611068285 A CN 201611068285A CN 106449182 A CN106449182 A CN 106449182A
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- polyaniline
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- 229920000767 polyaniline Polymers 0.000 title claims abstract description 77
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 71
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 66
- 239000000243 solution Substances 0.000 claims description 33
- 239000000463 material Substances 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 16
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 239000007772 electrode material Substances 0.000 abstract description 7
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 6
- 239000003990 capacitor Substances 0.000 abstract description 4
- 239000000084 colloidal system Substances 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 2
- 230000001351 cycling effect Effects 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 235000011150 stannous chloride Nutrition 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- -1 graphite alkene Chemical class 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
Classifications
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- 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
- H01G11/22—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
-
- 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
- H01G11/46—Metal oxides
-
- 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
- H01G11/48—Conductive polymers
-
- 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)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Manufacturing & Machinery (AREA)
Abstract
The invention discloses a preparation method of a polyaniline/graphene/tin dioxide composite material. Three-dimensional polyaniline/graphene oxide complex colloid is prepared by adopting a hydrothermal method and graphene oxide in the prepared colloid is reduced by utilizing SnCl2; and tin dioxide particles are deposited on the three-dimensional polyaniline/graphene oxide complex by adopting the hydrothermal method, so as to prepare the three-dimensional porous net-shaped polyaniline/graphene/tin dioxide composite material. The method disclosed by the invention has a simple, reliable and green and environment-friendly preparation process, and the prepared polyaniline/graphene/tin dioxide composite material has a regular space structure, good dispersibility, high energy density and power density and an excellent cycling performance, is an ideal super-capacitor electrode material and is particularly suitable for industrial production.
Description
Technical field
The invention belongs to novel energy field of material technology, particularly to one kind, ultracapacitor is prepared with hydro-thermal method and use three
The method of dimension holey polyaniline/Graphene/tin dioxide composite material.
Background technology
Ultracapacitor due to there is high-energy-density and power density and outstanding cycle performance etc. and as quick
Primary selection with high-power energy stocking system field.Electrode material in ultracapacitor rises to the performance of ultracapacitor
To vital effect, therefore, realizing the wide variety of most important thing of ultracapacitor is to prepare and develop high performance electricity
Pole material.
Conducting polymer, transition metal oxide and material with carbon element are three kinds of materials that electrode material for super capacitor is commonly used.
Overcome the shortcomings of that using the advantageous characteristic of these three materials homogenous material has that to prepare combination electrode material be super electricity at present
One of focus of container electrode investigation of materials.Ding etc. synthesizes SnO by dip coating2@PANI and then and redox graphene
It is compounded to form the SnO of 3-D nano, structure2@PANI/rGO trielement composite material, this materials show very high reversible than electric capacity simultaneously
There is outstanding high rate performance and cycle performance（H. Ding, et al. Ternary SnO2@PANI/rGO
nanohybrids as excellent anode materials for lithium-ion batteries[J].
Electrochimica Acta, 2015, 157: 205-210.）.Nguyen etc. adopts two-step method synthesizing graphite alkene/nanometer
SnO2/ PANI material, this composite has high rate capability（V.H. Nguyen, et al. Ultrasmall SnO2
nanoparticle-intercalated graphene@polyaniline composites as an active
electrode material for supercapacitors in different electrolytes[J].
Synthetic Metals, 2015, 207: 110-115.）.Liu etc. synthesized by tin dioxide nano-particle, Graphene and
The composite of polyaniline composition simultaneously studies the performance of its positive electrode as high performance lithium ion battery.This composite
Nanostructured can effectively adjust the volumetric expansion during tin ash lithiumation, the nanoparticle in suppression cyclic process simultaneously
Reunite and there is outstanding cyclical stability.（H. Liu, et al. A reduced graphene oxide/SnO2/
polyaniline nanocomposite for the anode material of Li-ion batteries[J].
Solid State Ionics, 2016, 294: 6-14. ）.
Therefore high-performance super capacitor electrode material is prepared for it in electrochemical energy storage using simple synthetic technology
The application in field is significant.The present invention is with three-dimensional graphene oxide, SnCl2It is raw material with three-dimensional porous polyaniline,
Three-dimensional porous netted polyaniline/Graphene/tin dioxide composite material is prepared using hydro-thermal method.
Content of the invention
It is an object of the invention to provide a kind of preparation method of polyaniline/Graphene/tin dioxide composite material.
Thinking of the present invention：Three-dimensional polyaniline/graphene oxide composite colloids are prepared with hydro-thermal method, and uses SnCl2To system
Graphene oxide in standby colloid is reduced, and then adopts hydro-thermal method on three-dimensional polyaniline/graphene oxide complex
Face deposition stannic oxide particle prepares three-dimensional porous netted polyaniline/Graphene/tin dioxide composite material.
Concretely comprise the following steps：
(1) graphene oxide is dissolved in deionized water, ultrasonic 10 min preparation graphene oxide solution.
(2) add three-dimensional porous polyaniline in the graphene oxide solution being obtained to step (1), be sufficiently stirred for lower addition
SnCl2Solution and HI solution, are transferred in autoclave after supersound process 5 min, react 4 h, then cool down at 180 DEG C
Mixed solution is obtained to room temperature.
(3) add NaOH solution in the mixed solution being obtained to step (2), after supersound process 5 min, react at 180 DEG C
2 h, after naturally cooling to room temperature, products therefrom is washed with deionized and is dried to neutrality, that is, polyaniline/graphite is obtained
Alkene/tin dioxide composite material.
Described three-dimensional porous polyaniline is 0.1 ~ 4 with the mass ratio of graphene oxide:1；Described graphene oxide is with HI's
Mass ratio is 1:2.56；Described SnCl2Ratio with the amount of the material of NaOH is 1:4；Described tin ash and graphene oxide
Mass ratio is 0.1 ~ 2:1.
The inventive method preparation process is simple, reliability, environmental protection, and obtained polyaniline/Graphene/tin ash is multiple
Condensation material has regular space structure, good dispersibility, high-energy-density and power density, outstanding cycle performance, is
A kind of preferable electrode material for super capacitor, is especially suitable for industrialized production.
Brief description
Fig. 1 is the scanning electron microscope (SEM) photograph of the polyaniline/Graphene/tin dioxide composite material of preparation in the embodiment of the present invention 3.
Specific embodiment
Embodiment 1：
(1) 0.5g three-dimensional graphene oxide is dissolved in 100mL deionized water, it is molten that ultrasonic 10 min prepare graphene oxide
Liquid.
(2) add the three-dimensional porous polyaniline of 0.05g in the graphene oxide solution being obtained to step (1), be sufficiently stirred for down
Add SnCl2Solution（Containing 0.0629 g SnCl2）With the HI solution of 10 mL 1 M, it is transferred to high pressure after supersound process 5 min anti-
Answer in kettle, at 180 DEG C, react 4 h, be subsequently cooled to room temperature and mixed solution is obtained.
(3) add NaOH solution in the mixed solution being obtained to step (2)（Containing 0.0531 g NaOH）, supersound process 5
After min, at 180 DEG C, react 2 h, after naturally cooling to room temperature, products therefrom is washed with deionized to be done to neutrality
Dry, that is, polyaniline/Graphene/tin dioxide composite material is obtained.
Described three-dimensional porous polyaniline is 0.1 with the mass ratio of graphene oxide:1, described SnCl2With the material of NaOH
The ratio of amount is 1:4；Described tin ash is 0.1 with the mass ratio of graphene oxide:1.
Embodiment 2：
(1) 0.5g three-dimensional graphene oxide is dissolved in 100mL deionized water, it is molten that ultrasonic 10 min prepare graphene oxide
Liquid.
(2) add the three-dimensional porous polyaniline of 0.05g in the graphene oxide solution being obtained to step (1), be sufficiently stirred for down
Add SnCl2Solution（Containing 0.1258 g SnCl2）With the HI solution of 10 mL 1 M, it is transferred to high pressure after supersound process 5 min anti-
Answer in kettle, at 180 DEG C, react 4 h, be subsequently cooled to room temperature and mixed solution is obtained.
(3) add NaOH solution in the mixed solution being obtained to step (2)（Containing 0.1062 g NaOH）, supersound process 5
After min, at 180 DEG C, react 2 h, after naturally cooling to room temperature, products therefrom is washed with deionized to be done to neutrality
Dry, that is, polyaniline/Graphene/tin dioxide composite material is obtained.
Described three-dimensional porous polyaniline is 0.1 with the mass ratio of graphene oxide:1, described SnCl2With the material of NaOH
The ratio of amount is 1:4；Described tin ash is 0.2 with the mass ratio of graphene oxide:1.
Embodiment 3：
(1) 0.5g three-dimensional graphene oxide is dissolved in 100mL deionized water, it is molten that ultrasonic 10 min prepare graphene oxide
Liquid.
(2) add the three-dimensional porous polyaniline of 0.05g in the graphene oxide solution being obtained to step (1), be sufficiently stirred for down
Add SnCl2Solution（Containing 0.1573 g SnCl2）With the HI solution of 10 mL 1 M, it is transferred to high pressure after supersound process 5 min anti-
Answer in kettle, at 180 DEG C, react 4 h, be subsequently cooled to room temperature and mixed solution is obtained.
(3) add NaOH solution in the mixed solution being obtained to step (2)（Containing 0.1327 g NaOH）, supersound process 5
After min, at 180 DEG C, react 2 h, after naturally cooling to room temperature, products therefrom is washed with deionized to be done to neutrality
Dry, that is, polyaniline/Graphene/tin dioxide composite material is obtained.
Described three-dimensional porous polyaniline is 0.1 with the mass ratio of graphene oxide:1, described SnCl2With the material of NaOH
The ratio of amount is 1:4；Described tin ash is 0.25 with the mass ratio of graphene oxide:1.
Embodiment 4：
(1) 0.5g three-dimensional graphene oxide is dissolved in 100mL deionized water, it is molten that ultrasonic 10 min prepare graphene oxide
Liquid.
(2) add the three-dimensional porous polyaniline of 0.05g in the graphene oxide solution being obtained to step (1), be sufficiently stirred for down
Add SnCl2Solution（Containing 0.3145 g SnCl2）With the HI solution of 10 mL 1 M, it is transferred to high pressure after supersound process 5 min anti-
Answer in kettle, at 180 DEG C, react 4 h, be subsequently cooled to room temperature and mixed solution is obtained.
(3) add NaOH solution in the mixed solution being obtained to step (2)（Containing 0.2654 g NaOH）, supersound process 5
After min, at 180 DEG C, react 2 h, after naturally cooling to room temperature, products therefrom is washed with deionized to be done to neutrality
Dry, that is, polyaniline/Graphene/tin dioxide composite material is obtained.
Described three-dimensional porous polyaniline is 0.1 with the mass ratio of graphene oxide:1, described SnCl2With the material of NaOH
The ratio of amount is 1:4；Described tin ash is 0.5 with the mass ratio of graphene oxide:1.
Embodiment 5：
(1) 0.5g three-dimensional graphene oxide is dissolved in 100mL deionized water, it is molten that ultrasonic 10 min prepare graphene oxide
Liquid.
(2) add the three-dimensional porous polyaniline of 0.05g in the graphene oxide solution being obtained to step (1), be sufficiently stirred for down
Add SnCl2Solution（Containing 0.6290 g SnCl2）With the HI solution of 10 mL 1 M, it is transferred to high pressure after supersound process 5 min anti-
Answer in kettle, at 180 DEG C, react 4 h, be subsequently cooled to room temperature and mixed solution is obtained.
(3) add NaOH solution in the mixed solution being obtained to step (2)（Containing 0.5308 g NaOH）, supersound process 5
After min, at 180 DEG C, react 2 h, after naturally cooling to room temperature, products therefrom is washed with deionized to be done to neutrality
Dry, that is, polyaniline/Graphene/tin dioxide composite material is obtained.
Described three-dimensional porous polyaniline is 0.1 with the mass ratio of graphene oxide:1, described SnCl2With the material of NaOH
The ratio of amount is 1:4；Described tin ash is 1 with the mass ratio of graphene oxide:1.
Embodiment 6：
(1) 0.5g three-dimensional graphene oxide is dissolved in 100mL deionized water, it is molten that ultrasonic 10 min prepare graphene oxide
Liquid.
(2) add the three-dimensional porous polyaniline of 0.05g in the graphene oxide solution being obtained to step (1), be sufficiently stirred for down
Add SnCl2Solution（Containing 1.2580 g SnCl2）With the HI solution of 10 mL 1 M, it is transferred to high pressure after supersound process 5 min anti-
Answer in kettle, at 180 DEG C, react 4 h, be subsequently cooled to room temperature and mixed solution is obtained.
(3) add NaOH solution in the mixed solution being obtained to step (2)（Containing 1.0616 g NaOH）, supersound process 5
After min, at 180 DEG C, react 2 h, after naturally cooling to room temperature, products therefrom is washed with deionized to be done to neutrality
Dry, that is, polyaniline/Graphene/tin dioxide composite material is obtained.
Described three-dimensional porous polyaniline is 0.1 with the mass ratio of graphene oxide:1, described SnCl2With the material of NaOH
The ratio of amount is 1:4；Described tin ash is 2 with the mass ratio of graphene oxide:1.
Embodiment 7：
The step repeating embodiment 1, the addition only changing three-dimensional porous polyaniline in step (2) is 0.125 g.
Embodiment 8：
The step repeating embodiment 1, the addition only changing three-dimensional porous polyaniline in step (2) is 0.25 g.
Embodiment 9：
The step repeating embodiment 1, the addition only changing three-dimensional porous polyaniline in step (2) is 0.5 g.
Embodiment 10：
The step repeating embodiment 1, the addition only changing three-dimensional porous polyaniline in step (2) is 1 g.
Embodiment 11：
The step repeating embodiment 1, the addition only changing three-dimensional porous polyaniline in step (2) is 2 g.
Embodiment 12：
The step repeating embodiment 2, the addition only changing three-dimensional porous polyaniline in step (2) is 0.125 g.
Embodiment 13：
The step repeating embodiment 2, the addition only changing three-dimensional porous polyaniline in step (2) is 0.25 g.
Embodiment 14：
The step repeating embodiment 2, the addition only changing three-dimensional porous polyaniline in step (2) is 0.5 g.
Embodiment 15：
The step repeating embodiment 2, the addition only changing three-dimensional porous polyaniline in step (2) is 1 g.
Embodiment 16：
The step repeating embodiment 2, the addition only changing three-dimensional porous polyaniline in step (2) is 2 g.
Embodiment 17：
The step repeating embodiment 3, the addition only changing three-dimensional porous polyaniline in step (2) is 0.125 g.
Embodiment 18：
The step repeating embodiment 3, the addition only changing three-dimensional porous polyaniline in step (2) is 0.25 g.
Embodiment 19：
The step repeating embodiment 3, the addition only changing three-dimensional porous polyaniline in step (2) is 0.5 g.
Embodiment 20：
The step repeating embodiment 3, the addition only changing three-dimensional porous polyaniline in step (2) is 1 g.
Embodiment 21：
The step repeating embodiment 3, the addition only changing three-dimensional porous polyaniline in step (2) is 2 g.
Embodiment 22：
The step repeating embodiment 4, the addition only changing three-dimensional porous polyaniline in step (2) is 0.125 g.
Embodiment 23：
The step repeating embodiment 4, the addition only changing three-dimensional porous polyaniline in step (2) is 0.25 g.
Embodiment 24：
The step repeating embodiment 4, the addition only changing three-dimensional porous polyaniline in step (2) is 0.5 g.
Embodiment 25：
The step repeating embodiment 4, the addition only changing three-dimensional porous polyaniline in step (2) is 1 g.
Embodiment 26：
The step repeating embodiment 4, the addition only changing three-dimensional porous polyaniline in step (2) is 2 g.
Embodiment 27：
The step repeating embodiment 5, the addition only changing three-dimensional porous polyaniline in step (2) is 0.125 g.
Embodiment 28：
The step repeating embodiment 5, the addition only changing three-dimensional porous polyaniline in step (2) is 0.25 g.
Embodiment 29：
The step repeating embodiment 5, the addition only changing three-dimensional porous polyaniline in step (2) is 0.5 g.
Embodiment 30：
The step repeating embodiment 5, the addition only changing three-dimensional porous polyaniline in step (2) is 1 g.
Embodiment 31：
The step repeating embodiment 5, the addition only changing three-dimensional porous polyaniline in step (2) is 2 g.
Embodiment 32：
The step repeating embodiment 6, the addition only changing three-dimensional porous polyaniline in step (2) is 0.125 g.
Embodiment 33：
The step repeating embodiment 6, the addition only changing three-dimensional porous polyaniline in step (2) is 0.25 g.
Embodiment 34：
The step repeating embodiment 6, the addition only changing three-dimensional porous polyaniline in step (2) is 0.5 g.
Embodiment 35：
The step repeating embodiment 6, the addition only changing three-dimensional porous polyaniline in step (2) is 1 g.
Embodiment 36：
The step repeating embodiment 6, the addition only changing three-dimensional porous polyaniline in step (2) is 2 g.
Claims (1)
1. a kind of preparation method of polyaniline/Graphene/tin dioxide composite material is it is characterised in that concretely comprise the following steps：
(1) graphene oxide is dissolved in deionized water, ultrasonic 10 min preparation graphene oxide solution；
(2) add three-dimensional porous polyaniline in the graphene oxide solution being obtained to step (1), be sufficiently stirred for lower addition SnCl2Molten
Liquid and HI solution, are transferred in autoclave after supersound process 5 min, react 4 h, be subsequently cooled to room temperature system at 180 DEG C
Obtain mixed solution；
(3) add NaOH solution in the mixed solution being obtained to step (2), after supersound process 5 min, at 180 DEG C, react 2 h,
After naturally cooling to room temperature, products therefrom is washed with deionized and is dried to neutrality, that is, be obtained polyaniline/Graphene/
Tin dioxide composite material；
Described three-dimensional porous polyaniline is 0.1 ~ 4 with the mass ratio of graphene oxide:1；Described graphene oxide and the quality of HI
Ratio is 1:2.56；Described SnCl2Ratio with the amount of the material of NaOH is 1:4；Described tin ash and the quality of graphene oxide
Than for 0.1 ~ 2:1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108010730A (en) * | 2017-11-20 | 2018-05-08 | 桂林理工大学 | The preparation method of polyaniline nano linear array/graphene film/tin dioxide composite material |
| CN108010729A (en) * | 2017-11-20 | 2018-05-08 | 桂林理工大学 | The preparation method of polypyrrole nano line array/graphene film/tin dioxide composite material |
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| CN108010730A (en) * | 2017-11-20 | 2018-05-08 | 桂林理工大学 | The preparation method of polyaniline nano linear array/graphene film/tin dioxide composite material |
| CN108010729A (en) * | 2017-11-20 | 2018-05-08 | 桂林理工大学 | The preparation method of polypyrrole nano line array/graphene film/tin dioxide composite material |
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