CN108648920A - A kind of preparation method of titanium dioxide nano thread-graphene composite material - Google Patents
A kind of preparation method of titanium dioxide nano thread-graphene composite material Download PDFInfo
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- CN108648920A CN108648920A CN201810255894.7A CN201810255894A CN108648920A CN 108648920 A CN108648920 A CN 108648920A CN 201810255894 A CN201810255894 A CN 201810255894A CN 108648920 A CN108648920 A CN 108648920A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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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 of titanium dioxide nano thread graphene composite material is related to a kind of preparation method of titanium dioxide nano thread graphene composite material.The invention solves the titanium dioxide problems relatively low as electrode material for super capacitor poorly conductive and performance.Graphene oxide is prepared first, then it is mixed with titanic oxide nano powder, and hydro-thermal reaction is carried out in sodium hydroxide lye, reaction product is finally carried out to acidification and heat treatment in hydrochloric acid, is obtained a kind of with high-specific surface area, high performance electrode material for super capacitor.Preparation method of the present invention has simply, the advantages of efficiently and being easy to mass produce.
Description
Technical field
The present invention relates to a kind of preparation methods of titanium dioxide nano thread-graphene composite material.
Background technology
Ultracapacitor is a kind of energy storage device being widely studied in recent years, its big, quick charge and discharge with specific capacity
Electricity has extended cycle life the advantages that big with discharge power.Have in information communication, space flight and aviation and science and techniques of defence etc. and answers extensively
With.According to energy storage mechnism difference, ultracapacitor can be divided into double electric layers supercapacitor and fake capacitance ultracapacitor.Double electricity
Layer capacitor mainly utilizes charge to generate the electrostatic attraction of opposite charges in the interface of electrode and electrolyte to which formation is double
Electric layer stores energy, and main electrode material is carbon-based material, such as activated carbon and carbon nanotube.Fake capacitance ultracapacitor,
Quick and reversible redox reaction mainly occurs using electrode surface or nearby was to realize energy storage, main material
Cross metal oxide and conducting polymer.
Currently, the transition metal oxides such as ruthenium-oxide, manganese oxide, nickel oxide and titanium dioxide are widely used in fake capacitance
In ultracapacitor.Especially ruthenium-oxide can show outstanding fake capacitance performance, and specific capacitance reaches 1300 F/g, still
It is seriously polluted in preparation process since cost is extremely expensive, therefore be difficult to be applied in business.And titanium dioxide is due to it
The advantages of electrochemical properties are stable, at low cost, nontoxic and easy preparation is as preparing the most potential material of electrode of super capacitor
One of material.Titanium dioxide nano thread is a kind of nano material of one-dimentional structure, the specific surface with bigger compared with nano particle
Product, and due to the particularity of structure, the efficiency of charge transmission can be improved as the direct channel of electron-transport.But
Since itself energy gap is big, the problem that conductivity is poor and specific surface area is low makes its application on ultracapacitor not
It is ideal.
Graphene is a kind of two-dimensional layered-structure material of only monoatomic thickness, and wherein carbon atom is sp2 hydridization.Graphite
Alkene has many excellent physical and mechanical properties：Such as good heat conductivity, electronic conductivity and mechanical performance.Therefore,
By graphene and titanium dioxide it is compound be a kind of very ideal selection.
Invention content
Technical problem to be solved by the invention is to provide a kind of preparations of titanium dioxide nano thread-graphene composite material
Method.
A kind of preparation method of titanium dioxide nano thread-graphene composite material, it is characterised in that titanium dioxide nano thread-
The preparation method of graphene electrode material for super capacitor carries out according to the following steps：
One, the preparation of graphene oxide：By 0.8 ~ 1 g graphite powders and 0.8 ~ 1 g sodium nitrate with 46 mL's under the conditions of ice-water bath
20 ~ 30 mins are mixed in the concentrated sulfuric acid in conical flask, and 6 g permanganic acid are added to above-mentioned mixed solution under the conditions of ice-water bath
Potassium stirs 40 ~ 60 mins, obtains the mixed solution of green purple, the mixed solution of green purple is protected under conditions of 30 ~ 40 DEG C
During which 1 h of temperature keeps being slightly agitated for, the distilled water of 35 ~ 45 mL is then added, 30 ~ 40 are kept the temperature under conditions of 85 ~ 95 DEG C
Stop heating after mins, obtain dark-brown mixed solution, 100 mL deionized waters and 6 mL are added to dark-brown mixed solution
30 ~ 35% hydrogen peroxide obtain the mixed solution of glassy yellow, then use mass concentration anti-for the hydrochloric acid solution and deionized water of 5 %
It is 5 ~ 7 that after backwashing, which washs bright yellow solution to pH, is collected by centrifugation, is freeze-dried 4 ~ 6 h, obtains stannic oxide/graphene nano piece;Step 1
In the rotating speed that is collected by centrifugation be 3000 r/min;
Two, the preparation of titanium dioxide nano thread-graphene composite material：0.2 g of graphene oxide that step 1 obtains is weighed to add
Enter into 75 mL deionized waters, 2 h of ultrasonic disperse, obtains graphene oxide dispersion at room temperature；By 0.01 ~ 1.2 g dioxies
Change titanium powder to be added in graphene oxide dispersion, first stir 30 ~ 60 mins, 30 ~ 60 mins of re-ultrasonic dispersion is mixed
Close the mixed dispersion liquid of uniform titanium dioxide and graphene oxide；It will be in the mixed dispersion liquid of titanium dioxide and graphene oxide
The mixing of 24 ~ 36 g sodium hydroxides is added, stirs 30 mins；Again by mixed solution at 180 ~ 220 DEG C, 24 ~ 26 h of hydro-thermal reaction,
By hydrothermal product, pickling three times, is then cleaned with deionized water to neutrality in hydrochloric acid, and washing product is freeze-dried 4 ~ 6 h,
The product after drying is finally heat-treated 2 ~ 3 h for 450 ~ 500 DEG C under protection of argon gas, obtains titanium dioxide nano thread-graphene
Composite material；When step 2 pickling, a concentration of 0.1 mol/L of hydrochloric acid；Argon flow amount when step 2 is heat-treated is 500
sccm。
Advantages of the present invention：
（1）Graphene oxide is reduced to graphite by the present invention by the direct synthesis of titanium dioxide nano wire of one step of hydro-thermal method
Alkene, and keep the two compound, a kind of titanium dioxide nano thread-graphene composite material is prepared, preparation method is simple；
（2）Composite material prepared by the present invention can play simultaneously titanium dioxide nano thread and graphene structure and performance it is excellent
Gesture, wherein titanium dioxide nano thread provide fake capacitance, and the titanium dioxide of one-dimentional structure provides larger specific surface area, stone
Black alkene improves the electric conductivity of material, the shortcomings that compensating for titanium dioxide poorly conductive, and then improves the specific capacitance of material, makes
The specific capacitance of composite material is obtained far above the ultracapacitor that independent titanium dioxide is raw material preparation.
Description of the drawings
Fig. 1 is the stereoscan photograph tested the titanium dioxide nano thread prepared in one and be amplified to 5000 times.
Fig. 2 is the scanning electricity tested the titanium dioxide nano thread-graphene composite material prepared in two and be amplified to 5000 times
Mirror photo.
Fig. 3 is the scanning electricity tested the titanium dioxide nano thread-graphene composite material prepared in five and be amplified to 5000 times
Mirror photo.
Fig. 4 is the scanning electricity tested the titanium dioxide nano thread-graphene composite material prepared in six and be amplified to 5000 times
Mirror photo.
Fig. 5 is to test the titanium dioxide nano thread-graphene composite material Raman collection of illustrative plates prepared in five.
The titanium dioxide nano thread prepared in Fig. 6 bit tests five-graphene composite material X ray diffracting spectrum.
Fig. 7 is that the constant current for titanium dioxide nano thread-graphene composite material that different titanium dioxide quality are prepared fills
Discharge curve.
Fig. 8 is experiment five, the titanium dioxide nano thread-graphene composite material prepared when titanium dioxide is 0.05 g
Under the current density of 1 Ag-1, the stable circulation linearity curve after recycling 1000 times.
Specific implementation mode
Below in conjunction with example, the present invention will be further described, it should be pointed out that example as described below be intended to convenient for pair
The understanding of the present invention, and do not play any restriction effect to it.
Specific implementation mode one：Present embodiment is a kind of preparation side of titanium dioxide nano thread-graphene composite material
Method specifically follows the steps below：
One, the preparation of graphene oxide：By 0.8 ~ 1 g graphite powders and 0.8 ~ 1 g sodium nitrate with 46 mL's under the conditions of ice-water bath
20 ~ 30 mins are mixed in the concentrated sulfuric acid in conical flask, and 6 g permanganic acid are added to above-mentioned mixed solution under the conditions of ice-water bath
Potassium stirs 40 ~ 60 mins, obtains the mixed solution of green purple, the mixed solution of green purple is protected under conditions of 30 ~ 40 DEG C
During which 1 h of temperature keeps being slightly agitated for, the distilled water of 35 ~ 45 mL is then added, 30 ~ 40 are kept the temperature under conditions of 85 ~ 95 DEG C
Stop heating after mins, obtain dark-brown mixed solution, 100 mL deionized waters and 6 mL are added to dark-brown mixed solution
30 ~ 35% hydrogen peroxide obtain the mixed solution of glassy yellow, then use mass concentration anti-for the hydrochloric acid solution and deionized water of 5 %
It is 5 ~ 7 that after backwashing, which washs bright yellow solution to pH, is collected by centrifugation, is freeze-dried 4 ~ 6 h, obtains stannic oxide/graphene nano piece;Step 1
In the rotating speed that is collected by centrifugation be 3000 r/min;
Two, the preparation of titanium dioxide nano thread-graphene composite material：0.2 g of graphene oxide that step 1 obtains is weighed to add
Enter into 75 mL deionized waters, 2 h of ultrasonic disperse, obtains graphene oxide dispersion at room temperature；By 0.01 ~ 1.2 g dioxies
Change titanium powder to be added in graphene oxide dispersion, first stir 30 ~ 60 mins, 30 ~ 60 mins of re-ultrasonic dispersion is mixed
Close the mixed dispersion liquid of uniform titanium dioxide and graphene oxide；It will be in the mixed dispersion liquid of titanium dioxide and graphene oxide
The mixing of 24 ~ 36 g sodium hydroxides is added, stirs 30 mins；Again by mixed solution at 180 ~ 220 DEG C, 24 ~ 26 h of hydro-thermal reaction,
By hydrothermal product, pickling three times, is then cleaned with deionized water to neutrality in hydrochloric acid, and washing product is freeze-dried 4 ~ 6 h,
The product after drying is finally heat-treated 2 ~ 3 h for 450 ~ 500 DEG C under protection of argon gas, obtains titanium dioxide nano thread-graphene
Composite material；When step 2 pickling, a concentration of 0.1 mol/L of hydrochloric acid；Argon flow amount when step 2 is heat-treated is 500
sccm。
Specific implementation mode two：The difference of present embodiment and specific implementation mode one is：By 0.01 ~ 0.033 g bis-
Titanium dioxide powder is added in graphene oxide dispersion, first stirs 30 ~ 60 mins, and 30 ~ 60 mins of re-ultrasonic dispersion is obtained
The mixed dispersion liquid of uniformly mixed titanium dioxide and graphene oxide, it is other same as the specific embodiment one.
Specific implementation mode three：The difference of present embodiment and specific implementation mode one or two is：By titanium dioxide with
The mixing of 24 ~ 30 g sodium hydroxides is added in the mixed dispersion liquid of graphene oxide, stirs 30 mins, other and specific embodiment party
Formula one or two is identical.
Specific implementation mode four：Unlike one of present embodiment and specific implementation mode one to three：It will mix again molten
Liquid at 200 ~ 220 DEG C, 24 ~ 26 h of hydro-thermal reaction, by hydrothermal product in hydrochloric acid pickling three times, then with deionized water clean to
Washing product is freeze-dried 4 ~ 6 h by neutrality, finally by 450 ~ 500 DEG C of heat treatment 2 ~ 3 under protection of argon gas of the product after drying
H obtains titanium dioxide nano thread-graphene composite material, other identical as one of specific implementation mode one to three.
Beneficial effects of the present invention are verified by following tests.
Experiment one：This experiment is contrast test, prepares titanium dioxide nano thread, specific method is：
0.6 g titania powders are added in 75 mL deionized waters, 30 mins, 30 mins of re-ultrasonic dispersion are first stirred,
Obtain uniformly mixed titanium oxide dispersion.The mixing of 30 g sodium hydroxides, stirring 30 will be added in titanium oxide dispersion
mins；Again by mixed solution at 200 DEG C, 24 h of hydro-thermal reaction, by hydrothermal product, pickling three times, then uses deionization in hydrochloric acid
Water is cleaned to neutrality, and washing product is freeze-dried 6 h, finally by the 450 DEG C of heat treatment 2 under protection of argon gas of the product after drying
H obtains titanium dioxide nano thread；
As shown in Figure 1, it can be seen that the titanium dioxide nano thread of preparation is in one-dimensional linear structure, structural integrity.
Experiment two：A kind of preparation method of titanium dioxide nano thread-graphene composite material, specifically according to the following steps
It carries out：
One, graphene oxide is prepared：The concentrated sulfuric acid of 1 g graphite powders and 1 g sodium nitrate under the conditions of ice-water bath with 46 mL is being bored
25 mins are mixed in shape bottle, 6 g potassium permanganate, stirring 45 is added to above-mentioned mixed solution under the conditions of ice-water bath
Mins obtains the mixed solution of green purple, and the mixed solution of green purple is kept the temperature 1 h under conditions of 35 DEG C, during which keeps suitable
Degree stirring, is then added the distilled water of 35 mL, stops heating after 35 mins are kept the temperature under conditions of 90 DEG C, obtains dark brown color contamination
Solution is closed, 30% hydrogen peroxide of 100 mL deionized waters and 6 mL is added to dark-brown mixed solution, obtains the mixing of glassy yellow
It is 7 that then hydrochloric acid solution and deionized water that solution is 5% with mass concentration washs bright yellow solution to pH repeatedly, and centrifugation is received
Collection is freeze-dried 4 h, obtains stannic oxide/graphene nano piece；
Two, the preparation of titanium dioxide nano thread-graphene composite material：0.2 g of graphene oxide that step 1 obtains is weighed to add
Enter into 75 mL deionized waters, 2 h of ultrasonic disperse, obtains graphene oxide dispersion at room temperature；By 1.2 g titanium dioxide
Powder is added in graphene oxide dispersion, first stirs 30 mins, and 30 mins of re-ultrasonic dispersion obtains uniformly mixed two
The mixed dispersion liquid of titanium oxide and graphene oxide；30 g hydrogen will be added in the mixed dispersion liquid of titanium dioxide and graphene oxide
Sodium oxide molybdena mixes, and stirs 30 mins；Again by mixed solution at 200 DEG C, 24 h of hydro-thermal reaction, by hydrothermal product deionized water
Cleaning is to neutrality, and then acid-leached product three times, is freeze-dried 6 h, finally by the product after drying in argon by pickling in hydrochloric acid
Gas shielded 2 h of lower 450 DEG C of heat treatment, obtain titanium dioxide nano thread-graphene composite material.
As shown in Fig. 2, when titania powder is 1.2 g, titanium dioxide nano thread-graphene composite wood is prepared
Material, titanium dioxide has grown into line and compound with graphene, but titanium dioxide nano thread quantity is more.
Experiment three：A kind of preparation method of titanium dioxide nano thread-graphene composite material, this experiment are different from experiment two
Point is that titania powder is that 0.2 g, other steps and parameter are identical as experiment two.
Experiment four：A kind of preparation method of titanium dioxide nano thread-graphene composite material, this experiment and experiment two to three
Difference is that titania powder is that 0.1 g, other steps and parameter are identical as experiment two to three.
Experiment five：A kind of preparation method of titanium dioxide nano thread-graphene composite material, this experiment and experiment two to four
Difference is that titania powder is that 0.05g, other steps and parameter are identical as experiment two to four.
As shown in figure 3, when titania powder is 0.05 g, titanium dioxide nano thread-graphene composite wood is prepared
Material, titanium dioxide have grown into line and compound with graphene, and titanium dioxide nano thread is uniformly dispersed.
Experiment six：A kind of preparation method of titanium dioxide nano thread-graphene composite material, this experiment and experiment two to five
Difference is that titania powder is that 0.033 g, other steps and parameter are identical as experiment two to five.
As shown in figure 4, when titania powder is 0.033 g, titanium dioxide nano thread-graphene composite wood is prepared
Material, titanium dioxide have grown into line and compound with graphene, but titanium dioxide nano thread negligible amounts, almost by graphene
It is fully wrapped around.
Experiment seven：A kind of preparation method of titanium dioxide nano thread-graphene composite material, this experiment and experiment two to six
Difference is not add titania powder, other steps and parameter are identical as experiment two to six.
As shown in figure 5, titanium dioxide nano thread-graphene composite material has by force at 1326 cm-1 and 1586 cm-1
Peak, intensity ratio (ID/IG) are less than 1, illustrate that the peak is the characteristic peak of graphene, and in 164,270,463,675 Hes
There is the characteristic peak of titanium dioxide nano thread at 881 cm-1, this illustrates in titanium dioxide nano thread-graphene composite material, dioxy
It is compound preferably in graphene to change titanium, graphene oxide has been reduced into graphene.
As shown in fig. 6, in titanium dioxide nano thread-graphene composite material, at 25.2 °, 28.6 °, 43.5 °,
Occur apparent diffraction maximum at 44.5 ° and 48.2 °, corresponds to (110) of titanium dioxide, (002), (003), (01) respectively
(020) crystal face.The diffraction maximum of graphene is not observed, this is because titanium dioxide has diffraction maximum at 25.2 °, is led
The diffraction maximum of no apparent graphene is caused to occur.
Experiment eight：Make collector with nickel foam, titanium dioxide nano thread-graphene composite material is prepared into as active material
The electrode arrived is working electrode, carries out Electrochemical Detection experiment, specific as follows：
One, collector, the electrode that titanium dioxide nano thread-graphene composite material is prepared as active material are made with nickel foam
For working electrode, silver chlorate is reference electrode, and platinum filament is to electrode, and 6 M KOH are electrolyte, are assembled into three-electrode system；
Two, under the three-electrode system in step 1, voltage range is 0-0.4 V, and current density is 1 Ag-1, passes through perseverance
Current charging and discharging（GCD）Test obtains the GCD curves of titanium dioxide nano thread-graphene composite material；
Three, under the three-electrode system in step 1, current density is 1 Ag-1, is tested by cyclical stability, obtains two
The stable circulation linearity curve of titanium oxide nano wire-graphene composite material.
As shown in fig. 7, curve 1 is the GCD curves for testing the titanium dioxide nano thread that an independent titanium dioxide is prepared, it is bent
Line 2 to curve 6 is that different quality titanium dioxide is that titanium dioxide nano thread-graphene that raw material is prepared is multiple in experiment two to six
The GCD curves of condensation material, curve 7 are not add titanium dioxide in experiment seven, only generate the GCD curves of graphene.Curve 2 is to song
The discharge time of line 6 is far more than curve 1 and curve 7, illustrates the titanium dioxide for preparing titanium dioxide and graphene after compound
The performance of nano wire-graphene composite material is obviously improved.Wherein, the discharge time longest of curve 5, illustrate be when graphene
0.2 g, performance is best when titanium dioxide is 0.05 g.
As shown in figure 8, the composite material prepared when titanium dioxide is 0.05 g is under the current density of 1 Ag-1
After cycle 1000 times, 93 % for retaining initial capacitance are remained to, preferable cyclical stability has been shown.
Claims (2)
1. a kind of preparation method of titanium dioxide nano thread-graphene composite material, it is characterised in that titanium dioxide nano thread-stone
The preparation method of black alkene electrode material for super capacitor carries out according to the following steps：
One, the preparation of graphene oxide：By 0.8 ~ 1 g graphite powders and 0.8 ~ 1 g sodium nitrate with 46 mL's under the conditions of ice-water bath
20 ~ 30 mins are mixed in the concentrated sulfuric acid in conical flask, and 6 g permanganic acid are added to above-mentioned mixed solution under the conditions of ice-water bath
Potassium stirs 40 ~ 60 mins, obtains the mixed solution of green purple, the mixed solution of green purple is protected under conditions of 30 ~ 40 DEG C
During which 1 h of temperature keeps being slightly agitated for, the distilled water of 35 ~ 45 mL is then added, 30 ~ 40 are kept the temperature under conditions of 85 ~ 95 DEG C
Stop heating after mins, obtain dark-brown mixed solution, 100 mL deionized waters and 6 mL are added to dark-brown mixed solution
30 ~ 35% hydrogen peroxide obtain the mixed solution of glassy yellow, then use mass concentration anti-for the hydrochloric acid solution and deionized water of 5 %
It is 5 ~ 7 that after backwashing, which washs bright yellow solution to pH, is collected by centrifugation, is freeze-dried 4 ~ 6 h, obtains stannic oxide/graphene nano piece;Step 1
In the rotating speed that is collected by centrifugation be 3000 r/min;
Two, the preparation of titanium dioxide nano thread-graphene composite material：0.2 g of graphene oxide that step 1 obtains is weighed to add
Enter into 75 mL deionized waters, 2 h of ultrasonic disperse, obtains graphene oxide dispersion at room temperature；By 0.01 ~ 1.2 g dioxies
Change titanium powder to be added in graphene oxide dispersion, first stir 30 ~ 60 mins, 30 ~ 60 mins of re-ultrasonic dispersion is mixed
Close the mixed dispersion liquid of uniform titanium dioxide and graphene oxide；It will be in the mixed dispersion liquid of titanium dioxide and graphene oxide
The mixing of 24 ~ 36 g sodium hydroxides is added, stirs 30 mins；Again by mixed solution at 180 ~ 220 DEG C, 24 ~ 26 h of hydro-thermal reaction,
By hydrothermal product, pickling three times, is then cleaned with deionized water to neutrality in hydrochloric acid, and washing product is freeze-dried 4 ~ 6 h,
The product after drying is finally heat-treated 2 ~ 3 h for 450 ~ 500 DEG C under protection of argon gas, obtains titanium dioxide nano thread-graphene
Composite material；When step 2 pickling, a concentration of 0.1 mol/L of hydrochloric acid；Argon flow amount when step 2 is heat-treated is 500
sccm。
2. a kind of application of titanium dioxide nano thread-graphene composite material, it is characterized in that the material is as electrode material application
In ultracapacitor.
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| CN103990444A (en) * | 2014-06-04 | 2014-08-20 | 沈阳化工大学 | Preparation method of graphene-homemade TiO2 nanowire photocatalyst |
| CN104941621A (en) * | 2015-05-26 | 2015-09-30 | 华南理工大学 | Composite photocatalyst for efficiently degrading antibiotics as well as preparation method and application thereof |
| CN105344350A (en) * | 2015-12-03 | 2016-02-24 | 江南大学 | Preparation method for molybdenum-doped TiO2 nanowire/graphene compound with high catalytic degradation activity under visible light |
| US20170062143A1 (en) * | 2015-08-24 | 2017-03-02 | Aruna Zhamu | Production process for a supercapacitor having a high volumetric energy density |
-
2018
- 2018-03-27 CN CN201810255894.7A patent/CN108648920A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103990444A (en) * | 2014-06-04 | 2014-08-20 | 沈阳化工大学 | Preparation method of graphene-homemade TiO2 nanowire photocatalyst |
| CN104941621A (en) * | 2015-05-26 | 2015-09-30 | 华南理工大学 | Composite photocatalyst for efficiently degrading antibiotics as well as preparation method and application thereof |
| US20170062143A1 (en) * | 2015-08-24 | 2017-03-02 | Aruna Zhamu | Production process for a supercapacitor having a high volumetric energy density |
| CN105344350A (en) * | 2015-12-03 | 2016-02-24 | 江南大学 | Preparation method for molybdenum-doped TiO2 nanowire/graphene compound with high catalytic degradation activity under visible light |
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