CN109517217A - A kind of tungsten-doped vanadium dioxide/graphene complex and the preparation method and application thereof - Google Patents
A kind of tungsten-doped vanadium dioxide/graphene complex and the preparation method and application thereof Download PDFInfo
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- CN109517217A CN109517217A CN201811400252.8A CN201811400252A CN109517217A CN 109517217 A CN109517217 A CN 109517217A CN 201811400252 A CN201811400252 A CN 201811400252A CN 109517217 A CN109517217 A CN 109517217A
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Abstract
The present invention discloses a kind of tungsten-doped vanadium dioxide/graphene complex and the preparation method and application thereof.Method is uniformly mixed comprising steps of weighing appropriate graphene oxide powder, vanadic anhydride, organic acid and ammonium tungstate and being added in solvent deionized water, obtains precursor liquid;The precursor liquid is calcined to obtain tungsten-doped vanadium dioxide/graphene complex after hydro-thermal reaction, cooling, washing, centrifuge washing, drying.Tungsten-doped vanadium dioxide/graphene complex produced by the present invention has good dispersibility and crystallinity; it is applied in New-type phase change intelligent temperature control material and energy-saving material and its anti-pollution and heat-proof quality can be improved; and preparation process of the present invention is simple, high-efficient, low energy consumption, it can be achieved that large-scale production.
Description
Technical field
The present invention relates to graphene composite material technical field more particularly to a kind of tungsten-doped vanadium dioxide/graphene are multiple
Close object and the preparation method and application thereof.
Background technique
Energy-saving and emission-reduction in recent years become the top priority of current various countries.And building energy consumption account for the 1/3 of social total energy consumption with
On.Therefore, the energy-saving and emission-reduction of building are the effective means for solving the problems, such as to build highly energy-consuming, while being also the pass for reducing energy consumption
Key.By developing energy-saving glass, it is expected to that greenhouse gas emission and energy consumption is greatly lowered, is finally reached energy-saving and environment-friendly purpose.
It applies on building glass coated with the coating based on heat-insulating and energy-saving powder at present, the energy-efficient life of mill construction can be met
It produces and requires, can also realize the reducing energy consumption carried out to existing simple glass.Infrared ray is the main source of external environment heat source, but
Existing heat-insulating and energy-saving powder is unsatisfactory to the absorption of infrared ray or reflecting effect.Therefore, it is necessary to make improvements.
Vanadium dioxide particle and graphene are formed by conductive network theoretically and may be implemented the total reflection to infrared light, and
It is not conventional diffusing reflection, absorption and transmission to infrared ray can be greatly reduced, to reduce temperature rise, realizes energy-efficient mesh
's.Graphene conductivity with higher simultaneously, can in time export electronics, and reaction can inhibit light induced electron and hole multiple eventually
It closes, light-catalyzed reaction efficiency is improved, so that the anti-pollution of coating can be improved.And vanadium dioxide/graphene composite powder is used
It is rarely reported in the research of transparent heat insulating glass nano paint, therefore studies the titanium dioxide for being used for transparent heat insulating glass nano paint
The research of vanadium/graphene composite powder is of great significance.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of tungsten-doped vanadium dioxide/graphenes
Compound and the preparation method and application thereof, it is desirable to provide a kind of tungsten-doped vanadium dioxide/graphene complex is for transparent heat-insulated
Glass nano coating.
Technical scheme is as follows:
A kind of preparation method of tungsten-doped vanadium dioxide/graphene complex, wherein comprising steps of
(1) graphene oxide powder is taken, is added in deionized water, ultrasonic disperse;
(2) vanadic anhydride, organic acid and ammonium tungstate are taken again, is added in system obtained by step (1), and stirring obtains precursor liquid;
(3) precursor liquid obtained by step (2) is transferred in reaction kettle and carries out hydro-thermal reaction;
(4) gained mixed liquor after step (3) reaction is successively carried out after cooling down, washing, be centrifugated, dry, is calcined, is obtained
To tungsten-doped vanadium dioxide/graphene complex.
Tungsten-doped vanadium dioxide/graphene complex preparation method, wherein in step (1), the oxidation stone
Black alkene is two-dimensional stannic oxide/graphene nano piece.
Tungsten-doped vanadium dioxide/graphene complex preparation method, wherein in step (1), the oxidation stone
The step of black alkene powder ultrasonic disperses is as follows: using 28-59kHz frequency, 500W power ultrasonic treatment, the processing time is 5-
60min。
Tungsten-doped vanadium dioxide/graphene complex preparation method, wherein in step (2), five oxidation
The mass ratio of the material of two vanadium and ammonium tungstate is 100:1-20:1.
Tungsten-doped vanadium dioxide/graphene complex preparation method, wherein in step (2), the organic acid
For one of citric acid and oxalic acid, wherein the mass ratio of the material of vanadic anhydride and citric acid is 1:3, the substance with oxalic acid
Amount ratio be 1:2.
Tungsten-doped vanadium dioxide/graphene complex preparation method, wherein in step (3), the hydro-thermal is anti-
The hydrothermal temperature answered is 180-200 DEG C, and the hydro-thermal time is 24-72h.
Tungsten-doped vanadium dioxide/graphene complex preparation method, wherein in step (4), the calcining temperature
Degree is 550 DEG C -650 DEG C, calcination time 1.5h-2.5h.
A kind of tungsten-doped vanadium dioxide/graphene complex, wherein use tungsten-doped vanadium dioxide of the present invention/
The preparation method of graphene complex is prepared.
A kind of tungsten-doped vanadium dioxide/graphene complex answering in insulating moulding coating or thermal insulation film of the present invention
With.
The utility model has the advantages that tungsten-doped vanadium dioxide/graphene complex produced by the present invention has good dispersibility and knot
Brilliant degree is applied in New-type phase change intelligent temperature control material and energy-saving material and its anti-pollution and heat-proof quality can be improved, and
Preparation process of the present invention is simple, high-efficient, low energy consumption, it can be achieved that large-scale production.
Detailed description of the invention
Fig. 1 is a kind of XRD spectrum of tungsten-doped vanadium dioxide/graphene complex of the embodiment of the present invention one.
Fig. 2 is a kind of EDS map of tungsten-doped vanadium dioxide/graphene complex of the embodiment of the present invention one.
Fig. 3 is that a kind of SEM Flied emission of tungsten-doped vanadium dioxide/graphene complex of the embodiment of the present invention one scans electricity
Mirror shape appearance figure.
Fig. 4 is that a kind of another SEM Flied emission of tungsten-doped vanadium dioxide/graphene complex of the embodiment of the present invention one is swept
Retouch Electronic Speculum shape appearance figure.
Fig. 5 is a kind of Raman spectrogram of tungsten-doped vanadium dioxide/graphene complex of the embodiment of the present invention one.
Fig. 6 is a kind of V of the embodiment of the present invention two0.99W0.01O2The DSC of/graphene complex detects figure.
Fig. 7 is a kind of V of the embodiment of the present invention three0.99W0.01O2The DSC of powder detects figure.
Specific embodiment
The present invention provides a kind of tungsten-doped vanadium dioxide/graphene complex and the preparation method and application thereof, to make this hair
Bright purpose, technical solution and effect are clearer, clear, and the present invention is described in more detail below.It should be appreciated that herein
Described specific embodiment is only used to explain the present invention, is not intended to limit the present invention.
The embodiment of the present invention provides a kind of preparation method of tungsten-doped vanadium dioxide/graphene complex, wherein including step
It is rapid:
(1) graphene oxide powder is taken, is added in deionized water, ultrasonic disperse;
(2) vanadic anhydride, organic acid and ammonium tungstate are taken again, is added in system obtained by step (1), and stirring obtains precursor liquid;
(3) precursor liquid obtained by step (2) is transferred in reaction kettle and carries out hydro-thermal reaction;
(4) gained mixed liquor after step (3) reaction is successively carried out after cooling down, washing, be centrifugated, dry, is calcined, is obtained
To tungsten-doped vanadium dioxide/graphene complex.
Vanadium dioxide crystal form is Type B in products therefrom after hydro-thermal reaction of the present invention, then passes through products therefrom after calcination processing
Middle vanadium dioxide crystal form is M type.Tungsten-doped vanadium dioxide/graphene complex produced by the present invention have it is good dispersibility and
Crystallinity is applied in New-type phase change intelligent temperature control material and energy-saving material and its anti-pollution and heat-proof quality can be improved,
And preparation process of the present invention is simple, high-efficient, low energy consumption, it can be achieved that large-scale production.
In step (1), in a preferred embodiment, the graphene oxide is two-dimensional stannic oxide/graphene nano
Piece.Because graphene nanometer sheet can make nanoparticle be preferably compounded in its curling accordion nanometer sheet surface and nanometer sheet
Interlayer.
In step (1), the step of graphene oxide powder ultrasonic disperse, is as follows: using 28-59kHz frequency, 500W
Power ultrasonic treatment, processing time are 5-60min.
In step (2), in a preferred embodiment, the mass ratio of the material of the vanadic anhydride and ammonium tungstate is
100:1-20:1.
In step (2), in a preferred embodiment, the organic acid be one of citric acid and oxalic acid,
In, the mass ratio of the material of vanadic anhydride and citric acid is 1:3, and the mass ratio of the material with oxalic acid is 1:2.
In step (3), in a preferred embodiment, the hydrothermal temperature of the hydro-thermal reaction is 180-200 DEG C.?
Vanadium dioxide crystal form prepared by this temperature range is preferable.
In step (3), in a preferred embodiment, the hydro-thermal time of the hydro-thermal reaction is 24-72h.Herein
The reaction of hydro-thermal time interval carries out relatively sufficiently, and prepared vanadium dioxide crystal form is preferable.
Step (4) specifically includes the following steps:
(41) gained mixed liquor after step (3) reaction is cooled to room temperature, obtains solidliquid mixture;
(42) obtained solidliquid mixture is washed 3 ~ 5 times with deionized water and dehydrated alcohol respectively;
(43) solidliquid mixture resulting after washing is centrifuged, removes moisture;The revolving speed being wherein centrifugated is
3000 ~ 5000 revs/min, the time is 10 ~ 30 minutes;
(44) reaction product after separation is placed in baking oven, is dried 4 ~ 8 hours at 60 ~ 80 DEG C and obtains composite nano powder;
(45) step (44) resulting composite nano powder is put into tube furnace and is calcined, obtain tungsten-doped vanadium dioxide/graphite
Alkene compound.
In step (4), in a preferred embodiment, the calcination temperature is 550 DEG C -650 DEG C.
In step (4), in a preferred embodiment, the calcination time is 1.5h-2.5h.
The embodiment of the present invention also provides a kind of tungsten-doped vanadium dioxide/graphene complex, wherein is mixed using the tungsten
The preparation method of miscellaneous vanadium dioxide/graphene complex is prepared.
The embodiment of the present invention also provides a kind of tungsten-doped vanadium dioxide/graphene complex in insulating moulding coating or heat-insulated
Application in film.
Below by specific embodiment, the present invention is further described.
Embodiment one
(1), 20mg graphene oxide powder is weighed, 35ml deionized water, ultrasonic disperse 30min is added;
(2), according still further to V0.99W0.01O2Component ratio weigh 0.609g vanadic anhydride, 1.101g citric acid and 0.013g tungsten
Sour ammonium is added in system obtained by step (1), and stirring at normal temperature 10min obtains precursor liquid;
(3), precursor liquid obtained by step (2) is transferred in autoclave, is reacted 24 hours at 200 DEG C;
(4), by step (3) reaction after mixed liquor be cooled to room temperature, by obtained solidliquid mixture use respectively deionized water and
Dehydrated alcohol washs 3 times;
(5), step (4) resulting solidliquid mixture is centrifuged, removes moisture, obtains tungsten-doped vanadium dioxide/stone
Black alkene compound, the revolving speed of centrifuge separation are 5000 revs/min, and the time is 10 minutes;
(6), the reaction product after step (5) separation is placed in baking oven, is dried 4 hours at 80 DEG C and obtains composite nano powder
Body;
(7), by step (6) resulting composite nano powder be put into 600 DEG C of calcining 2h in tube furnace obtain tungsten-doped vanadium dioxide/
Graphene complex.
Test result:
Fig. 1 is the XRD spectrum of the resulting tungsten-doped vanadium dioxide/graphene complex of the embodiment of the present invention.The production as seen from the figure
Object characteristic peak sharply protrudes, and crystal form is preferable, and without other miscellaneous peaks, illustrates that the incorporation of tungsten has no effect on the crystal form knot of vanadium dioxide
Structure meets vanadium dioxide standard card.
Fig. 2 is the EDS map of the resulting tungsten-doped vanadium dioxide/graphene complex of the embodiment of the present invention.As seen from the figure
Wolfram element successfully mixes in compound.
Fig. 3-4 is that the SEM Flied emission of the resulting tungsten-doped vanadium dioxide/graphene complex of the embodiment of the present invention scans electricity
Mirror shape appearance figure.Nanoparticle is evenly distributed on graphene nanometer sheet surface as seen from Figure 3.The visible nanoparticle of Fig. 4 is evenly dispersed
And it is tightly fixed to the graphene nanometer sheet interlayer of the accordion of curling.
Fig. 5 is the Raman spectrogram of the resulting tungsten-doped vanadium dioxide/graphene complex of the embodiment of the present invention.It can by figure
Know that nanoparticle and graphene success are compound.
Embodiment two
(1), 20mg graphene oxide powder is weighed, 35ml deionized water, ultrasonic disperse 30min is added;
(2), according still further to V0.99W0.01O2Component ratio weigh 0.609g vanadic anhydride, 0.973g oxalic acid and 0.013g wolframic acid
Ammonium is added in system obtained by step (1), and stirring at normal temperature 10min obtains precursor liquid;
(3), precursor liquid obtained by step (2) is transferred in autoclave, is reacted 24 hours at 200 DEG C;
(4), the mixed liquor of step (3) is cooled to room temperature, obtained solidliquid mixture is used into deionized water and anhydrous second respectively
Alcohol washs 3 times;
(5), step (4) resulting solidliquid mixture is centrifuged, removes moisture, obtains tungsten-doped vanadium dioxide/stone
Black alkene compound, the revolving speed of centrifuge separation are 5000 revs/min, and the time is 10 minutes;
(6), the reaction product after step (5) separation is placed in baking oven, is dried 4 hours at 80 DEG C and obtains composite nano powder
Body;
(7), by step (6) resulting composite nano powder be put into 600 DEG C of calcining 2h in tube furnace obtain tungsten-doped vanadium dioxide/
Graphene complex.
Test result:
Fig. 6 is the V of the embodiment of the present invention0.99W0.01O2The DSC of/graphene complex detects figure.The compound as can be seen from Figure
Phase transition temperature is 59.6 DEG C, and the compound phase transition temperature than Fig. 7 non-composite graphite alkene has dropped 2.2 DEG C.
Embodiment three
(1), according to V0.99W0.01O2Component ratio weigh 0.609g vanadic anhydride, 0.973g oxalic acid and 0.013g ammonium tungstate,
Stirring at normal temperature 10min, obtains precursor liquid;
(2), precursor liquid obtained by step (1) is transferred in autoclave, is reacted 24 hours at 200 DEG C;
(3), the mixed liquor of step (2) is cooled to room temperature, obtained solidliquid mixture is used into deionized water and anhydrous second respectively
Alcohol washs 3 times;
(4), step (3) resulting solidliquid mixture is centrifuged, removes moisture, obtains tungsten-doped vanadium dioxide/stone
Black alkene compound, the revolving speed of centrifuge separation are 5000 revs/min, and the time is 10 minutes;
(5), the reaction product after step (5) separation is placed in baking oven, is dried 4 hours at 80 DEG C and obtains nano-powder;
(6), step (6) resulting nano-powder is put into 600 DEG C of calcining 2h in tube furnace and obtains tungsten-doped vanadium dioxide powder.
Test result:
Fig. 7 is the V of the embodiment of the present invention0.99W0.01O2The DSC of powder detects figure.As a kind of reversible phase transition material, vanadium dioxide
Phase transition temperature near 68 DEG C, when the molar ratio of tungsten-doped vanadium dioxide is 1%, phase transition temperature is 61.8 as can be seen from Figure
DEG C, the phase transition temperature than pure vanadium dioxide has dropped 6.2 DEG C.
Example IV
(1), 20mg graphene oxide powder is weighed, 35ml deionized water, ultrasonic disperse 30min is added;
(2), according still further to V0.98W0.02O2Component ratio weigh 0.609g vanadic anhydride, 0.973g citric acid and 0.037g tungsten
Sour ammonium is added in system obtained by step (1), and stirring at normal temperature 10min obtains precursor liquid;
(3), precursor liquid obtained by step (2) is transferred in autoclave, is reacted 24 hours at 200 DEG C;
(4), the mixed liquor of step (3) is cooled to room temperature, obtained solidliquid mixture is used into deionized water and anhydrous second respectively
Alcohol washs 3 times;
(5), step (4) resulting solidliquid mixture is centrifuged, removes moisture, obtains tungsten-doped vanadium dioxide/stone
Black alkene compound, the revolving speed of centrifuge separation are 5000 revs/min, and the time is 10 minutes;
(6), the reaction product after step (5) separation is placed in baking oven, is dried 4 hours at 80 DEG C and obtains composite nano powder
Body;
(7), by step (6) resulting composite nano powder be put into 600 DEG C of calcining 2h in tube furnace obtain tungsten-doped vanadium dioxide/
Graphene complex.
In conclusion a kind of tungsten-doped vanadium dioxide/graphene complex provided by the invention and preparation method thereof with answer
With tungsten-doped vanadium dioxide/graphene complex produced by the present invention has good dispersibility and crystallinity, is applied to
Its anti-pollution and heat-proof quality, and preparation process of the present invention letter can be improved in New-type phase change intelligent temperature control material and energy-saving material
It is single, high-efficient, low energy consumption, it can be achieved that large-scale production.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (9)
1. a kind of preparation method of tungsten-doped vanadium dioxide/graphene complex, which is characterized in that comprising steps of
(1) graphene oxide powder is taken, is added in deionized water, ultrasonic disperse;
(2) vanadic anhydride, organic acid and ammonium tungstate are taken again, is added in system obtained by step (1), and stirring obtains precursor liquid;
(3) precursor liquid obtained by step (2) is transferred in reaction kettle and carries out hydro-thermal reaction;
(4) gained mixed liquor after step (3) reaction is successively carried out after cooling down, washing, be centrifugated, dry, is calcined, is obtained
To tungsten-doped vanadium dioxide/graphene complex.
2. the preparation method of tungsten-doped vanadium dioxide/graphene complex according to claim 1, which is characterized in that step
Suddenly in (1), the graphene oxide is two-dimensional stannic oxide/graphene nano piece.
3. the preparation method of tungsten-doped vanadium dioxide/graphene complex according to claim 1, which is characterized in that step
Suddenly in (1), the step of graphene oxide powder ultrasonic disperse, is as follows: 28-59kHz frequency is used, at 500W power ultrasound
Reason, processing time are 5-60min.
4. the preparation method of tungsten-doped vanadium dioxide/graphene complex according to claim 1, which is characterized in that step
Suddenly in (2), the mass ratio of the material of the vanadic anhydride and ammonium tungstate is 100:1-20:1.
5. the preparation method of tungsten-doped vanadium dioxide/graphene complex according to claim 1, which is characterized in that step
Suddenly in (2), the organic acid is one of citric acid and oxalic acid, wherein the mass ratio of the material of vanadic anhydride and citric acid
For 1:3, the mass ratio of the material with oxalic acid is 1:2.
6. the preparation method of tungsten-doped vanadium dioxide/graphene complex according to claim 1, which is characterized in that step
Suddenly in (3), the hydrothermal temperature of the hydro-thermal reaction is 180-200 DEG C, and the hydro-thermal time is 24-72h.
7. the preparation method of tungsten-doped vanadium dioxide/graphene complex according to claim 1, which is characterized in that step
Suddenly in (4), the calcination temperature is 550 DEG C -650 DEG C, calcination time 1.5h-2.5h.
8. a kind of tungsten-doped vanadium dioxide/graphene complex, which is characterized in that described in any item using claim 1-7
Tungsten-doped vanadium dioxide/graphene complex preparation method is prepared.
9. tungsten-doped vanadium dioxide/graphene complex answering in insulating moulding coating or thermal insulation film described in a kind of claim 8
With.
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CN114574169A (en) * | 2022-02-09 | 2022-06-03 | 中国科学院深圳先进技术研究院 | Vanadium dioxide-boron nitride phase-change heat-conducting composite material and preparation method and application thereof |
CN114574169B (en) * | 2022-02-09 | 2023-10-03 | 中国科学院深圳先进技术研究院 | Vanadium dioxide-boron nitride phase-change heat-conducting composite material and preparation method and application thereof |
WO2024040429A1 (en) * | 2022-08-23 | 2024-02-29 | 中国科学院深圳先进技术研究院 | Electromagnetic shielding composite material with temperature response characteristic, and preparation method therefor and application thereof |
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