CN107804872A - A kind of rutile phase hypovanadic oxide of porous laminated structure and preparation method thereof - Google Patents
A kind of rutile phase hypovanadic oxide of porous laminated structure and preparation method thereof Download PDFInfo
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- CN107804872A CN107804872A CN201610810435.1A CN201610810435A CN107804872A CN 107804872 A CN107804872 A CN 107804872A CN 201610810435 A CN201610810435 A CN 201610810435A CN 107804872 A CN107804872 A CN 107804872A
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Abstract
The present invention relates to a kind of rutile phase hypovanadic oxide of porous laminated structure and preparation method thereof, the sandwich construction that cellular construction of the rutile phase hypovanadic oxide of the porous laminated structure for single layered porous or the cellular construction accumulation by the single layered porous form, the cellular construction of the single layered porous are interconnected to form the stratiform two-dimensional structure with hole by particulate oxidation vanadium.The rutile phase hypovanadic oxide of porous laminated structure prepared by the present invention is that nanometer emptying aperture is combined to inside nano-powder so that the rutile phase hypovanadic oxide material of porous laminated structure improves visible light transmissivity while the solar energy regulation efficiency for ensureing material is constant.
Description
Technical field
The present invention relates to a kind of rutile phase hypovanadic oxide, and in particular to a kind of Rutile Type dioxy of porous laminated structure
Change vanadium and preparation method thereof, belong to Material Field.
Background technology
Due to the sustainable growth of world energy consumption, make the development of utilization and new technology of the people to novel renewable energy
Generate urgent demand.The discharge of carbon dioxide and other dusty gas not only causes pollution to environment, to the body of people
Body health also result in influence.Therefore, the demand to the energy and utilization become one of factor for improving people's living standard, section
Energy emission reduction has become the current top priority in various countries.It is estimated that it is building energy consumption to have more than 1/3 in social total energy consumption, therefore
It is one of energy-saving and emission-reduction, the emphasis for realizing sustainable development to promote building energy conservation.Because significant portion is used for sky in building energy consumption
Adjust, more than half in air conditioner energy source is lost in by window and extraneous heat exchange, therefore the intelligent power saving for passing through development of new
Window, energy consumption can be effectively reduced, reduce the discharge of greenhouse gases, be finally reached the purpose of energy-conserving and environment-protective.
At present, the energy-saving glass of market sale or energy-conservation pad pasting (abbreviation Energy Saving Windows) belong to low-launch-rate (Low~E)
Category, be characterized in that there is higher visible light transmissivity and relatively low far infrared transmissivity (winter is heat-insulated), can realize every
While heat insulation, carry out the infrared part in sunshine high blocking (being suitable for hot area) or high transmission (is suitable for trembling with fear
Cryogenic region).But its price is higher and can not carry out real-time monitoring to sunshine with the change of ambient temperature, belongs to " passive
Response " type, it is difficult to adapt to the most of climatic environments cold in winter and hot in summer in China.Other " active response " type energy-saving glass, such as
Electrochomeric glass, gas-discoloration glass, its is complicated, involves great expense, and is difficult popularization in a short time.By contrast, utilize
The thermochromism energy-saving glass of huge optical change development caused by vanadium dioxide phase transformation, due to the temperature change that can accord with one's environment
Realize that photo-thermal transflector automatically adjusts, without any artificial energy source, it is considered to be one of energy-saving glass material of most low-carbon environment-friendly.
Preparing thermochromism intelligent glass has two ways, i.e., prepares vanadium dioxide plated film glass using extensive magnetron sputtering
The physics preparation method of glass and vanadium dioxide nano powder is prepared with chemical means using nanometer technology in advance, then by nano-powder
Chemical preparation mode as pad pasting energy-saving glass is prepared by modes such as chemicalpistons.Compared with former mode, Hou Zheyou
Simple in equipment, generality is strong, cheap, is easy to large area production, and the remarkable advantage of wide application, it is easier to be market
Receive.But because vanadium oxygen system classes of compounds is various, only vanadium dioxide composition just has a variety of isomerism crystal knots
Structure, how extensive titania phase hypovanadic oxide powder is always challenge to research and production.Titania phase at present
Hypovanadic oxide powder is broadly divided into two methods：One kind is direct synthesis technique.Such as patent (Chinese invention patent publication number
CN102120615A) and document (Solar Energy Materials＆Solar Cells 95 (2011) 3520) utilizes hydro-thermal
Method handles 24 hours one-step synthesis rutile phase hypovanadic oxide powders more than 260 DEG C.Patent (Chinese invention patent publication number
CN104724757A solvent thermal reaction one-step synthesis rutile phase hypovanadic oxide powder at a lower temperature) is passed through.Another kind is
Vanadium dioxide presoma is first synthesized, then passes through the means titania phase hypovanadic oxide powders such as heat treatment or hydro-thermal again.Such as
Patent (Chinese invention patent publication number CN101863511A), B phases VO is obtained first with hydro-thermal method2Powder, then by above-mentioned powder
It is encapsulated in closed resistant to elevated temperatures container, is annealed in the range of 350~1200 DEG C, acquires rutile phase hypovanadic oxide powder
Body.Obtained as patent (Chinese invention patent publication number CN102120614) handles the tetravalent vanadium ion aqueous solution using alkaline reagent
Suspension presoma, is then transferred to hydrothermal reaction kettle by suspension, and required titanium dioxide can be made through hydro-thermal reaction, dry separation
Vanadium powder body.As document (Materials Research Bulletin 40 (2005) 315) first with hydro-thermal method synthesizes (NH4)0.5V2O5Nano wire, then above-mentioned powder is encapsulated in quartz ampoule, annealed two hours at 570 DEG C, obtain VO2Nano wire, and
Its electrology characteristic is characterized, and does not apply and is preparing energy-saving coatings, the related neck of energy-conservation pad pasting or energy-saving glass etc.
Domain.
The final application of nano-powder is compound with filmogen, is prepared into intelligent power saving coating, passes through different film forming
Means are prepared into intelligent power saving film.Weigh vanadium dioxide energy-conservation film properties refer mainly to indicate solar energy regulation rate and visible ray is saturating
Cross rate.And solar energy regulation rate is improved by improving vanadium dioxide solid content, it can seriously reduce the visible light transmissivity of film.
Solution at present, scheme one are to reduce the size of nano-powder, and scheme two is to introduce nanometer emptying aperture.For scheme two,
There are some patents to make report with document, will such as document (ACS Appl.Mater.Interfaces 2011,3,135-138)
The precursor liquid of organic film former and tetravalent vanadium ion is compound to be prepared into vanadium dioxide coating liquid, is obtained after film forming by high-temperature process
Vanadium dioxide energy-saving film, due to the presence of organic matter, substantial amounts of emptying aperture is formd after high-temperature process, it will be apparent that improve film
Visible light transmissivity, but this method can not mass produce, it is necessary to which high-temperature process, application are single；Such as document
(Materials Letters 110 (2013) 241-244), the precursor B phase hypovanadic oxide first synthesized, in Surface coating dioxy
SiClx, by heat treatment, laminar VO2 (M) the@SiO2 nano-powders that nanometer emptying aperture be present are obtained, successfully draw nanometer emptying aperture
Enter into nano-powder, but this nanometer emptying aperture is dispersed between stratum nucleare and shell, it is necessary to coat processing, cumbersome,
Condition is harsh.
The content of the invention
In view of the above-mentioned problems, it is an object of the invention to provide a kind of rutile phase hypovanadic oxide of porous laminated structure and
Its preparation method.
On the one hand, the invention provides a kind of rutile phase hypovanadic oxide of porous laminated structure, the porous laminated knot
What cellular construction of the rutile phase hypovanadic oxide of structure for single layered porous or the cellular construction accumulation by the single layered porous formed
Sandwich construction, the cellular construction of the single layered porous are interconnected to form the stratiform two dimension knot with hole by particulate oxidation vanadium
Structure.
The rutile phase hypovanadic oxide of porous laminated structure prepared by the present invention is that nanometer emptying aperture is combined into nano-powder
It is internal so that the rutile phase hypovanadic oxide material of porous laminated structure is in constant same of the solar energy regulation efficiency for ensureing material
Shi Tigao visible light transmissivities.
It is preferred that the particle size of the particulate oxidation vanadium in the rutile phase hypovanadic oxide of the porous laminated structure is
100nm~2 μm, preferably 100nm~1 μm, pore-size are 20nm~150nm, preferably 20nm~80nm, porosity ranges 1%
~20%, preferably 10%~20%.
It is preferred that stratiform thickness >=200nm, preferably 200nm of the rutile phase hypovanadic oxide of the porous laminated structure
~2 μm, the ratio of most long one side and stratiform thickness is (1~100)：1, preferably (10~60)：1.
On the other hand, present invention also offers a kind of preparation method of the rutile phase hypovanadic oxide of porous laminated structure,
Including：
The ammonium vanadium bronze phase (NH of layer structure4)0.6V2O5The preparation of vanadium dioxide presoma；
By the ammonium vanadium bronze phase (NH of layered structure4)0.6V2O5Vanadium dioxide presoma is in vacuum at 400~900 DEG C
Heat treatment 5~120 minutes, obtains the rutile phase hypovanadic oxide of porous laminated structure.
It is preferred that the ammonium vanadium bronze phase (NH of layer structure is synthesized using hydro-thermal method4)0.6V2O5Vanadium dioxide presoma.
Also, it is preferred that using ammonium metavanadate and formic acid as raw material, hydro-thermal reaction 6~100 hours, are obtained at 220~300 DEG C
To the ammonium vanadium bronze phase (NH of layered structure4)0.6V2O5Vanadium dioxide presoma, wherein the ammonium metavanadate and formic acid rub
You are than being 3.3:1~1:2.6.
The rutile phase hypovanadic oxide powder of the porous laminated structure of gained of the invention can be used for energy-saving coatings, energy-conservation pad pasting
Or the association area such as energy-saving glass.Present invention process is simple, cost is low, reproducible, high income, course of reaction safety, is not required to
Protection of reducing atmosphere is wanted, is adapted to large-scale production, the hypovanadic oxide powder good dispersion obtained, stability height.
Brief description of the drawings
Fig. 1 is the XRD of vanadium dioxide presoma prepared by embodiment 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of vanadium dioxide presoma prepared by embodiment 1；
Fig. 3 is the XRD of the rutile phase hypovanadic oxide of porous laminated structure prepared by embodiment 1；
Fig. 4 is the scanning electron microscope (SEM) photograph of the rutile phase hypovanadic oxide of porous laminated structure prepared by embodiment 1；
Fig. 5 be film obtained by the rutile phase hypovanadic oxide powder of porous laminated structure prepared by embodiment 1 at 25 DEG C and
Optical transmittance curve at a temperature of 90 DEG C；
Fig. 6 is the XRD of vanadium dioxide presoma prepared by embodiment 2；
Fig. 7 is the scanning electron microscope (SEM) photograph of vanadium dioxide presoma prepared by embodiment 2；
Fig. 8 is the XRD of the rutile phase hypovanadic oxide of porous laminated structure prepared by embodiment 2；
Fig. 9 is the scanning electron microscope (SEM) photograph of the rutile phase hypovanadic oxide of porous laminated structure prepared by embodiment 2；
Figure 10 is to implement film obtained by the rutile phase hypovanadic oxide powder of the 2 porous laminated structures prepared at 25 DEG C and 90
Optical transmittance curve at a temperature of DEG C；
Figure 11 is the XRD of vanadium dioxide presoma prepared by embodiment 3；
Figure 12 is the scanning electron microscope (SEM) photograph of vanadium dioxide presoma prepared by embodiment 3；
Figure 13 is the XRD of the rutile phase hypovanadic oxide of porous laminated structure prepared by embodiment；
Figure 14 is the scanning electron microscope (SEM) photograph of the rutile phase hypovanadic oxide of porous laminated structure prepared by embodiment 3；
Figure 15 be film obtained by the rutile phase hypovanadic oxide powder of porous laminated structure prepared by embodiment 3 at 25 DEG C and
Optical transmittance curve at a temperature of 90 DEG C.
Embodiment
The present invention is further illustrated below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, is not intended to limit the present invention.
The present invention is by by ammonium vanadium bronze phase (NH4)0.6V2O5The step of vanadium dioxide presoma one is heat-treated, and obtains having porous
The rutile phase hypovanadic oxide powder of layer structure, its sandwich are the cellular construction of single layered porous or the list of single layered porous
The sandwich construction that meta structure accumulation forms.
In the present invention, the cellular construction of the single layered porous is to be interconnected to form stratiform two dimension knot by particulate oxidation vanadium
Structure, and a large amount of holes in structure be present.Particulate oxidation vanadium obtains particle size 100nm~2 μm, and pore-size 20nm~
150nm, porosity ranges 1%~20%.
In the present invention, stratiform thickness >=200nm of the rutile phase hypovanadic oxide of the porous laminated structure, preferably
200nm~2 μm.The ratio of most long one side and stratiform thickness can be (1~100)：1, preferably (10~60)：1.
Illustrate to following exemplary that the present invention provides the preparation method of the rutile phase hypovanadic oxide of porous laminated structure.
Synthesize the ammonium vanadium bronze phase (NH of layer structure4)0.6V2O5Vanadium dioxide presoma.Specifically, hydro-thermal is first passed through
Reaction is contained (NH4)0.6V2O5The mixed solution (alternatively referred to as hydro-thermal reaction solution) of powder, then by gained hydro-thermal reaction solution
The ammonium vanadium bronze phase (NH obtained after filtering (filtering) and drying4)0.6V2O5Powder (ammonium vanadium bronze phase (NH4)0.6V2O5Vanadium dioxide
Presoma).
As an example, using ammonium metavanadate and formic acid as raw material, the hydro-thermal reaction 6-100h at 220-300 DEG C.Inclined vanadium
The mol ratio of sour ammonium and formic acid is 3.3:1-1:2.6.
To ammonium vanadium bronze phase (NH4)0.6V2O5Vanadium dioxide presoma is heat-treated, and obtains the golden red of porous laminated structure
Stone phase hypovanadic oxide.Heat treatment is to carry out under vacuo.Heat treatment temperature can be 400-900 DEG C.Heat treatment time can be 5-120
Minute.
The hypovanadic oxide powder good dispersion that the present invention is obtained, stability are high；Preparation method is also easy, cost is low, repeats
Property good, high income, be adapted to large-scale production.Powder prepared by the present invention can be widely used for the energy-saving coatings of building and automobile,
Save the association area such as pad pasting and energy-saving glass.
Embodiment is enumerated further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this
Invention is further described, it is impossible to is interpreted as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made belong to protection scope of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by this paper explanation
In the range of select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
Step A) 1.733g ammonium metavanadates and 0.205g formic acid are weighed, stirred 10 minutes in 40mL deionized waters.It is transferred to 100mL
In water heating kettle, reacted 6 hours under the conditions of 300 DEG C, after cold filtration clean dry, obtain vanadium dioxide presoma；
Step B) appropriate above-mentioned vanadium dioxide presoma is weighed, 400 DEG C are warming up under vacuum, are incubated 120 minutes, cooling
The rutile phase hypovanadic oxide powder of porous laminated structure is obtained afterwards；
Using XRD, SEM and spectrophotometer are to step A) vanadium dioxide presoma, step B) porous laminated structure gold
The performance of red stone phase hypovanadic oxide powder is characterized.
Fig. 1 is by step A) XRD of vanadium dioxide presoma is obtained, display presoma is rendered as (NH4)0.6V2O5Single crystalline substance
Phase.
Fig. 2 is by step A) obtain the scanning electron microscope (SEM) photograph of vanadium dioxide presoma, display is in square brick layer structure, length-width ratio≤
2, thickness >=200nm, the ratio of most long one side and stratiform thickness is (1~100)：1.
Fig. 3 is by step B) obtain porous laminated structure rutile phase hypovanadic oxide XRD, show ammonium vanadium bronze
(NH4)0.6V2O5Vanadium dioxide presoma is all converted to rutile phase hypovanadic oxide powder.
Fig. 4 is by step B) obtain porous laminated structure rutile phase hypovanadic oxide scanning electron microscope (SEM) photograph, size and Re Chu
Change is little before reason, still keeps the layer structure of presoma, its thickness >=200nm, length-width ratio≤2, most long one side and stratiform
The ratio of thickness is (1~100)：1.Simultaneously because heat treatment has NH3Generation, make it have porous.Vanadium oxide particle size
100nm~2 μm, pore-size 20nm~150nm, porosity ranges 1%~20%.
Fig. 5 is film obtained by the rutile phase hypovanadic oxide powder of porous laminated structure at a temperature of 25 DEG C and 90 DEG C
Optical transmittance curve.The rutile phase hypovanadic oxide of synthesized porous laminated structure has thermal discoloration as seen from the figure
Energy.
Embodiment 2
Step A) 1.733g ammonium metavanadates and 1.77g formic acid are weighed, stirred 10 minutes in 40mL deionized waters.It is transferred to 100mL
In water heating kettle, reacted 100 hours under the conditions of 220 DEG C, after cold filtration clean dry, obtain vanadium dioxide presoma；
Step B) appropriate above-mentioned vanadium dioxide presoma is weighed, 900 DEG C are warming up under vacuum, 5 minutes are incubated, after cooling
Obtain the rutile phase hypovanadic oxide powder of porous laminated structure；
Using XRD, SEM and spectrophotometer are to step A) vanadium dioxide presoma, step B) porous laminated structure gold
The performance of red stone phase hypovanadic oxide powder is characterized.
Fig. 6 is by step A) XRD of vanadium dioxide presoma is obtained, display presoma is rendered as (NH4)0.6V2O5Single crystalline substance
Phase.
Fig. 7 is by step A) obtain the scanning electron microscope (SEM) photograph of vanadium dioxide presoma, display is in square brick layer structure, length-width ratio≤
2, thickness >=200nm, the ratio of most long one side and stratiform thickness is (2~80)：1.
Fig. 8 is by step B) obtain porous laminated structure rutile phase hypovanadic oxide XRD, show ammonium vanadium bronze
(NH4)0.6V2O5Vanadium dioxide presoma is all converted to rutile phase hypovanadic oxide powder.
Fig. 9 is by step B) obtain porous laminated structure rutile phase hypovanadic oxide scanning electron microscope (SEM) photograph, size and Re Chu
Change is little before reason, still keeps the layer structure of presoma, its thickness >=200nm, length-width ratio≤2, most long one side and stratiform
The ratio of thickness is (2~80)：1.Simultaneously because heat treatment has NH3Generation, make it have porous.Vanadium oxide particle size
100nm~2 μm, pore-size 20nm~150nm, porosity ranges 1%~20%.
Figure 10 is film obtained by the rutile phase hypovanadic oxide powder of porous laminated structure at a temperature of 25 DEG C and 90 DEG C
Optical transmittance curve.The rutile phase hypovanadic oxide of synthesized porous laminated structure has thermal discoloration as seen from the figure
Energy.The rutile phase hypovanadic oxide powder of structure.
Embodiment 3
Step A) 1.733g ammonium metavanadates and 1.0g formic acid are weighed, stirred 10 minutes in 40mL deionized waters.It is transferred to 100mL water
In hot kettle, reacted 50 hours under the conditions of 270 DEG C, after cold filtration clean dry, obtain vanadium dioxide presoma；
Step B) appropriate above-mentioned vanadium dioxide presoma is weighed, 750 DEG C are warming up under vacuum, are incubated 60 minutes, cooling
The rutile phase hypovanadic oxide powder of porous laminated structure is obtained afterwards；
Using XRD, SEM and spectrophotometer are to step A) vanadium dioxide presoma, step B) porous laminated structure gold
The performance of red stone phase hypovanadic oxide powder is characterized.
Figure 11 is by step A) XRD of vanadium dioxide presoma is obtained, display presoma is rendered as (NH4)0.6V2O5It is single
Crystalline phase.
Figure 12 is by step A) obtain the scanning electron microscope (SEM) photograph of vanadium dioxide presoma, display is in square brick layer structure, length-width ratio
≤ 2, thickness >=200nm, the ratio of most long one side and stratiform thickness is (1~100)：1.
Figure 13 is by step B) obtain porous laminated structure rutile phase hypovanadic oxide XRD, show ammonium vanadium bronze
(NH4)0.6V2O5Vanadium dioxide presoma is all converted to rutile phase hypovanadic oxide powder.
Figure 14 is by step B) obtain porous laminated structure rutile phase hypovanadic oxide scanning electron microscope (SEM) photograph, size and Re Chu
Change is little before reason, still keeps the layer structure of presoma, its thickness >=200nm, length-width ratio≤2, most long one side and stratiform
The ratio of thickness is (1~100)：1.Simultaneously because heat treatment has NH3Generation, make it have porous.Vanadium oxide particle size
100nm~2 μm, pore-size 20nm~150nm, porosity ranges 1%~20%.
Figure 15 is film obtained by the rutile phase hypovanadic oxide powder of porous laminated structure at a temperature of 25 DEG C and 90 DEG C
Optical transmittance curve.The rutile phase hypovanadic oxide of synthesized porous laminated structure has thermal discoloration as seen from the figure
Energy.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not limited to the substantial technological content model of the present invention
Enclose, substantial technological content of the invention is broadly to be defined in the right of application, any technology that other people complete
Entity or method, if with the right of application defined in it is identical, also or a kind of equivalent change, will
It is considered as being covered by among the right.
Claims (6)
- A kind of 1. rutile phase hypovanadic oxide of porous laminated structure, it is characterised in that the rutile of the porous laminated structure The sandwich construction that cellular construction of the phase hypovanadic oxide for single layered porous or the cellular construction accumulation by the single layered porous form, institute The cellular construction for stating single layered porous is interconnected to form the stratiform two-dimensional structure with hole by particulate oxidation vanadium.
- 2. the rutile phase hypovanadic oxide of porous laminated structure according to claim 1, it is characterised in that the porous layer The particle size of particulate oxidation vanadium in the rutile phase hypovanadic oxide of shape structure is 100nm~2 μm, pore-size 20 The nm of nm~150, porosity ranges 1%~20%.
- 3. the rutile phase hypovanadic oxide of porous laminated structure according to claim 1 or 2, it is characterised in that described more The nm of the stratiform thickness of the rutile phase hypovanadic oxide of hole layer structure >=200, length-width ratio≤2, most long one side and stratiform thickness Than for（1~100）：1.
- 4. a kind of preparation method of the rutile phase hypovanadic oxide of structure porous laminated as any one of claim 1-3, It is characterised in that it includes：The ammonium vanadium bronze phase (NH of layer structure4)0.6V2O5The preparation of vanadium dioxide presoma；By the ammonium vanadium bronze phase (NH of layered structure4)0.6V2O5Vanadium dioxide presoma is in vacuum at 400~900 DEG C Heat treatment 5~120 minutes, obtains the rutile phase hypovanadic oxide of porous laminated structure.
- 5. preparation method according to claim 4, it is characterised in that the ammonium vanadium bronze of layer structure is synthesized using hydro-thermal method Phase (NH4)0.6V2O5Vanadium dioxide presoma.
- 6. preparation method according to claim 5, it is characterised in that using ammonium metavanadate and formic acid as raw material, 220~ Hydro-thermal reaction 6~100 hours at 300 DEG C, obtain the ammonium vanadium bronze phase (NH of layered structure4)0.6V2O5Vanadium dioxide forerunner Body, wherein the mol ratio of the ammonium metavanadate and formic acid is 3.3:1~1:2.6.
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| CN108675350A (en) * | 2018-05-22 | 2018-10-19 | 湘潭大学 | A kind of spherical vanadium bronze ball of string sodium-ion battery positive material and preparation method thereof |
| CN112751014A (en) * | 2021-02-04 | 2021-05-04 | 江苏警官学院 | Aqueous energy storage battery based on layered vanadium oxide negative electrode |
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