CN106167414A - A kind of preparation method of the vanadium dioxide film with heat reflectivity response - Google Patents
A kind of preparation method of the vanadium dioxide film with heat reflectivity response Download PDFInfo
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- CN106167414A CN106167414A CN201610546626.1A CN201610546626A CN106167414A CN 106167414 A CN106167414 A CN 106167414A CN 201610546626 A CN201610546626 A CN 201610546626A CN 106167414 A CN106167414 A CN 106167414A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/82—Asbestos; Glass; Fused silica
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/62218—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic films, e.g. by using temporary supports
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
The invention discloses the preparation method of a kind of vanadium dioxide film with heat reflectivity response；Including the sintering of glass fabric after pre-treatment, dipping precursor solution and the dipping of glass fibre.The vanadium dioxide film that the present invention prepares has good hot photo absorption property, has the sudden change of reflectance near 38 DEG C.When temperature is less than 38 DEG C, reflectance is at high level, when temperature is higher than 38 DEG C, and reflectance is in low-level, and this performance is reversible.The response of its heat reflectivity is utilized to can apply in greenhouse the negative-feedback regu-lation to temperature so that indoor temperature can maintain near 38 DEG C, beneficially the growth of greenhouse implants.The preparation method of the disclosed vanadium dioxide film having heat reflectivity response for carrier with glass fabric has the advantages such as energy-conservation, cheap, safe, simple, stable and the shortest.
Description
Technical field
The present invention relates to vanadium dioxide film and preparation method thereof, have for carrier with glass fibre particularly to one
The preparation method of the vanadium dioxide film of heat-reflectivity responses.
Background technology
Vanadium dioxide film is because of its relatively low phase transition temperature (about 68 DEG C), thus is paid close attention to widely.At phase alternating temperature
Near degree, its transformation rate is exceedingly fast, and after undergoing phase transition, its optical property, electric property, thermal conductivity and pcrmeability etc. can occur
Sudden change, therefore vanadium dioxide film has the highest using value at hot light, thermoelectricity, thermal-magnetizing material.But its phase transition temperature
Far above room temperature, it is impossible to the temperature negative-feedback regu-lation in greenhouse.
The method preparing vanadium dioxide film mainly has chemical gaseous phase deposition (CVD), ion sputtering and sol-gal process.
Sol-gal process is considered as a kind of the easiest method.
The domestic research for glass fibre is mainly used in the research of structural material, and the research to functional material is merely better than
Nothing.By finding the retrieval of existing patent documentation, the Chinese invention patent application of Application No. 201410236112.7 is open
A kind of Inorganic sol-gel preparation method of vanadium dioxide film；Obtained vanadium dioxide film optics performance of control is excellent
Different, it is seen that light transmittance reaches as high as 70%, and infrared regulation performance reaches as high as 60%, has wide in photoelectric functional material field
Application prospect.But, the substrate that this invention uses is transparent substrates, it is impossible to be applied to reflect the regulation of light；Furthermore, this invention is thin
Film needs to sinter under ventilation atmosphere, compared with the present invention, more complicated.Secondly, the phase transition temperature of this invention is 60～65 DEG C, nothing
Method is used in the temperature in controllable greenhouse.
Summary of the invention
It is an object of the invention to overcome phase transition temperature of vanadium dioxide to be too high to temperature negative feedback in greenhouse adjust
The defect of joint, it is provided that a kind of phase transition temperature is the vanadium dioxide with glass fibre for carrier with heat-reflectivity responses of 38 DEG C
The preparation method of thin film；The present invention utilizes glass fabric for carrier, utilizes sol-gal process, at its area load multilayer colloid
Thin film, is then sintered.The method has the advantages such as energy-conservation, cheap, safe, simple, stable and the shortest.
It is an object of the invention to be achieved through the following technical solutions:
The present invention relates to the preparation method of a kind of vanadium dioxide film with heat-reflectivity responses, with glass fabric
For carrier, sol-gal process is utilized to load multi-layer H at this carrier surfacexV2O5Presoma colloid, high temperature sintering, obtain described with
Glass fibre is the vanadium dioxide film that carrier has heat-reflectivity responses.
Preferably, described method comprises the steps:
S1, glass fabric is carried out pre-treatment, remove the wetting agent on its surface；
S2, by V2O5Powder heating prepares melted V2O5After, pour cold quenching-in water into and obtain HxV2O5Presoma colloid；
S3, by step S1 process after glass fabric immerse HxV2O5Presoma colloid, takes out and is dried；Repeatedly soak
Enter, drying process；
S4, step S3 gained glass fabric is carried out high temperature sintering under vacuum, be cooled to room temperature, obtain described
Vanadium dioxide film.
Preferably, in step S1, described glass fabric is alkali-free E type glass fabric.
Preferably, the density of described alkali-free E type glass fabric is 100～200m2/g。
Preferably, in step S1, described pre-treatment includes: glass fabric heats in the environment of 500～550 DEG C 2
～2.5h；It is then sonicated 1～2h.The purpose of pre-treatment is to remove the wetting agent of fiberglass surfacing and improve its surface to inhale
Attached performance；Heating the wetting agent on 2～2.5h removable surfaces at 500～550 DEG C, ultrasonic 1～2h adheres to leaching thereon to remove
Profit agent residue.
Preferably, in step S2, described heating is to be incubated 20～40min at 750～850 DEG C.More preferably 800 DEG C insulations
30min。
Preferably, described V2O5Powder is 1g:(20～100 with the amount ratio of cold water) ml.More preferably 1g:60ml.
Preferably, in step S2, the time every time immersed is 8～12 seconds, repeats immersion, drying process 8～12 times.More excellent
The time that choosing is immersed every time is 10 seconds, repeats immersion, drying process 10 times.
Preferably, in step S3, described vacuum condition is that vacuum is less than 10-2Pa。
Preferably, in step S3, described high temperature sintering includes: with the heating rate of 8～10 DEG C/min, from room temperature to
300～600 DEG C, then keep 1～5h at maximum temperature.More preferably 8 DEG C/min is warmed up to 500 DEG C, is incubated 1.5h.
Preferably, the thickness of described vanadium dioxide film is 130～200 μm.
Preferably, the phase transition temperature of described vanadium dioxide film is 38 DEG C.
The invention still further relates to the purposes of the vanadium dioxide film that a kind of above-mentioned preparation method prepares, described vanadium dioxide is thin
Film is applied in greenhouse temperature is carried out negative-feedback regu-lation.
The mechanism of described negative-feedback regu-lation is: temperature is less than 38 DEG C, and product reflectance is high, and the heat being reflected back greenhouse is high,
Temperature raises；Temperature is higher than 38 DEG C, and product reflectance is low, and the heat being reflected back greenhouse is low, and temperature reduces；Finally can maintain greenhouse
Room temperature near 38 DEG C.
The vanadium dioxide film that the present invention prepares has good hot photo absorption property, has reflectance near 38 DEG C
Sudden change: when temperature is less than 38 DEG C, reflectance is at high level, when temperature is higher than 38 DEG C, and reflectance is in low-level, and this
Performance is reversible；The negative-feedback regu-lation to temperature is can apply in greenhouse so that room hence with its heat-reflectivity responses
Interior temperature can maintain near 38 DEG C, beneficially the growth of greenhouse implants.
Compared with prior art, there is advantages that
1, the present invention is by controlling process conditions and parameter, it is thus achieved that have 4%V5+The vanadium dioxide film of doping, so that
Obtain its phase transition temperature and be reduced to 38 DEG C, can apply to the temperature negative-feedback regu-lation system in greenhouse.；
2, glass fabric is carrier by the present invention, on the one hand stable because of it, sintering process not with colloid reaction；Another
Aspect, the flexibility of glass fabric can make it easily be layered on inside greenhouse；
3, the feature that the vanadium dioxide film of the present invention has heat-reflectivity responses, performance is reversible, chemical stability is strong；
Except its heat-reflectivity responses can be utilized to be applied to the negative-feedback regu-lation of temperature in greenhouse, it is also possible to utilize glass fabric
Flexibility it can be produced in enormous quantities and the facility of tiling in greenhouse；
4, the preparation method of the present invention has the advantages such as energy-conservation, cheap, safe, simple, stable and the shortest.
Accompanying drawing explanation
By the detailed description non-limiting example made with reference to the following drawings of reading, the further feature of the present invention,
Purpose and advantage will become more apparent upon:
Fig. 1 is the super depth of field (VHX) figure of embodiment of the present invention products therefrom, and wherein, a is bare glass fibre low power figure, b
For the vanadium dioxide film low power figure of the present invention, c is high power figure in bare glass fibre, and d is the vanadium dioxide film of the present invention
Middle high power figure, e is that bare glass fibre is appeared place's high power figure, and f is that the attachment vanadium dioxide film of the present invention is appeared glass high power
Figure；
Fig. 2 is the SEM figure of embodiment of the present invention products therefrom, and wherein, a is bare glass fibre SEM figure, and b is the present invention
Vanadium dioxide film be attached on glass SEM figure；
Fig. 3 is the XPS figure of embodiment of the present invention products therefrom；
Fig. 4 is the TEM figure of embodiment of the present invention products therefrom；
Fig. 5 is HRTEM and the SAED figure of embodiment of the present invention products therefrom；Wherein, a is HRTEM figure, and b is SAED figure；
Fig. 6 is the angular resolution temperature-wavelength-reflectance circle of equal altitudes of embodiment of the present invention products therefrom, and incident illumination is vertical
Incidence, reflection light changes with the change of test angles；Wherein, temperature-wavelength-reflectance circle of equal altitudes when a is angle of reflection 0 °, b
For temperature-wavelength-reflectance circle of equal altitudes during angle of reflection 20 °, temperature-wavelength-reflectance circle of equal altitudes when c is angle of reflection 40 °,
Temperature-wavelength-reflectance circle of equal altitudes when d is angle of reflection 60 °；Reflection light changes with the change of test angles；
Fig. 7 is the temperature-wavelength-reflectance circle of equal altitudes of embodiment of the present invention products therefrom；
Fig. 8 is that total reflex strength of embodiment of the present invention products therefrom varies with temperature figure.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail.Following example will assist in those skilled in the art
It is further appreciated by the present invention, but limits the present invention the most in any form.It should be pointed out that, to those of ordinary skill in the art
For, without departing from the inventive concept of the premise, it is also possible to make certain adjustments and improvements.These broadly fall into the guarantor of the present invention
Protect scope.
Embodiment 1
Select 100m2/ g alkali-free E type glass fabric is carrier, and first carrier is placed in heat under the conditions of Muffle furnace 500 DEG C
Process 2h, to remove the wetting agent of fiberglass surfacing, the ultrasonic 1h of glass fabric after processing the most again, removes further
Remain in the wetting agent of fiberglass surfacing.By 5g V2O5Powder is placed in Muffle furnace and heats 30min at 800 DEG C, is melted
V2O5, pour into rapidly in 300ml cold distilled water and quench, stir 10min, filter removal residue and obtain brown sol solutions, this colloidal sol
Liquid solute main component is HxV2O5.Glass fabric through pre-treatment is impregnated 10s in the sol solutions such as prepared, then
Glass fibre is arranged in baking oven drying, and oven temperature is set to 60 DEG C, repeats above operation 10 times, obtains dark brown glass
Fiber cloth.Dark brown glass fabric piezoid is clamped, puts in quartz cell, and add a cover.Quartz cell is carefully placed into vacuum
In stove, it is evacuated to 10-2Pa.The temperature of vacuum drying oven is from room temperature to 500 DEG C, and is incubated 2h, heating rate be set to 8 DEG C/
Min, then cools to room temperature with stove.The product obtained is shown in (b), (d), (f) in Fig. 1.One layer two of glass fabric surface
Vanadium oxide is the thinnest, and therefore it can also be seen that the braiding structure of glass fabric, color is navy blue.Can be measured by the SEM figure of Fig. 2
Going out, film thickness scope is in 130-200 μm.Schemed it can be seen that thin film is mainly by V by the XPS of Fig. 34+And V5+Constitute, wherein V4+
The ratio accounted for is 96%.By the TEM of Fig. 4 it can be seen that the thickness range of thin film is in 130-200 μm；The HRTEM of Fig. 5 can see
Go out, VO in thin film2It is the VO with phase transition temperature mutually2Phase.The heat of product-reflectivity responses performance can be from Fig. 6, Fig. 7 and Fig. 8
Embody.Fig. 6 is the angular resolution temperature-wavelength-reflectance circle of equal altitudes of product, it can be seen that in any angle
Under reflection light, its heat-reflectivity responses performance is consistent: under 650～850nm wave bands, the reflection when temperature is less than 38 DEG C
Rate is in a high position, and when temperature is higher than 38 DEG C, reflectance declines about 30%.Illustrate the performance of its heat-reflectivity responses not with
Reflect the change of angular and disappear.Fig. 7 is temperature-wavelength-reflectance circle of equal altitudes that product is total, in its situation of change and Fig. 4
Consistent；Fig. 8 is that total reflex strength varies with temperature figure, it can be seen that undergo mutation 38 DEG C of its reflex strengths, reflex strength
Reduce by 22%.This preparation method is without using special installation, and energy consumption is low, and products obtained therefrom is cheap.
Embodiment 2
Select 120m2/ g alkali-free E type glass fabric is carrier, and first carrier is placed in heat under the conditions of Muffle furnace 450 DEG C
Process 3h, to remove the wetting agent of fiberglass surfacing, the ultrasonic 2h of glass fabric after processing the most again, removes further
Remain in the wetting agent of fiberglass surfacing.By 5g V2O5Powder is placed in Muffle furnace and heats 40min at 750 DEG C, is melted
V2O5, pour into rapidly in 100ml cold distilled water and quench, stir 10min, filter removal residue and obtain brown sol solutions, this colloidal sol
Liquid solute main component is HxV2O5.Glass fabric through pre-treatment is impregnated 8s in the sol solutions such as prepared, then will
Glass fibre is arranged in baking oven drying, and oven temperature is set to 55 DEG C, repeats above operation 8 times, obtains dark brown glass fibers
Wei Bu.Dark brown glass fabric piezoid is clamped, puts in quartz cell, and add a cover.Quartz cell is carefully placed into vacuum drying oven
In, it is evacuated to 10-2Pa.The temperature of vacuum drying oven is from room temperature to 600 DEG C, and is incubated 1h, heating rate be set to 6 DEG C/
Min, then cools to room temperature with stove, obtains product.Angular resolution temperature-contour the relation of wavelength-reflectance investigating this product understands,
Under the reflection light of any angle, its heat-reflectivity responses performance is consistent: under 650～850nm wave bands, when temperature is low
In 38 DEG C time, reflectance is in a high position, and when temperature is higher than 38 DEG C, reflectance declines about 25%；Investigate total reflection of this product
Intensity varies with temperature relation and understands, and undergos mutation 38 DEG C of its reflex strengths, and reflex strength reduces by 20%.
Embodiment 3
Select 80m2/ g alkali-free E type glass fabric is carrier, is first placed in by carrier under the conditions of Muffle furnace 550 DEG C at heat
Reason 1h, to remove the wetting agent of fiberglass surfacing, the ultrasonic 1.5h of glass fabric after processing the most again, removes further
Remain in the wetting agent of fiberglass surfacing.By 5g V2O5Powder is placed in Muffle furnace and heats 20min at 850 DEG C, is melted
V2O5, pour into rapidly in 500ml cold distilled water and quench, stir 10min, filter removal residue and obtain brown sol solutions, this colloidal sol
Liquid solute main component is HxV2O5.Glass fabric through pre-treatment is impregnated 12s in the sol solutions such as prepared, then
Glass fibre is arranged in baking oven drying, and oven temperature is set to 65 DEG C, repeats above operation 12 times, obtains dark brown glass
Glass fiber cloth.Dark brown glass fabric piezoid is clamped, puts in quartz cell, and add a cover.Quartz cell is carefully placed into very
In empty stove, it is evacuated to 10-2Pa.The temperature of vacuum drying oven is from room temperature to 300 DEG C, and is incubated 5h, and heating rate is set to 12
DEG C/min, then cool to room temperature with stove, obtain product.Investigate this product angular resolution temperature-the contour relation of wavelength-reflectance can
Knowing, under the reflection light of any angle, its heat-reflectivity responses performance is consistent: under 650～850nm wave bands, work as temperature
During less than 38 DEG C, reflectance is in a high position, and when temperature is higher than 38 DEG C, reflectance declines about 26%；Investigate the total anti-of this product
Penetrating intensity to vary with temperature knowable to relation, undergo mutation 38 DEG C of its reflex strengths, reflex strength reduces by 18%.
Above the specific embodiment of the present invention is described.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformation or amendment within the scope of the claims, this not shadow
Ring the flesh and blood of the present invention.
Claims (10)
1. have a preparation method for the vanadium dioxide film of heat-reflectivity responses with glass fibre for carrier, its feature exists
In, with glass fabric as carrier, utilize sol-gal process to load multi-layer H at this carrier surfacexV2O5Presoma colloid, high temperature
Sintering, obtains the described vanadium dioxide film with glass fibre for carrier with heat-reflectivity responses.
2. the preparation of the vanadium dioxide film with glass fibre for carrier with heat-reflectivity responses as claimed in claim 1
Method, it is characterised in that described method comprises the steps:
S1, glass fabric is carried out pre-treatment, remove the wetting agent on its surface；
S2, by V2O5Powder heating prepares melted V2O5After, pour cold quenching-in water into and obtain HxV2O5Presoma colloid；
S3, by step S1 process after glass fabric immerse HxV2O5Presoma colloid, takes out and is dried；Repeatedly immerse, do
Dry operation；
S4, step S3 gained glass fabric is carried out high temperature sintering under vacuum, be cooled to room temperature, obtain described dioxy
Change vanadium thin film.
3. the preparation of the vanadium dioxide film with glass fibre for carrier with heat-reflectivity responses as claimed in claim 2
Method, it is characterised in that in step S1, described glass fabric is alkali-free E type glass fabric；Described alkali-free E type glass fibers
The density of dimension cloth is 100～200m2/g。
4. the preparation of the vanadium dioxide film with glass fibre for carrier with heat-reflectivity responses as claimed in claim 2
Method, it is characterised in that in step S1, described pre-treatment includes: glass fabric heats in the environment of 500～550 DEG C 2
～2.5h；It is then sonicated 1～2h.
5. the preparation of the vanadium dioxide film with glass fibre for carrier with heat-reflectivity responses as claimed in claim 2
Method, it is characterised in that described V2O5Powder is 1g:(20～100 with the amount ratio of cold water) ml.
6. the preparation of the vanadium dioxide film with glass fibre for carrier with heat-reflectivity responses as claimed in claim 2
Method, it is characterised in that in step S2, the time every time immersed is 8～12 seconds, repeats immersion, drying process 8～12 times.
7. the preparation of the vanadium dioxide film with glass fibre for carrier with heat-reflectivity responses as claimed in claim 2
Method, it is characterised in that in step S3, described vacuum condition is that vacuum is less than 10-2Pa。
8. the preparation of the vanadium dioxide film with glass fibre for carrier with heat-reflectivity responses as claimed in claim 2
Method, it is characterised in that in step S3, described high temperature sintering includes: with the heating rate of 8～10 DEG C/min, from room temperature
To 300～600 DEG C, then keep 1～5h at maximum temperature.
9. the preparation of the vanadium dioxide film with glass fibre for carrier with heat-reflectivity responses as claimed in claim 2
Method, it is characterised in that the thickness of described vanadium dioxide film is 130～200 μm, phase transition temperature is 38 DEG C.
10. the purposes of the vanadium dioxide film that a preparation method as claimed in claim 1 prepares, it is characterised in that described two
Vanadium oxide film is applied in greenhouse temperature is carried out negative-feedback regu-lation.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110551459A (en) * | 2019-09-27 | 2019-12-10 | 武汉工程大学 | Temperature-control glass film and thermochromic intelligent window |
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| CN106167414B (en) | 2020-02-21 |
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