CN109485097A - A kind of caesium hafnium tungsten bronze and the preparation method and application thereof - Google Patents
A kind of caesium hafnium tungsten bronze and the preparation method and application thereof Download PDFInfo
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- CN109485097A CN109485097A CN201811543293.2A CN201811543293A CN109485097A CN 109485097 A CN109485097 A CN 109485097A CN 201811543293 A CN201811543293 A CN 201811543293A CN 109485097 A CN109485097 A CN 109485097A
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- tungsten bronze
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/006—Compounds containing tungsten, with or without oxygen or hydrogen, and containing two or more other elements
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
本发明公开了一种铯铪钨青铜及其制备方法与应用，其中，所述铯铪钨青铜的化学式为CsyHfxW1‑xO3，其中0≤x≤0.30，0.20≤y≤0.33。本发明所述铯铪钨青铜用于隔热涂料或隔热薄膜的制备，提高隔热涂料或隔热薄膜的透光隔热性能。
The invention discloses a cesium hafnium tungsten bronze and a preparation method and application thereof, wherein the chemical formula of the cesium hafnium tungsten bronze is Cs y Hf x W 1-x O 3 , wherein 0≤x≤0.30, 0.20≤y≤ 0.33. The cesium hafnium tungsten bronze of the invention is used for the preparation of heat insulating paint or heat insulating film, and improves the light transmission and heat insulating performance of the heat insulating paint or heat insulating film.
Description
Technical field
The present invention relates to tungsten bronze fields more particularly to a kind of caesium hafnium tungsten bronze and the preparation method and application thereof.
Background technique
Modern architecture mansion is for fashion beauty and improves indoor lighting, largely slim, transparent outer using glass, film etc.
Portion's material traditional mud wall of substitution, but these common materials do not play barrier action to solar radiation, make interior instead
It heats up excessively high, leads to the increase of air conditioning energy consumption, the serious waste energy.Energy-saving and emission-reduction are to realize one of the requirement of sustainable development,
Building energy conservation and vehicle energy saving are the important components of energy-saving and emission-reduction.Currently, building energy conservation and vehicle energy saving are to merit attention
A problem, it is indoor with it is outdoor or it is interior with carry out what energy exchange was mainly carried out by door glass outside vehicle, building and
The interior very big reason of energy consumption increase is that common door and window can not make the exchange of indoor and outdoor energy be controlled effectively.Improve
The spectral selection of door glass is to reduce one of the important research field of energy consumption.
It is that thermal coefficient is lower that applying at present, which has two classes respectively in the material for the spectral selection for improving window body glass,
Bright heat-barrier material and transparent heat-insulated material with near-infrared screening performance, the lower transparent heat-insulated material of thermal coefficient it is heat-insulated
Performance is to be improved, and current research concentrates on improving near-infrared screening performance.
Tungsten bronze type material is a kind of transparent heat-insulated functional material of environment protecting and power-saving type, since it is relative to indium oxide
Tin (ITO), tin-antiomony oxide (ATO), LaB6With the transparent heat-insulated material such as Low-E glass have excellent near-infrared screening performance,
The advantages that hypotoxicity, simple low cost and synthesis technology, which is widely used, makees the heat-proof coating material of forms.Currently, about double-doped
The report of miscellaneous tungsten bronze is fewer, is concentrated mainly on solid phase method for the report of the tungsten bronze of alkali metal and transition metal codope
Preparation, but solid phase method preparation required temperature is higher, particle size is larger, dispersed not high.Meanwhile it being prepared in the prior art
Tungsten bronze powder applying the transparent heat-insulated performance in insulating moulding coating or thermal insulation film also to need to further increase.
Therefore, the existing technology needs to be improved and developed.
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 caesium hafnium tungsten bronzes and preparation method thereof
With application, it is intended to which tungsten bronze powder crystallinity is poor in the prior art, partial size is larger and dispersed not high and septum pellucidum for solution
The limited problem of hot property.
A kind of caesium hafnium tungsten bronze, wherein the chemical formula of the caesium hafnium tungsten bronze is CsyHfxW1-xO3, wherein 0≤x≤
0.30,0.20≤y≤0.33.
A kind of preparation method of caesium hafnium tungsten bronze, wherein include:
Step A, tungstate dihydrate acid sodium is dissolved, aqueous citric acid solution is added, cesiated salt solution is then added, mixed liquor is formed, by chlorine
Change hafnium ethanol solution to be added in the mixed liquor, obtains precursor liquid；
Step B, the precursor liquid is transferred in autoclave and carries out hydro-thermal reaction, obtain crude product；
Step C, the crude product is calcined under protective atmosphere, obtains caesium hafnium tungsten bronze.
The preparation method of the caesium hafnium tungsten bronze, wherein in the step A, the amount of the substance of the tungstate dihydrate acid sodium
Ratio with the sum of the amount of substance of hafnium chloride and the amount of the substance of the citric acid is 1:6.
The preparation method of the caesium hafnium tungsten bronze, wherein in the step A, the cesium salt is cesium carbonate or cesium chloride.
The preparation method of the caesium hafnium tungsten bronze, wherein in the step B, the temperature of the hydro-thermal reaction is 180 ~
200℃。
The preparation method of the caesium hafnium tungsten bronze, wherein in the step B, time of the hydro-thermal reaction is 48 ~
72h。
The preparation method of the caesium hafnium tungsten bronze, wherein in the step C, the temperature of the calcination is 500 ~ 800
℃。
The preparation method of the caesium hafnium tungsten bronze, wherein in the step C, the time of the calcining is 2 ~ 4h.
The preparation method of the caesium hafnium tungsten bronze, wherein in the step C, the protective atmosphere is inert gas gas
Atmosphere or reducing atmosphere.
A kind of application of caesium hafnium tungsten bronze as described above, wherein the caesium hafnium tungsten bronze is applied to insulating moulding coating or thin
In the preparation of film.
The utility model has the advantages that caesium hafnium tungsten bronze of the present invention is codope tungsten bronze powder, wherein the caesium hafnium tungsten bronze
Position of the doped chemical hafnium part substitution element tungsten in crystal, tungsten will form two Lacking oxygens and increases after being replaced by the hafnium of tetravalence
The concentration of carrier applies the light transmission thermal insulation that insulating moulding coating or thermal insulation film are improved in insulating moulding coating or thermal insulation film
Energy.Meanwhile the preparation method of the caesium hafnium tungsten bronze has simple process, clean and environmental protection, the low feature of production cost is prepared
Tungsten bronze powder have the advantages that crystallinity preferably, partial size it is smaller and dispersed high.
Detailed description of the invention
Fig. 1 is the XRD diagram of caesium hafnium tungsten bronze powder made from the embodiment of the present invention 1.
Fig. 2 is the EDS figure of caesium hafnium tungsten bronze powder made from the embodiment of the present invention 1.
Fig. 3 is the SEM figure of caesium hafnium tungsten bronze powder made from the embodiment of the present invention 1.
Fig. 4 is another SEM figure of caesium hafnium tungsten bronze powder made from the embodiment of the present invention 1.
Fig. 5 is another SEM figure of caesium hafnium tungsten bronze powder made from the embodiment of the present invention 1.
Fig. 6 is another SEM figure of caesium hafnium tungsten bronze powder made from the embodiment of the present invention 1.
Fig. 7 is the XRD diagram of caesium hafnium tungsten bronze powder made from the embodiment of the present invention 2.
Fig. 8 is the EDS figure of caesium hafnium tungsten bronze powder made from the embodiment of the present invention 2.
Fig. 9 is the SEM figure of caesium hafnium tungsten bronze powder made from the embodiment of the present invention 2.
Figure 10 is another SEM figure of caesium hafnium tungsten bronze powder made from the embodiment of the present invention 2.
Figure 11 is another SEM figure of caesium hafnium tungsten bronze powder made from the embodiment of the present invention 2.
Specific embodiment
The present invention provides a kind of caesium hafnium tungsten bronze and the preparation method and application thereof, to make the purpose of the present invention, technical solution
And effect is clearer, clear, the present invention is described in more detail below.It should be appreciated that specific implementation described herein
Example is only used to explain the present invention, is not intended to limit the present invention.
A kind of caesium hafnium tungsten bronze, wherein the chemical formula of the caesium hafnium tungsten bronze is CsyHfxW1-xO3, wherein 0≤x≤
0.30,0.20≤y≤0.33.
Caesium hafnium tungsten bronze of the present invention is to form codope tungsten bronze nano powder using transient metal doped caesium tungsten bronze
Body, wherein doped chemical hafnium part replaces position of the tungsten in crystal, so as to improve the performance of tungsten bronze.Caesium hafnium of the present invention
Tungsten bronze can effectively improve the transparent heat-insulated performance of glass or film.
A kind of preparation method of caesium hafnium tungsten bronze, wherein include:
Step A, tungstate dihydrate acid sodium is dissolved, aqueous citric acid solution is added, cesiated salt solution is then added, mixed liquor is formed, by chlorine
Change hafnium ethanol solution to be added in the mixed liquor, obtains precursor liquid；
Step B, the precursor liquid is transferred in autoclave and carries out hydro-thermal reaction, obtain crude product；
Step C, the crude product is calcined under protective atmosphere, obtains caesium hafnium tungsten bronze.
Caesium hafnium tungsten bronze powder is prepared using hydro-thermal method in the present invention, the preparation method have process flow it is simple,
The features such as at low cost, is suitble to industrialized production.And the caesium hafnium tungsten bronze powder being prepared has crystallinity is preferable, partial size is small and
The relatively good advantage of dispersibility.
Preferably, in the step A, the sum of amount of substance of the amount of the substance of the tungstate dihydrate acid sodium and hafnium chloride and institute
The ratio for stating the amount of the substance of citric acid is 1:6.The citric acid also has and mentions for hydro-thermal reaction in addition to providing an acidic environment
For the effect of reducing atmosphere.The dosage of the citric acid can guarantee that entire hydro-thermal reaction is carried out in acid system, mention
The quality of high product.
Preferably, in the step A, the cesium salt is one of cesium carbonate or cesium chloride.The cesium salt, which has, to be stablized
Preferably, and cesium ion can be provided for hydro-thermal reaction.
Preferably, in the step B, the temperature of the hydro-thermal reaction is 180 ~ 200 DEG C, and the time of the hydro-thermal reaction is
48 ~ 72h is conducive to promote yield.
It preferably, further include being washed to crude product progress washing process, alcohol before the drying in the step C
Processing and drying process.By washing processing to crude product progress washing process and alcohol, the impurity in crude product is removed, then carry out
It is dried, improves the purity of caesium hafnium tungsten bronze.
Preferably, in the step C, the temperature of the drying is 80~100 DEG C.In the drying process, the dry temperature
Degree is higher, and drying time can be reduced, but also should not be too high, and product is prevented to be oxidized.
Preferably, in the step C, the temperature of the calcination is 500 ~ 800 DEG C, and the time of the calcining is 2 ~ 4h.This
The parameter for inventing the calcining can help to obtain the hafnium doping caesium tungsten bronze nano-powder that partial size is small and uniformity is good.
Preferably, in the step C, the protective atmosphere is inert gas atmosphere or reducing atmosphere.In calcination process,
Caesium tungsten bronze is adulterated for hafnium, inert gas atmosphere or reducing atmosphere are provided, prevent the oxidation for leading to product because of high temperature.
The present invention also provides a kind of applications of caesium hafnium tungsten bronze as described above, wherein the caesium hafnium tungsten bronze be applied to every
The preparation of hot coating or thermal insulation film.Caesium hafnium tungsten bronze of the present invention is added in insulating moulding coating or thermal insulation film, it can
Effectively improve the light transmission heat-proof quality of product.
Below by specific embodiment, next further description of the technical solution of the present invention.
In embodiment with XRD diffraction pattern spectrometer be the production of Japanese Shimadzu Corporation XRD-600, use using CuK α as
Excitaton source is scanned, 10-60 ° of scanning range of 10 °/min of scanning speed, and 0.02 ° of step-length.
The dispersibility of preparation-obtained caesium tungsten bronze and element composition are analyzed by SEM and EDS in embodiment,
Specifically with scanning electron microscope be HItachi company S-3400N(II) type.
Embodiment 1
(1) 2.9687g tungstate dihydrate acid sodium is dissolved, 11.5272g lemon acid dissolution formation aqueous citric acid solution is added to sodium tungstate
In solution, then 0.5376g cesium carbonate is dissolved and is added, forms mixed liquor；
(2) 0.3203g hafnium chloride is dissolved in 20mL ethanol solution, is then added in step (1) described mixed liquor, obtains forerunner
Liquid；
(3) precursor liquid is transferred in the autoclave of polytetrafluoroethyllining lining and carries out hydro-thermal reaction, 200 DEG C of hydrothermal temperature,
Hydro-thermal time 48h, obtains crude product；
(4) processing is washed into crude product centrifugation, washing, alcohol that hydro-thermal reaction obtains, after 80 DEG C of dryings, 600 DEG C under an argon atmosphere
2h is calcined, black-and-blue caesium hafnium tungsten bronze powder is obtained.
Fig. 1 is that this implements the XRD diagram of caesium hafnium tungsten bronze powder obtained, and Fig. 2 is that this implementation caesium hafnium tungsten obtained is green
The EDS of copper powder body schemes, and Fig. 3 is that this implements the SEM figure that the big multiple of caesium hafnium tungsten bronze powder obtained is 10000, and Fig. 4 is this reality
It applies the SEM that the big multiple of caesium hafnium tungsten bronze powder obtained is 20000 to scheme, Fig. 5 is this implementation caesium hafnium tungsten bronze powder obtained
The SEM that the big multiple of body is 30000 schemes, and Fig. 6 is that this implements the SEM figure that the big multiple of caesium hafnium tungsten bronze powder obtained is 40000.
It is found that this implementation caesium hafnium tungsten bronze powder obtained has, crystallinity is preferable, partial size is small for the analysis from figure, uniform particle diameter, divides
Dissipate the preferable feature of property.
Embodiment 2
(1) 2.9687g tungstate dihydrate acid sodium is dissolved, 11.5272g lemon acid dissolution formation aqueous citric acid solution is added to sodium tungstate
In solution, then 0.5556g cesium chloride is dissolved and is added, forms mixed liquor；
(2) 0.3203g hafnium chloride is dissolved in 20mL ethanol solution, is then added in step (1) described mixed liquor, obtains forerunner
Liquid；
(3) precursor liquid is transferred to reaction in the autoclave of polytetrafluoroethyllining lining and carries out hydro-thermal reaction, hydrothermal temperature 200
DEG C, hydro-thermal time 48h obtains crude product.
(4) processing is washed into crude product centrifugation, washing, alcohol that hydro-thermal reaction obtains, after 80 DEG C of dryings, under an argon atmosphere
600 DEG C of calcining 2h, obtain black-and-blue caesium hafnium tungsten bronze powder.
Fig. 7 is that this implements the XRD diagram of caesium hafnium tungsten bronze powder obtained, and Fig. 8 is that this implementation caesium hafnium tungsten obtained is green
The EDS of copper powder body schemes, and Fig. 9 is that this implements the SEM figure that the big multiple of caesium hafnium tungsten bronze powder obtained is 10000, and Figure 10 is this
Implement the SEM that the big multiple of caesium hafnium tungsten bronze powder obtained is 20000 to scheme, Figure 11 is this implementation caesium hafnium tungsten bronze obtained
The SEM that the big multiple of powder is 30000 schemes.The analysis from figure is it is found that this implementation caesium hafnium tungsten bronze powder obtained has crystallization
Property it is preferable, partial size is small, uniform particle diameter, the preferable feature of dispersibility.
Embodiment 3
(1) 2.6338g tungstate dihydrate acid sodium is dissolved, 11.5272g lemon acid dissolution formation aqueous citric acid solution is added to sodium tungstate
In solution, then 0.5376g cesium carbonate is dissolved and is added, forms mixed liquor；
(2) 0.6406g hafnium chloride is dissolved in 20mL ethanol solution, is then added in step (1) described mixed liquor, obtains forerunner
Liquid；
(3) precursor liquid is transferred in the autoclave of polytetrafluoroethyllining lining and carries out hydro-thermal reaction, 200 DEG C of hydrothermal temperature,
Hydro-thermal time 72h, obtains crude product.
(4) processing is washed into crude product centrifugation, washing, alcohol that hydro-thermal reaction obtains, after 80 DEG C of dryings, under an argon atmosphere
700 DEG C of calcining 2h, obtain black-and-blue caesium hafnium tungsten bronze powder.
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 (10)
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Cited By (1)
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| CN110373123A (en) * | 2019-07-30 | 2019-10-25 | 信义节能玻璃（芜湖）有限公司 | PVB glue film and preparation method thereof and laminated safety glass |
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