CN105565380B - One kind mixes tungsten vanadium dioxide ultrafine powder preparation method - Google Patents
One kind mixes tungsten vanadium dioxide ultrafine powder preparation method Download PDFInfo
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- CN105565380B CN105565380B CN201510516071.1A CN201510516071A CN105565380B CN 105565380 B CN105565380 B CN 105565380B CN 201510516071 A CN201510516071 A CN 201510516071A CN 105565380 B CN105565380 B CN 105565380B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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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
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The present invention relates to one kind mixes tungsten vanadium dioxide ultrafine powder preparation method, comprise the following steps：Step 1：Three hydrated sulfuric acid vanadyl are dissolved in distilled water, add the solubility sexavalence tungsten compound accounting for v element integral molar quantity 0.1～5%, add alkaline solution, adjust pH value of solution and reach 6～7, obtain suspension, carry out sucking filtration cleaning-drying and obtain mixing tungsten presoma powder body；Step 2：Aerosil is pulverized, silicon dioxide aerogel powder is sifted out by screen cloth；Step 3：Step 1 gained is mixed tungsten presoma powder body and step 2 gained silicon dioxide aerogel powder by 1～10：1 weight ratio is mixed, and obtains powder body is blended；Step 4：Step 3 gained blending powder body is carried out heat treatment under inert gas shielding, subsequently cools down；Heat treatment temperature is 600～1000 DEG C, and heat treatment time is 3～8h；Step 5：Blending powder body after being cooled down step 4 using 1000～3000 eye mesh screens is screened, and removes oarse-grained silicon dioxide aerogel powder.
Description
Technical field
The present invention relates to a kind of preparation method of hypovanadic oxide powder, more particularly, to one kind mix tungsten vanadium dioxide ultrafine powder
Preparation method.
Background technology
Vanadium dioxide (VO2) be a kind of thermal induced phase transition metallic compound, occur near 68 DEG C from cryogenic semiconductor to
The mutation of high-temperature metal phase.In phase transition process, there are 2～4 order of magnitude mutation, simultaneously with light refraction in the resistance of material
The mutation of rate, absorbance and reflectance, especially obvious in infrared and the change of near infrared band optical transmittance.Less than phase
During temperature, VO2Infrared and near-infrared transmitance higher；But when temperature is higher than phase transition temperature, VO2Infrared and near-infrared
Transmitance has significant decline.This physical characteristic is had based on it, can be used for intelligently regulating and controlling infrared transmittivity, to respond mesh
The front requirement to building energy conservation reduction of discharging.
But due to VO2Phase transition temperature at 68 DEG C about, and 68 DEG C of phase transition temperatures are comfortable with respect to human normal life
Slightly higher for temperature, therefore adjust VO2Phase transition temperature become VO to 15～30 DEG C2Intelligent temperature control characteristic subtracts in building energy conservation
The Important Action of row's aspect popularization and application.
Reduce VO2The method of phase transition temperature have multiple, sum up and main test this purpose by ion doping.Mix
Miscellaneous such as W6+、Mo6+、Nb5+、F-、Cr3+Plasma, wherein W6+Doping is to VO2Phase transition temperature influence amount larger.By adulterate W from
The form of son is VO2Phase transition temperature be reduced to room temperature and keep original phase transition performance.
One kind is had to pass through VO at present2After powder body is blended with resin or coating, it is coated in glass surface and makes intelligent temperature control glass
The method of glass, simplified intelligent temperature control process of glass.Because intelligent glass is higher to the uniformity requirements of film, this requires
VO2Diameter of particle is little, and homogeneous.
In preparation VO2In powder process, need to VO2Carry out heat treatment, to remove the water of crystallization of presoma, but forerunner
Body loses water of crystallization, forms VO2During crystal grain, due to the room of water of crystallization, crystal grain is made to be not good at it is intended to crystal lattice recombination.Crystal grain
Growth course by forming core, grow up and big crystal grain is annexed several stages of adjacent little crystal grain in some way and formed.VO2Crystal grain exists
Early growth period defect is many, and crystallite dimension is little, and surface activity is big.Rising with heat treatment temperature and the prolongation of heat treatment time,
Lattice is developed and is tended to perfect, and particle diameter is gradually increased, and big crystal grain fusion little crystal grain during growth, leads to crystal grain quick
Grow up, these are VO2Crystal grain after high-temperature heat treatment particle diameter than larger the reason.
Therefore in order to obtain ultra-fine VO2Powder body, it usually needs increase VO after high-temperature heat treatment2Pulverization process, this necessarily increases
Add production cost, be also readily incorporated impurity simultaneously.
Same problem also appears in ultra-fine mixes tungsten VO2In the preparation of powder body, in order to realize by mixing tungsten VO2Presoma
High-temperature heat treatment one step obtains ultra-fine VO2Powder body is it is necessary to carry out suitable adjustment to existing presoma high-temperature heat treatment process.
Content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of production time is short, low cost, be easy to
Large-scale production mix tungsten vanadium dioxide ultrafine powder preparation method.
For achieving the above object, the present invention can be achieved by the following technical programs：
One kind mixes tungsten vanadium dioxide ultrafine powder preparation method, comprises the following steps：
Step 1：Three hydrated sulfuric acid vanadyl are dissolved in distilled water, are simultaneously introduced and account for v element integral molar quantity 0.1～5%
Solubility sexavalence tungsten compound, is subsequently adding alkaline solution, and the slow pH value of solution that adjusts reaches 6～7, obtains suspension, will be suspended
Liquid carries out sucking filtration cleaning and obtains mixing tungsten presoma, will mix tungsten presoma and be dried and obtain mixing tungsten presoma powder body；
Step 2：Aerosil is pulverized, silicon dioxide aerogel powder is sifted out by screen cloth；
Step 3：Step 1 gained is mixed tungsten presoma powder body and step 2 gained silicon dioxide aerogel powder by 1～10：1
Weight ratio mixed, mixing velocity be 100～200r/min, obtain be blended powder body；
Step 4：Step 3 gained blending powder body is carried out heat treatment under inert gas shielding, subsequently cools down；Heat treatment temperature
Spend for 600～1000 DEG C, heat treatment time is 3～8h；
Step 5：Blending powder body after being cooled down step 4 using 1000～3000 eye mesh screens is screened, and removes bulky grain
Silicon dioxide aerogel powder.
Further, the drying equipment mixing tungsten presoma in step 1 is vacuum drying oven, and baking temperature is 60～80 DEG C,
Drying time is 24～48h.
Further, the tungsten compound of solubility sexavalence described in step 1 be one of sodium tungstate, ammonium tungstate or wolframic acid or
Multiple.
Further, alkaline solution described in step 1 is sodium hydroxide, the aqueous solution of sodium carbonate, sodium bicarbonate or ammonia
One or more of.
Further, the mesh number mixing tungsten presoma described in step 1 is more than 1000 mesh.
Further, aerosil described in step 3 is nano-hole aerogel, and density is less than 0.25g/cm3.
Further, the mesh number of step 3 gained silicon dioxide aerogel powder is 100～300 mesh.
Further, the equipment carrying out heat treatment in step 4 is Muffle furnace.
The present invention has the advantages that with respect to prior art：
1st, low cost, pollution-free, is conducive to green production；
2nd, the phase transition temperature mixing tungsten hypovanadic oxide powder can be controlled by mixing tungsten amount, in being hardly blended
Aeroge affects, and the phase transition temperature mixing tungsten hypovanadic oxide powder can as little as 14.9 DEG C；
3rd, mix tungsten presoma powder body mixing silicon dioxide aerogel powder, be conducive to the micro/nano level obtaining refining to mix tungsten two
Vanadium oxide powder body material；
4th, preparation method is easy and simple to handle, efficiency high, short preparation period, can enter Line Continuity large-scale production.
Present invention, avoiding single tungsten presoma powder body of mixing and produce fusion during high-temperature heat treatment removes water of crystallization, brilliant
Grain increases, thus eliminating VO after heat treatment2Pulverization process, improve and mix the ultra-fine VO of tungsten2Powder body preparation efficiency.
Mix tungsten vanadium dioxide ultrafine powder and dispersible and obtain sub- nanometer or nano pulp, and blended together with resin or organic coating
Membrane, is coated on glass door and window surface masking, obtains having transparent to the effect of region of ultra-red wavelength light transmission rate intelligent control
Heat insulating coatings.Directly existing windowpane can be transformed by film mode, according to outdoor temperature intelligent selection window
Family infrared transmittivity, increases indoor comfort level, has wide application and development prospect in building energy conservation.
Brief description
Fig. 1 is pure VO2, mix tungsten VO2, aeroge be blended heat treatment mix tungsten VO2DSC curve comparison diagram.
Specific embodiment
Below in conjunction with accompanying drawing and specific embodiment, the present invention is further illustrated：
One kind mixes tungsten vanadium dioxide ultrafine powder preparation method, comprises the following steps：
Step 1：Tungsten presoma is mixed in preparation
By three hydrated sulfuric acid vanadyl VOSO4·3H2O is dissolved in distilled water, be simultaneously introduced account for v element integral molar quantity 0.1～
5% solubility sexavalence tungsten compound simultaneously stirs, and is subsequently adding alkaline solution, and the slow pH value of solution that adjusts reaches 6～7, obtains
To canescence suspension；Suspension is carried out sucking filtration cleaning obtain unbodied mixing tungsten presoma；Tungsten presoma will be mixed put into very
Empty drying baker is dried, and baking temperature is 60～80 DEG C, and drying time is 24～48h, is dried, loose, non-caking
Mix tungsten presoma powder body, the mesh number that gained mixes tungsten presoma powder body is more than 1000 mesh.Solubility sexavalence tungsten compound used is
One or more of sodium tungstate, ammonium tungstate or wolframic acid, alkaline solution used is sodium hydroxide, sodium carbonate, sodium bicarbonate or
One or more of aqueous solution of ammonia.
Step 2：Prepare silicon dioxide aerogel powder
Aerosil is pulverized, silicon dioxide aerogel powder is sifted out by screen cloth.Titanium dioxide used
Silica aerogel is non-metallic ion, hydrophobic, high porosity nano-hole aerogel, and density is less than 0.25g/cm3；Gained
The mesh number of silicon dioxide aerogel powder is 100～300 mesh.
Step 3：Mix tungsten presoma powder body to be blended with silicon dioxide aerogel powder
Step 1 gained is mixed tungsten presoma powder body and step 2 gained silicon dioxide aerogel powder by 1～10：1 weight
Ratio is mixed, and mixing velocity is 100～200r/min, obtains powder body is blended.
Step 4：Blending powder body heat treatment
Step 3 gained blending powder body is put in Muffle furnace, and is passed through noble gases and protected, then carry out at heat
Reason, heat treatment temperature is 600～1000 DEG C, and heat treatment time is 3～8h, subsequently cools down.
Step 5：Remove silicon dioxide aerogel powder
Blending powder body after being cooled down step 4 using 1000～3000 eye mesh screens is screened, and removes oarse-grained dioxy
SiClx aerogel powder, you can obtain mixing tungsten vanadium dioxide ultrafine powder.
Embodiment 1
One kind mixes tungsten vanadium dioxide ultrafine powder preparation method, comprises the following steps：
Step 1：Tungsten presoma is mixed in preparation
By three hydrated sulfuric acid vanadyl VOSO4·3H2O is dissolved in distilled water, is simultaneously introduced and accounts for v element integral molar quantity 1%
Solubility sexavalence tungsten compound simultaneously stirs, by dilute for 0.01mol/L NaHCO3Solution syringe pump is dripped with the speed of 50mL/h
It is added to the VOSO being stirred continuously4In solution, control ph scope is 6～7, obtains canescence suspension；Suspension is taken out
Filtering is washed and is obtained unbodied mixing tungsten presoma；Tungsten presoma will be mixed put into vacuum drying oven and be dried, baking temperature will be 80
DEG C, drying time be 24h, be dried, loose, non-caking mix tungsten presoma powder body, gained mixes the mesh of tungsten presoma powder body
Number is more than 1000 mesh.Solubility sexavalence tungsten compound used is one or more of sodium tungstate, ammonium tungstate or wolframic acid, used
Alkaline solution be one or more of sodium hydroxide, aqueous solution of sodium carbonate, sodium bicarbonate or ammonia.
Step 2：Prepare silicon dioxide aerogel powder
Aerosil is pulverized, is screened by 100 mesh and 200 eye mesh screens, obtain 100～200 mesh
Silicon dioxide aerogel powder.Aerosil used is non-metallic ion, hydrophobic, high porosity nano-pore
Aeroge, density is less than 0.25g/cm3.
Step 3：Mix tungsten presoma powder body to be blended with silicon dioxide aerogel powder
The drying of step 1 gained mixed tungsten presoma powder body and step 2 gained silicon dioxide aerogel powder by 1.6:1
Weight ratio mixed, in mixer, 2min is mixed with the speed of 100r/min, obtains powder body is blended.
Step 4：Blending powder body heat treatment
Step 3 gained blending powder body is put in Muffle furnace, and is passed through noble gases and protected, then carry out at heat
Reason, heat treatment temperature is 700 DEG C, and heat treatment time is 4h, subsequently cools down.
Step 5：Remove silicon dioxide aerogel powder
Blending powder body after being cooled down step 4 using 1000 eye mesh screens is screened, and removes oarse-grained silicon dioxide gas
Gel powder body, you can obtain mixing tungsten vanadium dioxide ultrafine powder.
It will be seen from figure 1 that pure VO2Phase transformation peak value highest, mix tungsten VO2Take second place, aeroge be blended heat treatment mix tungsten
VO2Minimum.Therefore, the preparation method of the present invention is blended heat treatment and can effectively reduce phase alternating temperature by mixing tungsten amount and aeroge
Degree.
For a person skilled in the art, other can be made various corresponding according to above technical scheme and design
Change and deformation, and all these change and deformation all should belong within the protection domain of the claims in the present invention.
Claims (9)
1. one kind mixes tungsten vanadium dioxide ultrafine powder preparation method it is characterised in that comprising the following steps：
Step 1：Three hydrated sulfuric acid vanadyl are dissolved in distilled water, are simultaneously introduced and account for the solvable of v element integral molar quantity 0.1～5%
Property sexavalence tungsten compound, be subsequently adding alkaline solution, the slow pH value of solution that adjusts reaches 6～7, obtain suspension, suspension is entered
The cleaning of row sucking filtration obtains mixing tungsten presoma, will mix tungsten presoma and be dried and obtain mixing tungsten presoma powder body；
Step 2：Aerosil is pulverized, silicon dioxide aerogel powder is sifted out by screen cloth；
Step 3：Step 1 gained is mixed tungsten presoma powder body and step 2 gained silicon dioxide aerogel powder by 1～10：1 weight
Amount ratio is mixed, and obtains powder body is blended；
Step 4：Step 3 gained blending powder body is carried out heat treatment under inert gas shielding, subsequently cools down；Heat treatment temperature is
600～1000 DEG C, heat treatment time is 3～8h；
Step 5：Blending powder body after being cooled down step 4 using 1000～3000 eye mesh screens is screened, and removes oarse-grained two
Silica aerogel powder body.
2. according to claim 1 mix tungsten vanadium dioxide ultrafine powder preparation method it is characterised in that：Tungsten is mixed in step 1
The drying equipment of presoma is vacuum drying oven, and baking temperature is 60～80 DEG C, and drying time is 24～48h.
3. according to claim 1 mix tungsten vanadium dioxide ultrafine powder preparation method it is characterised in that：Described in step 1
Solubility sexavalence tungsten compound is one or more of sodium tungstate, ammonium tungstate or wolframic acid.
4. according to claim 1 or 3 mix tungsten vanadium dioxide ultrafine powder preparation method it is characterised in that：Institute in step 1
Stating alkaline solution is one or more of sodium hydroxide, aqueous solution of sodium carbonate, sodium bicarbonate or ammonia.
5. according to claim 1 mix tungsten vanadium dioxide ultrafine powder preparation method it is characterised in that：Described in step 1
The mesh number mixing tungsten presoma powder body is more than 1000 mesh.
6. according to claim 1 mix tungsten vanadium dioxide ultrafine powder preparation method it is characterised in that：Described in step 3
Aerosil is nano-hole aerogel, and density is less than 0.25g/cm3.
7. according to claim 1 mix tungsten vanadium dioxide ultrafine powder preparation method it is characterised in that：Step 3 gained two
The mesh number of silica aerogel powder body is 100～300 mesh.
8. according to claim 1 mix tungsten vanadium dioxide ultrafine powder preparation method it is characterised in that：Carry out in step 4
The equipment of heat treatment is Muffle furnace.
9. according to claim 1 mix tungsten vanadium dioxide ultrafine powder preparation method it is characterised in that：Mix described in step 3
The speed that tungsten presoma powder body is mixed with silicon dioxide aerogel powder is 100～200r/min.
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