CN105669194B - A kind of thermotropic infrared emittance vanadium dioxide preparation of sections method - Google Patents
A kind of thermotropic infrared emittance vanadium dioxide preparation of sections method Download PDFInfo
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Abstract
The invention discloses a kind of thermotropic infrared emittance vanadium dioxide preparation of sections method, it is initial feed to use metavanadate, citric acid and deionized water, after being uniformly mixed in a certain amount of ratio, being transferred in water heating kettle carries out hydro-thermal reaction, after question response terminates, by obtaining nano vanadium dioxide powder after centrifugation, washing and vacuum drying, then by pressed by powder flakiness, thermotropic infrared emittance vanadium dioxide thin slice is obtained final product after annealed treatment.Preparation process is simple of the invention, use raw material it is nontoxic, cost is relatively low, product crystallinity is preferable；Obtained vanadium dioxide thin slice can realize the mutation of near room temperature infrared emittance, mutation value is up to 0.34, the mechanical strength of thin slice is higher, it is not easy to break, it is easy to machining, various sizes of thin slice can be processed into actual applications is adhered directly onto required position, it is easy to use, had broad application prospects in infrared stealth and camouflage field.
Description
Technical field
The invention belongs to inorganic functional material field, it is related to the preparation method of thermotropic infrared emittance material, specifically relates to
And a kind of thermotropic infrared emittance vanadium dioxide preparation of sections method.
Background technology
Thermotropic infrared emittance material is a kind of intellectual material, and its own infrared emittance can be according to environment temperature
Change and from main regulation, had a wide range of applications in camouflage and thermal control field.In camouflage field, with the level of scouting
With multi-wavelength data acquisition, fusion and the continuous improvement of processing speed, the fixed signal characteristic matching technology of conventional camouflage equipment
Very big challenge is faced, if the infrared signature of camouflage equipment immobilizes, when external environment changes, camouflage equipment
Characteristic signal just occurs situation about being misfitted with background, and target can be caused to be exposed in long duration；And thermotropic emissivity material
Material can independently change the emissivity of itself with the change of temperature, actively adjust itself radiation intensity so that target and background begins
Last phase is merged, with excellent infrared self adaptation camouflage performance.In thermal control field, with the fast development of space technology, pass through
Cause that satellite surface manifests different emissivity in the period round the clock using thermotropic infrared emittance material, and then when regulating and controlling different
The caloradiance of Duan Weixing balances the heat in cabin, and the new thermal control technology for being capable of the change of dynamically adapting space environment is more next
More it is valued by people.
Vanadium dioxide is a kind of functional material with thermotropic emissivity property, its phase transition temperature close to room temperature,
There is metal-insulator transition at phase transition temperature and with the mutation of photoelectric properties, the change of its infrared emittance can before and after phase transformation
Up to 0.6.Therefore, the infrared intensity of goal of regulation and control is designed using the infrared emittance of vanadium dioxide material, makes its infrared spy
Property changing with environment and weather condition and automatically adjusting, such that it is able to realize optimal infrared stealth effect.Current titanium dioxide vanadium powder
The preparation method of body mainly has：Thermal decomposition method, induced with laser vapour deposition process, sol-gal process, chemical precipitation method and hydro-thermal method
Deng, wherein hydro-thermal method refer in the environment of HTHP, carry out in aqueous about chemically react method, the method by
In preparation process less pollution, consuming little energy, and be obtained in that narrow particle diameter distribution, reunion low degree, lattice development it is complete,
Purity powder higher and by extensive concern, be a very promising method for obtaining high-temperature-phase at a lower temperature.But
Existing VO2Generally elder generation Hydrothermal Synthesiss B phases, the D equal VO of powder Hydrothermal preparation method2Powder, then high-temperature phase-transitional is M phases again
VO2Powder, there are problems that complex technical process, time-consuming and, such as CN102502824A Chinese patents are disclosed
The preparation method of a kind of vanadium dioxide and its adulterated powder, VO is prepared first with hydro-thermal method2(B phases) powder, Ran Hou
In the atmosphere of high-purity argon gas or nitrogen, calcining obtains VO at 400 DEG C~700 DEG C2(M phases) powder.Problem based on the above, leads to
Cross using one step hydro thermal method to synthesize VO2(M phases) powder gradually receives everybody concern, CN101391814A Chinese patents
A kind of preparation method of rutile phase hypovanadic oxide powder is disclosed, hydro-thermal reaction is directly closed for 1~7 day at 200 DEG C~300 DEG C
Into Rutile Type VO2Powder, but the method take it is more, it is impossible to the fast and convenient preparation requirement required for meeting production,
And the raw material for using includes violent in toxicity V2O5Powder, it is impossible to reach environment-friendly requirement.
The preparation of hypovanadic oxide powder in the prior art is used mostly dopant, mainly reduces titanium dioxide by adulterating
The phase transition temperature of vanadium, but doping can cause the gap structure of monoclinic phase vanadium dioxide powder to change, and then to material
Light absorbs and optics performance of control produce influence, thus with the VO of doping2Powder is compared, the VO of pure monoclinic phase2Before powder phase transformation
The variable quantity of infrared emittance is bigger afterwards, with more excellent infrared performance of control, is more conducive to realize it in infrared stealth
Using.In addition, the application of hypovanadic oxide powder is mainly by being made coating in the prior art, but make coating needs
Addition resin, diluent and auxiliary agent etc., influence the variable quantity of its infrared emittance, so as to influence its performance, Liu Dongqing etc.
(referring to Liu Dongqing, Zheng Wenwei, Cheng Haifeng, bang is hidden, Du Panpan thermotropic emissivity VO2Coating is studied and applies the new skills of [J]
Art new technology, 2008 (11):117-119) by VO2Powder is prepared for VO2Coating, VO2Coating emissivity near 68 DEG C of transformation temperature
Undergo mutation, Sudden Changing Rate is 0.1, but the emissivity mutation value of coating is still smaller, limits its application.Therefore, need badly open
Send out advantages of nontoxic raw materials a kind of, with low cost, simple and effective, infrared emittance mutation are worth the system of pure monoclinic phase vanadium dioxide material high
Preparation Method.
The content of the invention
The technical problems to be solved by the invention are to overcome deficiency of the prior art, there is provided a kind of infrared hair of thermotropic
Rate vanadium dioxide preparation of sections method is penetrated, the method preparation process is simple, the raw material of use are nontoxic, low production cost, produced
The crystallinity of thing is good；Obtained thin slice is the nano material of monocline phase structure, with nanometer size effect, can realize approaching
The infrared emittance mutation of room temperature (about 68 DEG C), emissivity maximum sudden change value is 0.34, can directly be pasted thin slice when using
To required part, had broad application prospects in infrared stealth and camouflage field.
In order to solve the above technical problems, technical scheme proposed by the present invention is：
A kind of thermotropic infrared emittance vanadium dioxide preparation of sections method, comprises the following steps：
(1) metavanadate, citric acid and deionized water are mixed, stirring forms solution, is then turned resulting solution
Move on to and carry out hydro-thermal reaction in water heating kettle；
(2) product of gained is centrifuged after step (1) hydro-thermal reaction is terminated, and the product obtained after centrifugation spends successively
Alternately washing, the vacuum drying of ionized water and absolute ethyl alcohol, obtains hypovanadic oxide powder；
(3) hypovanadic oxide powder that step (2) is obtained first is suppressed into flakiness, is then annealed in argon gas atmosphere again
Treatment, obtains final product described thermotropic infrared emittance vanadium dioxide thin slice.
In above-mentioned preparation method, it is preferred that in the step (3), hypovanadic oxide powder is pressed into a diameter of 20mm's
Thin slice, pressing pressure is 16MPa~20MPa.
In above-mentioned preparation method, it is preferred that in the step (3), annealing temperature is 500 DEG C~800 DEG C, in annealing temperature
Under annealing time be 4h~10h.It is furthermore preferred that the annealing temperature is 600 DEG C~700 DEG C, specific cycle of annealing is：(a)
From room temperature to 600 DEG C~700 DEG C, heating rate is 5~8 DEG C/min；B () is incubated 4h~6h at 600 DEG C~700 DEG C；(c)
Room temperature is cooled to, rate of temperature fall is 4~6 DEG C/min.
In above-mentioned preparation method, it is preferred that in the step (1), metavanadate is selected from ammonium metavanadate, potassium metavanadate
The mol ratio of at least one, metavanadate and citric acid is 0.5~3:1, the filling rate of water heating kettle is 45%~85%.The water
The filling rate of hot kettle refers to the percentage that the material cumulative volume added in water heating kettle accounts for water heating kettle volume.It is furthermore preferred that described inclined
The mol ratio of vanadate and citric acid is 1~2:1, the filling rate of the water heating kettle is 60%~85%.
In above-mentioned preparation method, it is preferred that in the step (1), hydrothermal temperature is 165 DEG C~285 DEG C, during reaction
Between be 4h~48h.It is furthermore preferred that the hydrothermal temperature is 245 DEG C~285 DEG C, the reaction time is 8h~16h.
In above-mentioned preparation method, it is preferred that in the step (2), the product obtained after centrifugation uses deionized water, nothing successively
Water-ethanol alternately washing 3 times；Vacuum drying temperature is 50 DEG C~100 DEG C, and drying time is 8h~15h.It is furthermore preferred that described
Vacuum drying temperature is 60 DEG C~80 DEG C, and drying time is 10h~12h.
The preparation of hypovanadic oxide powder of the present invention uses a kind of nontoxic raw material metavanadate and the stronger lemon of reproducibility
Acid reaction, the VO of monoclinic phase can be just efficiently prepared using one step hydro thermal method2Powder (the hydro-thermal reaction time can foreshorten to 8~
16 hours), preparation time is greatly reduced, be conducive to the extensive preparation in industrial production；Obtained hypovanadic oxide powder is
Nano particle (refers to Fig. 3), due to its size be much smaller than infrared wavelength, therefore with the vanadium dioxide particle phase of conventional micron size
Than its transmissivity is much greater, so as to reduce reflectivity, causes its infrared emittance smaller, can preferably realize infrared
Stealthy function, with nanometer size effect.
Vanadium dioxide thin slice of the invention obtained be by powder it is repressed after made annealing treatment in argon gas atmosphere again after
Obtain, on the one hand can increase its mechanical strength, prevent from being damaged due to being machined caused thin slice in subsequent applications；The opposing party
The vanadium dioxide of a small amount of other phases in the powder obtained by preparation can be changed into the vanadium dioxide of monoclinic phase in face, so as to improve
The crystallinity of thin slice, increased variable quantity (the not annealed vanadium dioxide of infrared emittance before and after vanadium dioxide thin slice phase transformation
Infrared emittance changing value is 0.20 before and after thin slice phase transformation, infrared emittance change before and after the vanadium dioxide thin slice phase transformation after annealing
It is 0.34 to be worth, and refers to Fig. 5 and Fig. 6).Compared with coating obtained in utilization hypovanadic oxide powder of the prior art, present invention system
The vanadium dioxide thin slice for obtaining does not add any auxiliary agent, and the variable quantity of its infrared emittance is bigger, the infrared emittance after phase transformation
It is smaller, it is advantageously implemented in infrared stealth and the wide application in camouflage field.
If simple compressing tablet will be carried out obtained powder (by calcination processing) in the prior art, due to after heat treatment
Powder compressing tablet should not be molded, and the sheet surface roughness for obtaining is larger (similar in smaller pressure lower sheeting), can influence its phase
The variable quantity of infrared emittance before and after becoming, causes the change of infrared emittance before and after phase transformation smaller；Powder is carried out elder generation by the present invention
Made annealing treatment again after compressing tablet, the consistency of material can be increased so that the surface roughness of thin slice it is smaller (be similar to compared with
Big pressure lower sheeting), the change of infrared emittance is bigger before and after phase transformation, greatly improves its infrared performance of control, is easily applied to red
It is outer it is stealthy in.
The infrared emittance of obtained vanadium dioxide thin slice of the invention reduces with the increase of temperature, and infrared emittance is connecing
There is certain mutation during nearly room temperature, this is mainly due to VO2Metal-insulator phase transformation characteristic, this is carried out below briefly
Explanation.
Infrared emittance variation with temperature is mainly due to VO2Carriers concentration variation with temperature causes.VO2
At Tc (phase transition temperature)=68 DEG C occur from one-level displacement type phase transformation from low-temperature insulation state to high-temperature metal state Rapid reversible,
Work as T<It is monocline during Tc, in insulation figure, carrier concentration is relatively low；Work as T>VO during Tc2It is tetragonal, in metal
State, carrier concentration is sharply increased, and the reflectivity to photon is also increased dramatically, and causes infrared emittance to diminish rapidly.
The present invention compared with prior art, with following advantage：
(1) the obtained hypovanadic oxide powder of the present invention is nano particle, even size distribution, crystallinity preferably, with receiving
Rice dimensional effect.
(2) vanadium dioxide thin sheet preparation technique of the present invention is simple, and the raw material of use are nontoxic, and preparation time is short, are produced into
This is low.
(3) vanadium dioxide thin slice of the present invention can be realized being mutated close to the infrared emittance of room temperature, with existing titanium dioxide
Vanadium powder body or coating are compared, and with bigger infrared emittance variable quantity, mutation value reaches 0.34, the infrared emittance after phase transformation
It is smaller, had broad application prospects in infrared stealth and camouflage field.
(4) vanadium dioxide thin slice mechanical strength of the present invention is higher, not easy to break, is easy to machining, in actual applications
Various sizes of thin slice can be processed into and be adhered directly onto required position, it is easy to use.
Brief description of the drawings
Fig. 1 is the phase in version structural representation that vanadium dioxide is changed into tetragonal from monocline.
Fig. 2 is the XRD spectra of the thermotropic infrared emittance vanadium dioxide thin slice that the embodiment of the present invention 1 is prepared.
Fig. 3 is the SEM figures of the thermotropic infrared emittance hypovanadic oxide powder that the embodiment of the present invention 1 is prepared.
Fig. 4 is the DSC spectrograms of the thermotropic infrared emittance vanadium dioxide thin slice that the embodiment of the present invention 1 is prepared.
Fig. 5 is the vanadium dioxide thin slice (being obtained after repressed, without annealing) that the embodiment of the present invention 1 is prepared
Infrared emittance vary with temperature curve.
Fig. 6 is the infrared emittance of the thermotropic infrared emittance vanadium dioxide thin slice that the embodiment of the present invention 1 is prepared
Variation with temperature curve.
Specific embodiment
Embodiment 1
A kind of thermotropic infrared emittance vanadium dioxide preparation of sections method of the invention, comprises the following steps：
(1) 1.76g (0.015mol) ammonium metavanadates and 1.58g (0.0082mol) citric acid are added to 70ml deionizations
Magnetic agitation mixing is carried out in water, homogeneous solution is formed, mixing time is 30 minutes；Then the solution that will be obtained is transferred to
In 100ml water heating kettles, 16h is reacted at 245 DEG C；
(2) after the completion of reacting, after product is taken out after water heating kettle natural cooling, the product that will be obtained first is centrifuged, then will
The product obtained after centrifugation with alternately washing three times of deionized water, absolute ethyl alcohol, is finally vacuum dried at 60 DEG C successively,
Drying time is 12h, obtains final product VO2Powder；
(3) VO that 0.6g steps (2) are obtained is taken2Powder, is pressed into a diameter of using tablet press machine under the pressure of 20MPa
The thin slice (being designated as the vanadium dioxide thin slice not by annealing) of 20mm, then using following cycle of annealing in argon gas atmosphere
Made annealing treatment：A (), from room temperature to 600 DEG C, heating rate is 5 DEG C/min；B () is incubated 6h at 600 DEG C；C () is lowered the temperature
To room temperature, rate of temperature fall is 4 DEG C/min, that is, obtain thermotropic infrared emittance vanadium dioxide thin slice of the invention and (be designated as thermic
Become infrared emittance vanadium dioxide thin slice).
Fig. 1 is the phase in version structural representation that vanadium dioxide is changed into tetragonal from monocline, as temperature T<Tc (phases
Transition temperature) when, vanadium dioxide is monocline, with the rising of temperature, as temperature T>During Tc, vanadium dioxide is transformed into four directions
Structure, completes phase in version process, and infrared emittance is undergone mutation during this phase in version.Fig. 2 the present embodiment is prepared
Thermotropic infrared emittance vanadium dioxide thin slice XRD spectra, as can be seen from the figure 2 θ=26.9 °, 27.9 °,
33.4 °, 37.1 °, 39.9 °, 42.4 °, 44.7 °, 52.9 °, 55.6 °, 57.5 °, 60.6 ° and 65.0 ° have diffraction maximum, right respectively
Answer monocline VO2(- 111), (011), (- 102), (- 211), (002), (- 212), (012), (- 302), (- 311),
(220), (022), (- 313) and (- 402) crystal face, the collection of illustrative plates with standard PDF cards 43-1051 are corresponded, and show VO2Powder
Crystallinity it is good.The SEM figures of the thermotropic infrared emittance hypovanadic oxide powder that Fig. 3 is prepared for the present embodiment, from figure
In as can be seen that VO2The pattern almost spherical of powder, particle size is 70nm~80nm or so, even size distribution.Fig. 4 sheets
The DSC spectrograms of the thermotropic infrared emittance vanadium dioxide thin slice that implementation is prepared, it can be seen that 66.7 DEG C are
VO2Endothermic peak, 60.3 DEG C be VO2Exothermic peak, show the VO for obtaining2Thin slice has thermal induced phase transition property.
The method of testing of the present embodiment infrared emittance is as follows：Reference literature (Cao Yi, Cheng Haifeng, Zheng Wenwei, just great year,
Cheng Shaojun are based on coating wave band emissivity measurement [J] infrared techniques of thermal infrared imager, 2007,29 (6):In 316-320)
Measuring method, the infrared emittance of 7.5 μm~14 mu m wavebands is tested using FLIR thermal infrared imagers.Constant temperature water bath is heated to
Testing temperature is treated, sample is pasted onto using heat-conducting glue by water bath side, position is below the water surface and near center, thermal balance
30min；Thermal infrared imager is opened, starts automatic shooting function record infrared chart, operating personnel withdraw from a room during shooting, it is to avoid
The influence of human body radiation；The radiation temperature of sample surfaces is read with thermal infrared imager bundled software, and by being calculated difference
At a temperature of sample infrared emittance.
The vanadium dioxide thin slice annealed without process and the thermotropic that the present embodiment is prepared are tested using the above method
Infrared emittance of the infrared emittance vanadium dioxide thin slice at 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C and 90 DEG C, what is obtained is red
Emission rate variation with temperature curve as shown in Figure 5 and Figure 6, it can be seen that by annealing vanadium dioxide
The maximum sudden change value of infrared emittance is 0.20, thermotropic infrared emittance vanadium dioxide thin slice phase in version before and after thin slice phase in version
The maximum sudden change value of front and rear infrared emittance is 0.34.Annealed a small amount of other phases in obtained powder by argon gas atmosphere
Vanadium dioxide be changed into the vanadium dioxide of monoclinic phase, improve the mechanical strength and crystallinity of thin slice, increased vanadium dioxide
The variable quantity of infrared emittance before and after thin slice phase transformation.
Embodiment 2
A kind of thermotropic infrared emittance vanadium dioxide preparation of sections method of the invention, comprises the following steps：
(1) 1.76g (0.015mol) ammonium metavanadates and 1.58g (0.0082mol) citric acid are added to 70ml deionizations
Magnetic agitation mixing is carried out in water, homogeneous solution is formed, mixing time is 30 minutes；Then the solution that will be obtained is transferred to
In 100ml water heating kettles, 8h is reacted at 285 DEG C；
(2) after the completion of reacting, after product is taken out after water heating kettle natural cooling, the product that will be obtained first is centrifuged, then will
The product obtained after centrifugation with alternately washing three times of deionized water, absolute ethyl alcohol, is finally vacuum dried at 80 DEG C successively,
Drying time is 10h, obtains final product VO2Powder；
(3) VO that 0.6g steps (2) are obtained is taken2Powder, is pressed into a diameter of using tablet press machine under the pressure of 20MPa
The thin slice of 20mm, is then made annealing treatment using following cycle of annealing in argon gas atmosphere：A () is from room temperature to 600
DEG C, heating rate is 5 DEG C/min；B () is incubated 6h at 600 DEG C；C () is cooled to room temperature, rate of temperature fall is 4 DEG C/min, that is, obtain
Thermotropic infrared emittance vanadium dioxide thin slice of the invention.
After testing, the VO that the present embodiment is prepared2Powder even size distribution, VO2The mechanical strength of thin slice is higher, knot
Crystalline substance is good, is monocline phase structure, with thermal induced phase transition property；The method of testing of the present embodiment infrared emittance with embodiment 1,
The thermotropic infrared emittance vanadium dioxide thin slice that test the present embodiment is prepared is at 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C
With the infrared emittance at 90 DEG C, the maximum sudden change value for drawing infrared emittance before and after vanadium dioxide thin slice phase in version is 0.33.
Embodiment 3
A kind of thermotropic infrared emittance vanadium dioxide preparation of sections method of the invention, comprises the following steps：
(1) 2.07g (0.015mol) potassium metavanadates and 3.15g (0.0164mol) citric acid are added to 60ml deionizations
Magnetic agitation mixing is carried out in water, homogeneous solution is formed, mixing time is 30 minutes；Then the solution that will be obtained is transferred to
In 100ml water heating kettles, 12h is reacted at 285 DEG C；
(2) after the completion of reacting, after product is taken out after water heating kettle natural cooling, the product that will be obtained first is centrifuged, then will
The product obtained after centrifugation with alternately washing three times of deionized water, absolute ethyl alcohol, is finally vacuum dried at 70 DEG C successively,
Drying time is 11h, obtains final product VO2Powder；
(3) VO that 0.8g steps (2) are obtained is taken2Powder, is pressed into a diameter of using tablet press machine under the pressure of 20MPa
The thin slice of 20mm, is then made annealing treatment using following cycle of annealing in argon gas atmosphere：A () is from room temperature to 700
DEG C, heating rate is 8 DEG C/min；B () is incubated 6h at 700 DEG C；C () is cooled to room temperature, rate of temperature fall is 6 DEG C/min, that is, obtain
Thermotropic infrared emittance vanadium dioxide thin slice of the invention.
After testing, the VO that the present embodiment is prepared2Powder even size distribution, VO2The mechanical strength of thin slice is higher, knot
Crystalline substance is good, is monocline phase structure, with thermal induced phase transition property；The method of testing of the present embodiment infrared emittance with embodiment 1,
The thermotropic infrared emittance vanadium dioxide thin slice that test the present embodiment is prepared is at 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C
With the infrared emittance at 90 DEG C, the maximum sudden change value for drawing infrared emittance before and after vanadium dioxide thin slice phase in version is 0.31.
Embodiment 4
A kind of thermotropic infrared emittance vanadium dioxide preparation of sections method of the invention, comprises the following steps：
(1) 1.76g (0.015mol) ammonium metavanadates and 1.58g (0.0082mol) citric acid are added to 85ml deionizations
Magnetic agitation mixing is carried out in water, homogeneous solution is formed, mixing time is 30 minutes；Then the solution that will be obtained is transferred to
In 100ml water heating kettles, 8h is reacted at 285 DEG C；
(2) after the completion of reacting, after product is taken out after water heating kettle natural cooling, the product that will be obtained first is centrifuged, then will
The product obtained after centrifugation with alternately washing three times of deionized water, absolute ethyl alcohol, is finally vacuum dried at 60 DEG C successively,
Drying time is 12h, obtains final product VO2Powder；
(3) VO that 0.5g steps (2) are obtained is taken2Powder, is pressed into a diameter of using tablet press machine under the pressure of 16MPa
The thin slice of 20mm, is then made annealing treatment using following cycle of annealing in argon gas atmosphere：A () is from room temperature to 600
DEG C, heating rate is 5 DEG C/min；B () is incubated 4h at 600 DEG C；C () is cooled to room temperature, rate of temperature fall is 4 DEG C/min, that is, obtain
Thermotropic infrared emittance vanadium dioxide thin slice of the invention.
After testing, the VO that the present embodiment is prepared2Powder even size distribution, VO2The mechanical strength of thin slice is higher, knot
Crystalline substance is good, is monocline phase structure, with thermal induced phase transition property；The method of testing of the present embodiment infrared emittance with embodiment 1,
The thermotropic infrared emittance vanadium dioxide thin slice that test the present embodiment is prepared is at 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C
With the infrared emittance at 90 DEG C, the maximum sudden change value for drawing infrared emittance before and after vanadium dioxide thin slice phase in version is 0.30.
Embodiment 5
A kind of thermotropic infrared emittance vanadium dioxide preparation of sections method of the invention, comprises the following steps：
(1) 1.76g (0.015mol) ammonium metavanadates and 3.15g (0.0164mol) citric acid are added to 70ml deionizations
Magnetic agitation mixing is carried out in water, homogeneous solution is formed, mixing time is 30 minutes；Then the solution that will be obtained is transferred to
In 100ml water heating kettles, 16h is reacted at 245 DEG C；
(2) after the completion of reacting, after product is taken out after water heating kettle natural cooling, the product that will be obtained first is centrifuged, then will
The product obtained after centrifugation with alternately washing three times of deionized water, absolute ethyl alcohol, is finally vacuum dried at 80 DEG C successively,
Drying time is 10h, obtains final product VO2Powder；
(3) VO that 0.6g steps (2) are obtained is taken2Powder, is pressed into a diameter of using tablet press machine under the pressure of 20MPa
The thin slice of 20mm, is then made annealing treatment using following cycle of annealing in argon gas atmosphere：A () is from room temperature to 600
DEG C, heating rate is 5 DEG C/min；B () is incubated 6h at 600 DEG C；C () is cooled to room temperature, rate of temperature fall is 4 DEG C/min, that is, obtain
Thermotropic infrared emittance vanadium dioxide thin slice of the invention.
After testing, the VO that the present embodiment is prepared2Powder even size distribution, VO2The mechanical strength of thin slice is higher, knot
Crystalline substance is good, is monocline phase structure, with thermal induced phase transition property；The method of testing of the present embodiment infrared emittance with embodiment 1,
The thermotropic infrared emittance vanadium dioxide thin slice that test the present embodiment is prepared is at 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C
With the infrared emittance at 90 DEG C, the maximum sudden change value for drawing infrared emittance before and after vanadium dioxide thin slice phase in version is 0.32.
Embodiment 6
A kind of thermotropic infrared emittance vanadium dioxide preparation of sections method of the invention, comprises the following steps：
(1) 1.76g (0.015mol) ammonium metavanadates and 2.10g (0.011mol) citric acid are added to 70ml deionized waters
In carry out magnetic agitation mixing, form homogeneous solution, mixing time is 30 minutes；Then the solution that will be obtained is transferred to
In 100ml water heating kettles, 32h is reacted at 205 DEG C；
(2) after the completion of reacting, after product is taken out after water heating kettle natural cooling, the product that will be obtained first is centrifuged, then will
The product obtained after centrifugation with alternately washing three times of deionized water, absolute ethyl alcohol, is finally vacuum dried at 80 DEG C successively,
Drying time is 10h, obtains final product VO2Powder；
(3) VO that 0.6g steps (2) are obtained is taken2Powder, is pressed into a diameter of using tablet press machine under the pressure of 20MPa
The thin slice of 20mm, is then made annealing treatment using following cycle of annealing in argon gas atmosphere：A () is from room temperature to 600
DEG C, heating rate is 5 DEG C/min；B () is incubated 6h at 600 DEG C；C () is cooled to room temperature, rate of temperature fall is 4 DEG C/min, that is, obtain
Thermotropic infrared emittance vanadium dioxide thin slice of the invention.
After testing, the VO that the present embodiment is prepared2Powder even size distribution, VO2The mechanical strength of thin slice is higher, knot
Crystalline substance is good, is monocline phase structure, with thermal induced phase transition property；The method of testing of the present embodiment infrared emittance with embodiment 1,
The thermotropic infrared emittance vanadium dioxide thin slice that test the present embodiment is prepared is at 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C
With the infrared emittance at 90 DEG C, the maximum sudden change value for drawing infrared emittance before and after vanadium dioxide thin slice phase in version is 0.28.
Embodiment 7
A kind of thermotropic infrared emittance vanadium dioxide preparation of sections method of the invention, comprises the following steps：
(1) 2.07g (0.015mol) potassium metavanadates and 1.58g (0.0082mol) citric acid are added to 70ml deionizations
Magnetic agitation mixing is carried out in water, homogeneous solution is formed, mixing time is 30 minutes；Then the solution that will be obtained is transferred to
In 100ml water heating kettles, 32h is reacted at 205 DEG C；
(2) after the completion of reacting, after product is taken out after water heating kettle natural cooling, the product that will be obtained first is centrifuged, then will
The product obtained after centrifugation with alternately washing three times of deionized water, absolute ethyl alcohol, is finally vacuum dried at 60 DEG C successively,
Drying time is 12h, obtains final product VO2Powder；
(3) VO that 0.8g steps (2) are obtained is taken2Powder, is pressed into a diameter of using tablet press machine under the pressure of 20MPa
The thin slice of 20mm, is then made annealing treatment using following cycle of annealing in argon gas atmosphere：A () is from room temperature to 700
DEG C, heating rate is 8 DEG C/min；B () is incubated 6h at 700 DEG C；C () is cooled to room temperature, rate of temperature fall is 6 DEG C/min, that is, obtain
Thermotropic infrared emittance vanadium dioxide thin slice of the invention.
After testing, the VO that the present embodiment is prepared2Powder even size distribution, VO2The mechanical strength of thin slice is higher, knot
Crystalline substance is good, is monocline phase structure, with thermal induced phase transition property；The method of testing of the present embodiment infrared emittance with embodiment 1,
The thermotropic infrared emittance vanadium dioxide thin slice that test the present embodiment is prepared is at 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C
With the infrared emittance at 90 DEG C, the maximum sudden change value for drawing infrared emittance before and after vanadium dioxide thin slice phase in version is 0.29.
Claims (4)
1. a kind of thermotropic infrared emittance vanadium dioxide preparation of sections method, it is characterised in that comprise the following steps：
(1) metavanadate, citric acid and deionized water are mixed, stirring forms solution, is then transferred to resulting solution
Hydro-thermal reaction is carried out in water heating kettle；The hydrothermal temperature is 245 DEG C~285 DEG C, and the reaction time is 8h~16h；Metavanadic acid
Salt is selected from least one in ammonium metavanadate, potassium metavanadate, and the mol ratio of metavanadate and citric acid is 0.5~3:1, water heating kettle
Filling rate be 45%~85%；
(2) product of gained is centrifuged after step (1) hydro-thermal reaction is terminated, and the product obtained after centrifugation uses deionization successively
Alternately washing, the vacuum drying of water and absolute ethyl alcohol, obtains hypovanadic oxide powder；The hypovanadic oxide powder is nano particle；
(3) hypovanadic oxide powder that step (2) is obtained first is suppressed into flakiness, is then carried out at annealing in argon gas atmosphere again
Reason, obtains final product described thermotropic infrared emittance vanadium dioxide thin slice；The vanadium dioxide thin slice is monocline phase structure；By dioxy
Change the thin slice that vanadium powder body is pressed into a diameter of 20mm, pressing pressure is 16MPa~20MPa；The annealing temperature be 600 DEG C~
700 DEG C, specific cycle of annealing is：A (), from room temperature to 600 DEG C~700 DEG C, heating rate is 5~8 DEG C/min；B () exists
600 DEG C~700 DEG C insulation 4h~6h；C () is cooled to room temperature, rate of temperature fall is 4~6 DEG C/min.
2. preparation method as claimed in claim 1, it is characterised in that the mol ratio of the metavanadate and citric acid is 1~
2:1, the filling rate of the water heating kettle is 60%~85%.
3. preparation method as claimed in claim 1, it is characterised in that in the step (2), the product obtained after centrifugation is successively
With alternately washing 3 times of deionized water, absolute ethyl alcohol；Vacuum drying temperature is 50 DEG C~100 DEG C, and drying time is 8h~15h.
4. preparation method as claimed in claim 3, it is characterised in that the vacuum drying temperature is 60 DEG C~80 DEG C, is done
The dry time is 10h~12h.
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| CN1451633A (en) * | 2002-11-16 | 2003-10-29 | 中山大学 | Method for making vanadium dioxide and its adulterant nanoceramics |
| CN101391814A (en) * | 2008-10-31 | 2009-03-25 | 中国科学院上海硅酸盐研究所 | Method for preparing rutile phase hypovanadic oxide powder |
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