CN103254664A - Method for preparing intelligent temperature control type powder with mica coated by vanadium dioxide - Google Patents
Method for preparing intelligent temperature control type powder with mica coated by vanadium dioxide Download PDFInfo
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- CN103254664A CN103254664A CN201310176260XA CN201310176260A CN103254664A CN 103254664 A CN103254664 A CN 103254664A CN 201310176260X A CN201310176260X A CN 201310176260XA CN 201310176260 A CN201310176260 A CN 201310176260A CN 103254664 A CN103254664 A CN 103254664A
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Abstract
The invention discloses a method for preparing an intelligent temperature control type powder with mica coated by vanadium dioxide. The method is characterized in that an oxide V1-xMxO2 film of vanadium is prepared on the surface of sheet-shaped mica powder by adopting an organic sol-gel method, a drying method and a carbothermic method. The thermally induced phase transition properties of the V1-xMxO2 film is utilized by the powder and the infrared light transmittance (such as sunlight) can be automatically adjusted according to environment temperature so as to realize intelligent temperature control. Since the sheet-shaped structure mica powder is distributed in a medium parallelly, the intelligent temperature control efficiency of the powder is improved. Vanadium sol is coated on the surface of a substrate of the mica powder by virtue of the organic sol-gel method and the drying method, the process is simple, and adulteration is easy to realize. The method is readily available in raw materials, simple in industrial preparation and wide in product application. The implementation of the method can play a role in energy conservation.
Description
Technical field
The present invention relates to the preparation method that a kind of vanadium dioxide coats the intelligent temperature-control functional powder of mica, belong to functional type Composite Preparation field.
Background technology
Energy-saving and environmental protection, intelligence and safety are the themes of 21 century developing material.In the powder field, a variety of intelligent temperature control powders are arranged at present, Chinese patent 200410051967.9,200410051965.X.But the shortcoming of these intelligent temperature control powders is preparation technology and raw material complexity, be difficult for mixing, and cost is higher.
Ir radiation is the principal mode of energy emission in the sunlight, and the near infrared light energy accounts for 50% of sunlight total energy.Monocrystalline VO
2The significantly first-order phase transition from the monoclinic form semi-conductor to cubic rutile crystal type metallographic phase, VO can take place at 68 ℃
2Material is when phase transformation, and infrared transmittivity can be undergone mutation, and has lower infrared transmittivity when being higher than transformation temperature, has higher infrared transmittivity when being lower than transformation temperature, utilizes this character, VO
2Powder and thin-film material can be applied in intelligent temperature control, optical storage, sensing, field such as light-operated.At present about VO
2Powder body material or VO
2The applied research of thin-film material aspect intelligent temperature control mainly concentrates on micron order or nano level VO
2In the preparation and the application in products such as glass, plastics film thereof of powder.(J.Phy.Chem.Solids2001,62: 1229-1238) studied VO such as F.Guinneton
2Film and VO
2Particle is in the optical property of infrared light region.The result shows, continuous VO
2Film is than the VO that is dispersed in the medium
2Micro-nano powder has bigger infrared transmittivity before and after phase transformation changes and more high efficiency optical switch effect.But since preparation technology's restriction, big area VO
2The preparation difficulty of film is big, the cost height.
It is carrier that the present invention adopts flaky mica powder, coats one deck V on its surface
1-xM
xO
2Film.The mica sheet of high thickness to diameter ratio in applicating medium, have can parallel distribution characteristic, can form continuous protective layer, so with traditional spherical VO
2Powder is compared, the V of sheet
1-xM
xO
2/ mica powder physical efficiency improves under the coating high-temp reflectivity to infrared light, can produce better intelligent temperature control effect when being applied in this sheet function powder in the products such as paint, glass, plastics film, as can effectively reducing surface and the internal temperature that is exposed to the equipment under the solar radiation in summer, then can improve its surface and internal temperature winter, play effect cool in summer and warm in winter, save energy.
Summary of the invention
The objective of the invention is provides a kind of vanadium dioxide to coat the preparation method of the intelligent temperature-control functional powder of mica at the deficiencies in the prior art, is characterized in adopting the method for organosol gel, desiccating method and carbothermic reduction at flaky mica powder surface deposition one deck V
1-xM
xO
2Film forms, and the optimization thickness of film is 30-300nm.When temperature is lower than V
1-xM
xO
2During the thin film phase change temperature, the infrared transmittivity of powder is higher, when temperature is higher than its transformation temperature, and V
1-xM
xO
2The infrared transmittivity of film reduces, and the thermal radiation of the variation control infrared light by envrionment temperature realizes intelligent temperature control.
Purpose of the present invention is realized that by following technical measures wherein said raw material umber is parts by weight except specified otherwise.
The preparation method that vanadium dioxide coats the intelligent temperature-control functional powder of mica may further comprise the steps:
1) adopt the organosol gel method to prepare V
2O
5Colloidal sol or contain the V of doped element W, Mo, K, Ce or La
2O
5Colloidal sol;
2) the sheet mica micro mist is carried out surface treatment, remove its surface impurity, and etching sheet mica surface;
3) coat V at surface treated mica powder
2O
5Colloidal sol obtains the V that xerogel coats after the drying
2O
5/ mica powder;
4) with step 3 gained powder and carbon black with 240～360: 1 weight ratio mixes, and under protection of inert gas, in 400～600 ℃ of reduced anneal 1～5h of temperature, obtains the intelligent temperature-control functional powder that vanadium dioxide coats mica.
Described V
2O
5The preparation of organosol is to be the V of 99%～99.999wt% with purity
2O
55.0～10.0 parts of powders mix with 1: 8: 80 weight ratio with phenylcarbinol and isopropylcarbinol and stir evenly, again mixing liquid is incubated 3～4h in airtight container in 80～110 ℃ of oil baths of temperature, leaves standstill 3～5h then, treat that it layering occurs, remove by filter precipitation, obtain V
2O
5Organosol.
Mixing of described W, Mo, K, Ce or La element is that compound with containing W, Mo, K, Ce or La element is dissolved in the ethanol, stirs behind 0.5～1h and above-mentioned V
2O
5Powder is realized with the mixing liquid of phenylcarbinol and isopropylcarbinol mixes oil bath in encloses container method.
The surface treatment of described mica powder is successively at dehydrated alcohol with 4.0～10.0 parts of mica powders, concentration is that 36% hydrochloric acid and concentration are in the mixed solution of 30% hydrogen peroxide, and be that 25% ammoniacal liquor and concentration are in the mixed solution of 30% hydrogen peroxide in concentration, all with 1～3: 5 volume ratio mixes, respectively heated and boiled 0.5～2h.
The method for coating on described flaky mica powder surface is, V
2O
5Organosol and surface treated mica powder are according to 1～8: 100 weight ratio mixes, and carries out drying then.
Described carbon black specific surface is 100-600m
2/ g, V
2O
5/ mica and carbon black are with 240～360: 1 weight ratio mixes.
The temperature of described carbothermic reduction is 400～600 ℃, and under inert atmosphere, gas flow rate is 20～60ml/min, and annealing time is 1～5h, and the powder after the annealing is cooled to room temperature in inert atmosphere.
The preparation method that described vanadium dioxide coats the intelligent temperature-control functional powder of mica prepares the intelligent temperature-control functional powder that vanadium dioxide coats mica.
Performance test:
1, the intelligent temperature-control functional powder of the vanadium dioxide coating mica of the present invention's preparation has obtained confirmation through examination of infrared spectrum, as shown in Figure 1.
2, the intelligent temperature-control functional powder of the vanadium dioxide coating mica of the present invention's preparation is made laminated film in the UV light-cured resin, at wavelength X=4.55 μ m(wave number=2200cm
-1) infrared transmittivity with in the variation of temperature curve (thermic loop line), film raises with temperature at the infrared transmittivity at 4.55 mum wavelength places and reduces, when temperature reduced, infrared transmittivity was returned to the preceding initial value that heats up gradually, has realized reversible transition.
The present invention has following advantage:
1, carbon raises with temperature to the affinity of oxygen and increases in the carbothermic method, and various metals raise with temperature for the affinity of oxygen and reduce, so at high temperature but the reduction with carbon oxide compound is produced corresponding metal or the reduction high oxide is produced corresponding suboxide, and one of the primary product of carbon reduction is CO
2, can stop product by the phenomenon of other contaminating impurities;
2, organosol gel method raw material is easy to get, and technology is simple, and can not produce pollution to product, and preparation process is temperature required lower, and energy consumption is low.
3, powder utilizes the sheet structure of mica, can improve that powder has improved the intelligent temperature control performance of powder to the shield effectiveness of infrared light when being higher than transformation temperature;
Also kept the special color and luster effect of powder when 4, giving powder intelligent temperature control function;
5, because V
1-xM
xO
2Content ratio in the intelligent temperature-control functional powder of vanadium dioxide coating mica is not high, with respect to traditional intelligent temperature control function powder (pure V
1-xM
xO
2Powder), reduced cost.
6, raw material only needs flaky mica powder, high-purity V
2O
5, phenylcarbinol and isopropylcarbinol etc., raw material is simple and easy to.Not high to equipment requirements, cost of goods manifactured is low.
7, use organosol gel method and desiccating method and coat vanadium colloidal sol at the mica powder substrate surface, not high to material and the shape need of base material, realize easily mixing and coating.
Description of drawings
Fig. 1 is for adding V
1-xM
xO
2The high low temperature infrared transmittivity spectrogram of the light-cured resin film of/mica composite granule.
Fig. 1 is V
1-xM
xO
2/ mica function powder joins the laminated film of making in the UV light-cured resin (the shared weight of function powder is 5%), the infrared transmittivity contrast spectrogram under normal temperature and high temperature, and wave-number range is 4000～400cm
-1In the comparison diagram under high temperature and the normal temperature variation of infrared transmittivity as can be known, at 2200cm
-1The infrared transmittivity of wave band drops to 30.0%, changing value about 26.3% from 56.3%.The reason of laminated film infrared transmittivity reduction at high temperature is by VO in the function powder
2Thermal induced phase transition cause VO
2Make that at phase transformation temperature points generation thermal induced phase transition the infrared reflectance difference under low temperature and high temperature is bigger, and then make the infrared transmittivity of laminated film under low temperature and high temperature also show variation by a relatively large margin.(illustrate: at 3500～3200cm
-1The wide absorption peak of wave number is because the hydroxyl O-H stretching vibration in the water molecules causes; At 3000～2800cm
-1The complete absorption peak of wave number is owing to organic saturated c h bond stretching vibration in the resin causes; At 1800～1750cm
-1The complete absorption peak of wave number is owing to organic C=O key stretching vibration in the resin causes; At 1300～1000cm
-1The complete absorption peak of wave number is owing to organic C-O key stretching vibration in the resin causes.）
Fig. 2 is for adding VO
2The temperature variant thermic loop line of the infrared transmittivity figure of the light-cured resin film of/mica composite granule.
Fig. 2 is VO
2/ mica function powder joins the laminated film of making in the UV light-cured resin (the shared weight ratio of function powder is 5%), at wavelength X=4.55 μ m(wave number=2200cm
-1) infrared transmittivity with variation of temperature curve (thermic loop line), as can be observed from Figure, the infrared transmittivity of film behind the photocuring at 4.55 mum wavelength places raises with temperature and reduces, when temperature reduces, infrared transmittivity is returned to the initial value before heating up gradually, has realized reversible transition.
Embodiment
By the following examples the present invention is carried out concrete description; be necessary to be pointed out that at this present embodiment only is used for further specifying that the present invention carries out; can not be interpreted as limiting the scope of the invention, the person skilled in art can make some nonessential improvement and adjustment according to the content of foregoing invention.
1, with 10.0g purity is the V of 99wt%
2O
5Powder and phenylcarbinol and isopropylcarbinol with 1: 8: 80 weight ratio mix stir evenly after, in airtight container, in 110 ℃ of oil bath 4h of temperature, leave standstill 5h then, treat that it layering for some time occurs after, remove by filter precipitation, obtain V
2O
5Organosol;
2, with the 10.0g white mica powder successively at dehydrated alcohol, concentration is that 36% hydrochloric acid and concentration are in the mixed solution of 30% hydrogen peroxide, and concentration is that 25% ammoniacal liquor and concentration are in the mixed solution of 30% hydrogen peroxide, all with 2: 5 ratio heated and boiled 0.5h of volume ratio.With behind the deionized water repetitive scrubbing 100 ℃ of oven dry;
3, the organosol with gained in gained mica powder in the step 2 and the step 1 mixes with 1: 100 weight ratio, stirs, and obtains V after the drying
2O
5/ mica powder;
4, step 3 gained powder and the carbon black weight ratio with 240: 1 is mixed; under protection of inert gas; in 600 ℃ of annealing reduction 3.5h; temperature rise rate is 10 ℃/min; feed the emptying of 40ml/min rare gas element before the annealing process earlier; insulation finishes the back and feeds the protection of inert gas cooling, namely obtains the intelligent temperature-control functional powder that vanadium dioxide coats mica.
Embodiment 2
1, the 0.4g ammonium tungstate is added in the 80ml ethanol, stir 0.5h, it is dissolved fully;
2, with 10.0g purity be the V of 99.999wt%
2O
5Powder mixes with 1: 8: 80 weight ratio with phenylcarbinol and isopropylcarbinol, again gained liquid in the step 1 add wherein stir evenly after, in airtight container in 80 ℃ of oil bath 3h of temperature, leave standstill 3h then, after treating that it layering for some time occurs, remove by filter precipitation, obtain V
2-xW
xO
5Organosol;
3, get the 10.0g white mica powder successively at dehydrated alcohol, concentration is that 36% hydrochloric acid and concentration are in the mixed solution of 30% hydrogen peroxide, and concentration is that 25% ammoniacal liquor and concentration are in the mixed solution of 30% hydrogen peroxide, all with 1: 5 ratio heated and boiled 2h of volume ratio.With behind the deionized water repetitive scrubbing 100 ℃ of oven dry;
4, the colloidal sol with gained in gained mica powder in the step 3 and the step 2 mixes with 8: 100 weight ratio, stirs, and obtains V after the drying
2-xW
xO
5/ mica powder;
5, step 4 gained powder and the carbon black weight ratio with 360: 1 is mixed; under protection of inert gas; in 400 ℃ of annealing reduction 1h; temperature rise rate is 10 ℃/min; feed the emptying of 30ml/min rare gas element before the annealing process earlier; insulation finishes the back and feeds the protection of inert gas cooling, and the vanadium dioxide that namely obtains mixing tungsten coats the intelligent temperature-control functional powder of mica.
Embodiment 3
1, the 0.5g ammonium molybdate is dissolved in the 80ml ethanol, stirs 0.6h, it is dissolved fully;
2, with 5.0g purity be the V of 99.9wt%
2O
5Powder mixes with 1: 8: 80 weight ratio with phenylcarbinol and isopropylcarbinol, again gained liquid in the step 1 add wherein stir evenly after, in airtight container in 100 ℃ of oil bath 4h of temperature, leave standstill 4h then, after treating that it layering for some time occurs, remove by filter precipitation, obtain V
2-xMo
xO
5Organosol;
3, get the 4.0g white mica powder successively at dehydrated alcohol, concentration is that 36% hydrochloric acid and concentration are in the mixed solution of 30% hydrogen peroxide, and concentration is that 25% ammoniacal liquor and concentration are in the mixed solution of 30% hydrogen peroxide, all with 3: 5 ratio heated and boiled 1h of volume ratio.With behind the deionized water repetitive scrubbing 100 ℃ of oven dry;
4, the colloidal sol with gained in gained mica powder in the step 3 and the step 2 mixes with 3: 100 weight ratio, stirs, and obtains V after the drying
2-xMo
xO
5/ mica powder;
5, step 4 gained powder and the carbon black weight ratio with 260: 1 is mixed; under the rare gas element gas shield; in 600 ℃ of annealing reduction 5h; temperature rise rate is 10 ℃/min; feed the emptying of 50ml/min rare gas element before the annealing process earlier; insulation finishes the back and feeds the protection of inert gas cooling, and the vanadium dioxide that namely obtains mixing molybdenum coats the intelligent temperature-control functional powder of mica.
Embodiment 4
1, the 0.3g Potassium monofluoride is dissolved in the 80ml ethanol, stirs 0.8h, it is dissolved fully;
2, be 99.99wt%V with 8.0g purity
2O
5Powder mixes with 1: 8: 80 weight ratio with phenylcarbinol and isopropylcarbinol, again gained liquid in the step 1 add wherein stir evenly after, in airtight container in 100 ℃ of oil bath 4h of temperature, leave standstill 5h then, after treating that it layering for some time occurs, remove by filter precipitation, obtain V
2-xK
xO
5Organosol;
3, get the 5.0g white mica powder successively at dehydrated alcohol, concentration is that 36% hydrochloric acid and concentration are in the mixed solution of 30% hydrogen peroxide, and concentration is that 25% ammoniacal liquor and concentration are in the mixed solution of 30% hydrogen peroxide, all with 1: 5 ratio heated and boiled 0.5h of volume ratio.With behind the deionized water repetitive scrubbing 100 ℃ of oven dry;
4, the colloidal sol with gained in gained mica powder in the step 3 and the step 2 mixes with 7: 100 weight ratio, stirs, and obtains V after the drying
2-xK
xO
5/ mica powder;
5, step 4 gained powder and the carbon black weight ratio with 300: 1 is mixed; under the rare gas element gas shield; in 500 ℃ of annealing reduction 3h; temperature rise rate is 10 ℃/min; feed the emptying of 60ml/min rare gas element before the annealing process earlier; insulation finishes the back and feeds the protection of inert gas cooling, and the vanadium dioxide that namely obtains mixing potassium coats the intelligent temperature-control functional powder of mica.
Embodiment 5
1. the 0.3g lanthanum nitrate is dissolved in the 80ml ethanol, stirs 1h, it is dissolved fully;
2. be the V of 99wt% with 6.0g purity
2O
5Powder mixes with 1: 8: 80 weight ratio with phenylcarbinol and isopropylcarbinol, again gained liquid in the step 1 add wherein stir evenly after, in airtight container in 110 ℃ of oil bath 4h of temperature, leave standstill 4h then, after treating that it layering for some time occurs, remove by filter precipitation, obtain V
2-xLa
xO
5Organosol;
3. get the 6.0g white mica powder successively at dehydrated alcohol, concentration is that 36% hydrochloric acid and concentration are in the mixed solution of 30% hydrogen peroxide, and concentration is that 25% ammoniacal liquor and concentration are in the mixed solution of 30% hydrogen peroxide, all with 2: 5 ratio heated and boiled 1.5h of volume ratio.With behind the deionized water repetitive scrubbing 100 ℃ of oven dry;
4, the colloidal sol with gained in gained mica powder in the step 3 and the step 2 mixes with 1: 100 weight ratio, stirs, and obtains V after the drying
2-xLa
xO
5/ mica powder;
5, step 4 gained powder and the carbon black weight ratio with 320: 1 is mixed; under the rare gas element gas shield; in 450 ℃ of annealing reduction 4h; temperature rise rate is 10 ℃/min; feed the emptying of 40ml/min rare gas element before the annealing process earlier; insulation finishes the back and feeds the protection of inert gas cooling, and the vanadium dioxide that namely obtains mixing lanthanum coats the intelligent temperature-control functional powder of mica.
Embodiment 6
1. the 0.3g cerous nitrate is dissolved in the 80ml ethanol, stirs 0.5h, it is dissolved fully;
2. be the V of 99.9wt% with 10.0g purity
2O
5Powder mixes with 1: 8: 80 weight ratio with phenylcarbinol and isopropylcarbinol, again gained liquid in the step 1 add wherein stir evenly after, in airtight container in 90 ℃ of oil bath 3h of temperature, leave standstill 3h then, after treating that it layering for some time occurs, remove by filter precipitation, the V that obtains
2-xCe
xO
5Organosol;
3. get the 8.0g white mica powder successively at dehydrated alcohol, concentration is that 36% hydrochloric acid and concentration are in the mixed solution of 30% hydrogen peroxide, and concentration is that 25% ammoniacal liquor and concentration are in the mixed solution of 30% hydrogen peroxide, all with 3: 5 ratio heated and boiled 0.5h of volume ratio.With behind the deionized water repetitive scrubbing 100 ℃ of oven dry;
4, the colloidal sol with gained in gained mica powder in the step 3 and the step 2 mixes with 8: 100 weight ratio, stirs, and obtains V after the drying
2-xCe
xO
5/ mica powder;
5, step 4 gained powder and the carbon black weight ratio with 360: 1 is mixed; under the rare gas element gas shield; in 480 ℃ of reduction 3.5h that anneal down; temperature rise rate is 10 ℃/min; feed the emptying of 20ml/min rare gas element before the annealing process earlier; insulation finishes the back and feeds the protection of inert gas cooling, and the vanadium dioxide that namely obtains mixing cerium coats the intelligent temperature-control functional powder of mica.
Claims (8)
1. a vanadium dioxide coats the preparation method of the intelligent temperature-control functional powder of mica, it is characterized in that this method may further comprise the steps:
1) adopt the organosol gel method to prepare V
2O
5Colloidal sol or contain the V of doped element W, Mo, K, Ce or La
2O
5Colloidal sol;
2) the sheet mica micro mist is carried out surface treatment, remove its surface impurity, and etching sheet mica surface;
3) coat V at surface treated mica micro mist
2O
5Colloidal sol obtains the V that xerogel coats after the drying
2O
5/ mica powder;
4) with step 3 gained powder and carbon black with 240～360: 1 weight ratio mixes, and under protection of inert gas, in 400～600 ℃ of reduced anneal 1～5h of temperature, obtains the intelligent temperature-control functional powder that vanadium dioxide coats mica.
2. coat the preparation method of the intelligent temperature-control functional powder of mica according to the described vanadium dioxide of claim 1, it is characterized in that V
2O
5The preparation of organosol is to be the V of 99%～99.999wt% with purity
2O
55.0～10.0 parts of powders mix with 1: 8: 80 weight ratio with phenylcarbinol and isopropylcarbinol and stir evenly, again mixing liquid is incubated 3～4h in airtight container in 80～110 ℃ of oil baths of temperature, leaves standstill 3～5h then, treat that it layering occurs, remove by filter precipitation, obtain V
2O
5Organosol.
3. coat the preparation method of the intelligent temperature-control functional powder of micas according to claim 1 or 2 described vanadium dioxide, it is characterized in that: mixing of W, Mo, K, Ce or La element is that compound with containing W, Mo, K, Ce or La element is dissolved in the ethanol, stirs behind 0.5～1h and above-mentioned V
2O
5Powder is realized with the mixing liquid of phenylcarbinol and isopropylcarbinol mixes oil bath in encloses container method.
4. coat the preparation method of the intelligent temperature-control functional powder of mica according to the described vanadium dioxide of claim 1, the surface treatment that it is characterized in that mica powder is successively at dehydrated alcohol with 4.0～10.0 parts of mica powders, concentration is that 36% hydrochloric acid and concentration are in the mixed solution of 30% hydrogen peroxide, and concentration is that 25% ammoniacal liquor and concentration are in the mixed solution of 30% hydrogen peroxide, all with 1～3: 5 volume ratio mixes, respectively heated and boiled 0.5～2h.
5. coat the preparation method of the intelligent temperature-control functional powder of mica according to the described vanadium dioxide of claim 1, it is characterized in that the method for coating on sheet mica micro mist surface is, V
2O
5Organosol and surface treated mica powder are according to 1～8: 100 weight ratio mixes, and carries out drying then.
6. coat the preparation method of the intelligent temperature-control functional powder of mica according to the described vanadium dioxide of claim 1, it is characterized in that carbon black specific surface is 100-600m
2/ g, V
2O
5/ mica and carbon black are with 240～360: 1 weight ratio mixes.
7. coat the preparation method of the intelligent temperature-control functional powder of mica according to the described vanadium dioxide of claim 1, the temperature that it is characterized in that carbothermic reduction is 400～600 ℃, under inert atmosphere, gas flow rate is 20～60ml/min, annealing time is 1～5h, and the powder after the annealing is cooled to room temperature in inert atmosphere.
8. the preparation method who coats the intelligent temperature-control functional powder of mica according to the described vanadium dioxide of one of claim 1～7 prepares the intelligent temperature-control functional powder that vanadium dioxide coats mica.
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| CN107250240A (en) * | 2014-12-15 | 2017-10-13 | 巴斯夫欧洲公司 | It is used as the mica of the metal oxide-coated of fire retardant |
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