CN106928994B - A kind of photochromic composite nano powder and preparation method thereof, application - Google Patents
A kind of photochromic composite nano powder and preparation method thereof, application Download PDFInfo
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- CN106928994B CN106928994B CN201511008674.7A CN201511008674A CN106928994B CN 106928994 B CN106928994 B CN 106928994B CN 201511008674 A CN201511008674 A CN 201511008674A CN 106928994 B CN106928994 B CN 106928994B
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Abstract
The present invention relates to a kind of photochromic composite nano powders and preparation method thereof, application, the photochromic composite nano powder particle is core-shell structure, and shell is molybdenum trioxide, and kernel is titanium dioxide, wherein the titanium dioxide is anatase titanium dioxide nano particle, and shape is graininess.The preparation of the powder uses simple and quick one step hydro thermal method, i.e., mixes molybdenum source and titanium source, obtains molybdenum oxide through hydro-thermal reaction and coats Titanium dioxide nanoparticle;The photochromic composite nano powder can be applied to energy saving pad pasting, energy-saving glass or energy-saving wall field.The photochromic composite nano powder of foregoing invention has excellent dispersibility, stability has efficient photochromic properties, it can be achieved that the small-sized of molybdenum oxide.
Description
Technical field
The present invention relates to field of inorganic nano material, in particular to a kind of photochromic composite nano powder and its preparation side
Method.
Background technique
It is estimated that building energy consumption generally occupies the one third of social total energy consumption.Meanwhile energy for building is to world greenhouse
The contribution rate of gas discharge is up to 25%, so energy-saving and emission-reduction are the energy-efficient most important things in the world, and energy-saving and emission-reduction must be preferential
Consider building energy conservation.Data shows that building energy consumption 50% is carried out by windowpane, and windowpane is that building and extraneous photo-thermal are handed over
The main thoroughfare changed, therefore realize that building energy conservation mainly by the Intelligent energy-saving window of development of new, reduces energy consumption, reduce greenhouse gas
The discharge of body is finally reached energy-saving and environment-friendly purpose.
The Energy Saving Windows or energy saving pad pasting (abbreviation Energy Saving Windows) occurred at present are roughly divided into two classes, and one kind is that optical property is solid
Fixed Energy Saving Windows, using low-launch-rate (Low-E) glass currently on the market as representative, its advantage is that cheap, heat-proof quality
It is superior, it is most widely used, but the disadvantage is that cannot realize that the summer in winter is adjusted in real time because of seasonal variations, it is difficult to adapt to China's most of winters
The demand in thermally area of cold summer.It is another kind of, it is referred to as " intelligent type energy saving glass ", uses a variety of cause off-color materials to various objects
Reason stimulation generates corresponding optical change, is applicable to most of winter and warms up summer thermally area, energy conservation and indoor environment is made more to relax
It is suitable.Intelligent power saving glass is divided into electrochromism, gas-discoloration, thermochromism and four kinds photochromic.Electrochromic material needs
Apply voltage, structure is complicated, and preparation process requires high, causes expensive;Gas-discoloration needs to be passed through hydrogen and is just able to achieve
Bidirectional modulation;Thermochromism glass colour is short of aesthetic feeling;And it can be developed using the performance of molybdenum trioxide light color photic
Change colour Energy Saving Windows, and the automatic adjustment of illumination transmitance is realized due to that can comply with the variation of four seasons light intensity, and structure is simple, without artificial
The energy is expected to one of the energy-saving glass material as next low-carbon environment-friendly.
So-called photochromic material can be by specifically chemically reacting generation when referring to illumination of the compound A by wavelength h1
The structure product B different with spectrum property and reversible under the action of wavelength is the illumination or heat of h2 generate compound
The phenomenon that.Photochromic material is many kinds of, can generally divide organic photochromic and inorganic photochromic.It is wherein the most popular
One of inorganic photochromic material is molybdenum oxide.
Preparing photochromic intelligent glass, there are two types of modes, i.e., prepare molybdenum trioxide plated film glass using extensive magnetron sputtering
The physics preparation method of glass, and molybdenum trioxide nano powder is prepared with chemical means in advance using nanotechnology, then by nano powder
Body is prepared into the chemical preparation mode of pad pasting energy-saving glass by modes such as chemicalpistons.Compared with former mode, the latter
Since equipment is simple, generality is strong, cheap, is easy to the remarkable advantage of large area production and wide application, it is easier to be city
Field receives.
There are many method of molybdenum oxide preparation, and pattern is also very much, but there is a problem of one it is common: the particle size of preparation compared with
Greatly.Particle is minimum greatly to several hundred nanometers in Chinese patent (CN103288138A, CN102603005A, CN102153142A)
Greater than 50 nanometers.And this patent depends on the tiny feature of titan oxide particles, coats one layer of molybdenum oxide, integrally reduces particle
Size.
Simultaneously because the limitation of itself energy band of molybdenum trioxide semiconductor (in ultraviolet light range), material dimming scope and discoloration
Efficiency is much worse than ideal application.In order to solve this problem, unbodied molybdenum trioxide can be coated on and is matched with molybdenum trioxide
Metal oxide semiconductor, basic reason is that two kinds of matched semiconductors of energy band can form a kind of heterojunction structure, drop
Low energy bandwidth expands dimming scope, avoid light induced electron and hole in conjunction with improving photochromic efficiency.
Have with the matched conductor oxidate of molybdenum oxide energy band compared with more options, titanium dioxide performance is prominent, and main cause is
1) it since titanium oxide is as photochemical catalyst, has excellent performance, shows the light induced electron and hole ratio that it is generated under light conditions
General material is more, this has critical help to molybdenum trioxide photochromic efficiency is improved;2) titanium dioxide performance is stablized, weight
Renaturation is good;3) molybdenum trioxide and coated by titanium dioxide are configured new optical texture unit, and it is anti-that similar designs multilayer film obtains reflection
Only effect is the same.It can get bigger optical effect using the complicated optical effect of this core-shell structure.
Prepare the difficult point that above-mentioned core-shell structure is also this patent.Existing certain methods cladding has synthesized titanium oxide oxidation
Molybdenum composite material (Sensors and Actuators B (2011) 270, J.Am.Chem.Soc. (2000) 5138).But it is above-mentioned
Method is complicated for operation, time-consuming, energy consumption.And the compound coating of these patterns is all without research photochromic properties.
In conclusion now to molybdenum oxide study be short of the main reason for be, 1) compare it is organic and inorganic photic
Under off-color material, more researcher has been transferred to organic photochromic material, and having ignored improves molybdenum trioxide with chemical means
The research of performance.2) lack molybdenum oxide and the compound simple mature technology of titanium oxide.3) lack and be applied as saving by this cladding
The technology of energy film.Due to above, currently without one kind photochromic upper performance and all preferable nano particle of structure with
And energy saving film.
Summary of the invention
Technical problem to be solved by the present invention lies in provide a kind of photochromic composite nano powder and its preparation side
Method, the photochromic composite nano powder have efficient photochromic properties.
In the present invention, the photochromic composite nano powder is core-shell structure, and shell is molybdenum trioxide, and kernel is dioxy
Change titanium.Wherein the titanium dioxide is anatase titanium dioxide nano particle, and shape is little particle, and particle size is not
One, distribution 4-20nm, preferable particle size 5-10nm, the molybdenum trioxide are unbodied molybdenum trioxide nano particle,
Coat thickness 2-10nm.
The present invention provides a kind of photochromic composite nano powder preparation, including choose molybdenum acid solution or by other
Molybdate, which is dissolved in acid solution, obtains molybdenum acid solution as molybdenum source, and titanium source is added in the molybdenum acid solution, and it is molten to obtain presoma
Liquid;Alkali and reductant-oxidant are added in the precursor solution, obtains the molybdenum trioxide through hydro-thermal reaction and coats titanium dioxide
The composite nanometer particle of titanium.
Preferably, the amount of the titanium ion in molybdenum acid solution is added relative to its molar ratio of the amount of molybdenum ion 19:1-1:1.
Preferably, the molybdate is ammonium molybdate, sodium molybdate.The titanium source is preferably titanium tetrachloride or titanium sulfate.
Preferably, the acid solution is identical as the acid group of the titanium source.The preferred 2-3ml/L of acid solutions.The acid is molten
Liquid is preferably hydrochloric acid solution or sulfuric acid solution.The molybdenum acid solution concentration is preferably 0.0083-1.588g/ml.
Preferably, titanium ion and the hydrionic molar ratio 6:(15-20 of the acid solution).
Preferably, the aqueous slkali is ammonium hydroxide, sodium hydroxide or potassium hydroxide, more preferably ammonium hydroxide.
Preferably, the reductant-oxidant is 35% hydrogen peroxide, and the amount of the hydrogen peroxide of addition is that relatively every 1mL titanium source is added
0.1~1g.
The photochromic composite nano powder of the present invention is made of molybdenum oxide cladding Titanium dioxide nanoparticle;The system of the powder
It is standby to use simple and quick one step hydro thermal method, i.e., molybdenum source and titanium source are mixed, obtains molybdenum oxide cladding oxidation through hydro-thermal reaction
Titanium nano particle;The photochromic composite nano powder can be applied to energy saving pad pasting, energy-saving glass or energy-saving wall field.On
The photochromic composite nano powder of invention is stated, it can be achieved that the small-sized of molybdenum oxide, has excellent dispersibility, is stablized
Property, there are efficient photochromic properties.
Detailed description of the invention
Fig. 1 is X-ray diffraction (XRD) map of molybdenum trioxide cladding titanium dioxide nano particle prepared by embodiment 1;
Fig. 2 is the XRD diagram of pure zirconia titanium in the present invention;
Fig. 3 is transmission electron microscope (TEM) photo of molybdenum trioxide cladding titanium dioxide nano particle of the present invention, X-ray energy spectrum
Scheme (EDS) and chooses electron diffraction diagram;
Fig. 4 is the XRD diagram of pure zirconia molybdenum and SEM figure in the present invention;
Fig. 5 is the photochromic properties comparison of molybdenum trioxide cladding titanium dioxide nano particle of the present invention and pure phase molybdenum oxide
Figure;
Fig. 6 is the TEM comparison diagram of different molybdenum source/titanium sources;
Fig. 7 is the light modulation efficiency chart of different molybdenum source/titanium sources.
Specific embodiment
In the present invention, the photochromic composite nano powder is made of molybdenum oxide cladding Titanium dioxide nanoparticle.Institute
Stating molybdenum oxide cladding Titanium dioxide nanoparticle is core-shell structure, using anatase titanium dioxide nano particle as core, with amorphous
Molybdenum trioxide nano particle be shell.The titania nanoparticles are spherical shape, and the molybdenum trioxide nano particle is uniform
The titania nanoparticles are coated, the coated particle size distribution that different ratio is prepared is uneven, range 4-20nm.
The cladding thickness 2-10nm of the molybdenum trioxide.Efficiency is dimmed according to it, it is preferable that the coated particle partial size is 5-10nm.
The photochromic composite nano powder of the present invention is made of molybdenum oxide cladding Titanium dioxide nanoparticle;The system of the powder
It is standby to use simple and quick one step hydro thermal method, acid solution specially is added in molybdenum source and titanium source and prepares precursor solution, then
Alkali and reductant-oxidant are added, obtains the nano particle of the molybdenum oxide cladding titanium oxide through hydro-thermal reaction.The molybdenum salt can
Think ammonium molybdate, sodium molybdate.The titanium source can be titanium tetrachloride or titanium sulfate.
About the preparation of precursor solution, specifically the molybdates such as ammonium molybdate or sodium molybdate can be dissolved in concentration and be greater than
It is 0.0083~1.588g/ml molybdenum acid solution that concentration is obtained in 2mol/L acid solution, and at room temperature, stirring gained molybdenum acid solution is simultaneously
The titanium source with acid group identical as acid solution, such as titanium tetrachloride or titanium sulfate is added, obtains precursor solution.It can also be direct
Choosing concentration is 0.0083~1.588g/ml molybdenum acid solution as molybdenum source, and at room temperature, simultaneously tool is added in stirring gained molybdenum acid solution
There are the titanium source of acid group identical as acid solution, such as titanium tetrachloride or titanium sulfate, obtains precursor solution.About the dense of acid solution
Degree, is preferably greater than 2mol/L while being less than 3mol/L, adequately dissolves titanium source in this way, reduces its volatilization.
Aqueous slkali is added in the precursor solution, is alkalized, molybdenum titanium colloidal sol is obtained, colloidal sol is in neutrality or alkali at this time
Property.Then reductant-oxidant is added in the molybdenum titanium colloidal sol, is put into reaction kettle, obtains dispersion liquid using hydro-thermal reaction.Add
The aqueous slkali entered can be ammonium hydroxide, sodium hydroxide or potassium hydroxide, preferably ammonium hydroxide.Metatitanic acid structure is generated in order to neutralize acid solution,
It is unlikely to neutralize too the generation for influencing clad structure fastly again, the mass fraction of the aqueous slkali of addition is preferably 28%.And be added
The amount of aqueous slkali is monitored in terms of PH, until being dissolved as neutral or meta-alkalescence, is complexed with reaching whole titanium sources into metatitanic acid, absorption
Molybdenum source.What reductant-oxidant selected is concentration for 35% hydrogen peroxide, the amount of addition is that 0.1~1g is added in relatively every 1mL titanium source,
For the hydroxyl in desorption reaction precipitating.The reaction temperature of hydro-thermal reaction should be controlled at 150 degrees Celsius, the time in reaction time 6
Hour.The dispersion liquid is cooled to room temperature, successively by filtering, deionized water washing and dehydrated alcohol washing, is obtained after dry
It obtains molybdenum oxide and coats Titanium dioxide nanoparticle.Drying temperature is 70-90 degrees Celsius.
As an example, being further specifically described photochromic composite nano powder preparation of the invention comprising
Molybdenum source: 1) being dissolved in acid solution by following steps, obtains molybdenum acid solution, the molybdenum acid solution of stirring;2) it at room temperature, stirs
Simultaneously titanium source is added in the molybdenum acid solution, obtains precursor solution;3) aqueous slkali is added in the precursor solution, through alkalizing,
Obtain molybdenum titanium colloidal sol;4) reductant-oxidant is added in the molybdenum titanium colloidal sol, obtains dispersion liquid by hydro-thermal reaction;It 5) will be described
Dispersion liquid is cooled to room temperature, and by being filtered, washed, is obtained molybdenum oxide and is coated Titanium dioxide nanoparticle.Optionally, the molybdenum source is
Ammonium molybdate, sodium molybdate or molybdic acid, the titanium source are titanium tetrachloride or titanium sulfate, the acid of the acid group of the acid solution and the titanium source
Root is identical;The acid solutions are greater than 2ml/L, and the molybdenum acid solution concentration is 0.0083-1.588g/ml.Preferably, described
Acid solution is hydrochloric acid or sulfuric acid, and the titanium source is titanium tetrachloride, and the volume ratio of the titanium source and the acid solution is 6:(15-
20).Optionally, the aqueous slkali is ammonium hydroxide, sodium hydroxide or potassium hydroxide, it is preferable that the aqueous slkali is ammonium hydroxide, described molten
Glue is in neutrality or alkalinity.Optionally, the reductant-oxidant is hydrogen peroxide, it is preferable that the hydrogen peroxide concentration is 35%, is added
Amount be that 0.1~1g is added in every 1mL titanium source relatively.
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
This embodiment describes a kind of preparation methods of molybdenum trioxide cladding titanium dioxide nano particle, comprising:
S1: 0.1576g ammonium paramolybdate is added in the hydrochloric acid solution of 10ml, 2mol/L and obtains soluble molybdenum acid solution;
S2: 1ml titanium tetrachloride is added in soluble molybdenum acid solution under stirring at room temperature, obtains precursor solution;
S3: appropriate ammonium hydroxide is added dropwise in the precursor solution makes solution PH > 7, is alkalized, and obtains molybdenum titanium colloidal sol;
S4: in the molybdenum titanium colloidal sol, 0.5g hydrogen peroxide is added in relatively every 1mL titanium source, is put into reaction kettle, in temperature
It is reacted 6 hours at 150 DEG C, reaction terminates to obtain dispersion liquid;
S5: dispersion liquid is cooled to room temperature, and is successively washed through deionized water, and dehydrated alcohol washing through drying, obtains three oxygen
Change molybdenum cladding titanium dioxide (TiO2-MoO3Cladding) core-shell structure nanopowder body, it is named as TM-10.
Embodiment 2
The preparation of pure zirconia titanium: refering to the system of molybdenum trioxide cladding titanium dioxide nano particle described in embodiment 1
For step, step S1 hydrochloric acid solution is added without ammonium paramolybdate in embodiment 1, remaining step can be prepared pure with embodiment 1
Titanium oxide.
Fig. 1 is X-ray diffraction (XRD) map of molybdenum trioxide cladding titanium dioxide nano particle prepared by embodiment 1,
Fig. 2 is the XRD diagram of pure zirconia titanium prepared by embodiment 2.Comparison diagram 1 and Fig. 2 are as it can be seen that molybdenum trioxide packet prepared by embodiment 1
The characteristic peak for covering titania nanoparticles is TiO2, there is no other impurity peaks to occur in Fig. 1, illustrates molybdenum trioxide cladding two
TiO in Titanium dioxide nanoparticle2For crystalline state, MoO3For amorphous state.
Fig. 3: Fig. 3 is please referred to as the transmission electron microscope of molybdenum trioxide cladding titanium dioxide nano particle prepared by embodiment 1
(TEM) photo, X-ray energy spectrogram (EDS) and selection electron diffraction diagram.TEM figure and EDS figure combine as can be seen that embodiment 1
It is crystalline particulate state TiO among prepared sample2, around it is coated with amorphous state MoO3, shone in addition, choosing electronic diffraction
Piece has diffraction ring, further illustrates the TiO of crystallization2For polycrystalline state, thus, the cladding oxidation of molybdenum oxide prepared by embodiment 1
TiO in the nano particle of titanium2For polycrystalline state, MoO3For amorphous state.
Embodiment 3
In order to study TiO2-MoO3Improvement of the nanosphere to photochromic properties is coated, contrast sample is prepared.About pure phase
The preparation of molybdenum oxide: seeing the preparation step of molybdenum trioxide cladding titanium dioxide nano particle described in embodiment 1, real
It applies and casts out step S2 in example 1, pure zirconia titanium can be prepared with embodiment 1 in remaining step.
Fig. 4 is the XRD diagram of pure zirconia molybdenum and SEM figure in the present invention, and pure phase molybdenum oxide prepared by the present embodiment is oxidation
Molybdenum nanometer rods.XRD diagram in analysis chart 4, it is known that oxidation molybdenum structure is α-MoO3。
Embodiment 4
By molybdenum trioxide prepared by embodiment 1 is titanium dioxide nano powder coated and embodiment 3 prepared by pure phase oxygen
Change molybdenum powder body to evenly spread in ethanol solution respectively, obtains the photochromic properties that 0.3wt% sample solution tests them.
Referring to Fig. 5, Fig. 5 is the light-induced variable of molybdenum trioxide cladding titanium dioxide nano particle and pure phase molybdenum oxide of the present invention
Color performance comparison figure.As seen from Figure 5, molybdenum trioxide cladding titanium dioxide nano particle prepared by embodiment 1 is photochromic
Efficiency is 20 times of the photochromic efficiency of pure phase molybdenum oxide prepared in embodiment 3, it can be seen that, molybdenum trioxide cladding two
There is Titanium dioxide nanoparticle high light to cause discoloration.
Embodiment 5,6,7 and 8 is unitary variant comparative example, and referring to 1 preparation process of embodiment, what is uniquely changed is molybdenum ion
With the molar ratio of titanium ion.The molar ratio of molybdenum ion and titanium ion once corresponds to are as follows: 5:95,15:85,25:75,50:50.And according to
This is named as TM-5, TM-15, TM-25, its dependent variable of TM-50. no longer explains in detail in the patent, but cannot be limited with this
The interest field of the present invention.
Referring to Fig. 6, Fig. 6 is the TEM comparison diagram of different molybdenum source/titanium sources.With the increase of molybdenum source, particle mean size is more next
Smaller, particle dispersion is become better and better, and particle distribution range is smaller and smaller.TM-5 is distributed as 4-20nm, and TM-25 is narrowed down to
When 5-8nm. molybdenum source is excessive, particle is grown up again, and different types of particle occurs.Therefore TM-25 is minimum dimension cladding.
Referring to Fig. 7, Fig. 7 is the light modulation efficiency chart of different molybdenum source/titanium sources, solution prepares exemplary embodiment 4, sample solution
Concentration is prepared into 0.05wt%.Therefrom as it can be seen that the light modulation efficiency highest of optimum size TM-25.This be exactly before claims
The reason of middle particle size optimizes.
Above disclosed is only a preferred embodiment of the present invention, cannot limit the power of the present invention with this certainly
Sharp range, those skilled in the art can understand all or part of the processes for realizing the above embodiment, and weighs according to the present invention
Benefit requires made equivalent variations, still belongs to the scope covered by the invention.
Claims (8)
1. a kind of photochromic composite nano powder, which is characterized in that the photochromic composite nano powder particle is nucleocapsid
Structure, shell are molybdenum trioxide, and kernel is titanium dioxide, wherein the titanium dioxide is anatase titanium dioxide nanometer
Grain, shape are graininess, and clad structure particle diameter of nanometer powder is distributed as 4-20nm, and the molybdenum trioxide is unbodied three oxidation
Molybdenum nano particle, cladding thickness distribution is uneven, distribution 2-10nm.
2. a kind of preparation method of photochromic composite nano powder as described in claim 1 characterized by comprising choose
Other molybdates are dissolved in acid solution and obtain molybdenum acid solution as molybdenum source by molybdenum acid solution, and titanium is added in the molybdenum acid solution
Source obtains precursor solution;Aqueous slkali and reductant-oxidant are added in the precursor solution, is obtained through hydro-thermal reaction described
The composite nanometer particle of molybdenum trioxide cladding titanium dioxide.
3. photochromic composite nano powder preparation according to claim 2, which is characterized in that the molybdenum salt is molybdenum
Sour ammonium, sodium molybdate, the titanium source are titanium tetrachloride or titanium sulfate.
4. photochromic composite nano powder preparation according to claim 2, which is characterized in that the acid solution is dense
Spend 2-3ml/L.
5. photochromic composite nano powder preparation according to claim 2, which is characterized in that the molybdenum acid solution
Concentration is 0.0083-1.588g/ml, and the molar ratio of titanium ion and molybdenum ion is 19:1-1:1 in reaction solution.
6. photochromic composite nano powder preparation according to claim 2, which is characterized in that titanium ion with it is described
The hydrionic molar ratio of acid solution is 6:(15-20).
7. photochromic composite nano powder preparation according to claim 2, which is characterized in that the aqueous slkali is
Ammonium hydroxide, sodium hydroxide or potassium hydroxide.
8. according to claim 2-7 it is one of any described in photochromic composite nano powder preparation, which is characterized in that institute
Stating reductant-oxidant is 35% hydrogen peroxide of concentration, and the amount of addition is that 0.1~1g hydrogen peroxide is added in relatively every 1mL titanium source.
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CN112694120A (en) * | 2019-10-23 | 2021-04-23 | 中国科学院宁波工业技术研究院慈溪生物医学工程研究所 | Semiconductor nano particle with composite structure, preparation method and application thereof |
CN111944512B (en) * | 2020-08-17 | 2021-07-16 | 山东大学 | Ultra-small inorganic nano heterojunction photochromic material, erasable and rewritable medium prepared by adopting material and preparation method of erasable and rewritable medium |
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