CN103173207B - Thermochromic composite nanometer powder preparation method - Google Patents
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Abstract
The invention discloses a thermochromic composite nanometer powder preparation method. The method comprises the following steps of: preparing a vanadium dioxide precursor solution or a doped vanadium dioxide precursor solution by using a micro-emulsion method; wrapping the vanadium dioxide precursor or the doped vanadium dioxide precursor by using oxide with sintering inertness; and carrying out thermal treatment on the wrapped precursors. The composite nanometer powder prepared by the method has excellent dispersity, stability and thermochromic property. The preparation method disclosed by the invention has the advantages of simplicity, can be continuously controlled, is short in preparation period, good in repeatability and low in cost; large-scale production is easy to realize; and especially, the method can be used for obtaining the composite nanometer powder with controllable morphology and has practical value and application prospect.
Description
Technical field
The present invention relates to a kind of preparation method of thermochromism composite nano powder, specifically, relate to a kind ofly form nucleocapsid structure (VO by thering is the oxide compound parcel vanadium dioxide of sintering inertia or the vanadium dioxide of doping
2@SiO
2) the preparation method of thermochromism composite nano powder of nano particle composition, belong to functional materials preparing technical field.
Background technology
Because global energy resource is day by day poor, excessively carbon emission causes that environment goes from bad to worse, and energy-saving and emission-reduction have become the top priority of current various countries.According to estimates, in social total energy consumption, having more than 1/3 is building energy consumption, and energy-saving and emission-reduction are imperative, and energy-saving and emission-reduction must be paid the utmost attention to building energy conservation.Due to very most of for air-conditioning in building energy consumption, over half in air conditioner energy source run off by window and extraneous heat exchange, therefore by the Intelligent energy-saving window of development of new, can effectively reduce energy consumption, reduce the discharge of greenhouse gases, finally reach the object of energy-conserving and environment-protective.
Existing Energy Saving Windows generally adopts glass structure or the coated glass of hollow, and wherein, coated glass also has the regulating effect to insolation simultaneously, is one of main development direction of current Energy Saving Windows.Existing energy-conservation coated glass can roughly be divided into two classes, one class is the fixing Energy Saving Windows of optical property, taking the low radiation of Low-E(in the market) coated glass is as representative, low price, heat-proof quality is superior, be most widely used, but shortcoming is can not hold performance to light because of seasonal variation to regulate in real time, is difficult to adapt to China's thermally demand in district of most of cold summers; Another kind of be called as " intelligent power saving glass ", adopts multiple off-color material so that various physical stimulations are produced to corresponding optical change, can adapt to the demand of nearly all region and weather, energy-conservation and make indoor environment more comfortable.Typical Representative in intelligent power saving glass is electrochomeric glass, adopts additional switch and power supply to impel coated glass generation chemical transformation to reach light modulation object.Because electrochromism coated glass can be thought an electronic component substantially, its complex structure, preparation technology requires high, and needs switch and artificial energy source could realize light modulation, involves great expense, and is difficult in a short time realize large-scale production and application.By contrast, utilize a kind of thermochromism intelligent power saving glass of metal/semiconductor temperature control phase transformation research and development of particular matter, have simple in structure, just can realize completely the remarkable advantage such as full-automatic photo-thermal regulation and control of the temperature variation of according with one's environment without switch or any artificial energy source, the special most of thermally various building demands in district of cold summer of China that adapt to, and China takes its place in the front ranks of the world in this regard, be expected to obtain in a short time breakthrough, take the lead in realizing industrialization.The key substance of this thermochromism intelligent power saving glass is vanadium dioxide (VO
2).
Preparation thermochromism intelligent glass has two kinds of modes,, adopt extensive magnetron sputtering to prepare the physics preparation method of vanadium dioxide coated glass, prepare vanadium dioxide nano powder with chemical means in advance with employing nanotechnology, then nano-powder is prepared to the chemical preparation of the pad pasting energy-saving glass mode that becomes by modes such as chemicalpistons.Compared with front a kind of mode, the latter is because equipment is simple, and ubiquity is strong, cheap, and be easy to big area and produce, and the remarkable advantage such as wide application, more easily accepted by market.
As everyone knows, vanadium dioxide composition has some isomerism crystallizations, is defined as respectively A, B, and C, D, M and R phase, be R phase in the most stable crystalline phase of near room temperature, because having same crystalline structure with rutile, so be called again Rutile Type.Rutile phase hypovanadic oxide has thermochromic properties.So-called thermochromic properties, the optical property that refers to material as seen through, reflection or absorption etc., can change reversible change performance occurs with material temperature.If variable color occurs in visible-range, can be visually noticeable; And at visible ray wave band in addition, as the optical change that the infrared band of the sun (780-2500 nanometer) etc. occurs, though naked eyes are invisible, be also considered to sensu lato variable color.Research shows: rutile phase hypovanadic oxide is oblique crystal (M phase) when lower than 68 DEG C, is characteristic of semiconductor,, infrared rays is had to higher transmitance that is; When higher than 68 DEG C, be regular crystal (R phase), be metallic character, infrared rays is had to high-reflectivity.
But the vanadium dioxide nano particle that how to synthesize monodisperse and single one rutile phase is the challenge of this area always.Recently, successfully synthesize rutile phase hypovanadic oxide nano-powder (Solar Energy Materials & Solar Cells95 (2011) 3520, Chinese patent CN102120615A) in Japan and the domestic hydro-thermal reaction method of utilizing.But, above-mentioned utilize the direct titania phase hypovanadic oxide of hydrothermal method one step nano-powder need be more than 260 DEG C pyroprocessing 24 hours, power consumption, consuming time, productive rate is little in batches.And this by hydro-thermal reaction, directly synthetic nano-powder pattern is single, report is only confined to be similar to the particle that waits side's (for example three-dimensional dimension approaching near square or subsphaeroidal) at present.Because this square structure nano particle that waits is after glass surface is piled up, very easily by particle surface, incident light is produced to diffuse-reflectance, the increase of glass surface mist degree, light transmission are reduced, in addition, because the light refractive index of vanadium dioxide crystal is very high, to greatly increase the reflex components of particle and air interface, equally the transmitance of visible ray is produced to detrimentally affect.
Summary of the invention
The problems referred to above and the demand that exist for prior art, the object of this invention is to provide a kind of method of preparing thermochromism composite nano powder, to meet the application requiring of energy-saving material.
For achieving the above object, the technical solution used in the present invention is as follows:
A method of preparing thermochromism composite nano powder, comprises the steps:
A) prepare the vanadium dioxide precursor solution of vanadium dioxide precursor solution or doping with microemulsion method;
B) with the oxide compound with sintering inertia, the vanadium dioxide presoma of vanadium dioxide presoma or doping is wrapped up;
C) presoma after parcel is heat-treated.
As a kind of preferred version, described step a) comprises following operation:
1. be 100:(3～8 in mass ratio by preparing the required oil phase of microemulsion, tensio-active agent, cosurfactant, water): (5～20): the proportioning of (1～10) is mixed, stir to clarify vitreous state, make to form stable microemulsion system; Wherein: described oil phase is alkane solvents, described tensio-active agent is cats product, and described cosurfactant is alcoholic solvent, and described water is the tetravalent vanadium ion aqueous solution or the tetravalent vanadium ion aqueous solution that contains dopant ion;
2. in the microemulsion system forming, drip precipitation agent, make system become muddy state;
3. heating, makes system to boiling state, keeps 0.1～5 hour, is then cooled to room temperature, obtains the vanadium dioxide precursor solution of vanadium dioxide precursor solution or doping.
As further preferred version, described oil phase is hexane, decane, octane, dodecane, toluene or p-Xylol; Described tensio-active agent is palmityl trimethyl ammonium chloride (CTAC) or cetyl trimethylammonium bromide (CTAB); Described cosurfactant is butanols, amylalcohol or hexanol; Described water is that volumetric molar concentration is the tetravalent vanadium ion aqueous solution of 0.01～10.0mol/L or the tetravalent vanadium ion aqueous solution that contains dopant ion.
As further preferred version, the precipitation agent of step in is 2. ammonia soln, aqueous sodium hydroxide solution, ammonium bicarbonate aqueous solution, ammonium carbonate solution or ammonia.
As a kind of preferred version, described step b) comprises following operation: in vanadium dioxide precursor solution a) making to step or the vanadium dioxide precursor solution of doping, add the compound that has the oxide compound of sintering inertia or can be hydrolyzed to described oxide compound under acidity/alkaline condition; Stir, add ethanol to destroy microemulsion system, centrifugation, washing and dry.
The described oxide compound with sintering inertia is silicon oxide, aluminum oxide, zirconium white or titanium oxide.
Described acidic conditions can regulate and control with 0.01～1mol/L hydrochloric acid soln or sulphuric acid soln, and described alkaline condition can regulate and control with the ammonia soln of 0.01～1mol/L or sodium hydroxide solution.
As a kind of preferred version, the thermal treatment of step in c) is to carry out under vacuum or inert atmosphere.
As a kind of preferred version, the thermal treatment temp of step in c) is 400～1200 DEG C, and heat treatment time is 0.1～24 hour.
As further preferred version, the thermal treatment temp of step in c) is 600～1000 DEG C, and heat treatment time is 0.5～12 hour.
The tetravalent vanadium ion aqueous solution described in the present invention can be by (as tetravalence alkoxide of oxalic acid vanadyl or vanadylic sulfate or vanadium etc.) the direct water-soluble preparation of tetravalence vanadium source and is obtained, also can after reductive agent (as adopted hydrazine or oxalic acid etc.) effect, form and obtain by pentavalent vanadium source (as Vanadium Pentoxide in FLAKES, ammonium meta-vanadate etc.).
Because transformation temperature or the particle morphology etc. of rutile phase hypovanadic oxide can be adulterated and be obtained regulation and control by oligo-element.Because the effect of doped element kind and generation thereof is common practise, so the rutile phase hypovanadic oxide in the present invention comprises known element doping rutile phase hypovanadic oxide at present.Doping agent can, for the oxide compound of the doped element M of regulation, can be near 21～30 transition element, for example scandium, titanium, chromium, manganese, iron, cobalt, nickel, copper vanadium in the periodic table of elements as doped element M; Or zinc-tin and near element thereof, for example indium, antimony, tin, gallium, germanium, lead and bismuth, can be also common for regulating and controlling molybdenum and the tungsten of vanadium dioxide phase transition temperature.Doped element M can be that single element can be also the arbitrary combination in above-mentioned element.That is: can contain the single oxide of single doped element as the oxide compound of the M of doping agent, can be also the oxide compound that contains two or more doped elements, can also be the mixture being formed by the oxide compound of different doped elements.In the present invention, doped element can be controlled size and the pattern of gained doped vanadium dioxide powder.Doped element in doping agent and the mol ratio of tetravalent vanadium ion can be determined according to the doping of doped element, can select in the present invention 1:1000～l:1, preferably 3:97～3:7, more preferably 3:97～1:9.
Thermochromism composite nano powder of the present invention is to form nucleocapsid structure (VO by having the oxide compound parcel vanadium dioxide of sintering inertia or the vanadium dioxide of doping
2@SiO
2) nano particle composition, three-dimensional minimum size≤50 nanometer of described nano particle, the vanadium dioxide in described nano particle is rutile phase hypovanadic oxide VO
2(R), can be used for preparing energy-saving coatings, energy-conservation pad pasting, energy-saving glass or other energy-saving electric components and parts.
The composite nano powder of being prepared by the inventive method, has good dispersiveness, stability and thermochromic properties.And preparation method of the present invention is simple, can serialization control, preparation cycle is short, favorable repeatability, cost is low, is easy to large-scale production, especially, also can obtain the controlled composite nano powder of pattern by the inventive method, has practical value and application prospect.
Brief description of the drawings
The XRD figure of the composite nano powder that Fig. 1 obtains for the present invention;
The TEM figure of the composite nano powder that Fig. 2 obtains for embodiment 1;
The TEM figure of the composite nano powder that Fig. 3 obtains for embodiment 2;
The TEM figure of the composite nano powder that Fig. 4 obtains for embodiment 3;
The DSC figure of the composite nano powder of the Doped Tungsten that Fig. 5 obtains for embodiment 4 under different dopings;
Fig. 6 is that the composite nano powder that obtained by the present invention is made the spectrogram under high low temperature after film.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1
1. will prepare the required decane of microemulsion, cetyl trimethylammonium bromide, amylalcohol, water (the tetravalent vanadium ion aqueous solution of 0.1mol/L) in mass ratio for the proportioning of 100:4:6:4 is mixed, stir to clarify vitreous state, make to form stable microemulsion system;
2. in the microemulsion system forming, drip ammonium bicarbonate soln, make the pH < 6.5 of microemulsion system;
3. heating, makes system to boiling state, keeps 1 hour, is then cooled to room temperature, obtains vanadium dioxide precursor solution;
4. in the vanadium dioxide precursor solution making, add tetraethoxy (TEOS), stir 2～12h;
5. add ethanol to destroy microemulsion system, then centrifugation, washs and is dried, and obtains the vanadium dioxide presoma of Silica-coated;
6. by parcel after presoma under inert atmosphere in 600 DEG C of thermal treatment 1h, obtain composite nano powder of the present invention.
The XRD figure of the composite nano powder obtaining as shown in Figure 1, shows that the vanadium dioxide in obtained composite nano powder is all Rutile Type (R phase) vanadium dioxide.
The TEM figure of the composite nano powder that Fig. 2 obtains for the present embodiment, as seen from Figure 2: the pattern of the composite nano powder obtaining under acidic conditions (pH < 6.5) is bar-shaped, and length is no more than 1 μ m, and width is no more than 50nm.
Embodiment 2
1. will prepare the required decane of microemulsion, cetyl trimethylammonium bromide, amylalcohol, water (the tetravalent vanadium ion aqueous solution of 0.1mol/L) in mass ratio for the proportioning of 100:4:6:4 is mixed, stir to clarify vitreous state, make to form stable microemulsion system;
2. in the microemulsion system forming, drip ammonia soln, make pH=6.5～8.0 of microemulsion system;
3. heating, makes system to boiling state, keeps 1 hour, is then cooled to room temperature, obtains vanadium dioxide precursor solution;
4. in the vanadium dioxide precursor solution making, add tetraethoxy (TEOS), stir 2～12h;
5. add ethanol to destroy microemulsion system, then centrifugation, washs and is dried, and obtains the vanadium dioxide presoma of Silica-coated;
6. by parcel after presoma under inert atmosphere in 600 DEG C of thermal treatment 1h, obtain composite nano powder of the present invention.
The XRD figure of the composite nano powder obtaining as shown in Figure 1, shows that the vanadium dioxide in obtained composite nano powder is all Rutile Type (R phase) vanadium dioxide.
The TEM figure of the composite nano powder that Fig. 3 obtains for the present embodiment, as seen from Figure 3: the pattern of the composite nano powder obtaining under neutrallty condition (pH=6.5～8.0) is bar-shaped and particulate state, the size of particle is no more than 100nm, and the length of nanometer rod is no more than 1 μ m, and width is no more than 50nm.
Embodiment 3
1. will prepare the required decane of microemulsion, cetyl trimethylammonium bromide, amylalcohol, water (the tetravalent vanadium ion aqueous solution of 0.1mol/L) in mass ratio for the proportioning of 100:4:6:4 is mixed, stir to clarify vitreous state, make to form stable microemulsion system;
2. in the microemulsion system forming, drip the aqueous sodium hydroxide solution of 1mol/L, make the pH > 8 of microemulsion system;
3. heating, makes system to boiling state, keeps 1 hour, is then cooled to room temperature, obtains vanadium dioxide precursor solution;
4. in the vanadium dioxide precursor solution making, add tetraethoxy (TEOS), stir 2～12h;
5. add ethanol to destroy microemulsion system, then centrifugation, washs and is dried, and obtains the vanadium dioxide presoma of Silica-coated;
6. by parcel after presoma under inert atmosphere in 600 DEG C of thermal treatment 1h, obtain composite nano powder of the present invention.
The XRD figure of the composite nano powder obtaining as shown in Figure 1, shows that the vanadium dioxide in obtained composite nano powder is all Rutile Type (R phase) vanadium dioxide.
The TEM figure of the composite nano powder that Fig. 4 obtains for the present embodiment, as seen from Figure 4: the pattern of the composite nano powder obtaining under alkaline condition (pH > 8) is near-spherical, and size is no more than 100nm.
Embodiment 4
1. will prepare the required decane of microemulsion, cetyl trimethylammonium bromide, amylalcohol, water (the tetravalent vanadium ion aqueous solution of 0.1mol/L) in mass ratio for the proportioning of 100:4:6:4 is mixed, stir to clarify vitreous state, make to form stable microemulsion system; ;
2. in the microemulsion system forming, drip ammonium bicarbonate aqueous solution, make pH=4～7 of microemulsion system;
3. heating, makes system to boiling state, keeps 1 hour, is then cooled to room temperature, obtains vanadium dioxide precursor solution;
4. in the vanadium dioxide precursor solution making, add tetraethoxy (TEOS), stir 2～12h;
5. add ethanol to destroy microemulsion system, then centrifugation, washs and is dried, and obtains the vanadium dioxide presoma of Silica-coated;
6. by parcel after presoma under inert atmosphere in 600 DEG C of thermal treatment 1h, obtain composite nano powder of the present invention.
The XRD figure of the composite nano powder obtaining as shown in Figure 1, shows that the vanadium dioxide in obtained composite nano powder is all Rutile Type (R phase) vanadium dioxide.
The DSC figure of the composite nano powder of the Doped Tungsten that Fig. 5 obtains for the present embodiment under different dopings, W0, W1, W2 and the W3 in figure represents that respectively in raw material, the atomic ratio of W and V is 0,1%, 2% and 3%; As seen from Figure 5: along with the rising of W doping content, the transformation temperature of described composite nano powder declines, drop to 34.1 DEG C from 83.1 DEG C thereupon, can provide important references to the actual use of film.
The composite nano powder that above-described embodiment is obtained is dispersed in high transparent pressure sensitive adhesive double coated surface, and another side is attached in conventional clear glass, forms thermochromism pad pasting glass.Light transmission rate with spectrophotometric determination under differing temps (90 DEG C and 20 DEG C), it the results are shown in Fig. 6.As seen from Figure 6: at 2000nm, infrared conciliation rate reaches 45.7%, illustrate that the film of being prepared by composite nano powder provided by the invention has very strong infrared ability of regulation and control.
Visible in sum: the composite nano powder of being prepared by the inventive method, has good dispersiveness, stability and thermochromic properties.And, by the pH value of regulation and control microemulsion system, can obtain the composite nano powder of different-shape.
Finally be necessary described herein: above embodiment is only for being described in more detail technical scheme of the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.
Claims (6)
1. a method of preparing thermochromism composite nano powder, is characterized in that, comprises the steps:
A) prepare the vanadium dioxide precursor solution of vanadium dioxide precursor solution or doping with microemulsion method;
B) with the oxide compound with sintering inertia, the vanadium dioxide presoma of vanadium dioxide presoma or doping is wrapped up;
C) presoma after parcel is heat-treated;
Described step a) comprises following operation:
1. be 100:(3～8 in mass ratio by preparing the required oil phase of microemulsion, tensio-active agent, cosurfactant, water): (5～20): the proportioning of (1～10) is mixed, stir to clarify vitreous state, make to form stable microemulsion system; Wherein: described oil phase is alkane solvents, described tensio-active agent is cats product, and described cosurfactant is alcoholic solvent, and described water is the tetravalent vanadium ion aqueous solution or the tetravalent vanadium ion aqueous solution that contains dopant ion;
2. in the microemulsion system forming, drip precipitation agent, make system become muddy state;
3. heating, makes system to boiling state, keeps 0.1～5 hour, is then cooled to room temperature, obtains the vanadium dioxide precursor solution of vanadium dioxide precursor solution or doping;
Described oil phase is hexane, decane, octane, dodecane, toluene or p-Xylol; Described tensio-active agent is palmityl trimethyl ammonium chloride or cetyl trimethylammonium bromide; Described cosurfactant is butanols, amylalcohol or hexanol; Described water is that volumetric molar concentration is the tetravalent vanadium ion aqueous solution of 0.01～10.0mol/L or the tetravalent vanadium ion aqueous solution that contains dopant ion;
Described step b) comprises following operation: in vanadium dioxide precursor solution a) making to step or the vanadium dioxide precursor solution of doping, add the compound that has the oxide compound of sintering inertia or can be hydrolyzed to described oxide compound under acidity/alkaline condition; Stir, add ethanol to destroy microemulsion system, centrifugation, washing and dry;
The thermal treatment temp of step in c) is 400～1200 DEG C, and heat treatment time is 0.1～24 hour.
2. the method for claim 1, is characterized in that: the precipitation agent of step in is 2. ammonia soln, aqueous sodium hydroxide solution, ammonium bicarbonate aqueous solution, ammonium carbonate solution or ammonia.
3. the method for claim 1, is characterized in that: the described oxide compound with sintering inertia is silicon oxide, aluminum oxide, zirconium white or titanium oxide.
4. the method for claim 1, is characterized in that: 0.01～1mol/L hydrochloric acid soln or sulphuric acid soln regulation and control for described acidic conditions; Ammonia soln or the sodium hydroxide solution regulation and control of 0.01～1mol/L for described alkaline condition.
5. the method for claim 1, is characterized in that: the thermal treatment of step in c) is to carry out under vacuum or inert atmosphere.
6. the method for claim 1, is characterized in that: the thermal treatment temp of step in c) is 600～1000 DEG C, and heat treatment time is 0.5～12 hour.
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| CN105694615B (en) * | 2016-02-29 | 2019-01-29 | 中国科学院上海硅酸盐研究所 | A kind of hypovanadic oxide-based thermochromic composite of high-performance |
| CN112158883A (en) * | 2020-10-16 | 2021-01-01 | 成都先进金属材料产业技术研究院有限公司 | Process for preparing vanadium dioxide nano powder |
| CN114078631B (en) * | 2020-10-30 | 2023-02-28 | 宁波磁性材料应用技术创新中心有限公司 | Preparation method of soft magnetic composite material and metal magnetic powder core |
| CN114988472A (en) * | 2022-06-02 | 2022-09-02 | 哈尔滨工业大学 | Ultrasonic microemulsion synthesis method of M-phase superfine vanadium dioxide powder |
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| CN101538066A (en) * | 2008-12-25 | 2009-09-23 | 武汉理工大学 | Method for realizing mono-disperse modification and optimal orientation array of hypovanadic oxide nano wire |
| CN102602998A (en) * | 2011-01-25 | 2012-07-25 | 中国科学院上海硅酸盐研究所 | Vanadium dioxide powders and preparation method thereof |
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| CN102602998A (en) * | 2011-01-25 | 2012-07-25 | 中国科学院上海硅酸盐研究所 | Vanadium dioxide powders and preparation method thereof |
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Effective date of registration: 20220705 Address after: 215400 No.6 Liangfu Road, Taicang City, Suzhou City, Jiangsu Province Patentee after: Jiangsu Institute of advanced inorganic materials Address before: 200050 No. 1295 Dingxi Road, Shanghai, Changning District Patentee before: SHANGHAI INSTITUTE OF CERAMICS, CHINESE ACADEMY OF SCIENCES |