CN114890473A - VO (volatile organic compound) 2 /SiO 2 Method for preparing composite material - Google Patents
VO (volatile organic compound) 2 /SiO 2 Method for preparing composite material Download PDFInfo
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- CN114890473A CN114890473A CN202210656615.4A CN202210656615A CN114890473A CN 114890473 A CN114890473 A CN 114890473A CN 202210656615 A CN202210656615 A CN 202210656615A CN 114890473 A CN114890473 A CN 114890473A
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- 229910004298 SiO 2 Inorganic materials 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 239000012855 volatile organic compound Substances 0.000 title claims description 57
- 238000000498 ball milling Methods 0.000 claims abstract description 53
- 238000000137 annealing Methods 0.000 claims abstract description 39
- 239000004615 ingredient Substances 0.000 claims abstract description 25
- 239000002243 precursor Substances 0.000 claims abstract description 25
- 238000001238 wet grinding Methods 0.000 claims abstract description 22
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 12
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 10
- 239000012043 crude product Substances 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims description 60
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- 238000001035 drying Methods 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 14
- 238000009210 therapy by ultrasound Methods 0.000 claims description 11
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- 239000008103 glucose Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 6
- 238000003801 milling Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 claims description 3
- 229930091371 Fructose Natural products 0.000 claims description 3
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- 239000005715 Fructose Substances 0.000 claims description 3
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 claims description 3
- 229920002472 Starch Polymers 0.000 claims description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 239000008107 starch Substances 0.000 claims description 3
- 235000019698 starch Nutrition 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- ASJSAQIRZKANQN-CRCLSJGQSA-N 2-deoxy-D-ribose Chemical compound OC[C@@H](O)[C@@H](O)CC=O ASJSAQIRZKANQN-CRCLSJGQSA-N 0.000 claims description 2
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 claims description 2
- HMFHBZSHGGEWLO-SOOFDHNKSA-N D-ribofuranose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H]1O HMFHBZSHGGEWLO-SOOFDHNKSA-N 0.000 claims description 2
- 229920002527 Glycogen Polymers 0.000 claims description 2
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 2
- PYMYPHUHKUWMLA-LMVFSUKVSA-N Ribose Natural products OC[C@@H](O)[C@@H](O)[C@@H](O)C=O PYMYPHUHKUWMLA-LMVFSUKVSA-N 0.000 claims description 2
- HMFHBZSHGGEWLO-UHFFFAOYSA-N alpha-D-Furanose-Ribose Natural products OCC1OC(O)C(O)C1O HMFHBZSHGGEWLO-UHFFFAOYSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-PHYPRBDBSA-N alpha-D-galactose Chemical compound OC[C@H]1O[C@H](O)[C@H](O)[C@@H](O)[C@H]1O WQZGKKKJIJFFOK-PHYPRBDBSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- 229930182830 galactose Natural products 0.000 claims description 2
- 229940096919 glycogen Drugs 0.000 claims description 2
- 239000008101 lactose Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 19
- 238000005054 agglomeration Methods 0.000 abstract description 11
- 230000002776 aggregation Effects 0.000 abstract description 11
- 239000002105 nanoparticle Substances 0.000 abstract description 8
- 239000011858 nanopowder Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 238000006479 redox reaction Methods 0.000 abstract description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 38
- 230000000052 comparative effect Effects 0.000 description 29
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 18
- 239000000463 material Substances 0.000 description 18
- 239000000843 powder Substances 0.000 description 18
- 230000003287 optical effect Effects 0.000 description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 14
- 239000004570 mortar (masonry) Substances 0.000 description 9
- 238000001291 vacuum drying Methods 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 238000013329 compounding Methods 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- 238000002834 transmittance Methods 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
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- 238000006243 chemical reaction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Composite Materials (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Silicon Compounds (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a VO 2 /SiO 2 A preparation method of a composite material, belonging to VO 2 The field of composite material preparation. The preparation method adopted by the invention comprises the following steps: preparing mixed ingredients, obtaining a precursor, obtaining a crude product and obtaining a finished product. The invention adopts a mechanochemical method to prepare VO 2 /SiO 2 The composite material is prepared by subjecting a vanadium source and a reducing agent to oxidation-reduction reaction under the action of mechanochemistry, and SiO 2 Can effectively prevent precursor agglomeration in the ball milling process and VO in the annealing process 2 Agglomeration of the nanoparticles; the subsequent wet grinding process can open the soft agglomeration in the nano powder body and further improve the VO 2 Dispersibility of the nanoparticles. Furthermore, SiO 2 Has the anti-reflection effect. The method can realize VO 2 Large scale preparationAnd the obtained VO 2 /SiO 2 The composite material has high dispersibility.
Description
Technical Field
The invention belongs to VO 2 The field of composite material preparation, in particular to VO 2 /SiO 2 A method for preparing a composite material.
Background
Energy exhaustion and environmental pollution become two major problems which need to be solved urgently at present. Wherein, the building energy accounts for about 40 percent of the world energy consumption, and the building energy consumption as high as 50 percent is applied to the regulation and control of the indoor temperature. Therefore, how to reduce the energy required for regulating and controlling the indoor temperature is the key to reduce the energy consumption of the building.
Monoclinic phase VO 2 Is a thermochromic transition metal oxide, undergoes insulator-metal phase transition at about 68 ℃, and is accompanied by abrupt changes in resistivity, infrared transmittance, and the like. When the temperature is lower than the phase transition temperature, the material is an insulator phase, and most of visible light and near infrared light can penetrate VO 2 (ii) a When the temperature is higher than the phase transition temperature, the near infrared light transmittance abruptly decreases, while the visible light transmittance remains almost unchanged. In solar radiation, up to 53% of the energy is concentrated in the near infrared band. Thus, VO 2 The indoor temperature can be regulated. VO compared with other temperature regulating materials 2 The indoor temperature is adjusted mainly through near infrared light, the visible light is not adjusted, and the indoor brightness is still kept when the indoor temperature is adjusted. Thus, VO 2 The method has greater application potential in the field of intelligent windows.
At present, how to prepare high-performance VO on a large scale 2 Nanopowders remain a challenge. The ball milling method is a mechanochemical preparation method, has the advantages of high yield, short period, greenness and simplicity compared with a hydrothermal method, but is a solid-solid reaction, is easy to generate serious agglomeration phenomenon, and further reduces VO 2 Ability to modulate near infrared light. Therefore, how to reduce VO 2 (M) agglomeration in the ball milling process to prepare VO with high dispersibility 2 Nanoparticles are a difficult problem to solve at present.
Disclosure of Invention
The invention aims to provide a VO 2 /SiO 2 The preparation method of the composite material overcomes the defect of preparing high-performance VO in the prior art 2 The difficulty of the nano powder is high, the agglomeration is easy, and the like.
In order to achieve the above object or other objects, the present invention is achieved by the following aspects.
VO (volatile organic compound) 2 /SiO 2 The preparation method of the composite material comprises the following steps:
1) mixing a vanadium source, a reducing agent and SiO 2 Mixing to obtain mixed ingredients;
2) adding the mixed ingredients into a ball milling device, and adding grinding balls for ball milling to obtain a precursor;
3) putting the precursor obtained in the step 2) into a tube furnace for annealing to obtain VO 2 /SiO 2 A composite material crude product;
4) VO obtained by annealing in the step 3) 2 /SiO 2 Taking out the composite material crude product, adding the composite material crude product into a ball milling device, adding a solvent, and carrying out wet milling with grinding balls;
5) carrying out ultrasonic treatment, centrifugation and drying on the solution obtained after wet grinding in the step 4) to obtain VO with good dispersibility 2 /SiO 2 A composite material.
Further, the vanadium source is V 2 O 5 。
Further, the reducing agent is selected from one or more of glucose, fructose, galactose, ribose, deoxyribose, sucrose, maltose, lactose, starch, cellulose and glycogen. Preferably, the reducing agent is selected from glucose.
Further, the grinding ball is selected from one of alumina grinding ball, zirconia grinding ball, agate grinding ball, stainless steel grinding ball, polyurethane grinding ball and hard alloy grinding ball. Preferably, the milling balls are selected from one of alumina milling balls, zirconia milling balls and agate milling balls.
Furthermore, the diameter of the grinding ball is 1-10 mm.
Further, the molar ratio of the vanadium source to the reducing agent is (1-20): 1. preferably, the molar ratio of the vanadium source to the reducing agent is (5-15): 1.
further, a vanadium source and SiO 2 In a molar ratio of 1: (0.1-5). Preferably, the source of vanadium is mixed with SiO 2 In a molar ratio of 1: 1.
further, the mass ratio of the grinding balls to the mixed ingredients in the step 2) is (5-50): 1.
further, the grinding speed in the step 2) is 50-500 r/min.
Further, the grinding time in the step 2) is 5 min-24 h.
Further, the ball milling device may be a ball milling device commonly used in the field of ball milling. The ball milling device can be selected from a ball milling tank.
Further, the annealing temperature in the step 3) is 250-500 ℃, and the annealing time is 1-10 h.
Further, the solvent in the step 4) is ethanol. Preferably, the solvents ethanol and VO 2 /SiO 2 The mass ratio of the composite material crude product is (10-150): 1.
further, grinding balls in the step 4) and VO obtained in the step 3) 2 /SiO 2 The mass ratio of the composite material crude product is (5-100): 1.
further, the wet grinding speed in the step 4) is 50-500 r/min.
Further, the wet grinding time in the step 4) is 1-10 h.
Further, in the step 5), the centrifugal rotating speed is 800-1000 r/min, and the time is 1-30 min. Preferably, the centrifugation time is 10 min. In the step 5), the drying temperature is 10-100 ℃. Preferably, the drying temperature in step 5) is 40 ℃. The drying time in the step 5) is 5-24 h. Preferably, the drying time is 10 h. Further, the atmosphere during drying is vacuum. Further, the ultrasonic time in the step 5) is 1-5 h.
Further, VO prepared by the invention 2 /SiO 2 The average particle size of the composite material is 20-40 nm.
The invention adopts a mechanochemical method to prepare VO 2 /SiO 2 The composite material enables a vanadium source and a reducing agent to generate oxidation-reduction reaction under the mechanochemical action. SiO 2 2 Can haveEffectively prevent precursor agglomeration in the ball milling process and VO in the annealing process 2 And (4) agglomeration of the nano particles. The subsequent wet grinding process can open the soft agglomeration in the nano powder body and further improve the VO 2 Dispersibility of the nanoparticles. Furthermore, SiO 2 Has the anti-reflection effect. The method can realize VO 2 Large scale preparation, and the VO obtained 2 /SiO 2 The composite material has high dispersibility.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of the product obtained in example 1;
FIG. 2 is an X-ray diffraction (XRD) pattern of the product obtained in example 2;
FIG. 3 is a Scanning Electron Microscope (SEM) image of the product obtained in example 1;
FIG. 4 is a Scanning Electron Microscope (SEM) image of the product obtained in example 2;
FIG. 5 is a Scanning Electron Microscope (SEM) image of the product obtained in comparative example 1;
FIG. 6 is a Scanning Electron Microscope (SEM) image of the product obtained in comparative example 2;
FIG. 7 is a Scanning Electron Microscope (SEM) image of the product obtained in comparative example 3;
FIG. 8 is a graph of the optical properties (UV) of the product obtained in example 1;
FIG. 9 is a graph of the optical properties (UV) of the product obtained in example 2;
FIG. 10 is a graph of the optical properties (UV) of the product obtained in comparative example 1;
FIG. 11 is a graph of the optical properties (UV) of the product obtained in comparative example 2;
FIG. 12 is a graph of the optical properties (UV) of the product obtained in comparative example 3.
Detailed Description
The following description of the embodiments of the present invention is provided by way of specific examples, and other advantages and effects of the present invention will be readily apparent to those skilled in the art from the disclosure herein. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
It is to be noted that the features in the following embodiments and examples may be combined with each other without conflict. It is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention. Test methods in which specific conditions are not noted in the following examples are generally performed under conventional conditions or conditions recommended by each manufacturer.
When numerical ranges are given in the examples, it is understood that both endpoints of each of the numerical ranges and any value therebetween can be selected unless the invention otherwise indicated. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs and the description of the present invention, and any methods, apparatuses, and materials similar or equivalent to those described in the examples of the present invention may be used to practice the present invention.
Example 1
Mechanochemical method for preparing high-dispersity VO 2 /SiO 2 A method of compounding a material comprising the steps of:
(1) mixing vanadium pentoxide (2.89g), glucose (0.286g) and silicon dioxide (0.0478g) to obtain a mixed ingredient;
(2) grinding: adding the mixed ingredients into a ball milling device, adding 63.6g of zirconia grinding balls, and carrying out ball milling for 5 hours at the rotating speed of 350 r/min;
(3) taking materials: taking out the precursor in the ball milling tank by using a key;
(4) annealing: putting the precursor into an annealing furnace, annealing for 2h at 450 ℃ in a vacuum environment;
(5) wet grinding: adding 0.1g of the sample into a ball milling tank, adding 5ml of ethanol, adding 15g of zirconia grinding balls with the diameter of 1mm, and grinding for 2 hours;
(6) ultrasonic: taking out the mixed liquid, and carrying out ultrasonic treatment for 2 hours;
(7) centrifuging: placing the solution in a centrifuge at 10000r/min for 10 min;
(8) and (3) drying: and (3) putting the sample in a vacuum drying oven, drying at 40 ℃ for 8h, and grinding by means of a mortar to obtain the final powder.
The powder obtained was subjected to X-ray diffraction (XRD) measurement, and the results are shown in FIG. 1, in which all diffraction peaks were able to combine with monoclinic phase VO 2 The standard card corresponds to the obtained powder, and the obtained powder is VO 2 。
Example 2
Mechanochemical method for preparing high-dispersity VO 2 /SiO 2 A method of compounding a material comprising the steps of:
(1) mixing vanadium pentoxide (2.92g), maltose (0.263g) and silicon dioxide (0.0482g) to obtain a mixed ingredient;
(2) grinding: adding the mixed ingredients into a ball milling device, adding 63.6g of zirconia grinding balls, and carrying out ball milling for 5 hours at the rotating speed of 350 r/min;
(3) taking materials: taking out the precursor in the ball milling tank by using a key;
(4) annealing: putting the precursor into an annealing furnace, annealing for 2h at 450 ℃ in a vacuum environment;
(5) wet grinding: adding 0.1g of the sample into a ball milling tank, adding 5ml of ethanol, adding 15g of zirconia grinding balls with the diameter of 1mm, and grinding for 2 hours;
(6) ultrasonic: taking out the mixed liquid, and carrying out ultrasonic treatment for 2 hours;
(7) centrifuging: placing the solution in a centrifuge at 10000r/min for 10 min;
(8) and (3) drying: and (3) putting the sample in a vacuum drying oven, drying at 40 ℃ for 8h, and grinding by means of a mortar to obtain the final powder.
XRD test of the obtained powder shows that all diffraction peaks can be associated with monoclinic phase VO as shown in figure 2 2 The standard card corresponds to the obtained powder, and the obtained powder is VO 2 。
Example 3
Mechanochemical method for preparing high-dispersity VO 2 /SiO 2 A method of compounding a material comprising the steps of:
(1) mixing vanadium pentoxide (2.89g), fructose (0.286g) and silicon dioxide (0.0478g) to obtain a mixed ingredient;
(2) grinding: adding the mixed ingredients into a ball milling device, adding 63.6g of zirconia grinding balls, and carrying out ball milling for 5 hours at the rotating speed of 350 r/min;
(3) taking materials: taking out the precursor in the ball milling tank by using a key;
(4) annealing: putting the precursor into an annealing furnace, annealing for 2h at 450 ℃ in a vacuum environment;
(5) wet grinding: adding 0.1g of the sample into a ball milling tank, adding 5ml of ethanol, adding 15g of zirconia grinding balls with the diameter of 1mm, and grinding for 2 hours;
(6) ultrasonic: taking out the mixed liquid, and carrying out ultrasonic treatment for 2 hours;
(7) centrifuging: placing the solution in a centrifuge at 10000r/min for 10 min;
(8) and (3) drying: and (3) putting the sample in a vacuum drying oven, drying at 40 ℃ for 8h, and grinding by means of a mortar to obtain the final powder.
Obtaining VO through XRD test 2 And (3) powder.
Example 4
Mechanochemical method for preparing high-dispersity VO 2 /SiO 2 A method of compounding a material comprising the steps of:
(1) mixing vanadium pentoxide (2.93g), sucrose (0.251g) and silicon dioxide (0.0484g) to obtain a mixed ingredient;
(2) grinding: adding the mixed ingredients into a ball milling device, adding 63.6g of zirconia grinding balls, and carrying out ball milling for 5 hours at the rotating speed of 350 r/min;
(3) taking materials: taking out the precursor in the ball milling tank by using a key;
(4) annealing: putting the precursor into an annealing furnace, annealing for 2h at 450 ℃ in a vacuum environment;
(5) wet grinding: adding 0.1g of the sample into a ball milling tank, adding 5ml of ethanol, adding 15g of zirconia grinding balls with the diameter of 1mm, and grinding for 2 hours;
(6) ultrasonic: taking out the mixed liquid, and carrying out ultrasonic treatment for 2 hours;
(7) centrifuging: placing the solution in a centrifuge at 10000r/min for 10 min;
(8) and (3) drying: and (3) putting the sample in a vacuum drying oven, drying at 40 ℃ for 8h, and grinding by means of a mortar to obtain the final powder.
Obtaining VO through XRD test 2 And (3) powder.
Example 5
Mechanochemical method for preparing high-dispersity VO 2 /SiO 2 A method of compounding a material comprising the steps of:
(1) mixing vanadium pentoxide (2.93g), starch (0.250g) and silicon dioxide (0.0484g) to obtain a mixed ingredient;
(2) grinding: adding the mixed ingredients into a ball milling device, adding 63.6g of zirconia grinding balls, and carrying out ball milling for 5 hours at the rotating speed of 350 r/min;
(3) taking materials: taking out the precursor in the ball milling tank by using a key;
(4) annealing: putting the precursor into an annealing furnace, annealing for 2h at 450 ℃ in a vacuum environment;
(5) wet grinding: adding 0.1g of the sample into a ball milling tank, adding 5ml of ethanol, adding 15g of zirconia grinding balls with the diameter of 1mm, and grinding for 2 hours;
(6) ultrasonic: taking out the mixed liquid, and carrying out ultrasonic treatment for 2 hours;
(7) centrifuging: placing the solution in a centrifuge at 10000r/min for 10 min;
(8) and (3) drying: and (3) putting the sample in a vacuum drying oven, drying at 40 ℃ for 8h, and grinding by means of a mortar to obtain the final powder.
Obtaining VO through XRD test 2 And (3) powder.
Comparative example 1
Mechanochemical method for preparing high-dispersity VO 2 /SiO 2 A method of compounding a material comprising the steps of:
(1) mixing vanadium pentoxide (2.89g) and glucose (0.286g) to obtain a mixed ingredient;
(2) grinding: adding the mixed ingredients into a ball milling device, adding 63.6g of zirconia grinding balls, and carrying out ball milling for 5 hours at the rotating speed of 350 r/min;
(3) taking materials: taking out the precursor in the ball milling tank by using a key;
(4) annealing: putting the precursor into an annealing furnace, annealing for 2h at 450 ℃ in a vacuum environment;
(5) wet grinding:0.1g of the sample is added into a ball milling pot, and 3.6mg of SiO is added 2 Adding 5ml of ethanol, adding 15g of zirconia grinding balls with the diameter of 1mm, and grinding for 2 hours;
(6) ultrasonic: taking out the mixed liquid, and carrying out ultrasonic treatment for 2 hours;
(7) centrifuging: placing the solution in a centrifuge at 10000r/min for 10 min;
(8) and (3) drying: and (3) putting the sample in a vacuum drying oven, drying at 40 ℃ for 8h, and grinding by means of a mortar to obtain the final powder.
Comparative example 2
(1) Mixing vanadium pentoxide (2.89g) and glucose (0.286g) to obtain a mixed ingredient;
(2) grinding: adding the mixed ingredients into a ball milling device, adding 63.6g of zirconia grinding balls, and carrying out ball milling for 5 hours at the rotating speed of 350 r/min;
(3) taking materials: taking out the precursor in the ball milling tank by using a key;
(4) annealing: putting the precursor into an annealing furnace, annealing for 2h at 450 ℃ in a vacuum environment;
(5) wet grinding: adding 0.1g of the sample into a ball milling tank, adding 5ml of ethanol, adding 15g of zirconia grinding balls with the diameter of 1mm, and grinding for 2 hours;
(6) ultrasonic: taking out the mixed liquid, and carrying out ultrasonic treatment for 2 hours;
(7) centrifuging: placing the solution in a centrifuge at 10000r/min for 10 min;
(8) and (3) drying: and (3) putting the sample in a vacuum drying oven, drying at 40 ℃ for 8h, and grinding by means of a mortar to obtain the final powder.
Comparative example 3
(1) Mixing vanadium pentoxide (2.89g) and glucose (0.286g) to obtain a mixed ingredient;
(2) grinding: adding the mixed ingredients into a ball milling device, adding 63.6g of zirconia grinding balls, and carrying out ball milling for 5 hours at the rotating speed of 350 r/min;
(3) taking materials: taking out the precursor in the ball milling tank by using a key;
(4) annealing: putting the precursor into an annealing furnace, annealing for 2h at 450 ℃ in a vacuum environment;
(5) ultrasonic: taking out 0.1g of the sample, adding 10ml of ethanol, and carrying out ultrasonic treatment for 2 hours;
(7) centrifuging: placing the solution in a centrifuge at 10000r/min for 10 min;
(8) and (3) drying: and (3) putting the sample in a vacuum drying oven, drying at 40 ℃ for 8h, and grinding by means of a mortar to obtain the final powder.
Comparative example 4
(1) Mixing vanadium pentoxide (2.89g), glucose (0.286g) and silicon dioxide (0.0478g) to obtain a mixed ingredient;
(2) grinding: adding the mixed ingredients into a ball milling device, adding 63.6g of zirconia grinding balls, and carrying out ball milling for 5 hours at the rotating speed of 350 r/min;
(3) taking materials: taking out the precursor in the ball milling tank by using a key;
(4) annealing: putting the precursor into an annealing furnace, annealing for 2h at 450 ℃ in a vacuum environment;
(5) wet grinding: adding 0.1g of the sample into a ball milling tank, adding 5ml of ethanol, adding 15g of zirconia grinding balls with the diameter of 1mm, and grinding for 3 hours;
(6) ultrasonic: taking out the mixed liquid, and carrying out ultrasonic treatment for 2 hours;
(7) centrifuging: placing the solution in a centrifuge at 10000r/min for 10 min;
(8) and (3) drying: and (3) putting the sample in a vacuum drying oven, drying at 40 ℃ for 8h, and grinding by means of a mortar to obtain the final powder.
Morphology and Performance characterization
1. The samples obtained in example 1, example 2, comparative example 1, comparative example 2 and comparative example 3 were subjected to SEM characterization, and the results were shown in fig. 3, fig. 4, fig. 5, fig. 6 and fig. 7, respectively, from which it can be seen that the samples obtained in example 1, example 2, comparative example 1, comparative example 2 and comparative example 3 had average particle diameters of 34.0nm, 39.7nm, 36.9nm, 40.5nm and 50.1nm, respectively. Further analysis, it can be seen that: 1) SiO 2 2 The product dispersibility can be effectively improved, and the average particle size can be reduced; 2) compared with SiO 2 Directly react with VO 2 Wet milling of nanoparticles, SiO in the initial stage 2 Mixing with raw materials, ball milling to obtain SiO 2 Participate in the whole ball milling, annealing andthe obtained nano particles have better dispersibility and smaller particle size in the wet grinding process, which indicates that SiO is 2 The adding step has great influence on the dispersibility of the nano particles; 3) compared with the product of the comparative example 2, the product of the comparative example 3 has serious agglomeration phenomenon, which shows that the wet grinding can effectively open the agglomeration of the sample and improve the product dispersibility.
2. The solar transmittance of the samples obtained in example 1, example 2, comparative example 1, comparative example 2 and comparative example 3 was characterized by an ultraviolet-visible near-infrared spectrophotometer, and the results are shown in fig. 8, fig. 9, fig. 10, fig. 11 and fig. 12, respectively. The optical properties of the samples obtained in example 1 were T as calculated by the formula I lum ＝56.82％，ΔT sol 13.88%, the optical properties of the sample obtained in example 2 were T lum ＝58.04％，ΔT sol 11.05%, the optical properties of the sample obtained in comparative example 1 were T lum ＝64.84％，ΔT sol 9.96%, the optical properties of the sample of comparative example 2 are T lum ＝59.40％，ΔT sol 9.26%, the optical properties of the sample of comparative example 3 were T lum ＝59.03％，ΔT sol -0.87%. It can thus be found that: comparing example 1 with comparative example 1, it can be seen that SiO 2 The VO can be improved by participating in the whole ball milling, annealing and wet milling process 2 Optical properties; by comparing comparative example 1 with comparative example 2, SiO can be found 2 Can improve VO 2 Optical properties of (a); comparing comparative example 2 with comparative example 3, it can be seen that wet milling can increase VO 2 The optical properties of (1).
VO 2 The calculation formula of the optical performance of the thermotropic phase change film is shown as formula one:
the formula I is as follows:
wherein λ is the wavelength, T (λ) is the transmittance of the wavelength λ,
is the visual sensitivity of the human eye and is,
the spectrum of the solar radiation with the atmospheric mass number of 1.5.
In conclusion, VO with excellent optical performance can be obtained by the preparation method 2 /SiO 2 A composite material. SiO 2 2 The compounding, the adding step and the wet grinding of the mixture can effectively reduce the particle size of the product, improve the dispersibility of the product and further improve the VO 2 The optical properties of (1).
The foregoing embodiments are merely illustrative of the principles of the present invention and its efficacy, and are not to be construed as limiting the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. VO (volatile organic compound) 2 /SiO 2 The preparation method of the composite material is characterized by comprising the following steps:
1) mixing a vanadium source, a reducing agent and SiO 2 Mixing to obtain mixed ingredients;
2) adding the mixed ingredients into a ball milling device, and adding grinding balls for ball milling to obtain a precursor;
3) putting the precursor obtained in the step 2) into a tube furnace for annealing to obtain VO 2 /SiO 2 A composite material crude product;
4) VO obtained by annealing in the step 3) 2 /SiO 2 Taking out the composite material crude product, adding the composite material crude product into a ball milling device, adding a solvent, and carrying out wet milling with grinding balls;
5) carrying out ultrasonic treatment, centrifugation and drying on the solution obtained after wet grinding in the step 4) to obtain VO with good dispersibility 2 /SiO 2 A composite material.
2. The method of claim 1, wherein the source of vanadium is V 2 O 5 。
3. The method according to claim 1, wherein the reducing agent is one or more selected from glucose, fructose, galactose, ribose, deoxyribose, sucrose, maltose, lactose, starch, cellulose, and glycogen.
4. The preparation method according to claim 1, wherein the molar ratio of the vanadium source to the reducing agent is (1-20): 1.
5. the method of claim 1, wherein the source of vanadium is mixed with SiO 2 In a molar ratio of 1: (0.1-5).
6. The preparation method of claim 1, wherein the mass ratio of the grinding balls to the mixed ingredients in the step 2) is (5-50): 1.
7. the preparation method according to claim 1, wherein the annealing temperature in the step 3) is 250 ℃ to 500 ℃ and the annealing time is 1h to 10 h.
8. The method according to claim 1, wherein the solvent in step 4) is ethanol.
9. The method according to claim 1, wherein the milling balls in step 4) and the VO obtained in step 3) are mixed together 2 /SiO 2 The mass ratio of the composite material crude product is (5-100): 1.
10. the process of claim 1, wherein the VO obtained is 2 /SiO 2 The average particle size of the composite material is 20-40 nm.
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