CN110342574B - Preparation method of monoclinic-phase vanadium dioxide nano powder - Google Patents
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Abstract
The invention provides a preparation method of monoclinic phase vanadium dioxide nano powder, belonging to the preparation of VO by using a ball milling method2The field of powder. The method comprises the following steps: (1) preparing vanadium dioxide powder by a hydrothermal method; (2) mixing and stirring the vanadium dioxide powder prepared in the step (1) and a grinding aid; (3) adding the mixed ingredients obtained in the step (2) into a grinding device, adding grinding balls, and grinding; (4) and (4) cleaning and drying the ground material obtained in the step (3) to obtain the monoclinic phase vanadium dioxide. The ball milling method provided by the invention is used for preparing monoclinic phase VO2By forcing VO by mechanical force2The mixed phase is changed, and the grain diameter of the material is continuously reduced due to the grinding effect in the continuous ball milling process. The preparation method of the invention does not need heating, thus saving energy consumption; the phase transformation can be generated in a short time, the time is short, and the production efficiency is high.
Description
Technical Field
The invention belongs to a ball milling method for preparing VO2The field of powder, in particular to a preparation method of monoclinic phase vanadium dioxide nano powder.
Background
In recent years, in order to reduce the energy consumption of indoor air conditioners of modern buildings, "smart windows" have attracted much attention. The intelligent window can intelligently regulate and control the light transmittance and the heat transmittance through light, heat, electricity and other stimulus responses, and can be divided into a photochromic intelligent window, a thermochromic intelligent window and an electrochromic intelligent window.
Monoclinic phase vanadium dioxide VO2(M) has excellent thermochromic properties, and reflects near-infrared light when the ambient temperature is higher than the phase transition temperature and is in a metal state; below the phase transition temperature, is an insulating state, allowing light to pass freely. Regulating the sun due to monoclinic phase vanadium dioxideLight capability, therefore, currently monoclinic phase vanadium dioxide is one of the most ideal thermochromic smart window materials.
Vanadium (V) is a transition metal element and has active chemical property, and the V element shows +2 to +5 valences and various mixed valences thereof according to the chemical environment. And VO2The V element in the (1) is +4 valence, so the (4) is easy to be oxidized in the preparation process to obtain VO with +4/+5 mixed valence2/V2O5And (3) mixing the products. In addition, VO2There are also a number of isomeric forms, such as VO2(A)、VO2(B)、VO2(D)、VO2(P)、VO2(M), and the like. Thus, preparation of pure phase VO2(M), process conditions in the preparation process need to be precisely controlled.
At present, the method for preparing monoclinic phase vanadium dioxide is mainly a hydrothermal method, and the prepared particles have high purity, good crystallinity and large dispersibility. But the technological parameters are too many, the prepared product is often accompanied with other impurity phases and agglomeration, and the nanoscale VO is not easy to be directly obtained2(M) a powder. VO currently being made by phase transformation2Vanadium dioxide VO with mixed phase changed into monoclinic phase2(M) is mainly realized by high-temperature annealing under vacuum or inert atmosphere, but the method requires high-temperature heating and has large energy consumption, which undoubtedly increases the production cost, and on the other hand, the product is easy to agglomerate after high-temperature annealing, which also affects the product performance, such as: the article (Inorg. chem. front.,2016,3, 1035-2(D) Obtaining VO with particle size of more than 500nm and serious agglomeration after 3 hours of powder2(M) a powder.
Disclosure of Invention
The invention aims to provide a preparation method of monoclinic-phase vanadium dioxide nano powder, which overcomes the defects of the existing hydrothermal method and the preparation of VO by high-temperature phase transformation2(M) disadvantages and inadequacies of the powder technology.
In order to achieve the above object or other objects, the present invention is achieved by the following aspects.
A preparation method of monoclinic phase vanadium dioxide nano powder comprises the following steps:
(1) preparing vanadium dioxide powder by a hydrothermal method;
(2) mixing and stirring the vanadium dioxide powder prepared in the step (1) and a grinding aid;
(3) adding the mixed ingredients obtained in the step (2) into a grinding device, adding grinding balls, and grinding;
(4) and (4) cleaning and drying the ground material obtained in the step (3) to obtain the monoclinic phase vanadium dioxide.
Further, the vanadium dioxide powder in the step (1) is non-monoclinic phase vanadium dioxide. Preferably, the vanadium dioxide powder is selected from VO2(A)、VO2(B)、VO2(D)、VO2One or more of (P).
Among them, the hydrothermal method is a method conventional in the art.
Further, the mass ratio of the vanadium dioxide powder to the grinding aid is 1: (0-10).
Further, the mass ratio of the ingredients to the grinding balls in the step (3) is 1: (1-50).
Further, the grinding aid is selected from one or more of methanol, isoamyl alcohol, glycerol, acetone, aryl sulfonic acid, dodecylamine, tridecylamine, tetradecylamine, organosilicon, oleic acid, butyric acid, sodium stearate, sodium oleate, capric acid, lanolin, naphthenic acid, sodium naphthenate, sodium cyclamate, n-hexane, amyl acetate, sodium silicate, sodium hydroxide, sodium chloride, sodium carbonate, lithium hydroxide, lithium chloride, lithium carbonate, potassium hydroxide, potassium chloride, potassium carbonate, sodium hexametaphosphate, sodium tripolyphosphate, triethanolamine, polycarboxylate, sodium pyrophosphate and sodium citrate.
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 the group consisting of alumina milling balls, zirconia milling balls, agate milling balls.
Further, in the step (3), the rotating speed is 10-1800r/min, and the grinding is carried out for 5min-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, in the step (4), the ground material is centrifugally cleaned by a centrifugal machine, and the centrifugal speed is 50-1800 r/min. Drying at 30-100 deg.C for 1-5 h.
The ball milling method provided by the invention is used for preparing monoclinic phase VO2By forcing VO by mechanical force2The mixed phase is changed, and the grain diameter of the material is continuously reduced due to the grinding effect in the continuous ball milling process. The preparation method of the invention does not need heating, thus saving energy consumption; the phase transformation can be generated in a short time, the time is short, and the production efficiency is high.
Drawings
FIG. 1 shows a water-thermal synthesized VO obtained in example 12(A) X-ray diffraction (XRD) and VO of samples and final products2(A)、VO2(M) standard card comparison;
FIG. 2 shows the hydrothermal synthesis of VO obtained in example 22(D) X-ray diffraction (XRD) and VO of samples and final products2(B)、VO2(M) standard card comparison;
FIG. 3 shows a water-thermal synthesized VO obtained in example 32(D) X-ray diffraction (XRD) and VO of samples and final products2(D)、VO2(M) standard card comparison;
FIG. 4 is a Scanning Electron Microscope (SEM) of a sample obtained by hydrothermal method and a final product obtained by hydrothermal method in example 1, wherein the left side of the SEM shows VO obtained by hydrothermal method2(A) SEM picture of (1), and VO after ball milling treatment on the right picture2(M) SEM image;
FIG. 5 is a Scanning Electron Microscope (SEM) of the hydrothermal method of example 2, wherein the left side shows VO obtained by the hydrothermal method2(B) SEM picture of (1), and VO after ball milling treatment on the right picture2(M) SEM image;
FIG. 6 shows the hydrothermal synthesis of VO obtained in comparative example 12(D) X-ray diffraction (XRD) and VO of the sample2(D) Standard card comparison of (1);
FIG. 7 shows VO in comparative example 12(D) Annealing the powder to obtain powder X-ray diffraction (XRD) and VO2(M) standard card comparison;
FIG. 8 is a Scanning Electron Microscope (SEM) of a sample obtained by hydrothermal method and a final product in comparative example 1, wherein the left side is VO obtained by hydrothermal method2(D) SEM picture of (1), the right picture is VO obtained by annealing2(M) SEM image;
FIG. 9 is a Differential Scanning Calorimetry (DSC) chart of the product obtained in example 2.
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 specified in the following examples are generally carried out under conventional conditions or under conditions recommended by the respective manufacturers.
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.
The X-ray diffraction (XRD) test in the embodiment of the invention adopts the following instruments: d8 FOCUS.
Example 1
A preparation method of monoclinic phase vanadium dioxide nano powder comprises the following steps:
(1) hydrothermal preparation:
will V2O5(1.001g) into 20mL of deionized water, adding 1.5mL of concentrated sulfuric acid, stirring with a magnetic stirrer at 60-70 ℃ for 10min, and adding 0.520g N2H4·HO2The pH was adjusted to 3-4 using sodium hydroxide and transferred to a stainless steel autoclave lined with polytetrafluoroethylene. Sealing the autoclave, reacting at 230 deg.C for 24h, slowly cooling to room temperature to obtain product, centrifuging with deionized water twice, washing with ethanol once, removing residue, drying at 80 deg.C for 10h to obtain powder, performing X-ray diffraction (XRD) test, and mixing with VO2(A) Comparing with standard card, and obtaining VO powder as shown in figure 12(A) And (3) powder.
(2) Ball milling treatment:
1) 3.000g of VO obtained by multiple times of hydrothermal reaction in the step (1)2(A) Powder, mixed with oleic acid 2.324 g.
2) Adding the mixed ingredients into a ball milling tank, adding 50g of grinding balls, rotating at 1000r/min, and grinding for 4 h.
3) Transferring the ground material to a 50ml beaker, adding 30ml of ethanol, magnetically stirring for 5min, transferring to a centrifuge at a rotating speed of 3000r/min, centrifuging for 10min, and washing with ethanol for three times.
4) Placing the washing material in a constant temperature oven at 60 ℃ for baking for 10h to remove absolute ethyl alcohol, grinding by virtue of a mortar to obtain final powder, and performing X-ray diffraction (XRD) test on the powder, wherein the result is shown in figure 1, and the figure shows that other phase diffraction peaks of the powder obtained by the preparation method provided by the invention disappear and only contain VO2(M) diffraction Peak, indicating that the obtained powder is VO2(M) a powder.
Example 2
A preparation method of monoclinic phase vanadium dioxide nano powder comprises the following steps:
(1) hydrothermal preparation:
will V2O50.600g of oxalic acid and 0.790g of oxalic acid are added to 40mL of deionized water. Stirring with a magnetic stirrer for 1h to obtainThe blue transparent liquid was transferred to a teflon lined stainless steel autoclave. The autoclave was sealed and reacted at 210 ℃ for 24h, and then the autoclave was slowly cooled to room temperature. Obtaining a product, centrifugally washing the product with absolute ethyl alcohol for three times, removing residues, drying the product in vacuum at 55 ℃ for 12 hours to obtain powder, carrying out X-ray diffraction (XRD) test, and reacting the powder with VO2(B) Comparing with the standard card, as shown in FIG. 2, the obtained powder is VO2(B) And (3) powder.
(2) Ball milling treatment:
1) 1.123g of VO obtained by multiple times of hydrothermal reaction in the step (1)2(B) The powder was mixed with 1.234g of amyl acetate.
2) Adding the mixed ingredients into a ball milling tank, adding 45g of grinding balls, rotating at the speed of 200r/min, and grinding for 2 h.
3) Transferring the ground material to a 50ml beaker, adding 30ml of ethanol, magnetically stirring for 5min, transferring to a centrifuge at a rotating speed of 3000r/min, centrifuging for 10min, and washing with ethanol for three times.
4) Placing the washing material in a constant temperature oven at 60 ℃ for baking for 10h to remove absolute ethyl alcohol, grinding by virtue of a mortar to obtain final powder, and performing X-ray diffraction (XRD) test on the powder, wherein the result is shown in figure 2, and the figure shows that other phase diffraction peaks of the powder obtained by the preparation method provided by the invention disappear and only contain VO2(M) diffraction Peak, indicating that the obtained powder is VO2(M) a powder.
Example 3
A preparation method of monoclinic phase vanadium dioxide nano powder comprises the following steps:
(1) hydrothermal preparation:
will V2O5(0.8014g) is added into 20mL deionized water, stirred for 10min by a magnetic stirrer at the temperature of 60-70 ℃, and then 0.5200gN is added2H4·HO2The pH was adjusted to 7-8 using sodium hydroxide and transferred to a stainless steel autoclave lined with polytetrafluoroethylene. The autoclave was sealed and reacted at 260 ℃ for 24 hours, and then, the autoclave was slowly cooled to room temperature. Obtaining a product, centrifugally washing twice by deionized water, washing once by ethanol, removing residues, drying for 10 hours at 80 ℃ to obtain powder,performing X-ray diffraction (XRD) test and mixing with VO2(D) Comparing with the standard card, as shown in FIG. 3, the obtained powder is VO2(D) And (3) powder.
(2) Ball milling treatment:
1) 2.023g of VO obtained by multiple times of hydrothermal reaction in the step (1)2(D) Powder, mixed with 2.345g of butyric acid.
2) Adding the mixed ingredients into a ball milling tank, adding 60g of grinding balls, rotating at a speed of 1700r/min, and grinding for 1 h.
3) Transferring the ground material to a 50ml beaker, adding 30ml of ethanol, magnetically stirring for 5min, transferring to a centrifuge at a rotating speed of 3000r/min, centrifuging for 10min, and washing with ethanol for three times.
4) The washed materials are placed in a constant-temperature oven to be baked for 10 hours at 60 ℃, absolute ethyl alcohol is removed, the materials are ground by a mortar to obtain final powder, the powder is subjected to X-ray diffraction (XRD) test, the result is shown in figure 3, and the figure shows that other phase diffraction peaks of the powder obtained by the preparation method of the invention disappear and only contain VO2(M) diffraction Peak, indicating that the obtained powder is VO2(M) a powder.
Example 4
A preparation method of monoclinic phase vanadium dioxide nano powder comprises the following steps:
(1) hydrothermal preparation:
will V2O50.502g of oxalic acid and 0.691g of oxalic acid were added to 45mL of deionized water. Stirring with a magnetic stirrer for 2h to obtain a blue transparent liquid, and transferring into a polytetrafluoroethylene-lined stainless steel autoclave. The autoclave was sealed and reacted at 200 ℃ for 12 hours, and then, the autoclave was slowly cooled to room temperature. Obtaining a product, centrifugally washing the product with absolute ethyl alcohol for three times, removing residues, drying the product in vacuum at 55 ℃ for 12 hours, and obtaining VO through X-ray diffraction (XRD) test2(D)VO2(B) The mixed phase powder of (3).
(2) Ball milling treatment:
1) VO obtained by multiple times of hydrothermal in the step (1)2(D) And VO2(B) 2.023g of mixed phase powder and 3.265g of acetone were mixed.
2) Adding the mixed ingredients into a ball milling tank, adding 75g of grinding balls, rotating at 1200r/min, and grinding for 30 min.
3) Transferring the ground material to a 50ml beaker, adding 30ml of ethanol, magnetically stirring for 5min, transferring to a centrifuge at a rotating speed of 3000r/min, centrifuging for 10min, and washing with ethanol for three times.
4) Placing the washed materials in a constant-temperature oven, baking at 60 deg.C for 10h, removing anhydrous ethanol, and grinding with the help of mortar to obtain VO2(M) a powder.
Example 5
A preparation method of monoclinic phase vanadium dioxide nano powder comprises the following steps:
(1) hydrothermal preparation:
will V2O50.612g of oxalic acid and 0.621g of oxalic acid are added to 40mL of deionized water. Stirring with a magnetic stirrer for 2h to obtain a blue transparent liquid, and transferring into a polytetrafluoroethylene-lined stainless steel autoclave. The autoclave was sealed and reacted at 200 ℃ for 18h, and then the autoclave was slowly cooled to room temperature. Obtaining a product, centrifugally washing the product with absolute ethyl alcohol for three times, removing residues, drying the product in vacuum at 55 ℃ for 12 hours, and obtaining VO through X-ray diffraction (XRD) test2(D) And VO2(A) The mixed phase powder of (3).
(2) Ball milling treatment:
1) 3.356g of VO obtained by multiple times of hydrothermal reaction in the step (1)2(D) And VO2(A) The mixed phase powder of (3) was mixed with 3.214g of glycerin.
2) Adding the mixed ingredients into a ball milling tank, adding 80g of grinding balls, rotating at 500r/min, and grinding for 5 h.
3) Transferring the ground material to a 50ml beaker, adding 30ml of ethanol, magnetically stirring for 5min, transferring to a centrifuge at a rotating speed of 3000r/min, centrifuging for 10min, and washing with ethanol for three times.
4) Placing the washed materials in a constant-temperature oven, baking at 60 deg.C for 10h, removing anhydrous ethanol, and grinding with the help of mortar to obtain VO2(M) a powder.
Example 6
A preparation method of monoclinic phase vanadium dioxide nano powder comprises the following steps:
(1) hydrothermal preparation:
will V2O50.712g oxalic acid 0.522g was added to 40mL deionized water. Stirring with a magnetic stirrer for 2h to obtain a blue transparent liquid, and transferring into a polytetrafluoroethylene-lined stainless steel autoclave. The autoclave was sealed and reacted at 240 ℃ for 24h, and then the autoclave was slowly cooled to room temperature. Obtaining a product, centrifugally washing the product with absolute ethyl alcohol for three times, removing residues, drying the product in vacuum at 55 ℃ for 12 hours, and obtaining VO through X-ray diffraction (XRD) test2(D) And VO2(M) mixed phase powder.
(2) Ball milling treatment:
1) 1.568g of VO obtained by multiple times of hydrothermal reaction in the step (1)2(D) And VO2(M) mixed phase powder with 5.236g of n-hexane
And (4) mixing.
2) Adding the mixed ingredients into a ball milling tank, adding 100g of grinding balls, rotating at 100r/min, and grinding for 6 h.
3) Transferring the ground material to a 50ml beaker, adding 30ml of ethanol, magnetically stirring for 5min, transferring to a centrifuge at a rotating speed of 3000r/min, centrifuging for 10min, and washing with ethanol for three times.
4) Placing the washed materials in a constant-temperature oven, baking at 60 deg.C for 10h, removing anhydrous ethanol, and grinding with the help of mortar to obtain VO2(M) a powder.
Comparative example 1
30mmol of ammonium metavanadate and 40mmol of oxalic acid are added into 16ml of deionized water, and the mixture is stirred for 5 minutes to obtain 17ml of precursor. Then transferring the precursor solution into a 25ml stainless steel autoclave with a polytetrafluoroethylene lining, heating to 220 ℃, preserving heat for 18h, cooling the autoclave to room temperature, obtaining a product through centrifugal separation, transferring the product into a 50ml beaker, adding 30ml ethanol, magnetically stirring for 5min, transferring into a centrifuge at a rotating speed of 3000r/min, centrifuging for 10min, washing with ethanol for three times, and testing the obtained product through X-ray diffraction (XRD), wherein the result is VO (vacuum) shown in figure 62(D) Powder, then annealing at 550 ℃ for 3h under vacuum condition, testing the obtained product by X-ray diffraction (XRD), and displaying that the obtained powder is VO as shown in figure 72(M) a powder.
Performance characterization
1. FIG. 9 shows a graph of the product obtained in example 2 obtained by differential scanning calorimetry, in which the product obtained from the graph has a distinct phase transition temperature, a heating phase transition temperature and VO2(M) Standard phase transition temperature is close to 68 ℃.
2. SEM analysis is respectively carried out on the products of examples 1 and 2 and comparative example 1, and the results are respectively shown in figures 4, 5 and 8, and comparison of figures 4 and 5 shows that the product morphology of examples 1 and 2 is changed from the original hydrothermal nanoparticles into nearly circular particles with the diameter of 50nm-100nm after ball milling treatment, which shows that not only the target product can be obtained, but also the sample morphology can be changed and the particle size can be reduced after ball milling treatment. Comparing fig. 4, 5 and 8, it can be seen that the product obtained by ball milling (50nm-100nm) has a smaller particle size and improved particle dispersibility than the product obtained by comparative example 1 at a high temperature (500 nm).
In summary, the preparation method of the invention can promote VO2The mixed phase is subjected to phase transformation to obtain pure monoclinic phase VO2And the particle size of the material is continuously reduced due to the grinding effect in the continuous ball milling process. The preparation method of the invention does not need heating, thus saving energy consumption; the phase transformation can be generated in a short time, the time is short, and the production efficiency is high.
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 (2)
1. A preparation method of monoclinic phase vanadium dioxide nano powder is characterized by comprising the following steps:
(1) preparing vanadium dioxide powder by a hydrothermal method;
(2) mixing and stirring the vanadium dioxide powder prepared in the step (1) and a grinding aid;
(3) adding the mixed ingredients obtained in the step (2) into a grinding device, adding grinding balls, and grinding;
(4) cleaning and drying the ground material obtained in the step (3) to obtain monoclinic phase vanadium dioxide;
the mass ratio of the vanadium dioxide powder to the grinding aid is 1: (0-10);
in the step (3), the mass ratio of the ingredients to the grinding balls is 1: (1-50);
in the step (3), the rotating speed is 10-1800r/min, and the grinding time is 5min-24 h;
the vanadium dioxide powder in the step (1) is non-monoclinic phase vanadium dioxide selected from VO2(A)、VO2(B)、VO2(D)、VO2One or more of (P).
2. The method of claim 1, wherein the grinding aid is selected from one or more of methanol, isoamyl alcohol, glycerol, acetone, arylsulfonic acid, dodecylamine, tridecylamine, tetradecylamine, silicones, oleic acid, butyric acid, sodium stearate, sodium oleate, capric acid, lanolin, naphthenic acid, sodium naphthenate, sodium cyclamate, n-hexane, amyl acetate, sodium silicate, sodium hydroxide, sodium chloride, sodium carbonate, lithium hydroxide, lithium chloride, lithium carbonate, potassium hydroxide, potassium chloride, potassium carbonate, sodium hexametaphosphate, sodium tripolyphosphate, triethanolamine, polycarboxylate, sodium pyrophosphate, and sodium citrate.
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| CN110734088A (en) * | 2019-10-24 | 2020-01-31 | 成都先进金属材料产业技术研究院有限公司 | M-phase VO prepared by using invalid vanadium battery negative electrolyte2Method (2) |
| CN111186860A (en) * | 2020-01-06 | 2020-05-22 | 济南大学 | Preparation method for preparing monoclinic-phase vanadium dioxide nano powder from precursor obtained by thermal decomposition and ball milling |
| CN112125337A (en) * | 2020-10-16 | 2020-12-25 | 成都先进金属材料产业技术研究院有限公司 | Method for preparing nano vanadium dioxide by using pentavalent vanadium alkoxide as raw material |
| CN112209442B (en) * | 2020-10-16 | 2022-07-29 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing M-phase vanadium dioxide nano powder by salt-assisted ultrasonic pyrolysis method |
| CN112174206A (en) * | 2020-10-16 | 2021-01-05 | 成都先进金属材料产业技术研究院有限公司 | Method for directly preparing vanadium dioxide by taking vanadyl acetylacetonate as vanadium source |
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