CN112174205A - Vanadyl hydroxide stabilized ethanol solution dispersion system and preparation of M-phase VO by using same2Method for preparing nano powder - Google Patents
Vanadyl hydroxide stabilized ethanol solution dispersion system and preparation of M-phase VO by using same2Method for preparing nano powder Download PDFInfo
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Abstract
The invention discloses a vanadyl hydroxide stable ethanol solution dispersion system and a method for preparing M-phase VO by using the same2A method for preparing nano-powder, belonging to nano VO2The technical field of preparation. Aiming at the defects of complex process, large particle size, poor uniformity and the like of the conventional hydrothermal method, the invention firstly obtains a vanadyl hydroxide stable ethanol solution dispersion system in an ultrasonic dispersion-low-speed centrifugation mode, which is beneficial to preparing products with smaller particle size and better uniformity, and then prepares M-phase VO by using the dispersion system through the hydrothermal method2The nano powder has the advantages of good uniformity, high purity, high crystallinity and the like.
Description
Technical Field
The invention belongs to a nanometer VO2Preparation technical fieldIn particular to a vanadyl hydroxide stabilized ethanol solution dispersion system, and then the M-phase VO is prepared by using the system and adopting a hydrothermal method2A method for preparing nano powder.
Background
M-phase VO2The phase-change material has phase-change characteristics at about 68 ℃, the M phase in a monoclinic structure is changed into the R phase in a tetragonal rutile structure, the transmittance, the reflectivity, the resistivity, the magnetic susceptibility and the like of the material are all changed suddenly along with the phase change, and the process is reversible along with the increase and the decrease of the temperature. Thus, VO2The method is widely applied to the fields of intelligent windows, photoelectric switches, thermistors and the like. When the vanadium dioxide powder is used as an intelligent window, the form of the film is taken as the main mode, the preparation of the film is divided into two main types according to the technical route, the first type is direct film formation, the second type is preparation of vanadium dioxide powder into slurry, and the slurry is prepared into the film through coating, printing and other modes. The direct film-forming method has high requirements on equipment, and the film-forming process is often limited by the substrate material and size, in contrast, VO (volatile organic compounds)2The powder and the inorganic or organic transparent dispersing matrix are uniformly mixed to prepare coating slurry, and the coating slurry can be flexibly applied to various substrates in the modes of spraying, spin coating, printing and the like to form a composite film technology, so that the method is the most effective method for preparing large-area high-performance coatings. But the preparation of the slurry has higher requirements on the granularity and the uniformity of the powder, and the hydrothermal synthesis method has the greatest advantage of better uniformity of the particles, can realize the control on the crystal form and the morphology of the powder by changing process parameters and is used for preparing M-phase VO2The method is commonly used.
Synthesis of M-phase VO by existing hydrothermal method2The method mostly uses a pentavalent vanadium source as a raw material, adds a reducing agent, and prepares VO by a hydrothermal reduction method2Preparation of VO by such a method2The method has the advantages of complex process, high requirements on the purity and quality of the reducing agent and the problem of over reduction to generate vanadium trioxide.
CN104071843A discloses a preparation method of monodisperse M-phase vanadium dioxide nanoparticles, wherein vanadium pentoxide, oxalic acid and water are mixed according to a molar ratio of 1-2.5: 1: 500-800, adding a surfactant according to 4-6% of the volume of the mixed solution to obtain a precursor solution, then placing the precursor solution in a closed reactor, reacting at the temperature of 200-260 ℃ for at least 1h, performing solid-liquid separation to obtain orthogonal vanadium dioxide powder, then placing the powder in a nitrogen atmosphere, and annealing at the temperature of 300-600 ℃ for 0.5h to obtain the monodisperse M-phase vanadium dioxide nanoparticles with the particle size of 60-80 nm. The preparation method has obvious defects that the M phase cannot be prepared in one step, and the target product can be obtained only by heat treatment, so that the energy consumption and the process steps are increased, and the preparation cost is greatly increased.
Another research focus is to prepare M-phase product by one-step hydrothermal method from tetravalent vanadium source such as vanadyl sulfate, vanadyl oxalate, vanadyl dichloroxide, vanadyl acetylacetonate, etc. CN 102757094A discloses a preparation method of a stable phase A vanadium dioxide nanorod, which is characterized in that the pH value of a tetravalent vanadium ion aqueous solution is controlled within the range of 1-3, the tetravalent vanadium ion aqueous solution is directly added into a hydrothermal reaction kettle, the hydrothermal reaction kettle reacts for 0-720 h at the temperature of 180-220 ℃, the filling ratio of the reaction kettle is 50-90%, and the stable phase A vanadium dioxide nanorod is obtained after centrifugation, washing and drying. The method does not obtain M-phase VO with phase change function2The particle size of the product is relatively large and the uniformity is poor.
Disclosure of Invention
Aiming at the defects of complex process, large particle diameter, poor uniformity and the like of the existing hydrothermal method, the invention firstly provides a solution for stably dispersing a vanadyl hydroxide system in an ethanol solution environment, a precursor dispersion liquid with higher stability and better dispersibility is firstly obtained, and M-phase vanadium dioxide powder with high purity, high crystallinity and high uniformity is obtained through hydrothermal crystallization.
The invention firstly provides a vanadyl hydroxide stable ethanol solution dispersion system, which is prepared by the following method:
A. taking vanadyl sulfate solution, adjusting the pH of the system to 6.5-7.5 by adopting sodium hydroxide solution, filtering, washing, drying, and then grinding to obtain solid powder;
B. taking the solid powder obtained in the step A, and mixing the solid powder with the solid-liquid mass volume ratio of 1: 10-50, then carrying out ultrasonic dispersion, and after the ultrasonic dispersion, carrying out centrifugal separation on the obtained solution at the rotating speed of 3000-5000 rpm, wherein the obtained upper layer solution is the vanadyl hydroxide stable ethanol solution dispersion system.
In the step A, the concentration of the vanadyl sulfate solution is 0.1-1.0M.
Wherein, in the step A, the washing operation of the ethanol solution dispersion system stabilized by vanadyl hydroxide is as follows: washing with deionized water and absolute ethyl alcohol until no precipitate is separated out by dropwise adding a barium chloride solution into the filtrate; the drying operation comprises the following steps: drying at 60 deg.C under vacuum for 18 h.
Wherein, in the step B, the temperature of the ultrasonic dispersion is 50 ℃ and the time is 30 min.
And C, after centrifugal separation in the step B, repeating the step B on the obtained residual solid, and continuously preparing the vanadyl hydroxide stable ethanol solution dispersion system.
And C, in the vanadyl hydroxide stable ethanol solution dispersion system, centrifugally separating the obtained residual solid, and repeating the step B for 3-5 times.
The vanadyl hydroxide stabilized ethanol solution dispersion system provided by the invention is used as a precursor dispersion liquid with higher stability and better dispersibility, and is more favorable for preparing M-phase vanadium dioxide powder with excellent performance, so that the vanadyl hydroxide stabilized ethanol solution dispersion system is also used for preparing M-phase VO2The nanometer powder preparation process includes hydrothermal reaction of the ethanol solution dispersed system with stable vanadyl hydroxide solution, cooling and centrifugal separation to obtain M-phase VO2And (3) nano powder.
Wherein, the M-phase VO is prepared by using the vanadyl hydroxide to stabilize the ethanol solution dispersion system2In the method of the nano powder, the temperature of the hydrothermal reaction is 260-300 ℃ and the time is 2-24 h.
Wherein, the M-phase VO is prepared by using the vanadyl hydroxide to stabilize the ethanol solution dispersion system2In the method of nano-powder, the M-phase VO2The particle size of the nano powder is less than 100 nm.
In step B of the invention, the solid-liquid mass-volume ratio is as follows: solids by mass, liquids by volume, and both are of the same order of magnitude.
The invention has the beneficial effects that:
the invention adopts a mode of ultrasonic dispersion-low speed centrifugation to obtain a stable ethanol solution dispersion system, the dispersion system can not be settled after being placed for a long time (the dispersion system can stably exist for more than one month by verification), and the preparation of products with smaller particle size and better uniformity is facilitated; meanwhile, vanadyl sulfate is used as a raw material, so that the reduction step is reduced, the problems of excessive reduction for producing vanadium trioxide, introduction of impurities by a reducing agent, high waste liquid treatment cost and the like in the reduction process are solved, and the obtained VO2Is an M phase and has the advantages of good uniformity, high purity, high crystallinity and the like. The method has the advantages of simple process, low cost, easy popularization and suitability for large-scale production.
Drawings
FIG. 1 shows M-phase VO obtained in example 12XRD pattern of powder.
FIG. 2 shows M-phase VO obtained in example 12SEM image of powder.
Detailed Description
Specifically, the vanadyl hydroxide stabilized ethanol solution dispersion system is prepared by the following method:
A. taking vanadyl sulfate solution, adjusting the pH of the system to 6.5-7.5 by adopting sodium hydroxide solution, filtering, washing, drying, and then grinding to obtain solid powder;
B. taking the solid powder obtained in the step A, and mixing the solid powder with the solid-liquid mass volume ratio of 1: 10-50, then carrying out ultrasonic dispersion, and after the ultrasonic dispersion, carrying out centrifugal separation on the obtained solution at the rotating speed of 3000-5000 rpm, wherein the obtained upper layer solution is the vanadyl hydroxide stable ethanol solution dispersion system.
In general, when precursor powder of vanadyl hydroxide is dispersed in an ethanol solution, severe segregation is formed, that is, small particles are dispersed in the solution, and large particles are rapidly settled and precipitated at the bottom, so that the nucleation process of vanadium dioxide is affected due to local concentration difference of the precursor solution in the hydrothermal process, and crystal nuclei overgrow due to high local concentration to form crystals with poor uniformity. Therefore, the invention firstly solves the problem of precursor dispersibility, adopts an ultrasonic mode to accelerate monomer dissociation of the particle aggregate, enables monomer particles to be better dispersed in a solvent, and then obtains a precursor dispersion liquid with higher stability and better dispersibility by screening with a low-speed centrifugation method.
In the process for preparing the vanadyl sulfate stable ethanol solution dispersion system, in the step A, the concentration of the vanadyl sulfate solution is 0.1-1.0M.
In the step A, because the existence of the electrolyte can destroy the stability of a dispersion system, solid particles are agglomerated to form clusters, and therefore when vanadyl sulfate reacts with sodium hydroxide, deionized water and absolute ethyl alcohol are adopted for washing until no precipitate is separated out when a barium chloride solution is dropwise added into the filtrate, sulfate radicals are basically removed; then dried under vacuum at 60 ℃ for 18 h.
The invention firstly adopts ultrasonic dispersion, the temperature of the ultrasonic dispersion is controlled to be 50 ℃, and the time is 30 min; and then strictly controlling the centrifugal speed to be 3000-5000 rpm, and realizing selective separation of powder with different particle sizes and collection of small particle powder under the condition of low-speed centrifugation, thereby obtaining a vanadyl hydroxide stable ethanol solution dispersion system.
After the centrifugal separation in the step B, in order to avoid the waste of vanadium raw materials, repeating the step B on the obtained residual solid, and continuously preparing a vanadyl hydroxide stable ethanol solution dispersion system; through experiments, the vanadium raw material can be utilized to the maximum degree for 3-5 times, and after repeating for 3-5 times, no solid remains basically, and no value is provided for continuous recovery.
The vanadyl hydroxide stabilized ethanol solution dispersion system provided by the invention is used as a precursor dispersion liquid with higher stability and better dispersibility, and is more favorable for preparing M-phase vanadium dioxide powder with excellent performance, so that the vanadyl hydroxide stabilized ethanol solution dispersion system is also used for preparing M-phase VO2The nanometer powder preparation process includes hydrothermal reaction of the ethanol solution dispersed system with stable vanadyl hydroxide solution, cooling and centrifugal separation to obtain M-phase VO2Nano powder; wherein the temperature of the hydrothermal reaction is 260-300 ℃, and the time is 2-24 h.
In the invention, M-phase VO is prepared by using vanadyl hydroxide to stabilize ethanol solution dispersion system2The particle size of the nano powder is less than 100nm, and the nano powder is more favorable for being used as a raw material for producing the intelligent window.
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1
Weighing 3000mL of 0.1M vanadyl sulfate solution, adjusting the pH of the solution to 6.5 by using a sodium hydroxide solution, filtering and separating to obtain a solid product, repeatedly washing the solid product with deionized water and absolute ethyl alcohol for many times until no precipitate is separated out by using a barium chloride solution, then carrying out vacuum drying at 60 ℃ for 18h, cooling and grinding to obtain brown solid powder.
Taking 5g of the powder, adding 50mL of absolute ethyl alcohol, performing ultrasonic treatment at 50 ℃ for 30min, after the ultrasonic treatment is finished, centrifuging at 5000rpm and collecting a centrifugal upper layer solution for later use, repeating the step for 3 times on a solid product obtained by centrifuging, finally taking 70mL of collected supernatant, placing the supernatant in a 100mL high-temperature high-pressure reaction kettle, performing hydrothermal treatment at 260 ℃ for 24h, cooling to room temperature after the reaction is finished, and performing centrifugal separation to obtain powder.
Through detection, FIG. 1 shows the VO2The XRD pattern of the powder showed that the product was M-phase, and as can be seen from FIG. 2, the particle size of the powder was less than 100 nm.
Example 2
Weighing 3000mL of 0.5M vanadyl sulfate solution, adjusting the pH value of the solution to 7.0 by using a sodium hydroxide solution, filtering and separating to obtain a solid product, repeatedly washing the solid product with deionized water and absolute ethyl alcohol for many times until no precipitate is separated out by using a barium chloride solution, then carrying out vacuum drying at 60 ℃ for 18h, cooling and grinding to obtain brown solid powder.
Adding 150mL of absolute ethyl alcohol into 5g of the powder, performing ultrasonic treatment at 50 ℃ for 30min, centrifuging at 4000rpm after the ultrasonic treatment is finished, collecting a centrifugal upper layer solution for later use, repeating the step for 4 times on a solid product obtained by centrifuging, finally taking 60mL of collected supernatant, placing the supernatant in a 100mL high-temperature high-pressure reaction kettle, performing hydrothermal treatment at 280 ℃ for 16h, cooling to room temperature after the reaction is finished, and performing centrifugal separation to obtain VO2And (4) obtaining a target product.
Example 3
Weighing 3000mL of vanadyl sulfate solution with the concentration of 1.0M, adjusting the pH of the solution to 7.5 by using sodium hydroxide solution, filtering and separating to obtain a solid product, repeatedly washing the solid product by using deionized water and absolute ethyl alcohol for many times until no precipitate is separated out by using barium chloride solution, then carrying out vacuum drying at 60 ℃ for 18h, cooling and grinding to obtain brown solid powder.
Adding 250mL of absolute ethyl alcohol into 5g of the powder, performing ultrasonic treatment at 50 ℃ for 30min, centrifuging at 3000rpm after the ultrasonic treatment is finished, collecting a centrifugal upper layer solution for later use, repeating the steps for 5 times on a solid product obtained by centrifuging, finally taking 80mL of collected supernatant, placing the supernatant in a 100mL high-temperature high-pressure reaction kettle, performing hydrothermal treatment at 300 ℃ for 4h, cooling to room temperature after the reaction is finished, and performing centrifugal separation to obtain VO2And (4) obtaining a target product.
Claims (9)
1. The vanadyl hydroxide stabilized ethanol solution dispersion system is characterized in that: the preparation method comprises the following steps:
A. taking vanadyl sulfate solution, adjusting the pH of the system to 6.5-7.5 by adopting sodium hydroxide solution, filtering, washing, drying, and then grinding to obtain solid powder;
B. taking the solid powder obtained in the step A, and mixing the solid powder with the solid-liquid mass volume ratio of 1: 10-50, then carrying out ultrasonic dispersion, and after the ultrasonic dispersion, carrying out centrifugal separation on the obtained solution at the rotating speed of 3000-5000 rpm, wherein the obtained upper layer solution is the vanadyl hydroxide stable ethanol solution dispersion system.
2. The vanadyl hydroxide stabilized ethanol solution dispersion according to claim 1, wherein: in the step A, the concentration of the vanadyl sulfate solution is 0.1-1.0M.
3. The vanadyl hydroxide stabilized ethanol solution dispersion according to claim 1, wherein: in the step A, the washing operation comprises the following steps: washing with deionized water and absolute ethyl alcohol until no precipitate is separated out by dropwise adding a barium chloride solution into the filtrate; the drying operation comprises the following steps: drying at 60 deg.C under vacuum for 18 h.
4. The vanadyl hydroxide stabilized ethanol solution dispersion according to claim 1, wherein: in the step B, the temperature of the ultrasonic dispersion is 50 ℃, and the time is 30 min.
5. The vanadyl hydroxide stabilized ethanol solution dispersion according to any one of claims 1 to 4, wherein: and C, after centrifugal separation in the step B, repeating the step B on the obtained residual solid, and continuously preparing the vanadyl hydroxide stable ethanol solution dispersion system.
6. The vanadyl hydroxide stabilized ethanol solution dispersion according to claim 5, wherein: and repeating the step B for 3-5 times.
7. Preparation of M-phase VO by using vanadyl hydroxide to stabilize ethanol solution dispersion system2The method for preparing the nano powder is characterized by comprising the following steps: carrying out hydrothermal reaction on the vanadyl hydroxide stabilized ethanol solution dispersion system of any one of claims 1 to 6, and after the reaction is finished, cooling and centrifugally separating to obtain M-phase VO2And (3) nano powder.
8. Preparation of M-phase VO using vanadyl hydroxide stabilized ethanol solution dispersion according to claim 72The method for preparing the nano powder is characterized by comprising the following steps: the temperature of the hydrothermal reaction is 260-300 ℃, and the time is 2-24 h.
9. Use of hydrogen according to claim 7 or 8Preparation of M-phase VO by using vanadyl oxide stabilized ethanol solution dispersion system2The method for preparing the nano powder is characterized by comprising the following steps: the M-phase VO2The particle size of the nano powder is less than 100 nm.
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| CN116102063A (en) * | 2022-12-06 | 2023-05-12 | 成都先进金属材料产业技术研究院股份有限公司 | M-phase vanadium dioxide and preparation method thereof |
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