CN112777626A - Highly uniform zinc oxide submicron spheres with controllable particle size and preparation method thereof - Google Patents
Highly uniform zinc oxide submicron spheres with controllable particle size and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a highly uniform zinc oxide submicron sphere with controllable particle size and a preparation method thereof, belonging to the field of photonic crystal material preparation. The method adopts an alcohol-water system, reduces the temperature and pressure required by the synthesis of the zinc oxide microspheres, and synthesizes the zinc oxide polycrystalline submicron spheres with good monodispersity more cleanly. In the nucleation process, the temperature, the initial rotating speed, the zinc source and the deionized water are regulated and controlled to quickly carry out the nucleation process. During the growth process, mass transfer is further controlled by introducing the viscosity of a polyol control system, and the zinc oxide submicron spheres with stable particle sizes can be obtained through one-step reaction. According to the synthesis method, the zinc oxide submicron spheres with specific target particle size can be obtained only by changing the amount of the zinc source and the type and amount of the polyhydric alcohol. The adjustable particle size range of the zinc oxide submicron spheres prepared by the method is obviously enlarged, the adjustable particle size range is 100nm-800nm, and the monodispersity of the zinc oxide submicron spheres is good.
Description
Technical Field
The invention relates to a highly uniform zinc oxide submicron sphere with controllable particle size and a preparation method thereof, belonging to the field of photonic crystal material preparation.
Background
Zinc oxide is a II-VI semiconductor material with a theoretical refractive index of 2.1, with a direct band gap of about 3.4eV and an exciton binding energy of about 60meV, which makes it thermally stable at room temperature. Zinc oxide has been widely used in the fields of photolysis of water, nano-generators, high-sensitivity sensors, photonic crystals, and the like. Researches find that the semiconductor material with the micro-nano size level shows a plurality of unique physical and chemical phenomena, such as quantum effect, nonlinear optical effect and the like. The monodisperse microspheres eliminate the influence of the shape on the properties of the material, and the controllable particle size of the microspheres can further study the influence of the size of the material on the properties. Therefore, the preparation of the monodisperse zinc oxide microspheres with accurately controllable particle sizes has important significance for further research.
In the current research of synthesizing the zinc oxide microspheres with adjustable particle sizes, most reactions need high temperature and high pressure conditions, and the method has high cost and low efficiency. For example, thermal injection methods (see W.Ji, L.Li, W.Song, X.Wang, B.ZHao, Y.Ozaki, Angew.Chem.int.Ed.,2019,58, 14452-. The particle size range regulated by the zinc oxide spheres synthesized by the currently reported method is narrow, and is usually in the range of 10nm-200 nm. The research of synthesizing zinc oxide submicron spheres by using an alcohol-water system through a one-step method and accurately adjusting the particle size of the zinc oxide submicron spheres in a large range is not reported.
Disclosure of Invention
The invention aims to provide highly uniform zinc oxide submicron spheres with controllable particle size and a preparation method thereof. A preparation method of highly uniform zinc oxide submicron spheres with controllable particle size comprises the steps of increasing the rotating speed in a nucleation period to achieve the effect of explosive nucleation, and further controlling the mass transfer process in a stable growth period by controlling the viscosity according to the ratio of polyhydric alcohol to water to obtain the zinc oxide submicron spheres with target particle size; according to the synthesis method, the test steps can be accurately designed through the preset target particle size, and the zinc oxide submicron spheres with the target particle size can be accurately obtained by controlling the addition amount of the zinc source; meanwhile, the adjustable particle size range of the method is obviously enlarged, the adjustable particle size range is 100nm-800nm, the particle size of the zinc oxide submicron spheres is highly uniform, the zinc oxide submicron spheres are of a polycrystalline structure, and the particle size distribution coefficient is less than 10%.
The preparation method of the highly uniform zinc oxide submicron spheres with controllable particle size comprises the following steps:
1) according to the concentration of 0.2-1.2mmol/L, taking polyvinylpyrrolidone, stirring and dispersing in ethanol solution at room temperature;
2) according to the concentration of 0.1-1mol/L, taking a certain amount of zinc source, ultrasonically stirring and dispersing in a polyol solution at room temperature;
3) mixing the solutions obtained in the step 1) and the step 2), heating to 60-80 ℃, and stirring for 2-4 h;
4) adding deionized water into the solution obtained in the step 3) according to the volume ratio of 1-5 of polyol to deionized water, and stirring and dispersing;
5) the stirring speed is reduced, and the reaction is carried out for 1 to 2 hours at the temperature of between 60 and 80 ℃ by oil bath stirring;
6) and washing the obtained zinc oxide submicron spheres with ethanol for multiple times, centrifuging, drying and grinding to obtain the solid zinc oxide submicron spheres.
Further, in the above technical solution, the average molecular weight of polyvinylpyrrolidone is 10000-.
Further, in the above technical scheme, the polyhydric alcohol in step 2) is one or two of ethylene glycol, diethylene glycol, and 1, 2-propylene glycol.
Further, in the above technical scheme, the stirring time in the step 4) is 2-10 min.
Further, in the above technical solution, the zinc source includes zinc acetate dihydrate.
The invention uses the mixed solvent of the polyhydric alcohol and the ethanol, and utilizes the type and the quantity of the polyhydric alcohol which can be mixed and dissolved with the ethanol to regulate and control the viscosity and the surface energy of the system, thereby further influencing the nucleation speed, the mass transfer rate and the growth speed of the zinc oxide submicron spheres and obtaining the zinc oxide submicron spheres with uniform particle size.
The invention discusses that in systems with different temperatures, due to the fact that the saturation solubility of a zinc source is different, the supersaturation degree of the system can influence the nucleation efficiency, and the result shows that the higher the temperature is, the smaller the average grain diameter is, and the grain diameter distribution is more uniform in a 75 ℃ system.
Advantageous effects of the invention
The invention discloses a highly uniform zinc oxide submicron sphere with controllable particle size. According to the synthesis method, the test steps can be accurately designed through the preset target particle size, and the zinc oxide submicron spheres with the target particle size can be accurately obtained by adopting a one-step method; meanwhile, the adjustable particle size range of the method is obviously enlarged and can be adjusted to be 100nm-800 nm. The microsphere has uniform grain size, is of a polycrystalline structure, and has a grain size distribution coefficient of less than 10%. The zinc oxide submicron sphere can be widely applied to the fields of photolysis water, nano generators, high-sensitivity sensors, photonic crystals and the like. The obtained microspheres have rough surfaces and good effect in the field of catalysis.
Drawings
FIG. 1 is an X-ray diffraction pattern of the zinc oxide microspheres prepared in example 1.
FIG. 2 is a transmission electron micrograph of zinc oxide microspheres, wherein a) are 460. + -.10 nm zinc oxide microspheres prepared in example 1, and b) are 230. + -.10 nm zinc oxide microspheres prepared in example 24.
FIG. 3 is a scanning electron micrograph of zinc oxide microspheres, wherein a) are the 150. + -.10 nm zinc oxide microspheres prepared in example 2, b) are the 200. + -.10 nm zinc oxide microspheres prepared in example 28, c) are the 230. + -.10 nm zinc oxide microspheres prepared in example 27, d) are the 250. + -.10 nm zinc oxide microspheres prepared in example 19, e) are the 290. + -.10 nm zinc oxide microspheres prepared in example 26, f) are the 320. + -.10 nm zinc oxide microspheres prepared in example 3, g) are the 370. + -.10 nm zinc oxide microspheres prepared in example 16, h) are the 400. + -.10 nm zinc oxide microspheres prepared in example 14, i) are the 460. + -.10 nm zinc oxide microspheres prepared in example 1, j) are the 530. + -.10 nm zinc oxide microspheres prepared in example 25, k) are the 680. + -.10 nm microspheres prepared in example 24, l) are the 750. + -.10 nm zinc oxide microspheres prepared in example 4.
Fig. 4 is a particle size distribution diagram of the zinc oxide microspheres prepared in example 3.
FIG. 5 is a scanning electron micrograph of the zinc oxide microspheres prepared in example 3.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
The test methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials, unless otherwise specified, are commercially available or may be prepared by conventional methods.
Example 1
Through a multistep growth method for accurately regulating and controlling the particle size, the monodisperse zinc oxide submicron spheres with the particle size of 460 +/-10 nm are prepared. The preparation method comprises the following steps:
1) weighing 6.00g of polyvinylpyrrolidone with the average molecular weight of 40000, weighing 450ml of ethanol, and stirring and dispersing the polyvinylpyrrolidone in the ethanol solution at room temperature;
2) weighing 1.08g of zinc acetate dihydrate, measuring 50ml of ethylene glycol, and ultrasonically stirring and dispersing the zinc acetate dihydrate in an ethylene glycol solution at room temperature;
3) mixing the solutions obtained in the steps 1) and 2), heating to 75 ℃, and stirring for 2-4 h;
4) measuring 15ml of deionized water, adding the deionized water into the solution obtained in the step 3), and quickly stirring for 2 min;
5) stirring in an oil bath at 75 ℃ for reaction for 1.5 h;
6) and washing the obtained zinc oxide submicron spheres with ethanol for multiple times, centrifuging, drying and grinding to obtain the solid zinc oxide submicron spheres.
The transmission electron microscope image of the obtained zinc oxide submicron sphere is shown in figure 2a), and the prepared microsphere has good spherical morphology and uniform particle size, wherein the particle size is 460 +/-10 nm.
XRD test is carried out on the monodisperse 460 +/-10 nm zinc oxide microspheres, and the crystal structure of the microspheres is analyzed, as shown in figure 1, the diffraction peak position and the relative intensity of the obtained product are consistent with the standard wurtzite zinc oxide spectrum, and the standard card is JCPDS NO. 36-1451. In addition, other impurity peaks do not exist in the figure, and the fact that the product has high crystalline phase purity is proved.
The above results indicate that the prepared zinc oxide microspheres are polycrystalline structures, uniform inside and have no layered structure.
Example 2
Through a multistep growth method for accurately regulating and controlling the particle size, the monodisperse zinc oxide submicron spheres with the particle size of 150 +/-10 nm are prepared. The preparation method comprises the following steps:
1) weighing 6.00g of polyvinylpyrrolidone with the average molecular weight of 40000, weighing 450ml of ethanol, and stirring and dispersing the polyvinylpyrrolidone in the ethanol solution at room temperature;
2) weighing 0.54g of zinc acetate dihydrate, measuring 50ml of ethylene glycol, and ultrasonically stirring and dispersing the zinc acetate dihydrate in an ethylene glycol solution at room temperature;
3) mixing the solutions obtained in the steps 1) and 2), heating to 75 ℃, and stirring for 2-4 h;
4) measuring 15ml of deionized water, adding the deionized water into the solution obtained in the step 3), and quickly stirring for 2 min;
5) stirring in oil bath at 75 ℃ for reaction for 1.5 h;
6) and washing the obtained zinc oxide submicron spheres with ethanol for multiple times, centrifuging, drying and grinding to obtain the solid zinc oxide submicron spheres.
According to the characterization of a scanning electron microscope and the statistics of particle size distribution, the microsphere has good spherical morphology and uniform particle size, the particle size is 150 +/-10 nm, the particle size distribution is calculated to be less than 10%, and the particle size distribution is narrow.
Example 3
Through a multistep growth method for accurately regulating and controlling the particle size, the monodisperse zinc oxide submicron spheres with the particle size of 320 +/-10 nm are prepared. The preparation method comprises the following steps:
1) weighing 6.00g of polyvinylpyrrolidone with the average molecular weight of 40000, weighing 450ml of ethanol, and stirring and dispersing the polyvinylpyrrolidone in the ethanol solution at room temperature;
2) weighing 0.81g of zinc acetate dihydrate, weighing 50ml of ethylene glycol, and ultrasonically stirring and dispersing the zinc acetate dihydrate in an ethylene glycol solution at room temperature;
3) mixing the solutions obtained in the steps 1) and 2), heating to 75 ℃, and stirring for 2-4 h;
4) measuring 15ml of deionized water, adding the deionized water into the solution obtained in the step 3), and quickly stirring for 2 min;
5) stirring in oil bath at 75 ℃ for reaction for 1.5 h;
6) and washing the obtained zinc oxide submicron spheres with ethanol for multiple times, centrifuging, drying and grinding to obtain the solid zinc oxide submicron spheres.
Fig. 4 is a particle size distribution diagram of the zinc oxide microspheres prepared in this example, and the particle size distribution coefficient is calculated to be less than 10%, and the particle size distribution is narrow.
Fig. 3f) and fig. 5 are scanning electron micrographs of the zinc oxide microspheres prepared in this example with different magnifications, and the prepared microspheres have good spherical morphology and uniform particle size, with the particle size of 320 ± 10 nm.
Example 4
Through a multistep growth method for accurately regulating and controlling the particle size, the monodisperse zinc oxide submicron spheres with the particle size of 750 +/-10 nm are prepared. The preparation method comprises the following steps:
1) weighing 6.00g of polyvinylpyrrolidone with the average molecular weight of 40000, weighing 450ml of ethanol, and stirring and dispersing the polyvinylpyrrolidone in the ethanol solution at room temperature;
2) weighing 2.16g of zinc acetate dihydrate, measuring 50ml of ethylene glycol, and ultrasonically stirring and dispersing the zinc acetate dihydrate in an ethylene glycol solution at room temperature;
3) mixing the solutions obtained in the steps 1) and 2), heating to 75 ℃, and stirring for 2-4 h;
4) measuring 15ml of deionized water, adding the deionized water into the solution obtained in the step 3), and quickly stirring for 2 min;
5) stirring in oil bath at 75 ℃ for reaction for 1.5 h;
6) and washing the obtained zinc oxide submicron spheres with ethanol for multiple times, centrifuging, drying and grinding to obtain the solid zinc oxide submicron spheres.
According to the characterization of a scanning electron microscope and the statistics of particle size distribution, the microsphere has good spherical morphology and uniform particle size, the particle size is 790 +/-10 nm, the particle size distribution is calculated to be less than 10%, and the particle size distribution is narrow.
Examples 5 to 7
The mass of the polyvinylpyrrolidone obtained in the step 1) of the embodiment 1 is respectively replaced by 3.00g, 4.00g and 5.00g, so that the zinc oxide microspheres with the particle sizes of 520 +/-10 nm, 495 +/-10 nm and 475 +/-10 nm can be respectively prepared, and the particle size distribution coefficient is less than 10 percent.
Examples 8 to 10
Example 1 the molecular weight of polyvinylpyrrolidone obtained in step 1) is respectively replaced by 10000, 55000 and 130000, and zinc oxide microspheres with the particle size of 420 +/-10 nm, 500 +/-10 nm and 530 +/-10 nm can be respectively prepared, and the particle size distribution coefficient is less than 10%.
Examples 11 to 13
In example 1, the volume of the glycol obtained in step 1) is respectively replaced by 30ml, 40ml and 60ml, so that the zinc oxide microspheres with the particle sizes of 480 +/-10 nm, 470 +/-10 nm and 450 +/-10 nm can be respectively prepared, and the particle size distribution coefficients are all less than 10%.
Examples 14 to 16
In the embodiment 1, the stirring time in the step 4) is respectively replaced by 3min, 5min and 10min, so that the zinc oxide microspheres with the particle sizes of 400 +/-10 nm, 390 +/-10 nm and 370 +/-10 nm can be respectively prepared, and the particle size distribution coefficients are all less than 10%.
Examples 17 to 19
In example 2, the volume of the deionized water obtained in step 4) is replaced by 10mL, 20mL and 30mL respectively, so that the zinc oxide microspheres with the particle sizes of 130 +/-10 nm, 190 +/-10 nm and 250 +/-10 nm can be prepared respectively, and the particle size distribution coefficient is less than 10%.
Examples 20 to 23
In the step 2) of the examples 1,2, 3 and 4, the polyhydric alcohol is replaced by diethylene glycol, so that the zinc oxide microspheres with the particle sizes of 480 +/-10 nm, 170 +/-10 nm, 345 +/-10 nm and 830 +/-10 nm can be respectively prepared, and the particle size distribution coefficients are all less than 10%.
Examples 24 to 26
In the embodiment 1, the reaction temperature in the step 3) and the reaction temperature in the step 5) are the same, and the reaction temperatures are respectively 60 ℃, 70 ℃ and 80 ℃, so that the zinc oxide microspheres with the particle diameters of 680 +/-10 nm, 530 +/-10 nm and 290 +/-10 nm can be respectively prepared, and the particle diameter distribution coefficients of the synthesized zinc oxide submicron spheres are all less than 20%.
Examples 27 to 29
In the embodiment 2, the reaction temperature in the step 3) and the reaction temperature in the step 5) are the same, and the reaction temperatures are respectively replaced by 60 ℃, 70 ℃ and 80 ℃, so that the zinc oxide microspheres with the particle diameters of 230 +/-10 nm, 200 +/-10 nm and 110 +/-10 nm can be respectively prepared, and the particle diameter distribution coefficients are all less than 10%.
FIG. 3 is a scanning electron microscope image of zinc oxide microspheres with different particle sizes prepared in different examples, which shows that the prepared microspheres with different particle sizes have excellent monodispersity, uniform particle size, good morphology and certain surface roughness.
Claims (6)
1. A method for preparing highly uniform zinc oxide submicron spheres with controllable particle size is characterized by comprising the following steps:
1) according to the concentration of 0.2-1.2mmol/L, taking polyvinylpyrrolidone, stirring and dispersing in ethanol solution at room temperature;
2) according to the concentration of 0.1-1mol/L, taking a zinc source, ultrasonically stirring and dispersing in a polyol solution at room temperature;
3) mixing the solutions obtained in the step 1) and the step 2), heating to 60-80 ℃, and stirring for 2-4 h;
4) adding deionized water into the solution obtained in the step 3) according to the volume ratio of 1-5 of polyol to deionized water, and stirring and dispersing;
5) stirring in oil bath at 60-80 deg.C for 1-2 h;
6) and washing the obtained zinc oxide submicron spheres with ethanol for multiple times, centrifuging, drying and grinding to obtain the solid zinc oxide submicron spheres.
2. The method for preparing highly uniform zinc oxide submicron spheres with controllable particle size as claimed in claim 1, wherein the average molecular weight of polyvinylpyrrolidone is 10000-130000.
3. The method for preparing highly uniform zinc oxide submicron spheres with controllable particle size according to claim 1, wherein the polyol in step 2) is one or two of ethylene glycol, diethylene glycol and 1, 2-propylene glycol.
4. The method for preparing highly uniform zinc oxide submicron spheres with controllable particle size according to claim 1, wherein the stirring time in step 4) is 2-10 min.
5. The method of claim 1, wherein said zinc source comprises zinc acetate dihydrate.
6. The highly uniform zinc oxide submicron spheres with controllable particle sizes are characterized in that the zinc oxide submicron spheres have uniform particle sizes and are of polycrystalline structures, the particle size regulation range of the microspheres is 800nm and 100-800nm, and the particle size distribution coefficient is less than 10%.
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