CN114132956A - Preparation method of ZnS microspheres - Google Patents
Preparation method of ZnS microspheres Download PDFInfo
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- CN114132956A CN114132956A CN202111477881.2A CN202111477881A CN114132956A CN 114132956 A CN114132956 A CN 114132956A CN 202111477881 A CN202111477881 A CN 202111477881A CN 114132956 A CN114132956 A CN 114132956A
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- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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Abstract
The invention relates to the technical field of ZnS microsphere preparation, in particular to a method for preparing ZnS microspheres by organic carboxylic acid auxiliary liquid phase, which comprises the following steps: (1) preparing a zinc salt aqueous solution; (2) adding organic carboxylic acid into the zinc salt aqueous solution, and fully stirring to obtain a transparent mixed solution; (3) dissolving a sulfur source in the transparent mixed solution to obtain a reaction precursor solution; (4) transferring the reaction precursor solution to a reaction device for reaction; (5) and after the reaction device is cooled to room temperature, centrifugally cleaning the product to obtain the ZnS microsphere. According to the preparation method of the ZnS microsphere, the organic carboxylic acid is added into the zinc salt aqueous solution and then reacts with the sulfur source, so that the nucleation rate of ZnS can be reduced at the initial stage of the reaction; in the later stage of the reaction, promoting the crystal-forming ions to synchronously diffuse towards all directions of crystal nucleus to form spherical particles; the ZnS microsphere prepared by the method has good dispersibility, regular appearance and smooth surface, and has good application value.
Description
Technical Field
The invention relates to the technical field of ZnS microsphere preparation, in particular to a method for preparing ZnS microspheres by organic carboxylic acid auxiliary liquid phase.
Background
Zinc sulfide (ZnS) is a typical type of II-IV semiconductor material, and has a large band gap energy (3.5-3.8eV) in both wurtzite (α -ZnS) and sphalerite (β -ZnS) structures, and due to the advantages of low toxicity, low preparation cost, and the like, ZnS materials are gaining attention in the fields of photocatalysis, cathode ray, luminescent materials, photo/electroluminescence, flat panel display, solar cells, and the like. For example, Cu blue phosphors and Mn green afterglow materials have been used for commercial illumination since the last century, while ZnS: Ag, Cl blue and ZnS: Cu, Cl green phosphors have been widely used in cathode ray tubes; in addition, the excellent piezoelectric properties of ZnS have led to extensive research in the field of stress emitting materials in recent years; the color change behavior of ZnS: Cu under the action of external electric field has attracted the interest of scholars in the field of electrochromism in recent years. In conclusion, ZnS is an optical material substrate with excellent performance and rich functional types.
For optical materials, the characteristics of the particle morphology, dispersibility, size distribution, etc., of the material greatly affect its luminescent and color rendering properties. Practical application shows that whether the particle morphology of the material is regular or not directly influences the light scattering and light attenuation degree of the material; the dispersibility of the particles is good, which is related to the radiation absorption capability and the luminous intensity. It is worth mentioning that the spherical particles are ideal in morphology of high-quality optical materials, have good dispersibility and uniform size, and can form a compact and uniform light emitting layer through close packing when a device is packaged, so that the resolution of a fluorescent component is improved, light scattering is effectively reduced, and the optimal light emitting and color developing states are presented.
The current method for preparing spherical particles mainly comprises the following steps: template method, uniform precipitation method, hydrothermal method, spray pyrolysis method, etc. However, these methods have the disadvantages of complicated operation, long reaction time, harsh reaction conditions, difficult removal of template in the product, rough surface of the product, etc. when synthesizing ZnS spherical particles. In addition, the method needs to adopt specific raw materials and can realize the preparation of ZnS spherical particles under specific conditions. Therefore, the method for preparing the ZnS spherical particles with wide requirements on raw materials, high reaction condition tolerance, good dispersity, regular appearance and smooth surface is provided, and the method has great significance in the fields of luminescence, electrochromism and the like.
Disclosure of Invention
In order to solve the problems, the invention provides a method for preparing ZnS microspheres by organic carboxylic acid auxiliary liquid phase, the preparation method has wide raw material selection range and wide reaction conditions, and the prepared ZnS microspheres have high purity and good particle dispersibility.
A preparation method of ZnS microspheres comprises the following steps:
(1) preparing a zinc salt aqueous solution;
(2) adding organic carboxylic acid into the zinc salt aqueous solution, and fully stirring to obtain a transparent mixed solution;
(3) dissolving a sulfur source in the transparent mixed solution to obtain a reaction precursor solution;
(4) transferring the reaction precursor solution to a reaction device for reaction;
(5) and after the reaction device is cooled to room temperature, centrifugally cleaning the product to obtain the ZnS microsphere.
Further, in the step (1), the zinc salt is selected from one or more of zinc sulfate, zinc chloride, zinc nitrate, zinc acetate and zinc citrate; preferably, the zinc salt is hydrated zinc acetate.
Further, the concentration of the zinc salt aqueous solution in the step (1) is 0.001-1 mmol/mL; preferably, the concentration of the aqueous solution of zinc salt is 0.01 to 0.1 mmol/mL.
Further, in the step (2), the organic carboxylic acid is selected from one or more of citric acid, acetic acid, malic acid, tartaric acid, maleic acid, succinic acid and ethylenediamine tetraacetic acid.
Further, the molar ratio of the organic carboxylic acid to the zinc ions is 0.5:1-200: 1; preferably, the molar ratio of the organic carboxylic acid to the zinc ion is 1:1 to 100: 1.
The organic carboxylic acid plays roles of complexing and adsorbing in the reaction, is used for regulating and controlling the generation speed of ZnS and preventing agglomeration of ZnS microspheres as a product; due to the different molecular structures of different organic carboxylic acids, there are differences in the number of complexing sites (ligands) that can be provided, resulting in different molar ratios of organic carboxylic acid to zinc ion in the example applications. The inventor finds out through experimental research that the molar ratio of the organic carboxylic acid to the zinc ions is preferably 2:1-10:1 for polybasic carboxylic acids such as citric acid, malic acid and the like; the molar ratio of the organic carboxylic acid to the zinc ion is preferably 50:1 to 100:1 with respect to the monocarboxylic acid such as acetic acid.
Further, in the step (3), the sulfur source is selected from one or more of thiourea, lithium sulfide, sodium sulfide, potassium sulfide and ammonium sulfide; preferably, the sulfur source is thiourea.
Further, the molar ratio of the sulfur source to the zinc ions is 1:1-20: 1; preferably, the molar ratio of the sulfur source to the zinc ions is 1:1 to 3: 1.
Further, the reaction is a hydrothermal reaction or a microwave reaction; the heating temperature of the hydrothermal reaction is 120-300 ℃, and the temperature of the reaction liquid for terminating the microwave reaction is 50-120 ℃.
Further, the time of the hydrothermal reaction is 1-96h, and the time of the microwave reaction is 0.1-2 h; preferably, the hydrothermal reaction time is 3-24h, and the microwave reaction time is 0.2-0.5 h.
Performing hydrothermal reaction in a drying oven, wherein the reaction vessel is a hydrothermal reaction kettle;
the reaction vessel is a flask/beaker for carrying out the microwave reaction, which is carried out in a microwave reactor.
Further, the particle size of the ZnS microspheres is 0.1 to 20 μm.
When a proper amount of organic carboxylic acid is introduced into the reaction system, the introduced organic carboxylic acid is mixed with free ions Zn2+Complexation occurs; as the temperature of the reaction system increases, the added sulfur source gradually decomposes to produce S2-Due to Zn2+In a complex state with organic carboxylic acid molecules, resulting in S2-With Zn2+The reaction speed is reduced, and the nucleation rate of ZnS is reduced; following the contraryShould proceed further, ZnS crystal nucleus grows gradually, S2-With Zn2+The carboxylic acid molecules are discharged to the surface of the crystal nucleus and form a uniform protective layer on the surface of the crystal nucleus, so that the diffusion speed of the crystal-forming ions to all directions of the crystal nucleus tends to be consistent, and finally spherical particles are formed. In addition, the adsorption of carboxylic acid molecules on the surface of the particles prevents agglomeration between the particles, thereby obtaining monodisperse spherical particles.
Compared with the prior art, the invention has the beneficial effects that:
1. the preparation method of ZnS microspheres of the invention adds organic carboxylic acid into zinc salt aqueous solution, and then reacts with sulfur source, so that organic carboxylic acid and Zn are utilized at the initial stage of reaction2+Complex formation is carried out, and the nucleation rate of ZnS is reduced; in the later stage of the reaction, carboxylic acid molecules are discharged to the surface of the crystal nucleus to form a uniform protective layer, so that crystal-forming ions are promoted to synchronously diffuse towards all directions of the crystal nucleus to form spherical particles; meanwhile, the adsorption effect of carboxylic acid molecules on the surfaces of the particles is utilized, so that the agglomeration among the particles can be prevented, and the monodisperse spherical particles are obtained. The ZnS microsphere prepared by the method has good dispersibility, regular appearance and smooth surface, and has good application value.
2. The preparation method of the ZnS microsphere has wide selection range of raw materials including a zinc source, a sulfur source and organic carboxylic acid, wide reaction conditions, suitability for various reaction modes, simple operation, good adaptability to the existing ZnS microsphere manufacturing system and good production and popularization values.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIGS. 1-2 are XRD and SEM images of ZnS microspheres prepared in example 1 of the present invention, respectively;
FIGS. 3 to 6 are SEM images of ZnS microspheres prepared in examples 2 to 5 of the present invention, respectively;
FIGS. 7 to 8 are SEM images of products prepared in comparative examples 1 to 2 of the present invention;
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of ZnS microspheres comprises the following steps:
(1) 2mmol of zinc acetate dihydrate (Zn (CH)3COO)2·2H2O) is dissolved in 50mL deionized water, and magnetic stirring is carried out for 10 min;
(2) to the resulting solution was added 10mmol of citric acid monohydrate (C)6H8O7·H20) Continuously stirring the particles to obtain a transparent mixed solution;
(3) weighing 3mmol of thiourea, adding the thiourea into the transparent mixed solution, and continuing stirring until the thiourea is completely dissolved to obtain a reaction precursor solution;
(4) transferring the reaction precursor solution to a 100mL hydrothermal kettle, placing the hydrothermal kettle in a drying oven at 200 ℃, and reacting for 6 h;
(5) and after the reaction kettle is cooled to room temperature, firstly separating the product from the mother liquor by adopting a centrifugal machine at the rotating speed of 1000r/min, then adjusting the rotating speed to 6000r/min, washing the product with deionized water for three times, and washing the product with alcohol for one time to obtain the ZnS microspheres.
The XRD and SEM characterization patterns are shown in figure 1-2, and the prepared ZnS microsphere is of a hexagonal wurtzite structure, has good crystallinity and is free from impurity phase generation; the particles are regular spheres and have good dispersibility, and the size of the particles is between 1 and 10 mu m.
Example 2
This embodiment includes most of the operation steps of embodiment 1, and the difference is that:
(2) to the resulting solution was added 20mmol of citric acid monohydrate (C)6H8O7·H20) Continuously stirring the particles to obtain a transparent mixed solution;
the SEM characteristic diagram is shown in FIG. 3, and it can be seen that the particles are all less than 10 μm, the sphericity is high, and the dispersibility is good.
Example 3
This embodiment includes most of the operation steps of embodiment 1, and the difference is that:
(3) weighing 2mmol of thiourea, adding the thiourea into the transparent mixed solution, and continuing stirring until the thiourea is completely dissolved to obtain a reaction precursor solution;
the SEM characteristic diagram is shown in FIG. 4, and it can be seen that the particles are all less than 10 μm, the sphericity is high, and the dispersibility is good.
Example 4
(1) 2mmol of zinc acetate dihydrate (Zn (CH)3COO)2·2H2O) is dissolved in 70mL deionized water, and magnetic stirring is carried out for 10 min;
(2) adding 20mL of acetic acid solution with the purity of 36 wt% into the obtained solution, and continuously stirring to obtain transparent mixed solution;
(3) weighing 5mmol of thiourea, adding the thiourea into the transparent mixed solution, and continuing stirring until the thiourea is completely dissolved to obtain a reaction precursor solution;
(4) transferring the reaction precursor solution to a 100mL hydrothermal kettle, placing the hydrothermal kettle in a drying oven at 200 ℃, and reacting for 12 h;
(5) and after the reaction kettle is cooled to room temperature, firstly separating the product from the mother liquor by adopting a centrifugal machine at the rotating speed of 1000r/min, then adjusting the rotating speed to 6000r/min, washing the product with deionized water for three times, and washing the product with alcohol for one time to obtain the ZnS microspheres.
The SEM characteristic diagram is shown in FIG. 5, and it can be seen that the particles are all less than 10 μm, the sphericity is high, and the dispersibility is good.
Example 5
(1) 2mmol of zinc acetate dihydrate (Zn (CH)3COO)2·2H2O) is dissolved in 100mL deionized water, and is magnetically stirred for 10 min;
(2) to the resulting solution was added 15mmol of malic acid (C)4H6O5) Continuously stirring to obtain a transparent mixed solution;
(3) weighing 5mmol of thiourea, adding the thiourea into the transparent mixed solution, and continuing stirring until the thiourea is completely dissolved to obtain a reaction precursor solution;
(4) transferring the reaction precursor solution into a 250mL two-mouth flask, transferring the flask into a microwave reactor, and carrying out microwave reaction for 10min at a heating speed of 10 ℃/min;
(5) after the reaction, the flask was taken out, and the temperature of the reaction solution was measured to be 96 ℃;
(6) and after the reaction liquid is cooled to room temperature, firstly separating the product from the mother liquid at the rotating speed of 1000r/min by using a centrifugal machine, then adjusting the rotating speed to 6000r/min, washing the product with deionized water for three times, and washing the product with alcohol for one time to obtain the ZnS microspheres.
The SEM characteristic diagram is shown in FIG. 6, and it can be seen that the particles are all less than 10 μm, the sphericity is high, and the dispersibility is good.
Comparative example 1
This comparative example includes most of the operating steps of example 1, with the following exceptions: no organic carboxylic acid is added.
The SEM representation is shown in FIG. 7, and the product is an agglomerate of irregular fine particles with a particle size in the submicron range, which is significantly smaller than that of the spherical particles obtained in example 1, indicating that the nucleation rate is not well controlled without using carboxylic acid; the agglomerated state of the particles further indicates that the particles are stuck to each other in a state where the carboxylic acid is absent from the surface; moreover, the irregular shape of the particles indicates that the surface of the particles is not protected by the carboxylic acid, so that the particles cannot grow at a uniform speed in all directions and cannot be transformed into spherical particles.
Comparative example 2
This comparative example includes most of the operating steps of example 1, with the following exceptions:
(3) weighing 100mmol of thiourea, adding the thiourea into the transparent mixed solution, and continuing stirring until the thiourea is completely dissolved;
the SEM representation is shown in FIG. 8, the product is irregular and has a rough surface, and monodisperse zinc sulfide microspheres cannot be obtained.
In conclusion, the preparation method of the ZnS microsphere, provided by the invention, has the advantages that the organic carboxylic acid is introduced into a reaction system, the morphology of the ZnS microsphere can be well controlled, the reaction raw material selection is wide, the reaction conditions are wide, and the prepared ZnS microsphere has good dispersibility, regular morphology, smooth surface and good application value.
The present invention has been further described with reference to specific embodiments, but it should be understood that the detailed description should not be construed as limiting the spirit and scope of the present invention, and various modifications made to the above-described embodiments by those of ordinary skill in the art after reading this specification are within the scope of the present invention.
Claims (10)
1. The preparation method of the ZnS microsphere is characterized by comprising the following steps of:
(1) preparing a zinc salt aqueous solution;
(2) adding organic carboxylic acid into the zinc salt aqueous solution, and fully stirring to obtain a transparent mixed solution;
(3) dissolving a sulfur source in the transparent mixed solution to obtain a reaction precursor solution;
(4) transferring the reaction precursor solution to a reaction device for reaction;
(5) and after the reaction device is cooled to room temperature, centrifugally cleaning the product to obtain the ZnS microsphere.
2. The method for preparing ZnS microspheres of claim 1, wherein in step (1), the zinc salt is selected from one or more of zinc sulfate, zinc chloride, zinc nitrate, zinc acetate and zinc citrate.
3. The method for preparing ZnS microspheres according to claim 1, wherein the concentration of said aqueous solution of zinc salt in step (1) is in the range of 0.001 to 1 mmol/mL.
4. The method for preparing ZnS microspheres of claim 1, wherein said organic carboxylic acid in step (2) is selected from one or more of citric acid, acetic acid, malic acid, tartaric acid, maleic acid, succinic acid, ethylenediaminetetraacetic acid.
5. The method for preparing ZnS microspheres according to claim 1, wherein the molar ratio of organic carboxylic acid to zinc ion is in the range of 0.5:1 to 200: 1.
6. The method for preparing ZnS microspheres of claim 1, wherein said sulfur source in step (3) is selected from one or more of thiourea, lithium sulfide, sodium sulfide, potassium sulfide and ammonium sulfide.
7. The method for preparing ZnS microspheres of claim 1, wherein the molar ratio of the sulfur source to the zinc ion is in the range of 1:1 to 20: 1.
8. The method for producing ZnS microspheres according to claim 1, wherein the reaction is a hydrothermal reaction or a microwave reaction; the heating temperature of the hydrothermal reaction is 120-300 ℃, and the temperature of the reaction liquid for terminating the microwave reaction is 50-120 ℃.
9. The method for preparing ZnS microspheres of claim 8, wherein the hydrothermal reaction time is in the range of 1 to 96h and the microwave reaction time is in the range of 0.1 to 2 h.
10. The method for producing ZnS microspheres according to claim 1, wherein the particle size of the ZnS microspheres is 0.1 to 20 μm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114835154A (en) * | 2022-03-31 | 2022-08-02 | 宁波大学 | Preparation method of monodisperse ZnS colloidal microspheres with adjustable particle size |
| CN115466559A (en) * | 2022-09-19 | 2022-12-13 | 中国科学院兰州化学物理研究所 | Friction luminous paint |
| CN115569653A (en) * | 2022-09-15 | 2023-01-06 | 广州大学 | Polymerization nanoparticle heterogeneous water treatment catalyst, preparation method and application |
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