阅读说明：本技术 一种微米级玫瑰石状SnO2制备方法 (Micron-grade rosette SnO2Preparation method ) 是由 张芳聪 姚文俐 于 2021-07-02 设计创作，主要内容包括：本发明属于功能材料制备领域,涉及一种微米级玫瑰石状SnO-(2)制备方法。包括以下步骤：(1)称取碳酸钠溶于去离子水中,配制成一定浓度的碳酸钠水溶液作为沉淀剂；(2)将可溶性锡盐溶于适量酸中,其中锡盐与酸的摩尔比为1：0.5～1.5,再加入去离子水使溶液中的Sn～(2+)浓度为0.1～0.2mol/L的锡盐溶液；(3)将一定量锡盐溶液加入微波反应器中加热至50～70℃,再将上述适量的碳酸钠溶液以100～1000mL/min的流速加入锡盐溶液中,随后恒温搅拌2～10分钟；(4)微波沉淀反应结束后,过滤、洗涤后,得到沉淀物,将沉淀物在90～100℃中干燥6～10小时,得到固体烘干物；(5)将上述固体烘干物置于空气或氧气气氛中,以1～5℃/min加热升温到400℃～600℃,并保温1～6小时,得到本发明所述的一种微米级玫瑰石状SnO-(2)。(The invention belongs to the field of functional material preparation, and relates to micron-sized rosette-shaped SnO 2 A preparation method. The method comprises the following steps: (1) weighing sodium carbonate, dissolving the sodium carbonate in deionized water, and preparing a sodium carbonate aqueous solution with a certain concentration as a precipitator; (2) dissolving a soluble tin salt in a proper amount of acid, wherein the molar ratio of the tin salt to the acid is 1: 0.5-1.5, and adding deionized water to lead Sn in the solution 2+ Tin salt solution with the concentration of 0.1-0.2 mol/L; (3) adding a certain amount of tin salt solution into a microwave reactor, heating to 50-70 ℃, adding the proper amount of sodium carbonate solution into the tin salt solution at the flow rate of 100-1000 mL/min, and then stirring at constant temperature for 2-10 minutes; (4) after the microwave precipitation reaction is finished, filtering and washing to obtain a precipitate, and drying the precipitate at 90-100 ℃ for 6-10 hours to obtain a solid dried substance; (5) placing the solid dried substance in air or oxygen atmosphere, heating to 400-600 ℃ at the speed of 1-5 ℃/min, and preserving heat for 1-6 hours to obtain the micron-sized rose-stone-shaped SnO 2 。)

1. Micron-grade rosette SnO₂The preparation method is characterized by comprising the following steps:

(1) weighing sodium carbonate, dissolving the sodium carbonate in deionized water to prepare a sodium carbonate aqueous solution, wherein the molar concentration of the sodium carbonate aqueous solution is 0.1-0.5 mol/L;

(2) dissolving a soluble tin salt in an acid, wherein the molar ratio of tin salt to acid is 1: 0.5 to 1.5, and then adding deionized water to prepare Sn²⁺Tin salt solution with the concentration of 0.1-0.2 mol/L;

(3) adding a tin salt solution into a microwave liquid phase reactor, heating to 50-70 ℃, adding the prepared sodium carbonate aqueous solution into the tin salt solution at a rate of 100-1000 mL/min, and magnetically stirring for 2-10 minutes;

(4) after the microwave precipitation reaction is finished, filtering the precipitate to be neutral by using deionized water, and drying the precipitate at the temperature of 90-100 ℃ for 6-10 hours to obtain a solid dried substance;

(5) placing the solid drying object in a certain atmosphere for high-temperature reaction, heating to 400-600 ℃ at the speed of 1-5 ℃/min, and preserving heat for 1-6 hours to obtain the micron-sized rosette-shaped SnO₂。

2. The micron-sized rosette-shaped SnO according to claim 1₂The preparation method is characterized by comprising the following steps: the tin salt in the step (2) is one of stannous chloride and stannous sulfate.

3. The micron-sized rosette-shaped SnO according to claim 1₂The preparation method is characterized by comprising the following steps: the acid in the step (2) is one of concentrated hydrochloric acid and concentrated sulfuric acid.

4. The micron-sized rosette-shaped SnO according to claim 1₂The preparation method is characterized by comprising the following steps: the atmosphere in the step (5) is air or oxygen atmosphere.

Technical Field

The invention belongs to the field of functional material preparation, and relates to micron-sized rosette-shaped SnO₂A preparation method.

Background

Tin is an important industrial material in national economy, and has rich sources and low price. SnO₂As a functional material, the functional material has been widely applied to the fields of battery electrode materials, semiconductor materials, thin film materials, catalysts, cosmetics and the like. SnO₂When used as an electrode material of a lithium ion battery, the material has theoretical specific capacity which is about 3 times that of a graphite electrode, and can meet the requirement of a battery electrode with high energy density. At the same time, SnO₂As an n-type wide bandgap semiconductor material, its optical, electrical and catalytic properties strongly depend on its microstructure, morphologyAnd doping, different microstructures have a significant impact on their electrical and optical properties. In addition, the composite material can be widely applied to a plurality of fields such as conductive fibers, rubber, ceramics, plastics, coatings, conductive fillers for antistatic coatings, low-emissivity glass for buildings, infrared absorption heat insulation materials, semiconductor gas sensitive elements, humidity sensitive elements and the like, and has great economic and social benefits.

Currently synthesized SnO₂In the conventional method, tin dioxide materials with various morphologies, such as nano microspheres, nano flowers, nano rods, nano sheets and the like, are prepared by adopting different experimental methods. The invention assists microwave liquid phase synthesis, optimizes reaction parameters, and can quickly synthesize a precursor of the material so as to prepare the tin dioxide material with special morphology.

Disclosure of Invention

The invention provides micron rose-stone-shaped SnO aiming at regulating and controlling the shape of a reaction precursor₂A preparation method.

The technical scheme of the invention is as follows: micron rose stone-shaped SnO₂The preparation method is characterized by comprising the following steps:

(1) weighing sodium carbonate, dissolving the sodium carbonate in deionized water to prepare a sodium carbonate aqueous solution, wherein the molar concentration of the sodium carbonate aqueous solution is 0.1-0.5 mol/L;

(2) dissolving a soluble tin salt in an acid, wherein the molar ratio of tin salt to acid is 1: 0.5 to 1.5, and then adding deionized water to prepare Sn²⁺Tin salt solution with the concentration of 0.1-0.2 mol/L;

(3) adding a tin salt solution into a microwave liquid phase reactor, heating to 50-70 ℃, adding the prepared sodium carbonate aqueous solution into the tin salt solution at a rate of 100-1000 mL/min, and magnetically stirring for 2-10 minutes;

(4) after the microwave precipitation reaction is finished, filtering the precipitate to be neutral by using deionized water, and drying the precipitate at the temperature of 90-100 ℃ for 6-10 hours to obtain a solid dried substance;

(5) drying the solidCarrying out high-temperature reaction in a certain atmosphere, heating to 400-600 ℃ at a speed of 1-5 ℃/min, and preserving heat for 1-6 hours to obtain the micron-sized rose-stone-shaped SnO₂。

The tin salt in the step (2) is one of stannous chloride and stannous sulfate.

The acid in the step (1) in the step (2) is one of concentrated hydrochloric acid and concentrated sulfuric acid.

The atmosphere in the step (5) is air or oxygen atmosphere.

The invention has the beneficial effects that: (1) the invention adopts soluble tin salt and sodium carbonate to prepare the precipitator, and the microwave precipitation reaction time is short; (2) the invention does not need surfactant or template, the process is simple, the post-treatment is convenient; (3) the tin dioxide prepared by the preparation method has a micron-sized roseite-shaped appearance.

Description of the drawings fig. 1 is a view showing micron-sized rosy-like SnO prepared according to example 1₂XRD pattern of (a). FIG. 2 is a micron-sized rosette-like SnO prepared according to example 1₂SEM image of (d).

Detailed Description

The examples of the present invention are as follows, but do not limit the present invention.

Example 1

(1) Weighing 0.02mol of anhydrous sodium carbonate, adding a proper amount of deionized water to a constant volume of 100mL, wherein the molar concentration of the sodium carbonate is 0.2 mol/L;

(2) 0.02mol of stannous chloride was first dissolved in an appropriate amount of 2mL concentrated hydrochloric acid (12 mol/L) with a molar ratio of tin to acid of 1: 1.2, adding a proper amount of deionized water to a constant volume of 200mL to ensure that Sn in the solution is dissolved²⁺The concentration is 0.1 mol/L;

(3) heating the solution to 60 ℃ under the assistance of microwave, adding the sodium carbonate solution into the tin salt solution at the speed of 400mL/min, and then stirring and reacting for 5 minutes at constant temperature;

(4) after the microwave reaction is finished, cooling, carrying out solid-liquid separation on the obtained product, washing the product for a plurality of times by using deionized water, and drying the precipitate at 100 ℃ for 6 hours to obtain a solid dried substance;

(5) placing the above solid dried material in a boxThe resistance furnace carries out solid-phase reaction in the air atmosphere, and the micron-sized rosette SnO is obtained by heating to 550 ℃ at the speed of 2 ℃/min and preserving the heat for 2h₂；

(6) Micron-sized rosette-shaped SnO prepared in this example₂The phase and morphology of the compound are respectively shown in figure 1 and figure 2, wherein figure 1 is SnO₂Fig. 2 shows the prepared SnO₂Is in a shape of flake aggregated rosettes.

Example 2

(1) Weighing 0.04mol of anhydrous sodium carbonate, adding a proper amount of deionized water to a constant volume of 80mL, wherein the molar concentration of the sodium carbonate is 0.5 mol/L;

(2) 0.04mol of stannous chloride is first dissolved in an appropriate amount of 1.64mL of concentrated hydrochloric acid (12 mol/L) with a molar ratio of tin to acid of 1: 0.5, adding a proper amount of deionized water to a constant volume of 200mL to ensure that Sn in the solution is dissolved²⁺The concentration is 0.2 mol/L;

(3) heating the solution to 70 ℃ under the assistance of microwave, adding the sodium carbonate solution into the tin salt solution at a rate of 200mL/min, and then stirring and reacting for 2 minutes at constant temperature;

(4) after the microwave reaction is finished, cooling, carrying out solid-liquid separation on the obtained product, washing the product for a plurality of times by using deionized water, and drying the precipitate at 100 ℃ for 6 hours to obtain a solid dried substance;

(5) carrying out solid-phase reaction on the solid drying object in air atmosphere, heating to 600 ℃ at a speed of 1 ℃/min, and preserving heat for 1h to obtain the micron-sized rosette-shaped SnO₂。

Example 3

(1) Weighing 0.02mol of anhydrous sodium carbonate, adding a proper amount of deionized water to a constant volume of 200mL, wherein the molar concentration of the sodium carbonate is 0.1 mol/L;

(2) 0.02mol of stannous sulfate was first dissolved in an appropriate amount of 1.63mL of concentrated sulfuric acid (18.4 mol/L) with a molar ratio of tin to acid of 1: 1.5, adding a proper amount of deionized water to a constant volume of 125mL to ensure that Sn in the solution is dissolved²⁺The concentration is 0.16 mol/L;

(3) heating the solution to 50 ℃ under the assistance of microwave, adding the sodium carbonate solution into the tin salt solution at the speed of 1000mL/min, and then stirring and reacting for 10 minutes at constant temperature;

(4) after the microwave reaction is finished, cooling, carrying out solid-liquid separation on the obtained product, washing the product for a plurality of times by using deionized water, and drying the precipitate at 90 ℃ for 10 hours to obtain a solid dried substance;

(5) carrying out solid-phase reaction on the solid drying object in an oxygen atmosphere, heating to 400 ℃ at a speed of 5 ℃/min, and preserving heat for 6h to obtain the micron-sized rosette-shaped SnO₂。