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Preparation method of room-temperature ball-milling solid phase chemical reaction of rare earth mixing with nano stannic oxide

A technology of nano-tin dioxide and solid-phase chemical reaction, which is applied in the direction of tin oxide, etc., can solve the problems of antimony and tin ion hydrolysis out of synchronization, difficulty in achieving uniform mixing, and difficulty in large-scale industrial production, achieving shortened chemical reaction time, The effect of speeding up the chemical reaction and preventing the hydrolysis of tin ions

Inactive Publication Date: 2010-06-23
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From the content of the above Chinese patent application, it can be seen that the traditional solid-phase method is simple to operate and low in cost, but the reaction speed is slow, and it is difficult to achieve uniform mixing during doping; the cost of hydrothermal method, sol-gel method and metal alkoxide hydrolysis method Higher, the chemical co-precipitation method has strict requirements on the precipitation conditions such as pH value, and it is easy to cause the hydrolysis of antimony and tin ions to be out of sync, which is not conducive to the realization of real doping, and it is difficult to carry out large-scale industrial production

Method used

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  • Preparation method of room-temperature ball-milling solid phase chemical reaction of rare earth mixing with nano stannic oxide
  • Preparation method of room-temperature ball-milling solid phase chemical reaction of rare earth mixing with nano stannic oxide

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Embodiment 1

[0026] In this embodiment, the reactants are stannous chloride and cerium chloride, and the ligand is oxalic acid. The process flow is as follows: figure 1 As shown, there are the following steps in sequence

[0027] 1. Ingredients

[0028] The molar ratio of the total amount of stannous chloride, cerium chloride and oxalic acid is 1:2, wherein the molar ratio of tin and cerium ions is 94:6

[0029] 2. Mixing

[0030] Mix the proportioned stannous chloride, cerium chloride and oxalic acid until uniform;

[0031] 3. Preparation of precursors by ball milling solid-phase chemical reaction at room temperature

[0032] The uniformly mixed stannous chloride, cerium chloride and oxalic acid are ball milled at room temperature and normal pressure, so that they react to form precursors under the action of mechanical shear force and impact force generated during the ball milling process, and the speed of the ball mill is controlled at 300 rpm, ball milling for 60 minutes can complet...

Embodiment 2

[0040] In this embodiment, the reactants are stannous sulfate and cerium sulfate, and the ligand is ammonium carbonate. The process flow is as follows: figure 1 As shown, there are the following steps in sequence:

[0041] 1. Ingredients

[0042] The molar ratio of stannous sulfate, cerium sulfate total amount and ammonium carbonate is 1: 3, wherein tin, cerium ion molar ratio is 93: 7;

[0043] 2. Mixing

[0044] Mix the proportioned stannous sulfate, cerium sulfate and ammonium carbonate until uniform;

[0045] 3. Preparation of precursors by ball milling solid-phase chemical reaction at room temperature

[0046] The uniformly mixed stannous sulfate, cerium sulfate and ammonium carbonate are ball milled at room temperature and normal pressure, so that they can react to form precursors under the action of mechanical shear force and impact force generated during the ball milling process. The speed of the ball mill is 350 rpm / min, ball milling for 50 minutes can completely...

Embodiment 3

[0054] In this embodiment, the reactants are tin chloride and lanthanum chloride, and the ligand is oxalic acid. The process flow is as follows: figure 1 As shown, there are the following steps in sequence:

[0055] 1. Ingredients

[0056] The molar ratio of tin chloride, lanthanum chloride total amount and oxalic acid is 1: 4, wherein tin, lanthanum ion molar ratio is 96: 4;

[0057] 2. Mixing

[0058] Mix tin chloride, lanthanum chloride and oxalic acid in proportion until uniform;

[0059] 3. Preparation of precursors by ball milling solid-phase chemical reaction at room temperature

[0060]The uniformly mixed reaction system is ball milled at room temperature and normal pressure, so that it reacts to form a precursor under the action of mechanical shear force and impact force generated during the ball milling process. It can completely react tin chloride, lanthanum chloride and oxalic acid to form precursors;

[0061] 4. Precursor removal

[0062] The precursor is re...

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Abstract

The invention discloses a preparation method of room-temperature ball-milling solid phase chemical reaction of rare earth mixing with nano stannic oxide, relates to a preparation technology of the rare earth mixing with the nano stannic oxide, which can be applied for antistatic coating, plastics, fibre and other fields. Inorganic salts containing stannum and rare earth are taken as reactants, oxalic acid, ammonium carbonate, ammonium bicarbonate, sodium oxalate or sodium carbonate is taken as a ligand, the processing steps are sequentially dosing, mixing and preparing precursors of the room-temperature ball-milling solid phase chemical reaction, and the targeted product can be obtained after impurity removing, drying and thermal decomposition. The preparation method is characterized in that the reaction process does not use water, the stannum ion can be prevented from hydrolysis, uniform mixing can be realized, a solid phase reaction system is broken by utilizing the shearing force and the impact force generated during the ball milling process, the specific surface area of the reactant is increased, the reaction rate is increased, micro-fine and uniform precursors can be prepared, then the processes of cleaning, drying and controlling the thermolysis temperature and time are carried out, and thereby the rare earth mixing with nano stannic oxide powder, the particle size distribution of which is 30 to 80nm and has controllable morphology, can be obtained.

Description

1. Technical field [0001] The invention patent belongs to the "nano-oxide powder preparation technology", which involves a rare earth-doped nano-tin dioxide and its preparation method that can be used in antistatic coatings, plastics, fibers and other fields. 2. Background technology [0002] Antimony-doped tin dioxide (ATO) powder has been widely used due to its excellent properties such as high electrical conductivity, light color transparency, good stability and weather resistance, especially after the powder is nano-sized, due to its large specific A series of new features such as surface area have greatly improved its performance. At present, its preparation methods mainly include: chemical co-precipitation method, hydrothermal method, sol-gel method, metal alkoxide hydrolysis method, solid phase method, etc. For example: the patent application number 200510031786.4 uses ammonium stannate chloride and antimony oxychloride as raw materials, adds a small amount of compou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G19/02
Inventor 朱达川刘乙江涂铭旌
Owner SICHUAN UNIV
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