Method for controllably preparing oxide powder of titanium

A technology of oxide powder and titanium powder, applied in the direction of low-value titanium oxide, titanium oxide/hydroxide, etc., can solve the problems of difficult to quantify the amount of oxygen, increase the risk, unstable oxygen content, etc., and achieve the reaction time. Shortening, crystallinity and purity assurance, effect of accelerated diffusion

Active Publication Date: 2017-12-01
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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Problems solved by technology

Second, the method of gas-solid reaction is adopted to react with transition metal titanium and oxygen, and the ratio of titanium to oxygen of the target product is controlled by controlling the amount of oxygen in the reaction vessel. This reaction can react v...

Method used

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  • Method for controllably preparing oxide powder of titanium
  • Method for controllably preparing oxide powder of titanium
  • Method for controllably preparing oxide powder of titanium

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preparation example Construction

[0026] The method for preparing titanium oxide powder provided by the present invention is exemplarily described below.

[0027] Mix titanium powder and perchlorate in a vacuum-tight quartz tube. Specifically, a certain mass of titanium powder and perchlorate was weighed according to different proportions, transferred to a quartz tube, and then vacuum-packed in the quartz tube. Among them, the vacuum sealing device should make the inside of the quartz tube in a vacuum state (the pressure should be less than 10 -3 Torr), and then use the oxyhydrogen flame device to complete the vacuum packaging of the quartz glass tube. The particle diameter of the titanium powder may range from 1 to 50 microns. The perchlorate described in the present invention can be selected from potassium perchlorate, lithium perchlorate, sodium perchlorate, etc. if it satisfies high decomposition of oxygen and halides.

[0028] The vacuum-encapsulated quartz tube is placed in a muffle furnace for high-t...

Embodiment 1

[0034] Weigh 22.8 mg of potassium perchlorate and 189.4 mg of titanium metal powder, mix well, transfer to the quartz tube, and then -3 Under the vacuum condition of Torr, the quartz glass tube was sealed with a hydrogen-oxygen flame gun tube sealing device. Then transfer the quartz tube to a muffle furnace, slowly raise the temperature to 450 degrees, and keep it warm for 20 hours. After the sintering is completed, it is cooled to room temperature with the furnace. After opening the tube, soak it in distilled water to dissolve the potassium chloride produced during the reaction. Then, filter, and finally, after vacuum drying in a 60-degree oven, you can get Ti 6 O powder.

Embodiment 2

[0036] Weigh 43.4 mg of potassium perchlorate and 180 mg of titanium metal powder, mix well, transfer to a quartz tube, and then -3 Under the vacuum condition of Torr, the quartz glass tube was sealed with a hydrogen-oxygen flame gun tube sealing device. Then transfer the quartz tube to a muffle furnace, slowly raise the temperature to 450 degrees, and keep it warm for 20 hours. After the sintering is completed, it is cooled to room temperature with the furnace. After opening the tube, soak it in distilled water to dissolve the potassium chloride produced during the reaction. Then, filter, and finally, after vacuum drying in a 60-degree oven, you can get Ti 3 O powder.

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Abstract

The invention relates to a method for controllably preparing oxide powder of titanium. The method comprises the steps of weighing titanium powder and perchlorate, mixing the titanium powder and the perchlorate, then, putting the mixture into a vacuum-tight quartz tube, and carrying out a reaction for 10 to 30 hours at the high temperature of 400 DEG C to 1,100 DEG C, thereby obtaining the oxide powder of titanium. According to the method, a halide is produced during the reaction and can serve as a cosolvent of the reaction; and due to the addition of the halide cosolvent, the diffusion is accelerated, the reaction time is greatly shortened, and the crystallinity and purity of oxides of transition-metal titanium are guaranteed.

Description

technical field [0001] The method belongs to the field of synthesis and preparation, and aims at low-temperature and rapid synthesis of titanium oxide powders with different oxygen contents by controlling the feeding ratio. It provides convenience for studying the electrical and magnetic aspects of titanium oxide powder. Background technique [0002] There are many kinds of titanium oxides with different properties, and they have a wide range of applications in energy fields such as photovoltaics and catalysis. The physical and chemical properties of titanium oxides vary with the oxygen content. Moreover, as the ratio of titanium to oxygen increases, the forbidden band width of titanium oxide gradually narrows. When the ratio of titanium to oxygen is 1:1, it even transforms into a metallic phase. For example, black titanium dioxide has remarkable performance in photocatalytic degradation, and the conductivity of metal phase titanium monoxide is excellent, which is almost ...

Claims

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Application Information

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IPC IPC(8): C01G23/04
CPCC01G23/043C01P2002/72
Inventor 黄富强王东黄冲
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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