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Methods for preparing transition metal monoxide powder, target material and film

A transition metal and monoxide technology, applied in the field of synthesis and preparation, can solve the problems of restricting large-scale production and application, increasing unsafe factors, etc., achieve simple target preparation methods, shorten reaction time, and reduce high temperature resistance requirements Effect

Active Publication Date: 2017-05-17
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, synthesis methods two and three can prepare titanium monoxide powder, but the use or generation of hydrogen in the reaction artificially increases unsafe factors and limits large-scale production and application

Method used

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  • Methods for preparing transition metal monoxide powder, target material and film
  • Methods for preparing transition metal monoxide powder, target material and film
  • Methods for preparing transition metal monoxide powder, target material and film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Take by weighing 3.7474 grams of metal titanium powder, 6.2526 grams of titanium dioxide, take by weighing 5 grams of potassium chloride (0.5 times the mass) as a flux, after fully grinding, transfer to the quartz tube, then in less than 10 -3 Under the condition of Torr's vacuum, the quartz tube was encapsulated with an oxyhydrogen flame. Then place it in a muffle furnace at 900°C for 5 hours and take it out for quenching. Potassium chloride is washed away with distilled water, and TiO pure phase powder can be obtained after vacuum drying. Weigh 20 grams of the prepared TiO powder, place it in a graphite mold with a Φ of 1 inch, and compact it. Subsequently, the plasma discharge sintering method is used to sinter at 800 degrees Celsius and an argon atmosphere for 5 minutes to obtain a TiO dense target with a Φ of 1 inch.

[0044] figure 1 It is the XRD figure of the obtained TiO sample of the embodiment of the present invention 1; As attached figure 1 As shown, the...

Embodiment 2

[0046] Take by weighing 3.7474 grams of metal titanium powder, 6.2526 grams of titanium dioxide, take by weighing 20 grams of potassium chloride (2 times the quality) as a flux, after fully grinding, transfer to the quartz tube, then in less than 10 -3 Under the condition of Torr's vacuum, the quartz tube was encapsulated with an oxyhydrogen flame. Then place it in a muffle furnace at 900°C for 5 hours and take it out for quenching. Potassium chloride is washed away with distilled water, and TiO pure phase powder can be obtained after vacuum drying.

[0047] Figure 6 It is the XRD pattern of the TiO sample obtained in Example 2 of the present invention. The XRD spectrum peak is consistent with the TiO standard peak, and no other miscellaneous peaks appear, indicating that potassium chloride twice the mass of the reactant is used as a sintering aid. Under these conditions, pure TiO samples can be obtained.

Embodiment 3

[0049] Take by weighing 4.4969 grams of metal titanium powder, 7.5031 grams of titanium dioxide, take by weighing 6 grams of potassium chloride (2 times the quality) as a flux, after fully grinding, transfer to a quartz tube, then in less than 10 -3 Under the condition of Torr's vacuum, the quartz tube was encapsulated with an oxyhydrogen flame. Then place it in a muffle furnace at 1100 degrees Celsius to react for 5 hours, take it out and quench it directly. Potassium chloride is washed away with distilled water, and TiO pure phase powder can be obtained after vacuum drying.

[0050] Figure 7 It is the XRD pattern of the TiO sample obtained in Example 3 of the present invention. The XRD spectrum peak is consistent with the TiO standard peak, and no other miscellaneous peaks appear, indicating that potassium chloride twice the mass of the reactant is used as a sintering aid. Under these conditions, pure TiO samples can be obtained.

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Abstract

The invention provides methods for preparing transition metal monoxide powder, target material and film. The methods comprise the following steps: transition metal M powder and transition metal M oxide powder in a mole ratio being 1:1-1.2:1 are taken as reaction raw materials and sufficiently mixed with alkali halide with mass being 0.5-2.5 times, preferably, 0.5-2 times of the total mass of the reaction raw materials, the mixture is packaged in a reactor in a vacuum manner and reacts at 900-1,100 DEG C for 5-10 h, and the transition metal monoxide powder is obtained; the transition metal monoxide powder is subjected to spark plasma sintering, and the transition metal monoxide target material is obtained; a film grows on the transition metal monoxide target material, and the transition metal monoxide film is obtained. The transition metal monoxide powder, target material and film can be prepared rapidly at low temperature with the methods.

Description

technical field [0001] The method belongs to the field of synthesis preparation, and aims at preparing transition metal-oxide (such as titanium monoxide) pure-phase powder and target material at low temperature and rapidly. The synthesis method is a solid-phase flux method and discharge plasma sintering. It provides convenience for the study of electrical and magnetic applications of transition metal oxide powders. At the same time, transition metal oxide films are grown by magnetron sputtering or pulsed laser deposition using transition metal oxides as targets. , can be used to further explore and study the physical properties of transition metal oxides. Background technique [0002] By adjusting the band gap of titanium dioxide by experimental means, titanium dioxide can realize the full-spectrum response of sunlight, and its conductivity has been greatly improved, so it has a wide range of applications in energy, which makes researchers study different oxidation degrees o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G1/02
CPCC01G1/02C01P2002/72C01P2002/85C01P2004/03C01P2004/61C01P2004/62C01P2006/32C01P2006/80
Inventor 黄富强王东黄冲
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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