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Supercell structure directly developed nano-grade beta-Li2TiO3 powder supercritical preparation method

A nano-scale, supercritical technology, applied in the fields of nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, can solve the problems of long preparation cycle, destruction of supercellular structure, complicated operation, etc., and achieve preparation cycle time. Short, lower activation barrier, uniform distribution effect

Active Publication Date: 2015-08-26
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method introduces K + Impurities, and need later calcination to powder, destroy β-Li 2 TiO 3 Supercellular structure with long preparation cycle and complex operation

Method used

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  • Supercell structure directly developed nano-grade beta-Li2TiO3 powder supercritical preparation method
  • Supercell structure directly developed nano-grade beta-Li2TiO3 powder supercritical preparation method

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preparation example Construction

[0044] A Nanoscale β-Li Directly Developed by a Supercellular Structure 2 TiO 3 The supercritical preparation method of powder comprises the following steps:

[0045] 1) Weigh TiO according to the molar ratio of Li:Ti (1.85~2.25):1 2 powder and LiOH·H 2 O powder, put the two into the high-pressure container (the material is Hastelloy, the pressure range is 50-200MPa), and then add distilled water to the high-pressure container according to the volume ratio of distilled water accounting for 20%-80% of the volume of the high-pressure container, and mix Uniform, and control Li + The concentration is 0.1~2mol / L;

[0046] 2) Put the high-pressure container in a high-temperature drying oven, and react at 375-450°C for 5-20 hours;

[0047] 3) Place the high-pressure container in an oven, and dry at 50-80°C for 8-12 hours to obtain β-Li 2 TiO 3 Powder;

[0048] 4) the β-Li obtained in step 3) 2 TiO 3 The powder is ground evenly to obtain nano-sized β-Li 2 TiO 3 Powder.

Embodiment 1

[0051] 1) Weigh TiO according to the molar ratio of Li:Ti of 1.90:1 2 powder and LiOH·H 2 O powder, add the two into a high-pressure vessel (the material is Hastelloy, and the pressure range is 50-200MPa), then add distilled water to the high-pressure vessel according to the volume ratio that distilled water accounts for 50% of the volume of the high-pressure vessel, mix evenly, and Control Li + The concentration is 1mol / L;

[0052] 2) Put the high-pressure container in a high-temperature drying oven and react at 400°C for 10 hours;

[0053] 3) Put the high-pressure container in an oven and dry at 80°C for 10 hours to obtain β-Li 2 TiO 3 Powder;

[0054] 4) the β-Li obtained in step 3) 2 TiO 3 The powder is ground evenly to obtain nano-sized β-Li 2 TiO 3 Powder.

[0055] figure 1 It is the nanoscale β-Li prepared in this embodiment 2 TiO 3 The XRD pattern of the powder shows that supercells have begun to develop, The value is 0.22.

Embodiment 2

[0057] 1) Weigh TiO according to the molar ratio of Li:Ti of 2.15:1 2 powder and LiOH·H 2 O powder, add the two into a high-pressure vessel (the material is Hastelloy, and the pressure range is 50-200MPa), then add distilled water to the high-pressure vessel according to the volume ratio that distilled water accounts for 40% of the volume of the high-pressure vessel, mix evenly, and Control Li + The concentration is 0.5mol / L;

[0058] 2) Place the high-pressure container in a high-temperature drying oven and react at 380°C for 10 hours;

[0059] 3) Place the high-pressure container in an oven and dry at 70°C for 12 hours to obtain β-Li 2 TiO 3 Powder;

[0060] 4) the β-Li obtained in step 3) 2 TiO 3 The powder is ground evenly to obtain nano-sized β-Li 2 TiO 3 Powder.

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Abstract

The invention discloses a supercell structure directly developed nano-grade beta-Li2TiO3 powder supercritical preparation method. The method comprises the following steps: (1) TiO2 powder and LiOH.H2O Powder are weighed according to a molar ratio that Li:Ti is (1.85-2.25):1; the two are added into a high-pressure container; distilled water is added into the high-pressure container; and the mixture is well mixed, wherein the concentration of Li<+> is controlled to be 0.1-2mol / L; (2) the high-pressure container is placed in a high-temperature drying box, and a sufficient reaction is carried out under a temperature of 375-450 DEG C; (3) the high-pressure container is placed in a baking oven, and drying is carried out, such that beta-Li2TiO3 powder is obtained; and (4) the beta-Li2TiO3 powder obtained in the step (3) is uniformly ground, such that the nano-grade beta-Li2TiO3 powder is obtained. The preparation method provided by the invention has the advantage of simple operation. The prepared beta-Li2TiO3 powder has high atomic ordering degree and good supercell structure development.

Description

technical field [0001] The invention belongs to the field of functional material powder prepared by supercritical hydrothermochemical method, and specifically relates to a nano-scale β-Li with supercellular structure directly developed 2 TiO 3 Supercritical preparation method of powder. Background technique [0002] Lithium metatitanate (β-Li 2 TiO 3 ) as one of the most potential solid-state tritium breeder materials has received extensive attention. β-Li 2 TiO 3 The excellent tritium release performance and low activation characteristics benefit from its well-developed supercellular structure and its high stability. At present, the preparation of nanoscale β-Li 2 TiO 3 Powder methods include solid phase method, wet chemical method and so on. The crystallinity of the powder prepared by the solid phase method is poor. The general wet chemical method requires later calcination, and the obtained powder has poor development of supercells. Other methods also have prob...

Claims

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Application Information

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IPC IPC(8): C01G23/00B82Y30/00
CPCY02P20/54
Inventor 于成龙王斐郝欣王秀峰曹舒尧高丹鹏崔云王道益沈清李嘉胤贾钦相宁青菊江红涛王莉丽
Owner SHAANXI UNIV OF SCI & TECH
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