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Wet chemical method for preparing beta-Li2TiO3 pellets

A wet chemical method and small ball technology, applied in the field of wet chemical preparation of β-Li2TiO3 small balls, can solve the problems of failing to guarantee the sphericity and relative density of the small balls, and achieve convenient recycling and reproduction, good supercell development, good shape regular effect

Active Publication Date: 2015-07-22
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method uses the powder coating method to prepare ceramic microspheres with a diameter of 0.2-3 mm, but the sphericity and relative density of the balls cannot be guaranteed.

Method used

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  • Wet chemical method for preparing beta-Li2TiO3 pellets
  • Wet chemical method for preparing beta-Li2TiO3 pellets
  • Wet chemical method for preparing beta-Li2TiO3 pellets

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preparation example Construction

[0039] A β-Li 2 TiO 3 The preparation method of bead, comprises the following steps:

[0040] 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 a high-pressure vessel, the material of the high-pressure vessel is polytetrafluoroethylene, Hastelloy or stainless steel, the pressure range is 2-100MPa, and then according to distilled water accounts for 10-80% of the volume of the high-pressure vessel Volume ratio Add distilled water to the high-pressure vessel, mix well, and control the Li + The concentration is 0.1~2mol / L;

[0041] 2) Put the high-pressure container in step 1) in an oven, perform hydrothermal reaction at 100-180°C for 20-30 hours, and then dry at 40-80°C for 30-50 hours to obtain β-Li 2 TiO 3 The hydrothermal precursor;

[0042] 3) the β-Li obtained in step 2) 2 TiO 3 β-Li 2 TiO 3 Powder;

[0043] 4) Utilize H with a mass fraction of 10% to 50% 2 o 2 Aqueous solution dissolving step 3) o...

Embodiment 1

[0051] 1) Weigh TiO according to the molar ratio of Li:Ti of 1.85:1 2 powder and LiOH·H 2 O powder, put the two into a high-pressure container, the material of the high-pressure container is polytetrafluoroethylene, Hastelloy or stainless steel, the pressure range is 2-100MPa, and then the volume ratio of distilled water to the volume of the high-pressure container is 30%. Add distilled water to the high-pressure vessel, mix well, and control the Li + The concentration is 0.5mol / L;

[0052] 2) Put the high-pressure container of step 1) in an oven, and after hydrothermal reaction at 100°C for 20h, dry at 60°C for 30h to obtain β-Li 2 TiO 3 The hydrothermal precursor;

[0053] 3) the β-Li obtained in step 2) 2 TiO 3 β-Li 2 TiO 3 Powder;

[0054] 4) Utilize the H that the mass fraction is 40% 2 o 2 Aqueous solution dissolving step 3) obtained β-Li 2 TiO 3 Powder, wherein, every 1.5mLH 2 o 2 Dissolve 1.5g β-Li in aqueous solution 2 TiO 3 Powder, then add chelating...

Embodiment 2

[0062] 1) Weigh TiO according to the molar ratio of Li:Ti of 1.95:1 2 powder and LiOH·H 2 O powder, add the two into a high-pressure vessel, the material of the high-pressure vessel is polytetrafluoroethylene, Hastelloy or stainless steel, the pressure range is 2-100MPa, and then the volume ratio of distilled water to 60% of the volume of the high-pressure vessel Add distilled water to the high-pressure vessel, mix well, and control the Li + The concentration is 1.2mol / L;

[0063] 2) Place the high-pressure container in step 1) in an oven, and after hydrothermal reaction at 120°C for 25h, dry at 50°C for 35h to obtain β-Li 2 TiO 3 The hydrothermal precursor;

[0064] 3) the β-Li obtained in step 2) 2 TiO 3 β-Li 2 TiO 3 Powder;

[0065] 4) Utilize the H that mass fraction is 30% 2 o 2 Aqueous solution dissolving step 3) obtained β-Li 2 TiO 3 Powder, where, every 2mLH 2 o 2 Dissolve 1g β-Li in aqueous solution 2 TiO 3 powder, and then add a chelating agent and a...

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Abstract

The invention discloses a wet chemical method for preparing beta-Li2TiO3 pellets. The wet chemical method comprises the following steps: 1, taking TiO2 powder, LiOH.H2O powder and distilled water and placing the TiO2 powder, the LiOH.H2O powder and the distilled water in a high pressure container to uniformly mix; 2, after performing the hydrothermal reaction, drying to obtain a beta-Li2TiO3 hydrothermal precursor; 3, after uniformly grinding the beta-Li2TiO3 hydrothermal precursor, sintering to form beta-Li2TiO3 powder; 4, dissolving the beta-Li2TiO3 powder by utilizing H2O2 aqueous solution and then adding a chelating agent and an additive to prepare suspension; 5, placing the suspension into a water bath to carry out heating and concentration; 6, dropwise adding concentrated slurry into a mixed gel bath of acetone and carbon tetrachloride at room temperature so as to form wet gel pellets; 7, placing the wet gel pellets at room temperature to enable the wet gel pellets to be sufficiently cured; 8, drying the cured gel pellets to obtain dry gel pellets; 9, after placing the dry gel pellets in a heating device for heating, carrying out heat preservation to obtain the beta-Li2TiO3 pellets. The beta-Li2TiO3 pellets prepared according to the method disclosed by the invention are regular in morphology, have a good degree of sphericity and small particle sizes, are uniformly distributed and have high phase purity.

Description

technical field [0001] The invention belongs to the technical field of indirect wet method preparation of pellets for tritium proliferation, in particular to a method for preparing β-Li 2 TiO 3 Wet chemistry method for pellets. Background technique [0002] Lithium metatitanate (β-Li 2 TiO 3 ) because of its considerable lithium atom density, high chemical stability and thermal conductivity, low tritium solubility, good compatibility with structural materials, and excellent tritium release performance and low activation characteristics at low temperatures, it is regarded as It is one of the most promising candidates for solid-state tritium breeders. At present, many different β-Li have been reported 2 TiO 3 Preparation method of pellets. For example, X.W.Wu et al. published an indirect wet method to prepare β-Li 2 TiO 3 Ball article. In citric acid and Li 2 TiO 3 Under the conditions of powder molar ratio of 1:1 and sintering at 1050°C for 6 hours, Li with a diam...

Claims

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Application Information

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IPC IPC(8): C01G23/00
Inventor 于成龙王斐郝欣张艾琳宋双王道益曹舒尧沈清
Owner SHAANXI UNIV OF SCI & TECH
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