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Preparation method of pyrochlore type rare-earth titanate powder

A rare earth titanate, rare earth nitrate technology, applied in titanate, chemical instruments and methods, titanium compounds, etc., can solve the problem of affecting the stoichiometric ratio, difficult to control the sol gelation rate, and inability to achieve pure phase powder It can solve the problems of body preparation, etc., to achieve the effects of no industrial waste, prevention of precipitation, and high product purity.

Active Publication Date: 2018-08-24
XINYI DONGFANG SHUOHUA OPTICAL MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when using the sol-gel method to prepare titanate powder, it is difficult to control the gelation rate of the sol, and the ions cannot completely enter the network during the chemical reaction complexation process, which affects the stoichiometric ratio and cannot achieve a pure phase powder. preparation of

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1 prepares Dy 2 Ti 2 o 7

[0018] A preparation method of pyrochlore type rare earth titanate powder, comprising the following steps

[0019] (1) Weighing: According to the general chemical formula Dy 2 Ti 2 o 7 The stoichiometric ratio of each element in, respectively weighs 36.653g dysprosium nitrate (Dy(NO3)3.xH2O) and 28.422g titanium isopropoxide, wherein the purity of dysprosium nitrate is higher than 99.99%;

[0020] (2) Sol gelation: ① Dissolve the rare earth nitrate raw material in absolute ethanol at room temperature, the mass volume ratio of rare earth nitrate to absolute ethanol is 0.1mol: 1L, stir for 20min to obtain solution A; ② room temperature Next, add 1ml of acetylacetone and titanium isopropoxide to absolute ethanol at the same time, the mass volume ratio of acetylacetone to absolute ethanol is 0.1:1L, and the mass volume ratio of titanium isopropoxide to absolute ethanol is 0.05mol: 1L, stirred for 20min to obtain solution B; ③ mix...

Embodiment 2

[0025] Embodiment 2 prepares Sm 2 Ti 2 o 7

[0026] A preparation method of pyrochlore type rare earth titanate powder, comprising the following steps

[0027] (1) Weighing: according to the general chemical formula Sm 2 Ti 2 o 7 The stoichiometric ratio of each element in , respectively weighed 133.335g samarium nitrate (Sm(NO 3 ) 3 .6H 2 O) and 85.266g titanium isopropoxide, wherein the purity of dysprosium nitrate is higher than 99.99%;

[0028] (2) Sol gelation: ① Dissolve the rare earth nitrate raw material in absolute ethanol at room temperature, the mass volume ratio of rare earth nitrate to absolute ethanol is 0.3mol: 1L, stir for 25min to obtain solution A; ② room temperature Next, add acetylacetone and titanium isopropoxide to absolute ethanol at the same time, the mass volume ratio of acetylacetone to absolute ethanol is 0.15mol:1L, and the mass volume ratio of titanium isopropoxide to absolute alcohol is 0.1mol: 1 L, stirred for 25 minutes to obtain solut...

Embodiment 3

[0033] Embodiment 3 prepares Dy 2 Ti 2 o 7

[0034] A preparation method of pyrochlore type rare earth titanate powder, comprising the following steps

[0035] (1) Weighing: According to the general chemical formula Dy 2 Ti 2 o 7 The stoichiometric ratio of each element in, weigh 183.265g dysprosium nitrate (Dy(NO 3 ) 3 .xH 2 O) and 142.11g titanium isopropoxide, wherein the purity of dysprosium nitrate is higher than 99.99%;

[0036] (2) Sol gelation: ① Dissolve the rare earth nitrate raw material in absolute ethanol at room temperature, the mass volume ratio of rare earth nitrate to absolute ethanol is 0.5mol: 1L, stir for 30min to obtain solution A; ② room temperature Next, add 2ml of acetylacetone and titanium isopropoxide to absolute ethanol at the same time, the mass volume ratio of acetylacetone to absolute ethanol is 0.2mol:1L, the mass volume ratio of titanium isopropoxide to absolute ethanol is 0.15mol : 1L, stirred for 30min to obtain solution B; ③ mixed s...

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Abstract

The invention discloses a preparation method of pyrochlore type rare-earth titanate powder. The preparation method adopts a soft chemical sol-gel method to prepare and comprises the following specificsteps: (1) weighing rare-earth nitrate powder and alcoholate of titanium respectively according to a stoichiometric ratio; (2) dissolving the rare-earth nitrate raw material into absolute ethyl alcohol at room temperature to obtain a solution A; adding acetylacetone and the alcoholate of titanium into the absolute ethyl alcohol at the same time to obtain a solution B; mixing the solution A and the solution B to obtain transparent sol; dropwise adding a diluted nitric acid solution into the transparent sol under the condition that the temperature is 40 to 60 DEG C and continuously stirring; monitoring the pH (Potential of Hydrogen) value; stopping dropwise adding until the pH value is 4.0 to 5.0; standing for 15 to 30min to obtain transparent wet gel; (3) drying the wet gel for 12 to 24h under the condition that the temperature is 100 to 120 DEG C; grinding to obtain powder; (4) putting the powder into a muffle furnace; keeping heat for 2 to 4h under the condition that the temperatureis 750 to 850 DEG C, so as to obtain the pyrochlore type rare-earth titanate powder. The preparation method disclosed by the invention has the advantages of simple preparation technology and low energy consumption; the prepared powder has uniform chemical composition and high product purity.

Description

technical field [0001] The invention belongs to the field of optical materials, and relates to a rare earth titanate, in particular to a preparation method of a pyrochlore type rare earth titanate powder. Background technique [0002] Rare earth titanate (RE 2 Ti 2 o 7 ) is an important chemical product, which has a wide range of applications and researches in many fields such as photovoltaic devices, photocatalysts, water purification, and electrolytes. At present, the methods for synthesizing rare earth titanates mainly include high-temperature solid-phase synthesis, sol-gel method, ultrasonic spray pyrolysis, and pulsed laser deposition. Among them, the sol-gel method has always been popular as one of the most suitable techniques for synthesizing rare earth titanate powders. However, when using the sol-gel method to prepare titanate powder, it is difficult to control the gelation rate of the sol, and the ions cannot completely enter the network during the chemical rea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/00B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01G23/003C01P2004/32C01P2004/64
Inventor 张乐顾灵诚邵岑周天元高光珍王骋陈浩
Owner XINYI DONGFANG SHUOHUA OPTICAL MATERIALS CO LTD
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