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Method for preparing rare earth titanate nanocrystalline with controllable size through self-propagating combustion

A technology of rare earth titanate and self-propagating combustion, which is applied in nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science. The effect of simplicity, short reaction time and simple equipment

Active Publication Date: 2013-10-02
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods have disadvantages such as complex process, high equipment requirements, small output, high cost and time-consuming.

Method used

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  • Method for preparing rare earth titanate nanocrystalline with controllable size through self-propagating combustion
  • Method for preparing rare earth titanate nanocrystalline with controllable size through self-propagating combustion
  • Method for preparing rare earth titanate nanocrystalline with controllable size through self-propagating combustion

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Add 10ml of tetrabutyl titanate to 20ml of water, stir to hydrolyze tetrabutyl titanate to obtain white precipitated titanium oxyhydroxide, add 4.5ml of 16mol L -1 The nitric acid solution completely dissolves the precipitate to obtain titanyl nitrate.

[0018] (2) Mix the above-mentioned titanyl nitrate solution, 12.827 g of neodymium nitrate and 4.393 g of glycine according to the molar ratio of 1:1:2, and then put them in an evaporating dish, place the evaporating dish on a magnetic stirrer and heat while stirring, magnetic The surface temperature of the stirrer is 250° C., the speed of magnetic stirring is 2500 rpm, and the liquid is volatilized under stirring.

[0019] (3) Stop stirring when sparks appear, sparks spread and burn rapidly, and finally get fluffy powder neodymium titanate (Nd 2 Ti 2 o 7 ), with an average grain size of about 28 nm.

[0020] Neodymium titanate (Nd 2 Ti 2 o 7 ) X-ray diffraction, SEM and TEM images are shown in Fig. 1, Fig. 2...

Embodiment 2

[0022] (1) Add 10ml of tetrabutyl titanate to 20ml of water, stir to hydrolyze tetrabutyl titanate to obtain white precipitated titanium oxyhydroxide, add 4.5ml of 16mol L -1 The nitric acid solution completely dissolves the precipitate to obtain titanyl nitrate.

[0023] (2) Mix the above-mentioned titanyl nitrate solution, 12.827 g of neodymium nitrate and 6.590 g of glycine according to the molar ratio of 1:1:3 and place them in an evaporating dish, place the evaporating dish on a magnetic stirrer and heat while stirring. The surface temperature of the stirrer is 350° C., the speed of magnetic stirring is 2500 rpm, and the liquid is volatilized under stirring.

[0024] (3) Stop stirring when sparks appear, sparks spread and burn rapidly, and finally get fluffy powder neodymium titanate (Nd 2 Ti 2 o 7 ), with an average grain size of about 41 nm.

Embodiment 3

[0026] (1) Add 5ml of tetraisopropyl titanate to 5ml of water, stir to hydrolyze tetraisopropyl titanate to obtain white precipitated titanium oxyhydroxide, add 5ml of 8mol·L -1 The nitric acid solution completely dissolves the precipitate to obtain titanyl nitrate.

[0027] (2) Mix the above-mentioned titanyl nitrate solution, 7.574 g of gadolinium nitrate and 3.149 g of aminoacetic acid according to the molar ratio of 1:1:2.5, and then place them in an evaporating dish, place the evaporating dish on a magnetic stirrer and heat while stirring. The surface temperature of the stirrer is 300° C., the speed of magnetic stirring is 2000 rpm, and the liquid is volatilized under stirring.

[0028] (3) Stop stirring when sparks appear, sparks spread and burn rapidly, and finally get fluffy powder gadolinium titanate (Gd 2 Ti 2 o 7 ), with an average grain size of about 40 nm.

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Abstract

The invention discloses a method for preparing rare earth titanate nanocrystalline with the controllable size through self-propagating combustion. The method comprises the following steps of: hydrolyzing titanic alkoxide to obtain oxygen titanium hydroxide, and dissolving the oxygen titanium hydroxide in a salpeter solution to obtain nitric acid oxygen titanium; placing rare earth nitrate, the nitric acid oxygen titanium and glycine in an evaporating dish, and placing the evaporating dish on a magnetic stirring apparatus so as to volatilize liquid; continuously heating under the stirring condition, stopping stirring when sparkle occurs, wherein the sparkle rapidly spread and burns, and obtaining fluffy rare earth titanate powder on the evaporating dish in the end. According to the method, the glycine is taken as a fuel and is subjected to self-propagating combustion by using heat generated by the oxidation-reduction reaction happening between the rare earth metal titanate and the glycine, so that the rare earth titanate nanocrystalline is rapidly synthesized. The regulation and control of crystalline size of the rare earth titanate can be realized by adjusting and controlling the molar ratio of nitrate ions to the glycine. The method disclosed by the invention has the advantages of being short in reaction time, simple in technology and environment-friendly; equipment is simple; and the production cycle is short.

Description

technical field [0001] The invention relates to the technical field of preparing nanocrystals, in particular to a method for preparing size-controllable rare earth titanate nanocrystals by a self-propagating combustion method. Background technique [0002] Rare earth titanates are important chemical products and have been widely used and researched in many fields such as photocatalysis, optics, energy storage, ferroelectricity and magnetism. At present, the methods for synthesizing rare earth titanates mainly include high-temperature solid-phase synthesis, sol-gel method, polymerization complexation method, and pulsed laser deposition. However, these methods have disadvantages such as complex process, high equipment requirements, small output, high cost and time-consuming. Therefore, it is necessary to develop an economical and practical technology to synthesize rare earth titanates. [0003] The self-propagating combustion method is a new method for rapidly synthesizing c...

Claims

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Application Information

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IPC IPC(8): C01G23/00B82Y30/00
Inventor 薛珲陈庆华钱庆荣朱兰瑾黄宝铨刘欣萍唐澍芬
Owner FUJIAN NORMAL UNIV
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