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Preparation method for SLTON perovskite NOx powder

An oxynitride, perovskite-type technology, applied in chemical instruments and methods, calcium/strontium/barium compounds, tantalum compounds, etc., can solve the problems of limiting the production of SLTON powder, taking a long time, etc., to meet the requirements, preparation Low cost, good dispersion effect

Inactive Publication Date: 2014-10-01
BOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional solid-state reaction technology for preparing SLTON powder is time-consuming and requires high temperature conditions (see Rooke, J.; Weller, M. T., Synthesis and Characterization of Perovskite-Type Oxynitrides. Solid State Phenomena, 2003, 90-91: 417 -422), the reaction is usually carried out at 1000 ~ 1300 ° C, which limits the production of SLTON powder

Method used

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  • Preparation method for SLTON perovskite NOx powder
  • Preparation method for SLTON perovskite NOx powder
  • Preparation method for SLTON perovskite NOx powder

Examples

Experimental program
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Embodiment 1

[0030] Accurately weigh strontium nitrate, lanthanum nitrate, tantalum pentachloride and urea in a molar ratio of 1:1:2:10 and put them into methanol aqueous solution (volume ratio of alcohol to water: 1:1) to stir and dissolve for more than 30 minutes . The solution was dried at 90 °C for 4 h, put into a mortar and ground finely, and the grinding time was 30 minutes. Put the above mixture into a crucible and put it into a box-type resistance furnace for calcination reaction at a reaction temperature of 800 °C and a reaction time of 4 h. After the reaction, it was naturally cooled to room temperature, and the product was nitrided under an ammonia atmosphere. The nitriding temperature was 850 °C for 6 hours. After cooling, the SLTON powder was obtained. The purity of its products is not less than 99.8%, and the impurity content: carbon is less than 0.12%; chlorine is less than 0.04%.

Embodiment 2

[0032] Accurately weigh strontium nitrate, lanthanum nitrate, tantalum pentachloride and citric acid in a molar ratio of 1:1:2:20 and put them into methanol aqueous solution (volume ratio of alcohol to water: 1:1) to stir and dissolve for more than 30 minutes. minute. The solution was dried at 200 °C for 6 h, put into a mortar and ground finely, and the grinding time was 30 minutes. Put the above mixture into a crucible and put it into a box-type resistance furnace for calcination reaction at a reaction temperature of 800 °C and a reaction time of 4 h. After the reaction, it was naturally cooled to room temperature, and the product was nitrided under an ammonia atmosphere. The nitriding temperature was 900 °C for 7 hours. After cooling, the SLTON powder was obtained. The purity of its products is not less than 99.7%, and the impurity content: carbon is less than 0.15%; chlorine is less than 0.04%.

Embodiment 3

[0034] Accurately weigh strontium chloride, lanthanum chloride, tantalum pentachloride and citric acid in a molar ratio of 1:1:2:20 and put them into methanol aqueous solution (alcohol-water volume ratio 1:1) and stir to dissolve. more than 30 minutes. The solution was dried at 200 °C for 6 h, put into a mortar and ground finely, and the grinding time was 30 minutes. The above mixture was put into a crucible and put into a box-type resistance furnace for calcination reaction at a reaction temperature of 800 °C and a reaction time of 5 h. After the reaction, it was naturally cooled to room temperature, and the product was nitrided under an ammonia atmosphere. The nitriding temperature was 900 °C for 8 hours. After cooling, the SLTON powder was obtained. The purity of its products is not less than 99.6%, and the impurity content: carbon is less than 0.15%; chlorine is less than 0.09%.

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Abstract

The invention discloses a preparation method for SLTON perovskite-type NOx powder. The method comprises the following steps: completely resolving a soluble strontium salt, a soluble lanthanum salt, a soluble tantalum salt and a combustion adjuvant in a methanol-water mixed solution, drying the solution, carrying out grinding till the raw materials are completely mixed uniformly, carrying out high-temperature calcination to form a precursor, and conducting nitriding high-temperature processing on the precursor to obtain the target product, wherein the molar ratio of the soluble tantalum salt to the combustion adjuvant is 1 to (1 to 500); the soluble strontium salt is one or the mixture of strontium chloride and strontium nitrate; the soluble lanthanum salt is one or the mixture of lanthanum chloride and lanthanum nitrate; the soluble tantalum salt is one or the mixture of tantalum pentachloride and tantalum ethylate; the combustion adjuvant is one or the mixture of urea, oxalic acid, citric acid and hexamethylenetetramine. The method has the advantages that the product purity is high; the impurity content is low; suitability for batch production and the fields of ferroelectricity, photo-electricity, photocatalysis, fuel cells and the like is realized.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic non-metallic materials, and in particular relates to a preparation method of perovskite type nitrogen oxide powder. Background technique [0002] Perovskite-structured transition metal oxynitrides, such as niobium- and tantalum-based semiconductor materials, have received considerable attention in recent decades because of their attractive properties and potential applications. As a new type of high-efficiency photocatalyst, tantalum-based oxynitride has attracted more and more attention. Sr 0.5 La 0.5 TaO 1.5 N 1.5 (abbreviated as SLTON) is an important lead-free perovskite-type ferroelectric material. It is mainly used in the fields of photocatalysis, dyes and pigments, magnetoresistive materials and purifiers. Since SLTON is a photocatalyst that responds to the visible spectrum (wavelength greater than 500 nm), it has received increasing attention in recent years. The t...

Claims

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Application Information

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IPC IPC(8): C01G35/00C01F17/00C01F11/00C04B35/58
Inventor 许家胜张杰
Owner BOHAI UNIV
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