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Nitridation synthesis of nitrogen oxide material SmTiO2N and application of nitrogen oxide material SmTiO2N in field of photocatalysis

A nitrogen oxide, photocatalytic technology, applied in hydrogen/syngas production, physical/chemical process catalyst, chemical/physical process, etc., can solve problems such as nitriding synthesis, and achieve the effect of low temperature and shortened nitriding time

Active Publication Date: 2021-02-19
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Nitride SmTiO for post-lanthanide Sm 2 The problem that N cannot be synthesized by nitriding by traditional methods, the present invention aims to develop a new nitriding process, using alkali metal salts of composite metals instead of composite metal oxides as nitriding precursors, and nitriding through a suitable ammonia flow atmosphere, Realize rapid and low temperature synthesis of SmTiO 2 The preparation route of N

Method used

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  • Nitridation synthesis of nitrogen oxide material SmTiO2N and application of nitrogen oxide material SmTiO2N in field of photocatalysis
  • Nitridation synthesis of nitrogen oxide material SmTiO2N and application of nitrogen oxide material SmTiO2N in field of photocatalysis
  • Nitridation synthesis of nitrogen oxide material SmTiO2N and application of nitrogen oxide material SmTiO2N in field of photocatalysis

Examples

Experimental program
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Effect test

Embodiment 1

[0048] (1) Synthesis of composite bimetallic sodium salt NaSmTiO by solid phase method 4 (Concrete method reference: Journal of SolidState Chemistry 161,225~232 (2001)), the NaSmTiO that adopts excessive deionized water to wash synthesis 4 Until the washing liquid is neutral, dry the solid sample NaSmTiO 4 Synthesized as SmTiO 2 Precursor of N;

[0049] (2) Take 0.5gNaSmTiO 4 In the quartz hanging basket, place the quartz hanging basket on the air flow baffle in the center of the quartz tube, seal the quartz tube and connect the NH 3 piping;

[0050] (3) Turn on NH 3 , the flow rate is 100ml / min, purging at room temperature for 30min, then heating up to 950℃ at 2℃ / min, nitriding at a constant temperature of 950℃ for 6h, and taking it out after cooling down to room temperature naturally after nitriding;

[0051] (4) Disperse the obtained powder in 20 mL of nitric acid with a concentration of 1 mol / L, stir for 30 minutes, centrifuge the powder sample and wash it with water...

Embodiment 2

[0053] (1) Synthesis of composite bimetallic sodium salt NaSmTiO by solid phase method 4 (Concrete method reference: Journal of SolidState Chemistry 161,225~232 (2001)), the NaSmTiO that adopts excessive deionized water to wash synthesis 4 Until the washing liquid is neutral, dry the solid sample NaSmTiO 4 Synthesized as SmTiO 2 Precursor of N;

[0054] (2) Take 0.5g NaSmTiO 4 In the corundum porcelain boat, place the corundum porcelain boat in the center of the horizontal tube furnace, seal and connect the NH 3 piping;

[0055] (3) Turn on NH 3 , the flow rate is 200ml / min, after purging at room temperature, the temperature is raised to 850°C at 5°C / min, and the constant temperature is 850°C for nitriding for 8 hours. After the nitriding is completed, the temperature is naturally lowered. Take out the powder after reaching room temperature;

[0056] (4) Disperse the obtained powder in 20 mL of aqua regia (concentrated hydrochloric acid mixed with concentrated nitric ac...

Embodiment 3

[0058] (1) Synthesis of composite bimetallic sodium salt NaSmTiO by solid phase method 4 (Concrete method reference: Journal of SolidState Chemistry 161,225~232 (2001)), the NaSmTiO that adopts excessive deionized water to wash synthesis 4 Until the washing liquid is neutral, dry the solid sample NaSmTiO 4 Synthesized as SmTiO 2 Precursor of N;

[0059] (2) Take 0.5gNaSmTiO 4 In the quartz hanging basket, place the quartz hanging basket on the air flow baffle in the center of the quartz tube, seal the quartz tube and connect the NH 3 piping;

[0060] (3) Turn on NH 3 , the flow rate is 400ml / min, purging at room temperature for 30min, then heating up to 800℃ at 1℃ / min, constant temperature nitriding for 20h, after nitriding, naturally cool down to room temperature and take out;

[0061] (4) Disperse the obtained powder in 20 mL of aqua regia, stir for 2 hours, centrifuge the powder sample and wash it with water, and then dry it to obtain the pure phase of SmTiO 2 N powd...

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Abstract

The invention belongs to the field of preparation of novel nitrogen oxide materials, and discloses a method for synthesizing a samarium and titanium perovskite structure nitrogen oxide new material byusing alkali metal salt of composite metal as a nitridation precursor. The alkali metal salt of the composite bimetal adopted by the method is described as MSmTiO4 (M=Li, Na, K) by a chemical formula, and the alkali metal salt can be quickly and massively synthesized in preparation by a solid-phase method. Nitriding is completed in a flowing bed with NH3, nitriding is conducted for 20-0.1 h at the high temperature ranging from 800 DEG C to 950 DEG C, and the corresponding nitrogen oxide SmTiO2N of the perovskite structure is generated. According to the method, the SmTiO2N is synthesized for the first time to form the nitrogen oxide material, the synthesized SmTiO2N is fine particle powder rich in pore channels, and the light absorption range is wide. The nitrogen oxide material SmTiO2N has remarkable photocatalytic activity when being applied to photocatalytic dye degradation, photocatalytic water decomposition hydrogen production and photocatalytic water decomposition oxygen production reactions.

Description

technical field [0001] The invention relates to the preparation and application of a perovskite structure nitrogen oxide samarium titanium nitrogen oxide semiconductor photocatalyst. Background technique [0002] AB(O, N) 3 Oxide-nitride materials have received extensive attention due to their novel optical, electrical, magnetic, and photocatalytic properties. This type of nitrogen oxide has a lower theoretical bandgap value (1.5-2.5eV) than oxides, and can catalyze the splitting of water in the visible light range (wavelength 400-800nm); at the same time, it has both metal oxides and nitrides. It has the advantages of good chemical stability and thermal stability. It is very stable in water and strong acid and strong alkali. It starts to decompose when it is above 600°C in the air and above 800°C in an inert atmosphere. Among them, the A-site elements of the perovskite structure are composed of lanthanide elements, and titanium elements are used as the B-site elements. In...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J35/10C02F1/30C01B3/04C02F101/30
CPCB01J27/24C02F1/30C01B3/042C02F2305/10C02F2101/308C01B2203/0277B01J35/60B01J35/39Y02E60/36
Inventor 章福祥鲍云锋祁育郭向阳
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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