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A kind of synthesis method of nano-ceramic and nano-carbide composite material

A technology of nano ceramics and composite materials, applied in the nano field, can solve the problems of easy loss of activity and difficulty in controlling the size of carbides, and achieve the effect of enhancing catalytic performance and increasing contact area

Active Publication Date: 2018-04-03
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the size of carbides obtained by all preparation methods is difficult to control, and the size is usually on the micron scale, and it is easy to lose activity in catalytic reactions
In addition, current researchers lack research on the influence of carbide size control on its catalytic performance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Accurately weigh 10.5g La(NO 3 ) 3 ·6H 2 O, 10g Cr(NO 3 ) 3 9H 2 O, 2g Y (NO 3 ) 3 ·6H 2 O, 12gZr(NO 3 ) 4 ·5H 2 O, add deionized water and stir until dissolved to obtain solution A;

[0023] (2) Weigh 16.5g of ethylenediaminetetraacetic acid, add deionized water and stir well until dissolved to obtain solution B;

[0024] (3) The above-mentioned solution B is slowly added to the solution A, and the pH value is adjusted to 2 with concentrated nitric acid, and the solution is slowly evaporated by heating;

[0025] (4) Pour it into an evaporating dish after heating and evaporating to form a sol, and use an electric furnace to heat and burn to form the primary powder of metal composite oxide;

[0026] (5) After calcining the primary powder at 500°C for 2 hours, nano-ceramic yttria-stabilized zirconia (YSZ) and chromium-containing oxide lanthanum chromate (LaCrO 3 ), and YSZ:LaCrO 3 Mass ratio 40:60;

[0027] (6) The calcined sample was crushed and sieved...

Embodiment 2

[0029] (1) Accurately weigh 4.2gLa(NO 3 ) 3 ·6H 2 O, 1.72g (NH 4 ) 6 Mo 7 o 24 4H 2 O, 3.26g Y (NO 3 ) 3 ·6H 2 O, 21.1gZr(NO 3 ) 4 · 5 H2O, add deionized water and stir until dissolved to obtain solution A;

[0030] (2) Weigh 31.5g of polyacrylic acid, add deionized water and stir until dissolved to obtain solution B;

[0031] (3) The above-mentioned solution B is slowly added to the solution A, and the pH value is adjusted to 2 with concentrated nitric acid, and the solution is slowly evaporated by heating;

[0032] (4) Pour it into an evaporating dish after heating and evaporating to form a sol, and use an electric furnace to heat and burn to form the primary powder of metal composite oxide;

[0033] (5) The primary powder was calcined at 800°C for 2 hours to obtain nano-ceramic yttria-stabilized zirconia (YSZ) and molybdenum-containing oxide lanthanum molybdate (La 2 Mo 2 o 9 ), and YSZ:La 2 Mo 2 o 9 Mass ratio 70:30;

[0034] (6) The calcined sample wa...

Embodiment 3

[0036] (1) Accurately weigh 4.24g (NH 4 ) 10 W 12 o 41 4H 2 O, 2.35g Y (NO 3 ) 3 ·6H 2 O, 14.9g Zr(NO 3 ) 4 ·5H 2 O, add deionized water and stir until dissolved to obtain solution A;

[0037] (2) Weigh 37.5g of ammonium citrate, add deionized water and stir until dissolved to obtain solution B;

[0038] (3) The above-mentioned solution B is slowly added to the solution A, and the pH value is adjusted to 3 with concentrated nitric acid, and the solution is slowly evaporated by heating;

[0039] (4) Pour it into an evaporating dish after heating and evaporating to form a sol, and use an electric furnace to heat and burn to form the primary powder of metal composite oxide;

[0040] (5) After calcining the primary powder at 700°C for 2 hours, nano-ceramic yttria-stabilized zirconia (YSZ) and tungsten oxide (WO 3 ), and YSZ:WO 3 Mass ratio 50:50;

[0041] (6) The calcined sample was crushed and sieved, and 200 mg of a 60-80 mesh sample was taken in a quartz reaction tu...

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Abstract

The invention discloses a synthesis method of nano ceramics and nano carbide composite materials. The specific steps include: weighing the metal salt, fully stirring and dissolving to obtain solution A; weighing the complexing agent and adding water and stirring and dissolving to obtain solution B; slowly adding solution B to solution A, continuing to stir and heating and evaporating the solution to form a sol; Pour the sol into an evaporating dish, heat and burn to obtain the primary powder of composite oxides containing tungsten, chromium and molybdenum, and then calcinate it at a temperature of 500-1000°C to obtain nano-ceramics and composite materials containing tungsten, chromium and molybdenum oxides; The temperature-programmed reduction process is carried out under the atmosphere, and kept for 1-50 hours, and then rapidly lowered to room temperature under the reducing atmosphere to obtain nano-ceramic and nano-carbide composite materials. This method can effectively stabilize carbides by adding nano ceramics, and can effectively control the size of carbides from several nanometers to hundreds of nanometers as the metal ratio is changed.

Description

technical field [0001] The invention belongs to the field of nanotechnology, and in particular relates to a synthesis method of nano ceramics and nano carbide composite materials. technical background [0002] Carbide is a kind of interstitial compound with metal-like properties, that is, smaller carbon atoms occupy the gaps in the densely packed layer of metal atoms, forming a simple crystal structure. Due to their unique electronic structure and surface properties, carbides can exhibit noble metal-like catalytic performance in catalytic reactions. Mainly used in hydrogenation / dehydrogenation reaction, hydrodesulfurization / hydrodenitrification reaction, ammonia synthesis and decomposition reaction energy (such as tungsten carbide, molybdenum carbide, etc.), it is an important research direction for people to study alternative precious metal materials; in addition, Carbide is also a kind of substance with high melting point and hardness, high thermal stability and mechanica...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/22
Inventor 程谟杰王鑫
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI