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Synthesizing nano crystal cobalt aluminium spinelle pigment by using solution combustion method

A technology of solution combustion and nanocrystals, applied in the direction of fibrous fillers, dyeing physical treatment, etc., can solve the problems of long time required for the synthesis process and complicated process, and achieve the effects of narrow particle size distribution, simple reaction process and simple equipment

Inactive Publication Date: 2009-08-05
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the above methods can prepare nanocrystalline CoAl 2 o 4 , but the common disadvantage is that the process is relatively complicated and the synthesis process takes a long time
However, there is no low-temperature solution combustion method to synthesize nanocrystalline CoAl 2 o 4 report

Method used

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  • Synthesizing nano crystal cobalt aluminium spinelle pigment by using solution combustion method
  • Synthesizing nano crystal cobalt aluminium spinelle pigment by using solution combustion method
  • Synthesizing nano crystal cobalt aluminium spinelle pigment by using solution combustion method

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Use aluminum nitrate, cobalt acetate and citric acid as raw materials, according to Co 2+ :Al 3+ : citric acid molar ratio = 1:2:2 ingredients, the method is as follows: respectively dissolve aluminum nitrate, cobalt acetate and citric acid in deionized water to make a solution, stir continuously after mixing, adjust the pH to 7 with ammonia water, and stir fully Afterwards, heat in a microwave cavity. The microwave frequency is 2.45GHz, and the input power is 500W. As the water vapor evaporates, the solution concentrates, forming a gel. When reaching a certain temperature, the gel ignites and spontaneously burns for about 5 minutes, and a fluffy foamy powder is obtained. The above powder was heat-treated in air at 700°C for 2 hours to obtain the final product, whose XRD pattern is as follows: figure 2 , TEM photo as Figure 5 . CoAl 2 o 4 The average particle size of the powder (calculated by the Scherrer equation) is 19nm, and the specific surface area is 59m...

Embodiment 2

[0027] Use aluminum sulfate, cobalt nitrate and citric acid as raw materials, according to Co 2+ :Al 3+: citric acid molar ratio = 1:2:3 ingredients, the method is as follows: respectively dissolve aluminum sulfate, cobalt nitrate and citric acid in deionized water to make a solution, stir continuously after mixing, adjust the pH to 7 with ammonia water, and stir thoroughly Afterwards, heat on an electric stove. As the water evaporates, a gel is formed. Then put the gel in a muffle furnace. When the temperature reaches 300°C, the gel will ignite and spontaneously burn for about 15 minutes, and a fluffy foamy powder will be obtained. The above powder was heat-treated in air at 900°C for 1 hour to obtain the final product, whose XRD pattern is as follows: image 3 , TEM photo as Image 6 . Obtained CoAl 2 o 4 The average particle size of the powder (calculated by the Scherrer equation) is 31nm and the specific surface area is 43m 2 / g.

Embodiment 3

[0029] Use aluminum nitrate, cobalt nitrate, and urea as raw materials, according to Co 2+ :Al 3+ : urea molar ratio=1:2:10 ingredients, the method is as follows: respectively dissolve aluminum nitrate, cobalt nitrate, and urea in deionized water to make a solution, stir continuously after mixing, and heat in a microwave cavity. The microwave frequency is 2.45GHz, and the input power is 500W. As the water vapor evaporates, the solution concentrates, forming a gel. When reaching a certain temperature, the gel ignites and burns spontaneously for about 2 minutes, and a fluffy foamy powder is obtained. The above powder was heat treated in air at 500°C for 3 hours to obtain the final product, whose XRD pattern is as follows: Figure 4 , TEM photo as Figure 7 . Obtained CoAl 2 o 4 The average particle size of the powder (calculated by the Scherrer equation) is 42nm and the specific surface area is 37m 2 / g.

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Abstract

The invention discloses a method for preparing nanocrystalline cobalt-aluminum spinel (CoAl2O4) pigments through low-temperature combustion, which belongs to the field of nanocrystalline pigment preparation. The present invention is with soluble aluminum salt (aluminum nitrate, aluminum acetate, aluminum sulfate), soluble cobalt salt (cobalt nitrate, cobalt acetate, cobalt sulfate), citric acid or urea as starting material, Co2+: Al3+: citric acid three The mixing molar ratio is 1:(2-3):(1-6), or the mixing molar ratio of Co2+:Al3+:urea is 1:(2-3):(3-15). The solutions are mixed to form a complex, and citric acid or urea is used as a complexing agent and also as a fuel. The mixed solution is ignited by electric heating or microwave heating to obtain a fluffy powder, and then heat-treated at 500-1000°C to obtain nanocrystalline CoAl2O4 with a particle size of 10-100nm. The present invention is characterized in that the technological process is simple and efficient, and the combustion process is completed within 15 minutes. The process is low in energy consumption, easy to operate, and suitable for large-scale industrial production.

Description

technical field [0001] The present invention relates to nanocrystalline CoAl 2 o 4 Synthetic method of powder, especially the synthesis of nanocrystalline CoAl by electric heating or microwave heating to induce solution combustion 2 o 4 The method belongs to the field of nanocrystalline pigment preparation. Background technique [0002] CoAl with spinel structure 2 o 4 Blue pigment has excellent thermal stability and chemical stability, has been widely used in the coloring (P.A.Lewis, Pigment handbook, John Wiley and Sons, New York, Vol. 1, 1998). CoAl 2 o 4 The traditional preparation method of spinel is a solid-state reaction method, generally using cobalt carbonate and alumina as raw materials, mixing the two according to a certain ratio, ball milling, and then calcining at a high temperature of ~ 1300 ° C, and further crushing to achieve Specifies the granularity. Since the solid-state reaction requires long-distance diffusion of metal ions to complete, the rea...

Claims

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Application Information

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IPC IPC(8): C09C3/04C09C1/40
Inventor 李伟东李家治郭景坤
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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