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Preparation method of high-dispersion zirconium oxide nano powder

A technology of nano-powder and zirconia, which is applied in zirconia, nano-structure manufacturing, nano-technology, etc., can solve problems such as low surface tension, high cost of organic solvents, and large investment in equipment, so as to improve powder dispersion and facilitate The effect of industrialized production and less investment in equipment

Inactive Publication Date: 2010-10-06
SHANDONG UNIV OF TECH
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to reduce the agglomeration of nanoparticles, in the titration process: people try to add some surfactants or other organic substances in the reaction system, so that they can control the reaction nucleation process on the one hand; On the particle, it can enhance the steric hindrance effect between the particles and improve the dispersion performance of the particles, but the effect is not good
In the washing process: wash the precipitated precursor with absolute ethanol or other organic solvents, replace the surface adsorbed water with ethoxy groups or other organic functional groups, and reduce the hard agglomeration of the colloidal particles due to the bridging effect of hydroxyl groups; at the same time, due to the organic solvent With a lower surface tension, it will also reduce the capillary force generated during the dehydration process, reduce the bonding strength between particles, and reduce the generation of aggregates, but the effect is not good, and it can only be dispersed by using a special process during the drying process good nano powder
In the drying process: the use of supercritical drying, vacuum freeze drying and azeotropic distillation processes can better eliminate agglomeration, but supercritical drying and vacuum freeze drying have high requirements for equipment, and the equipment investment is large. The production efficiency is affected by the size of the equipment box. Low; azeotropic distillation uses organic solvents, the cost is high, and the efficiency is low due to the influence of the volume of distillation equipment

Method used

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  • Preparation method of high-dispersion zirconium oxide nano powder
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  • Preparation method of high-dispersion zirconium oxide nano powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] (1) 3.2g of ZrOCl 2 ·8H 2 O is dissolved in the water of 100ml and is configured into 0.1mol / L zirconium oxychloride solution, under stirring condition, 0.2mol / L sodium borohydride solution is titrated in the zirconium oxychloride solution, generates gel, then gel is used Deionized water was suction-filtered and washed several times until the lotion was neutral to obtain 12g of gel; (2) 12g of camphene was added to the gel, and mixed by ball milling at 50°C to form a slurry; (3) at room temperature After solidification and molding, the solidified slurry is left in the air environment at room temperature for 7 days. After the camphene is completely volatilized, it is placed in a sintering furnace and calcined at 700°C to obtain highly dispersed zirconia nanopowder.

[0017] Through XRD test, it can be seen that the powder crystal type is monoclinic phase; through SEM test, it can be seen that the particle size of zirconia nano powder is about 40nm, without hard agglomer...

Embodiment 2

[0019] (1) 4.3g of Zr(NO 3 ) 4 ·5H 2 O is dissolved in 100ml of water to form a 0.1mol / L zirconium nitrate solution. Under agitation, titrate a 0.5mol / L sodium borohydride solution into the zirconium nitrate solution to form a gel, and then extract the gel with deionized water. Filter and wash several times until the lotion is neutral to obtain 20g of gel; (2) add 20g of camphene to the gel, and mix it by ball milling at 50°C to form a slurry; (3) solidify and form at room temperature, and The solidified slurry is placed in the air environment at room temperature for 7 days, and after the camphene is completely volatilized, it is placed in a sintering furnace and calcined at 700°C to obtain highly dispersed zirconia nanopowder.

Embodiment 3

[0021] (1) 9.6g of ZrOCl 2 ·8H 2 O is dissolved in 100ml of water to form a 0.3mol / L zirconium oxychloride solution. Under stirring conditions, titrate 1mol / L ammonium carbonate solution into the zirconium oxychloride solution to form a gel, and then deionize the gel Water was filtered and washed several times until the lotion was neutral, and 45 g of gel was obtained; (2) 90 g of camphene was added to the gel, and mixed by ball milling at 60 ° C to form a slurry; (3) solidified at room temperature , put the solidified slurry in the air environment at room temperature for 7 days, after the camphene is completely volatilized, put it in a sintering furnace, and calcined at 800 ° C to obtain highly dispersed zirconia nanopowder.

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Abstract

The invention provides a preparation method of high-dispersion zirconium oxide nano powder, which belongs to the technical field of nano material preparation. The preparation method is characterized by comprising the following steps of: (1) titrating a precipitating agent into a zirconium salt solution while stirring to produce gel, and then, suction filtering and washing the gel with ion water for several times until the washing solution becomes neutral; (2) adding camphene into the gel, and ball milling to form a slurry at the temperature of 50-70 DEG C; (3) concreting and shaping the slurry at room temperature, placing the concreted slurry in an air environment at room temperature for 7-10 days, placing the slurry in a sintering furnace after the camphene completely volatilizes, and calcining at 700-900 DEG C to obtain the high-dispersion zirconium oxide nano powder. The zirconium oxide nano powder obtained by the invention has good dispersion, no hard agglomeration, granules smaller than 50 nm, simple process, safe operation, low cost and easy industrialization.

Description

technical field [0001] The invention provides a preparation method of highly dispersed zirconia nano powder, which belongs to the technical field of nano material preparation. Background technique [0002] There are many methods for preparing zirconia nanopowders, including gas-phase method and liquid-phase method. The liquid-phase chemical method has a stronger competitive advantage, because the industrial process control and equipment amplification technology related to this method have already been developed. More mature and lower cost. Liquid-phase methods include sol-gel method, alcohol salt hydrolysis method, hydrothermal method, emulsion method and co-precipitation method, etc. Among them, sol-gel method is a method that is particularly valued in liquid-phase wet chemical method. The advantages of low temperature, simple process and easy control are an effective method for industrial production. However, serious agglomeration will occur during the preparation proces...

Claims

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Application Information

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IPC IPC(8): C01G25/02B82B3/00
Inventor 魏春城牛金叶孟凡涛田贵山周立娟
Owner SHANDONG UNIV OF TECH
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