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Method for preparing metal cation modified cubic phase zirconia nanometer particles

A metal cation and phase zirconia technology, applied in zirconia and other directions, can solve problems such as increasing costs, and achieve the effects of low equipment requirements, high yield, and easy availability of varieties

Inactive Publication Date: 2009-01-07
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method works well, most of the modified metals can only choose expensive metals such as gold and platinum, which greatly increases the cost of preparation

Method used

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  • Method for preparing metal cation modified cubic phase zirconia nanometer particles
  • Method for preparing metal cation modified cubic phase zirconia nanometer particles
  • Method for preparing metal cation modified cubic phase zirconia nanometer particles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 1.6g of sodium hydroxide into a 50ml beaker containing 30ml of benzyl alcohol, and stir for about 4 hours until the sodium hydroxide is dispersed in the benzyl alcohol, and the solution is a viscous transparent colloid; then add 1.611g (5mmol ) ZrOCl 2 ·8H 2Slowly add O to the above transparent colloid, stir until ZrOCl 2 ·8H 2 O was also dispersed in the colloid, and then 5ml of oleic acid was added dropwise to the above mixture, and the mixture was a yellow viscous solid at this time. After stirring vigorously for 3 hours, the reactant was transferred to a 50 ml stainless steel reaction kettle with a polytetrafluoroethylene liner, sealed well, and placed in a constant temperature oven at 160° C. for 24 hours. When the reaction kettle is naturally cooled to room temperature, take the white solid in the bottom layer of the kettle, put it in a 40ml centrifuge tube, add 30ml of pure water, centrifuge at a speed of 7000r / min for 5 minutes, wash repeatedly 7 to 8 tim...

Embodiment 2

[0029] Add 2.807g of potassium hydroxide to a 50ml beaker containing 30ml of benzyl alcohol, and stir for about 4 hours until the potassium hydroxide is dispersed in the benzyl alcohol, and the solution is a viscous transparent colloid; then 1.611g (5mmol ) ZrOCl 2 ·8H 2 Slowly add O to the above transparent colloid, stir until ZrOCl 2 ·8H 2 O was also dispersed in the colloid, and then 5ml of oleic acid was added dropwise to the above mixture, and the mixture was a yellow viscous solid at this time. After stirring vigorously for 3 hours, the reactant was transferred to a 50ml stainless steel reaction kettle with a polytetrafluoroethylene liner, sealed well, and placed in a constant temperature oven at 160°C for 24 hours to react. When the reaction kettle is naturally cooled to room temperature, take the white solid in the bottom layer of the kettle, put it in a 40ml centrifuge tube, add 30ml of pure water, centrifuge at a speed of 7000r / min for 5 minutes, wash repeatedly 7...

Embodiment 3

[0031] Disperse the sodium or potassium modified zirconia sample prepared in 100mg of Example 2, 3 into 20ml, 0.5M M n+ (M=Li, Cs, Mg, Ca, Sr, Ba, Al, Fe, Co) aqueous solution (the preparation of each aqueous solution uses the chloride salt or nitrate of the corresponding ion), after 12 hours of immersion After stirring, centrifuge and wash with deionized water for 3 to 4 times until the corresponding cations are not detected in the cleaning solution, then dry naturally or in vacuum to obtain zirconia nanoparticles with cubic structure modified by other ions. From Figure 6 It can be concluded from the X-ray powder diffraction that the ion-exchanged zirconia material still has a cubic structure. Figure 7 and Figure 8 They are the surface photovoltage and surface photocurrent spectra of various cation-modified cubic zirconia, and it can be seen from the figure that Al ion-modified zirconia materials have obvious advantages.

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Abstract

The invention belongs to the preparation field of inorganic nanometer materials, and specifically relates to a method for preparing a ZrO2 nano particle with uniform particle size distribution and surface modified metal cations. The method comprises the steps of adding 30-50 millimole of alkali into an organic solvent without water; fully agitating; adding 5-10 millimole of zircon salt into the solution; agitating until complete dispersion to form a colloid; adding 0-10ml of oleic acid in droplets; placing the colloid in a stainless reactor with an inner polyfluortetraethylene lining; sealing well; and placing the reactor in a constant temperature oven with the temperature of 120-180 DEG C for reaction for 24-36 hours, so as to obtain cubic phase ZrO2 nano particles at the lowermost layer. The prepared nano particles have particle size of 4.5nm or so, and narrow dispersion, can stably disperse in solvents, such as water, ethanol, etc. and have practical application value. The method has the advantages of simplicity, less time consumption, high yield, lower pressure in reaction process and suitability for industrialized production.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic nanomaterials, in particular to a method for preparing metastable inorganic nanomaterials, in particular to a ZrO surface-modified metal cation with uniform particle size distribution 2 Methods for the preparation of nanoparticles. Background technique [0002] Due to the multifunctionality of zirconia materials, it has always been widely concerned, and it has always been a research hotspot from the field of structural ceramics to functional ceramics. With the rapid development of nanotechnology, ZrO 2 The application of technology has also been extended to various scientific fields, among which the development of light energy utilization is particularly rapid, including photocatalytic degradation of toxic organic matter, photolysis of water to prepare hydrogen, dye-sensitized solar cells, etc., and even in new digital cameras. There are applications in the photosensitive element CMOS. I...

Claims

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Application Information

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IPC IPC(8): C01G25/02C04B35/48
Inventor 陈接胜吴同舜李国栋
Owner JILIN UNIV
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