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Method for preparing zirconium dioxide nano powder by low-temperature calcination of zirconium sol

A technology of nanopowder and zirconia, applied in zirconia, nanotechnology for materials and surface science, nanotechnology, etc., can solve the problem of high energy consumption

Active Publication Date: 2016-06-01
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

On the other hand, zirconium precursors obtained by these methods, such as Zr(OH) 4 , ZrO(OH) 2 and ZrOC 2 o 4 2H 2 O, etc., generally require high-temperature calcination over 600°C-700°C to completely decompose to obtain zirconia powder, so the energy consumption is high
[0009] KaiJiang et al. in "Low-EnergyPathtoDenseHfO 2 A pure water-based HfO 2 The preparation method of sol, this method avoids using expensive hafnium alkoxide, with cheap water-soluble HfOCl 2 ·8H 2 O is the starting material, after obtaining Hf(OH) 4 After the hydrate is precipitated, a mixture of nitric acid and hydrogen peroxide is added to cause a degumming reaction, and finally a hafnium sol precursor with colloidal particles smaller than 2nm is obtained; but the author of this article only limits the application of this sol to the preparation of microelectronics and optical devices. HfO 2 nano film

Method used

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  • Method for preparing zirconium dioxide nano powder by low-temperature calcination of zirconium sol
  • Method for preparing zirconium dioxide nano powder by low-temperature calcination of zirconium sol
  • Method for preparing zirconium dioxide nano powder by low-temperature calcination of zirconium sol

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Dissolve zirconium oxychloride octahydrate in deionized water to form a clear solution with a concentration of 0.12mol / L, then add 1mol / L ammonia water to form a suspension, and measure the pH value to 7.8; the suspension is centrifuged to obtain Zr(OH ) 4 Hydrate precipitated, washed the precipitate with water to remove chloride ions; then quantitatively added 2mol / L nitric acid and 10mol / L hydrogen peroxide mixture to the precipitate for degumming reaction; vigorously stirred for 1 day to obtain a clear zirconium sol precursor, measured The clear sol has a pH value of 0.8.

[0029] Filter the clarified zirconium sol precursor to remove possible undissolved precipitated particles; then heat and evaporate water at 70°C to obtain a transparent zirconium xerogel. After the zirconium xerogel is calcined and decomposed at 330° C., the amorphous zirconium dioxide nanopowder is obtained.

[0030] From attached image 3 It can be seen from the X-ray diffraction pattern of t...

Embodiment example 2

[0032] Dissolve zirconium oxychloride octahydrate in deionized water to form a clear solution with a concentration of 0.12mol / L, then add 1mol / L ammonia water to form a suspension, and measure the pH value to 9.0; the suspension is filtered to obtain Zr(OH ) 4 Hydrate precipitated, washed the precipitate with water to remove chloride ions; then quantitatively added 2mol / L nitric acid and 10mol / L hydrogen peroxide mixture to the precipitate for degumming reaction; vigorously stirred for 1 day to obtain a clear zirconium sol precursor, measured The clear sol has a pH of 0.6.

[0033] Filter the clarified zirconium sol precursor to remove possible undissolved precipitated particles; then heat and evaporate water at 75°C to obtain a transparent zirconium xerogel. After the zirconium xerogel is calcined and decomposed at 405°C, the nanometer powder of zirconium dioxide mixed with amorphous amorphous state and tetragonal phase is obtained.

[0034] From attached Figure 4 It can ...

Embodiment example 3

[0036] Dissolve zirconium oxychloride octahydrate in deionized water to form a clear solution with a concentration of 0.12mol / L, then add 1mol / L ammonia water to form a suspension, and measure the pH value to 8.5; the suspension is centrifuged to obtain Zr(OH ) 4 Hydrate precipitated, washed the precipitate with water to remove chloride ions; then quantitatively added 2mol / L nitric acid and 10mol / L hydrogen peroxide mixture to the precipitate for degumming reaction; vigorously stirred for 1 day to obtain a clear zirconium sol precursor, measured The pH value of the clear sol was 0.7.

[0037] Filter the clarified sol precursor to remove possible undissolved precipitated particles; then heat and evaporate water at 80°C to obtain a transparent zirconium xerogel. Finally, the dry gel is calcined and decomposed at 430° C. to obtain a stable tetragonal phase zirconia nanopowder.

[0038] From attached Figure 5 It can be seen from the X-ray diffraction pattern that the powder is...

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Abstract

The invention provides a method for preparing zirconium dioxide nano powder by low-temperature calcination of zirconium sol. The method comprises the following steps: dissolving a raw material water-soluble zirconium inorganic salt in deionized water; adding an alkaline precipitant to generate a suspension, and centrifuging or filtering to obtain precipitate; adding mixed liquid of monobasic acid or monobasic acid and hydrogen peroxide into the precipitate, and continuously stirring for peptization to obtain a clear zirconium sol precursor; and finally, drying and dehydrating the zirconium sol precursor and calcining and decomposing in different temperature intervals, wherein amorphous zirconium dioxide nano powder as well as zirconium dioxide nano powder of which tetragonal phase can be kept stable without doping can be obtained, and the average particle size of the powder can be controlled between 3nm and 10nm. The preparation method of high-performance zirconium dioxide nano powder has the following advantages: the powder has small particle size, narrow distribution and good dispersity; the adopted raw material reagent is easily available and cheap; and the equipment requirements and operation technology are simple, the energy consumption is low, pollution is avoided, and industrial production is easy to realize.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and relates to a method for preparing high-purity, ultrafine, non-doped tetragonal phase-stabilized zirconia nanometer powder by using low-temperature calcined zirconium sol. Background technique [0002] Zirconia (ZrO 2 ) has unique physical and chemical properties, such as good thermal and chemical stability, high strength and fracture toughness, low thermal conductivity, good wear resistance and corrosion resistance, etc., so in addition to being used in traditional refractory materials, It is also widely used in the field of functional ceramics such as piezoelectric components and ceramic capacitors, as well as in the fields of advanced structural ceramics, functional coatings, oxygen sensors and catalyst carriers. [0003] Zirconia (ZrO 2 ) has three stable crystal forms: monoclinic, tetragonal and cubic. The stable form of zirconia bulk material at normal temperature and pre...

Claims

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Application Information

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IPC IPC(8): C01G25/02B82Y30/00
CPCC01G25/02C01P2002/72C01P2004/04C01P2004/64
Inventor 周大雨杨喜锐侯晓多高晓霞刘晓英陈国清
Owner DALIAN UNIV OF TECH
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