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Novel method of preparing nano zirconium oxide powder for dentistry

A nano-zirconia and powder technology, applied in the field of nano-materials, can solve the problems of large powder particle size, high cost and poor dispersibility, and achieve the effects of uniform powder particle size, fast reaction and low cost

Active Publication Date: 2016-07-13
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Precursors prepared by co-precipitation are prone to agglomeration during drying and calcination, resulting in larger particle size and poor dispersion; powders prepared by sol-gel method are also easy to agglomerate, and the preparation cycle is longer and the cost is higher. It is not suitable for mass production; the powder prepared by the microemulsion method usually needs to introduce a surfactant, such as the Chinese invention patent 201010220457.5 "a method for preparing dental colored nano-zirconia" mentioned "take n-octane, non-ionic surfactant , n-hexanol by volume ratio: 15-20: 2.1-6.4: 2-2.7 mixed to form a transparent emulsion, the above-mentioned transparent emulsion is divided into two parts, one part is added with soluble zirconium salt and coloring agent, and the other part is added with alkaline substances Aqueous solution to obtain microemulsion system of soluble zirconium salt and coloring agent and microemulsion system of alkaline substance respectively”, the preparation process of this method is loaded down with trivial details, and the cost is high
The traditional solid-phase mechanical mixing method generally uses ball milling technology, which requires a long time for ball milling, the powder particle size is large, and the particle size distribution is uneven

Method used

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  • Novel method of preparing nano zirconium oxide powder for dentistry
  • Novel method of preparing nano zirconium oxide powder for dentistry
  • Novel method of preparing nano zirconium oxide powder for dentistry

Examples

Experimental program
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Effect test

Embodiment 1

[0032] ZrOCl 2 ·8H 2 O and YCl 3 ·6H 2 After O is dissolved in deionized water respectively, stir and mix; the concentration of the mixed solution of zirconium salt and yttrium salt is 0.8mol / L, and the total amount of the mixed solution is 1mol. ZrOCl 2 ·8H 2 O is 0.97mol, YCl 3 ·6H 2 O is 0.03mol; Add the dispersant dehydrated alcohol to the mixed solution and the ammonia solution respectively, stir and constant volume; the amount of dehydrated alcohol accounts for 20% of the volume of the zirconium salt, yttrium salt mixed solution and the volume of the ammonia solution respectively; the amount of the ammonia solution On the basis of satisfying the amount required for the chemical reaction with zirconium salt and yttrium salt, the excess amount is 10%, so as to adjust the pH value of the precipitation reaction at about 8.7. Inject the mixed solution of zirconium salt, yttrium salt and ammonia solution into the reactor at room temperature at a flow rate of 60L / h, and a...

Embodiment 2

[0034] ZrOCl 2 ·8H 2 O and YCl 3 ·6H 2 After O is dissolved in deionized water respectively, stir and mix; the concentration of the mixed solution of zirconium salt and yttrium salt is 0.8mol / L, and the total amount of the mixed solution is 1mol. ZrOCl 2 ·8H 2 O is 0.95mol, YCl 3 ·6H 2 O is 0.05mol; Add the dispersant dehydrated alcohol to the mixed solution and the ammonia solution respectively, stir and constant volume; On the basis of satisfying the amount required for the chemical reaction with zirconium salt and yttrium salt, the excess amount is 10%, so as to adjust the pH value of the precipitation reaction at about 8.7. Inject the mixed solution of zirconium salt, yttrium salt and ammonia solution into the reactor at room temperature at a flow rate of 60L / h, and at the same time vigorously stir to form a white precipitate at a stirring speed of 800rpm; without aging, quickly use a large amount of deionized Dilute with water to obtain a white slurry; filter the w...

Embodiment 3

[0036] ZrOCl 2 ·8H 2 O and YCl 3 ·6H 2 After O is dissolved in deionized water respectively, stir and mix; the concentration of the mixed solution of zirconium salt and yttrium salt is 0.8mol / L, and the total amount of the mixed solution is 1mol. ZrOCl 2 ·8H 2 O is 0.92mol, YCl 3 ·6H 2 O is 0.08mol; Add the dispersant absolute ethanol to the mixed solution and the ammonia solution respectively, stir and constant volume; the amount of absolute ethanol accounts for 20% of the volume of the zirconium salt, the yttrium salt mixed solution and the ammonia solution volume; On the basis of satisfying the amount required for the chemical reaction with zirconium salt and yttrium salt, the excess amount is 10%, so as to adjust the pH value of the precipitation reaction at about 8.7. Inject the mixed solution of zirconium salt, yttrium salt and ammonia solution into the reactor at room temperature at a flow rate of 60L / h, and at the same time vigorously stir to form a white precipi...

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Abstract

The invention provides a novel method of preparing nano zirconium oxide powder for dentistry.The novel method includes: selecting soluble zirconium oxide as a raw material, soluble yttrium salt as a stabilizer and ammonia water as a precipitator, and adopting a quick co-precipitation method to generate a zirconium oxide precursor under vigorous stirring; immediately using a lot of deionized water for dilution without aging, suction-filtering, washing, dehydrating, drying, and calcining to obtain zirconium oxide powder.Crystal shape of nano zirconium oxide is square-phase zirconium oxide particles, average particle size of primary particles is 2-3 nm, and particle size is 10 nm and 25 nm after the particles are treated at 800 DEG C for 2 h.The method is simple and convenient in preparation process, low in cost, short in period, high in repeatability and suitable for batch production, and the powder is uniform in granularity and is nanoscale.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and in particular relates to a method for preparing dental nanometer zirconia powder. Background technique [0002] At present, the liquid-phase preparation methods of dental zirconia powder mainly include coprecipitation method, sol-gel method and microemulsion method. Precursors prepared by co-precipitation are prone to agglomeration during drying and calcination, resulting in larger particle size and poor dispersion; powders prepared by sol-gel method are also easy to agglomerate, and the preparation cycle is longer and the cost is higher. It is not suitable for mass production; the powder prepared by the microemulsion method usually needs to introduce a surfactant, such as the Chinese invention patent 201010220457.5 "a method for preparing dental colored nano-zirconia" mentioned "take n-octane, non-ionic surfactant , n-hexanol by volume ratio: 15-20: 2.1-6.4: 2-2.7 mixed to form ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02B82Y40/00
CPCC01G25/02C01P2002/72C01P2004/04C01P2004/64
Inventor 陈智慧丁建宁袁宁一李志伟邱建华
Owner CHANGZHOU UNIV
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