Synthesis of tetragonal phase stabilized nano and submicron sized nanoparticles
View Patent ↗Novel, monodispersed, spherical ZrO 2 particles in the size range of approximately 10 to approximately 600 nm exhibiting metastable tetragonal crystal structure at room temperature and novel methods of preparation. The ZrO 2 particles are approximately 100% in the tetragonal phase at room temperature and can be pure and free of foreign oxides. The novel method can include mixing zirconium-alkoxide and an alcohol, forming preparation one, followed by separately dissolving completely de-ionized water and a polymeric steric stabilizer in an alcohol forming preparation two. Next the preparations can be mixed with vigorous stirring while subjecting the materials to hydrolysis and condensation reactions with very slow stirring. Next, there is waiting for the formation of a sol from the mixture, followed by drying at approximately 80 degrees C. to form resultant material followed by crushing the resultant material.
1. A method for the synthesis of nanocrystalline ZrO 2 powder, pure and free of foreign oxides, in particle sizes of approximately 10 to approximately 30 nm in diameter, comprising the steps of:
preparing equal parts of an alcohol solution wherein a first part is mixed with deionized water and a second part is mixed with a zirconium-alkoxide;
under processing conditions using an R-value of 60, wherein the R-value comprises the ratio of molar concentration of water to zirconium-alkoxide;
adding a polymeric steric stabilizer to the first part of an alcohol solution with deionized water, wherein the stabilizer is in a concentration of approximately 1.0 to approximately 2.0 g/L and stirring until homogenized and forming a solution one;
dissolving the zirconium alkoxide in the second part of the alcohol solution and forming a solution two;
mixing the solution one and the solution two together;
stirring the mixture for approximately 4 hours;
holding the stirred mixture under static conditions for approximately 24 hours to complete the hydrolysis and condensation reactions;
drying at approximately 80 degrees C. to remove solvent and form resultant material;
crushing the resultant material to obtain nanocrystalline ZrO 2 powder, pure and free of foreign oxides, with particle sizes of approximately 10 nm to approximately 30 nm in diameter that form loose agglomerates and exhibit tetragonal crystal structure at room temperature; and
calcining at temperatures ranging from approximately 400° C. to approximately 800° C. wherein the nanocrystalline ZrO 2 powder, pure and free of foreign oxides, with particle sizes of approximately 10 nm to approximately 30 nm in diameter undergoes a gradual transformation from tetragonal to monoclinic phase with an increase in calcination temperature from approximately 400 to approximately 800 degrees C.
2. The method, as in claim 1 wherein said polymeric steric stabilizer is an organic polymer containing —OH or ether group.
3. The method, as in claim 1 , wherein said polymeric steric stabilizer is one of the group consisting of hydroxypropyl cellulose polymer (HPC), polyvinylalcohol, ethylene glycol, and hexamethyldisilazane.
4. The method, as in claim 1 , wherein said zirconium-alkoxide is zirconium (IV) n-propoxide and said alcohol is anhydrous alcohol.
5. The method, as in claim 1 , wherein said synthesis takes place in air under normal atmospheric conditions.
6. The method, as in claim 3 , wherein said polymeric steric stabilizer is HPC polymer.
7. The method, as in claim 6 , wherein said HPC polymer has a molecular weight of approximately 80,000 to approximately 1,000,000 g/mol.