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US 12,552,717 B2Granted
Lithography-based process for the production of transparent ceramic bodies with at least two zones of different composition and transparent ceramic bodies thus obtained
AssigneeConsiglio Nazionale Delle Ricerche
InventorsValentina Biasini, Jan Hostaša, Laura Esposito, Andreana Piancastelli, Guido Toci, Martin Schwentenwein, Dominik Philipp Brouczek
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Abstract
It is described a process for producing transparent ceramic bodies with at least two zones having different garnet composition, in particular in which one of said zones has composition Y3AI5O12. The invention is especially useful for the production of transparent ceramic bodies having preset complex shapes and/or a controlled complex distribution of doping ions.
Claims12
A process for the production of a transparent ceramic body, comprising the steps of:
- a) preparing a first suspension comprising:
- 1) a solvent;
- 2) a mixture of powders of oxides, hydroxides, nitrates or chlorides of metals in the stoichiometric ratio required to produce an oxide phase A3B5O12+x, wherein is −0.1≤x≤0.1, A is selected among Y, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu and mixtures thereof, and B is selected among Al, Fe, Cr, Sc, Ga and mixtures thereof;
- 3) a sintering aid selected among silicon oxide in the form of powder, a tetraalkylorthosilicate, calcium oxide powder, a calcium oxide precursor, magnesium oxide powder, a magnesium oxide precursor, or a mixture thereof;
- 4) a dispersant selected among polyethylene glycol, menhaden fish oil, phosphate esters, dicarboxylic acids, stearic acid and silanes;
- b) extracting the solvent from the suspension of step a) obtaining a mixture;
- c) preparing a homogeneous slurry comprising the mixture of step b) and a photocurable resin;
- d) preparing at least a second suspension comprising:
- 1′) a solvent;
- 2′) a mixture of powders of oxides, hydroxides, nitrates or chlorides of metals in the stoichiometric ratio required to produce an oxide phase A3B5O12+x, wherein is −0.1≤x≤0.1, A is selected among Y, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu and mixtures thereof, and B is selected among Al, Fe, Cr, Sc, Ga and mixtures thereof;
- 3′) a sintering aid selected among silicon oxide in the form of powder, a tetraalkylorthosilicate, calcium oxide powder, a calcium oxide precursor, magnesium oxide powder, a magnesium oxide precursor, or a mixture thereof;
- 4′) a dispersant selected among polyethylene glycol, menhaden fish oil, phosphate esters, dicarboxylic acids, stearic acid and silanes;
- e) extracting the solvent from the suspension of step d) obtaining a mixture;
- f) preparing a homogeneous slurry comprising the mixture of step e) and a photocurable resin;
- g) operating at a temperature between 20 and 30° C., forming a deposit comprising layers of the slurries of steps c) and f) by a layer-by-layer 3D printing technique wherein, after the deposition of each layer of slurry, a photopolymerization operation of the photocurable resin is carried out, and a cleansing operation of a series of photopolymerized layers of a first composition is carried out before depositing on it or next to it a layer of slurry of a second composition to remove the non-polymerized slurry of first composition, obtaining a consolidated body;
- h) subjecting the consolidated body of step g) to a thermal treatment in air or in an oxygen-rich atmosphere at a temperature in the range 100 to 1000° C. for removing the organic and volatile components of the consolidated body, obtaining a degreased body;
- i) subjecting the degreased body of step h) to a sintering thermal treatment in vacuum at a temperature in the range from 1600° C. to 1900° C. for a time in the range from 6 h to 32 h obtaining a sintered body;
- or
- i′) subjecting the degreased body of step h) to a sintering thermal treatment in vacuum at a temperature in the range from 1400° C. to 1800° C. for a time in the range from 2 h to 20 h followed by hot isostatic pressing with an applied pressure in the range from 100 to 300 bar at a temperature in the range from 1400° C. to 1800° C. for a time in the range from 1 h to 4 h obtaining a sintered body;
- in which said first suspension and said at least one second suspension have different compositions.
17 more elements
Dependencies are inferred from the claim text.