Glass scintillators and methods of manufacturing the same

Patent metadata

Field	Value
Publication number	US-11130283-B2
Application number	US-202117163823-A
Country	US
Kind code	B2
Filing date	Feb 1, 2021
Priority date	Jan 29, 2020
Publication date	Sep 28, 2021
Grant date	Sep 28, 2021

Abstract

Doped glass scintillators and methods of fabricating the same are provided. Doped glass scintillators can be fabricated by a stereolithography process, and doping can be carried out before the green body composite formation so that homogeneity of the dopant is improved. The structures retain an amorphous structure through the fabrication process, and the vacuum sintering process assists with keeping the dopants in their luminescence-producing oxidation state.

First claim

What is claimed is:

1. A transparent glass ceramic scintillator, comprising a glass substrate doped with a dopant, the transparent glass ceramic scintillator being produced by the following process:
preparing a filler comprising a ceramic powder, the filler being prepared by a sol gel synthesis that includes adding the dopant to the ceramic powder as it is being synthesized;
after preparing the filler, preparing a liquid composite comprising a polymeric matrix and the filler, the matrix being a photocurable pre-polymer resin mix and the filler being a ceramic powder, the matrix comprising a photocurable pre-polymer resin mix, and the preparing of the liquid composite comprising adding the dopant into a mixture of the photocurable pre-polymer resin mix and the ceramic powder;
after preparing the liquid composite, performing a stereolithography process on the liquid composite to produce a green body ensemble;
after performing the stereolithography process, performing a debinding process on the green body ensemble to produce a brown body ensemble that is free of chlorine;
dissolving the dopant in a first solvent at a predetermined ratio to form a dopant solution;
after performing the debinding process, immersing the brown body ensemble in the dopant solution for varying times; and
after immersing the brown body ensemble in the dopant solution, performing a sintering process on the brown body ensemble to give the transparent glass ceramic scintillator,

the transparent glass ceramic scintillator having no crystalline phase.

2. The transparent glass ceramic scintillator according to claim 1 , the performing of the stereolithography process comprising:
dispersing the liquid composite on a stirrer to form a monomeric sludge;
degassing the sludge using a vacuum pump to produce a liquid glass composite;
performing 3D printing on the liquid glass composite on a layer-by-layer basis to produce a printed ensemble of a predetermined geometry; and
rinsing the printed ensemble in a second solvent and post-curing the rinsed printed ensemble by exposing it to ultraviolet light to produce the green body ensemble.

3. The transparent glass ceramic scintillator according to claim 1 , the performing of the debinding process comprising subjecting the green body ensemble to gradual temperature ramps and isothermal treatments sufficient enough to eliminate the polymeric matrix without altering a 3D-printed shape of the green body ensemble, thereby producing the brown body ensemble.

4. The transparent glass ceramic scintillator according to claim 1 , the performing of the sintering process comprising thermally treating the brown body ensemble in a vacuum at a predetermined temperature for a predetermined time, the predetermined temperature being below at least one of a softening temperature and a melting temperature of the ceramic powder.

5. The transparent glass ceramic scintillator according to claim 1 , the dopant comprising cerium, europium, gadolinium, praseodymium, dysprosium, terbium, copper, or titanium.

6. The transparent glass ceramic scintillator according to claim 1 , the dopant comprising cerium.

7. The transparent glass ceramic scintillator according to claim 6 , the dopant being cerium III chloride or cerium III acetate.

8. The transparent glass ceramic scintillator according to claim 1 , the ceramic powder comprising silicate materials.

9. The transparent glass ceramic scintillator according to claim 8 , the ceramic powder comprising borosilicate.

10. The transparent glass ceramic scintillator according to claim 1 , the adding of the dopant to the ceramic powder as it is being synthesized comprising adding the dopant at a first concentration of below 5 mol %.

11. The transparent glass ceramic scintillator according to claim 1 , the adding of the dopant into the mixture of the photocurable pre-polymer resin mix and the ceramic powder comprising adding the dopant at a second concentration of below 5 mol %.

12. The transparent glass ceramic scintillator according to claim 1 , the predetermined ratio at which the dopant is dissolved in the first solvent to form the dopant solution being below 5 mol %.

13. A transparent glass ceramic scintillator, comprising a glass substrate doped with a dopant, the transparent glass ceramic scintillator being produced by the following process:
preparing a filler comprising a ceramic powder, the filler being prepared by a sol gel synthesis that includes adding the dopant to the ceramic powder as it is being synthesized;
after preparing the filler, preparing a liquid composite comprising a polymeric matrix and the filler, the matrix being a photocurable pre-polymer resin mix and the filler being a ceramic powder, the matrix comprising a photocurable pre-polymer resin mix, and the preparing of the liquid composite comprising adding the dopant into a mixture of the photocurable pre-polymer resin mix and the ceramic powder;
after preparing the liquid composite, performing a stereolithography process on the liquid composite to produce a green body ensemble;
after performing the stereolithography process, performing a debinding process on the green body ensemble to produce a brown body ensemble that is free of chlorine;
dissolving the dopant in a first solvent at a predetermined ratio to form a dopant solution;
after performing the debinding process, immersing the brown body ensemble in the dopant solution for varying times; and
after immersing the brown body ensemble in the dopant solution, performing a sintering process on the brown body ensemble to give the transparent glass ceramic scintillator,
the transparent glass ceramic scintillator having no crystalline phase,
the performing of the stereolithography process comprising:
dispersing the liquid composite on a stirrer to form a monomeric sludge;
degassing the sludge using a vacuum pump to produce a liquid glass composite;
performing 3D printing on the liquid glass composite on a layer-by-layer basis to produce a printed ensemble of a predetermined geometry; and
rinsing the printed ensemble in a second solvent and post-curing the rinsed printed ensemble by exposing it to ultraviolet light to produce the green body ensemble,

the performing of the debinding process comprising subjecting the green body ensemble to gradual temperature ramps and isothermal treatments sufficient enough to eliminate the polymeric matrix without altering a 3D-printed shape of the green body ensemble, thereby producing the brown body ensemble,
the performing of the sintering process comprising thermally treating the brown body ensemble in a vacuum at a predetermined temperature for a predetermined time, the predetermined temperature being below at least one of a softening temperature and a melting temperature of the ceramic powder,
the dopant being cerium III chloride or cerium III acetate,
the ceramic powder comprising borosilicate,
the adding of the dopant to the ceramic powder as it is being synthesized comprising adding the dopant at a first concentration of below 5 mol %,
the adding of the dopant into the mixture of the photocurable pre-polymer resin mix and the ceramic powder comprising adding the dopant at a second concentration of below 5 mol %, and
the predetermined ratio at which the dopant is dissolved in the first solvent to form the dopant solution being below 5 mol %.

Assignees

• Okpowe Omena
• Pala Nezih
• Wang Chunlei
• The Florida International Univ Board Of Trustees

Inventors

• Okpowe Omena
• Pala Nezih
• Wang Chunlei

Classifications

• B33Y80/00

  Products made by additive manufacturing · CPC title

• B33Y40/10

  Pre-treatment · CPC title

• B29C64/165 Primary

  using a combination of solid and fluid materials, e.g. a powder selectively bound by a liquid binder, catalyst, inhibitor or energy absorber · CPC title

• B29C64/35

  Cleaning · CPC title

• C03C3/095

  containing rare earths · CPC title