Method of forming rare earth oxide ceramic scintillator with ammonium dispersion of oxalate precipitates

• US 5,116,560 A
• Filed: 03/22/1991
• Issued: 05/26/1992
• Est. Priority Date: 03/22/1991
• Status: Expired due to Fees

• Current Assignee: General Electric Company
• Original Assignee: General Electric Company
• Inventors: Dole, Stephen Lee, Venkataramani, Subramaniam
• Primary Examiner(s): DERRINGTON, JAMES H
• Application Number:
  US07/673,608
• Time in Patent Office: 431 Days
• Field of Search: 264/1.2, 264/65, 252/301.4 R
• US Class Current: 264/1.22
• CPC Class Codes: C01F 17/241 containing two or more rare earth metals, e.g. NdPrO3 or LaNdPrO3
• CPC Class Codes: C04B 35/50 based on rare-earth compounds non-oxide rare earth compounds C04B35/5156
• CPC Class Codes: C09K 11/7787 Oxides C09K11/7785 takes precedence
• CPC Class Codes: G01T 1/202 the detector being a crystal
• CPC Class Codes: G01T 1/2023 Selection of materials see provisionally also G01T1/202

Abstract

A method of forming polycrystalline rare earth oxide ceramic scintillators formed by dissolving a mixture of oxides of the scintillator in an aqueous hydrochloric or nitric acid solution to form a rare earth solution, precipitating oxalates from the rare earth solution, calcining the oxalates to form the respective oxides, cold pressing the oxides to form a compact, and sintering the compact in a reducing atmosphere or vacuum to form the scintillator, the method being improved by precipitating the oxalates by admixing the rare earth solution with an oxalic solution comprised of, oxalic acid and ammonium ions in an amount that disperses the oxalate precipitates.

Claims

1. A method of forming a polycrystalline rare earth oxide ceramic scintillator containing an oxide of a rare earth activator selected from the group consisting of europium, neodymium, ytterbium, dysprosium, terbium and praseodymium, having improved transparency that does not require milling, said scintillator being formed by dissolving a mixture of oxides of the scintillator composition in an aqueous hydrochloric or nitric acid solution to form a rare earth solution, precipitating oxalates from the rare earth solution, calcining the oxalates to form oxides, cold pressing the oxides to form a compact, and sintering the compact in a reducing atmosphere or vacuum to form the scintillator, the improvement comprising:

precipitating the oxalates by admixing the rare earth solution with an oxalic solution comprised of, oxalic acid and ammonium ions in an amount that disperses the oxalate precipitates.

2. The method of claim 1 wherein the ammonium ions are in a ratio of at least about 1 mole of ammonium ions per mole of rare earth ions.

3. The method of claim 2 wherein the ammonium ions are in a ratio of about 1 to 2 moles of ammonium ions per mole of rare earth ions.

4. The method of claim 2 further comprising the step of washing the oxalate precipitates with water to remove excess ammonium or oxalate salts.

5. The method of claim 4 wherein the water has a pH between about 2 and 10.

6. The method of claim 2 further comprising the step of milling the oxalates

7. The method of claim 6 wherein the step of milling is vibration milling with a rigid organic polymer milling media.

8. A method of forming a polycrystalline yttria-dolinia scintillator having improved transparency that does not require milling said scintillator being formed by dissolving a mixture of oxides of the scintillator composition in an aqueous hydrochloric or nitric acid solution to form a rare earth solution, precipitating oxalates from the rare earth solution, calcining the oxalates to form oxides, cold pressing the oxides to form a compact, and sintering the compact in a reducing atmosphere or vacuum to form the scintillator, the improvement comprising:

precipitating the oxalates by admixing the rare earth solution with an oxalic solution comprised of, oxalic acid and ammonium ions in an amount that disperses the oxalate precipitates.

9. The method of claim 8 wherein the ammonium ions are in a ratio of at least about 1 mole of ammonium ions per mole of rare earth ions.

10. The method of claim 9 wherein the ammonium ions are in a ratio of about 1 to 2 moles of ammonium ions per mole of rare earth ions.

11. The method of claim 9 further comprising the step of washing the oxalate precipitates with water to remove excess ammonium or oxalate salts.

12. The method of claim 11 wherein the water has a pH between about 2 and 10.

13. The method of claim 9 further comprising the step of milling the oxalates.

14. The method of claim 13 wherein the step of milling is vibration milling with a rigid organic polymer milling media.

15. A method of forming a polycrystalline lutetia-gadolinia scintillator having improved transparency that does not require milling said scintillator being formed by dissolving a mixture of oxides of the scintillator composition in an aqueous hydrochloric or nitric acid solution to form a rare earth solution, precipitating oxalates from the rare earth solution, calcining the oxalates to form oxides, cold pressing the oxides to form a compact, and sintering the compact in a reducing atmosphere or vacuum to form the scintillator, the improvement comprising:

precipitating the oxalates by admixing the rare earth solution with an oxalic solution comprised of, oxalic acid and ammonium ions in an amount that disperses the oxalate precipitates.

16. The method of claim 15 wherein the ammonium ions are in a ratio of at least about 1 mole of ammonium ions per mole of rare earth ions.

17. The method of claim 16 wherein the ammonium ions are in a ratio of about 1 to 2 moles of ammonium ions per mole of rare earth ions.

18. The method of claim 16 further comprising the step of washing the oxalate precipitates with water to remove excess ammonium or oxalate salts.

19. The method of claim 18 wherein the water has a pH between about 2 and 10.

20. The method of claim 16 further comprising the step of milling the oxalates.

21. The method of claim 20 wherein the step of milling is vibration milling with a rigid organic polymer milling media.