IP Library Granted Patent US 12,054,848
Granted Patent B2
US 12,054,848 · App. 17/191,743 · Granted Aug 6, 2024

Crystals for detecting neutrons, gamma rays, and x rays and preparation methods thereof

Inventors: Yu Wang (Meishan, CN); Weiming Guan (Meishan, CN); Min Li (Meishan, CN)
Assignee: MEISHAN BOYA ADVANCED MATERIALS CO., LTD.
C30B15/002C07F5/003C30B15/14C30B15/20G01T1/2023G01T3/06
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Quick Facts
Patent No.
US 12,054,848
App. No.
17/191,743
Granted
Aug 6, 2024
Kind
B2
Abstract

The present disclosure discloses a method for growing a crystal for detecting neutrons, gamma rays, and/or x rays. The method may include weighting reactants based on a molar ratio of the reactants according to a reaction equation (1−x−z)X 2 O 3 +SiO 2 +2xCeO 2 +zZ 2 O 3 →X 2(1−x−Z) Ce 2x Z 2z SiO 5 +z/2O 2 ↑ or (1−x−y−z)X 2 O 3 +yY 2 O 3 +SiO 2 +2xCeO 2 +zZ 2 O 3 →X 2(1−x−y−z) Y 2y Ce 2x Z 2z SiO 5 +x/20 2 ↑; placing the reactants on which a second preprocessing operation has been performed into a crystal growth device after an assembly processing operation is performed on at least one component of the crystal growth device; introducing a flowing gas into the crystal growth device after sealing the crystal growth device; and activating the crystal growth device to grow the crystal based on the Czochralski technique.

Claims (40)

1. A method for growing a crystal, wherein:

a formula of the crystal is X 2(1-x-y-z) Y 2y Ce 2x Z 2z SiO 5 , wherein:

X consists of at least one of Ga, La, Pr, Ce, Nd, Pm, Sm, Eu, Tb, Dy, Ho, Er, Tm, Yb, Mn, Mg, Ca, Al, Fe, Sr, or Ba;

Z consists of at least one of Ga, Li, B, Gd, or Tb,

x=0.3%˜6%;

y=5%˜30%; and

z=0.3%˜6%; and

the method comprises:

weighting reactants based on a molar ratio of the reactants according to a reaction equation after a first preprocessing operation is performed on the reactants, wherein:

the reactants include X 2 O 3 , Y 2 O 3 , SiO 2 , Z 2 O 3 , and the Ce-containing compound;

the Ce-containing compound includes Ce 2 O 3 , Ce (CO 3 ) 2 , CeCl 3 , CeF 3 , CeS, CeBr 3 , CeRu 2 , CeCo 2 , CeRh 3 , CeN, CePd 3 , CeI 3 , CeF 4 , or CeCl 4 ; and

a weight of SiO 2 exceeds a theoretical weight value of the SiO 2 calculated according to the reaction equation by 0.01%˜0.999%;

placing the reactants on which a second preprocessing operation has been performed into a crystal growth device after an assembly processing operation is performed on at least one component of the crystal growth device;

introducing a flowing gas into the crystal growth device after sealing the crystal growth device, a flow rate of the flowing gas being 5 L/min˜12 L/min or 19.1 L/min˜20 L/min; and

activating the crystal growth device to grow the crystal based on a Czochralski technique.

2. The method of claim 1 , wherein the first preprocessing operation includes a roasting operation under 800° C.˜1400° C.

3. The method of claim 1 , wherein the at least one component of the crystal growth device includes a crucible, and the assembly processing operation includes at least one of:

performing an acid soaking and cleaning operation on the crucible;

determining whether a vertical distance between an upper edge of the crucible and an upper edge of an induction coil mounted in the crystal growth device is 0 mm˜+50 mm, wherein “+” represents that the upper edge of the crucible is higher than the upper edge of the induction coil, and “−” represents that the upper edge of the crucible is lower than the upper edge of the induction coil; or

cleaning an impurity in the crucible.

4. The method of claim 1 , wherein the second preprocessing operation includes at least one of an ingredient mixing operation or a pressing operation.

5. The method of claim 1 , wherein the flowing gas includes one or more of oxygen, nitrogen, or inert gas.

6. The method of claim 1 , wherein the flowing gas includes oxygen, a volume ratio of the oxygen being 0.001%˜10%.

7. The method of claim 1 , further comprising:

adding a seed crystal, the seed crystal including at least one of Cerium-doped Lutetium(-yttrium) oxyorthosilicate, Lanthanum-doped Lutetium(-yttrium) oxyorthosilicate, Praseodymium-doped Lutetium(-yttrium) oxyorthosilicate, or Neodymium-doped Lutetium(-yttrium) oxyorthosilicate.

8. The method of claim 7 , wherein a distance between the seed crystal and an upper surface of the reactants is 5 mm˜100 mm or a predetermined distance during melting the reactants during the crystal growth.

9. The method of claim 7 , further comprising:

sinking the seed crystal to 0.1 mm˜50 mm below a surface of a melt of the reactants by controlling a pulling rod during temperature adjustment; and

pulling up the pulling rod after maintaining a constant temperature for at least 0.1 hours˜1 hour.

10. The method of claim 1 , wherein a growth rate of the crystal is 0.01 mm/h˜6 mm/h during the crystal growth.

11. The method of claim 1 , wherein during a shouldering process of the crystal growth,

a shoulder angle is 30 degrees˜70 degrees, and

a shoulder length is 40 mm˜90 mm.

12. The method of claim 10 , wherein a constant diameter during the shouldering process is 10 mm˜200 mm.

13. The method of claim 1 , wherein during an ending process of the crystal growth,

an ending angle is 30 degrees˜70 degrees, and

an ending length is 40 mm˜90 mm.

14. The method of claim 1 , wherein at least one process in the crystal growth is controlled by a proportional-integral-derivative (PID) controller, the at least one process comprising at least one of a necking process, a shouldering process, a constant diameter growth process, an ending process, or a cooling process.

15. The method of claim 1 , wherein a melting time of a heat treatment for melting the reactants is 10 hours˜30 hours during the crystal growth.

16. The method of claim 1 , wherein a temperature decreasing time of the crystal during the crystal growth is 20 hours˜100 hours.

Assignments (2)
CHANGE OF NAME Recorded May 13, 2026
From: MEISHAN BOYA ADVANCED MATERIALS CO., LTD.
To: BOYA ADVANCED MATERIALS CO., LTD.
Reel/Frame 075565/0780 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 24, 2021
From: WANG, YU; GUAN, WEIMING; LI, MIN
To: MEISHAN BOYA ADVANCED MATERIALS CO., LTD.
Reel/Frame 056321/0900 →
Continuity (3)
Continuation In Part 16903322 · Jun 16, 2020
Continuation PCTCN2019101680 · Aug 21, 2019
Related Publication 20210189588A1 · Jun 24, 2021