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Annealing method for improving luminous efficiency of cerium-doped yttrium aluminum garnet crystal

A yttrium aluminum garnet, crystal luminescence technology, applied in crystal growth, chemical instruments and methods, single crystal growth and other directions, can solve problems such as affecting the luminous efficiency of crystals, and achieve improved scintillation performance, transmission performance, and luminous intensity. Effect

Active Publication Date: 2009-09-30
杭州光学精密机械研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the weak reducing atmosphere in the growth environment of the graphite heating element will also cause some Ce in the Ce:YAG crystal to 3+ ion reduction to Ce 2+ ions, and the carbon in the heating element is easy to enter the crystal to form defects, thus affecting the luminous efficiency of the crystal
[0004] At present, there is no mature annealing process to improve the luminous efficiency of Ce:YAG crystal grown by graphite heating method. Ce 3+ ion concentration while suppressing Ce 4+ ions to achieve the best luminous efficiency and further expand the application prospects of Ce:YAG crystals

Method used

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  • Annealing method for improving luminous efficiency of cerium-doped yttrium aluminum garnet crystal
  • Annealing method for improving luminous efficiency of cerium-doped yttrium aluminum garnet crystal
  • Annealing method for improving luminous efficiency of cerium-doped yttrium aluminum garnet crystal

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Experimental program
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Effect test

Embodiment 1

[0029] The Ce:YAG crystal was air annealed at 1100℃.

[0030] Annealing process steps:

[0031] (1) Clean with alcohol first, the size is 20×15×2mm 3 The Ce:YAG crystal removes impurities on the surface of the crystal to avoid furnace pollution caused by volatilization of impurities.

[0032] (2) Put the Ce:YAG sample on the pure YAG crystal substrate, and put the sample up to increase the contact area with the annealing atmosphere.

[0033] (3) Start the heating program, and raise the temperature from room temperature to 1000° C. at a rate of 100° C. / hour, and then increase the temperature from 1000° C. to 1100° C. at a rate of 50° C. / hour.

[0034] (4) Constant temperature at 1100° C. for 20 hours.

[0035] (5) Cool down from 1100°C to 1000°C at a rate of 50°C / hour, and then from 1000°C to room temperature at a rate of 100°C / hour. The Ce:YAG crystal sample taken out at last is intact and not cracked.

Embodiment 2

[0037] The Ce:YAG crystal was air annealed at 1100℃.

[0038] Annealing process steps:

[0039] (1) Clean the Ce:YAG crystal with a size of 20×15×5 mm3 with alcohol to remove impurities existing on the surface of the crystal, so as to avoid contamination of the furnace caused by volatilization of impurities.

[0040] (2) Put the Ce:YAG sample on the pure YAG crystal substrate, and put the sample up to increase the contact area with the annealing atmosphere.

[0041] (3) Start the heating program, and raise the temperature from room temperature to 1000° C. at a rate of 100° C. / hour, and then increase the temperature from 1000° C. to 1100° C. at a rate of 50° C. / hour.

[0042] (4) Constant temperature at 1100° C. for 35 hours.

[0043](5) Cool down from 1100°C to 1000°C at a rate of 50°C / hour, and then from 1000°C to room temperature at a rate of 100°C / hour. The Ce:YAG crystal sample taken out at last is intact and not cracked.

Embodiment 3

[0045] The Ce:YAG crystal was air annealed at 1200℃.

[0046] Annealing process steps:

[0047] (1) Clean with alcohol first, the size is 20×15×2mm 3 The Ce:YAG crystal removes impurities on the surface of the crystal to avoid furnace pollution caused by volatilization of impurities.

[0048] (2) Put the Ce:YAG sample on the pure YAG crystal substrate, and put the sample up to increase the contact area with the annealing atmosphere.

[0049] (3) Start the heating program, and raise the temperature from room temperature to 1000°C at a rate of 100°C / hour, and then increase the temperature from 1000°C to 1200°C at a rate of 50°C / hour.

[0050] (4) Constant temperature at 1200° C. for 15 hours.

[0051] (5) Cool down first from 1200°C to 1000°C at a rate of 50°C / hour, and then from 1000°C to room temperature at a rate of 100°C / hour. The Ce:YAG crystal sample taken out at last is intact and not cracked. The transmission and luminescence effects before and after annealing are a...

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Abstract

The invention relates to an annealing method for improving luminous efficiency of a cerium-doped yttrium aluminum garnet crystal, which is characterized by performing low temperature oxygen annealing or high temperature hydrogen annealing on the cerium-doped yttrium aluminum garnet (Ce:YAG) crystal grown by a graphite heater method. The method comprises the following steps: cleaning the crystal with acetone or alcohol first; placing the Ce:YAG crystal on a white stone or a pure YAG crystal substrate in a hearth; raising the temperature; annealing at a constant temperature; reducing the temperature to room temperature; and taking the Ce:YAG crystal out of the hearth. The annealing method can effectively eliminate the carbon-related defect in the crystal and improve the permeability of the crystal; and Ce<2+> ions formed in the growth process in the crystal are oxidized, thus the concentration of Ce<3+> ions needs to be increased and Ce<4+> ions are inhibited as much as possible at the same time to avoid quenching effect caused by the Ce<4+> ions so that the luminous intensity of the Ce:YAG crystal is improved to the utmost extent.

Description

technical field [0001] The invention relates to crystal heat treatment, in particular to an annealing method for improving the luminous efficiency of cerium-doped yttrium-aluminum garnet crystal, which is mainly used for growing cerium-doped yttrium-aluminum garnet (hereinafter referred to as Ce:YAG) crystal annealing method to obtain the best luminous efficiency. The Ce:YAG crystal grown by the graphite heating method has more carbon-related defects and variable-valence Ce ions, and the carbon defects can be eliminated and the Ce can be increased by a suitable annealing process. 3+ ions and reduce the quenching center, thereby effectively enhancing the luminous efficiency. Ce:YAG crystals treated by annealing process can be widely used in high energy physics, nuclear physics, nuclear medicine, oil well detection and white light LED and other fields. Background technique [0002] Yttrium aluminum garnet doped with cerium ions (Ce:Y 3 Al 5 o 12 Or Ce:YAG) single crystal ...

Claims

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Application Information

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IPC IPC(8): C30B33/02C30B29/28
Inventor 曹顿华赵广军董勤陈建玉丁雨憧程艳
Owner 杭州光学精密机械研究所
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