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Annealing method for infrared nonlinear single crystal of multi-component compound containing easily volatile components

A nonlinear crystal and compound technology, applied in the field of annealing and modification of inorganic compound single crystal, can solve the problems of high annealing cost, inconvenient operation, complicated structure of annealing experimental device, etc., and achieve the effect of avoiding secondary volatilization

Inactive Publication Date: 2012-08-01
ANHUI INST OF OPTICS & FINE MECHANICS - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The structure of the annealing experimental device is complex, inconvenient to operate, and the annealing cost is high

Method used

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  • Annealing method for infrared nonlinear single crystal of multi-component compound containing easily volatile components
  • Annealing method for infrared nonlinear single crystal of multi-component compound containing easily volatile components
  • Annealing method for infrared nonlinear single crystal of multi-component compound containing easily volatile components

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: ZnGeP2 single crystal annealing method

[0025] see figure 1 , 2 , first design and manufacture three-stage annealing furnace: annealing zone 1, gradient zone 2, high temperature zone 3, the lengths of which are 30cm, 20cm, 30cm respectively. Then the quartz crucible 4 was cleaned and dried with deionized water. Will be annealed ZnGeP 2 Wafer 5 placed on one end of crucible 4, ZnGeP 2 The polycrystalline powder is put into the carbon-coated boat 7 and placed on the other end of the crucible 4, and is vacuumed to 10°C at room temperature. -3 Seal the crucible after Pa. Then put the quartz crucible 4 after fusing into the appropriate position of the three-stage annealing furnace, place one end of the quartz crucible 4 with the polycrystalline material 6 in the high temperature zone 3, and place the one end of the quartz crucible 4 with the annealing wafer 5 in the annealing furnace. within Zone 1.

[0026] The high temperature zone 3 is raised to 930°...

Embodiment 2

[0029] Example 2: AgGaS 2 single crystal annealing method

[0030] Same as Example 1, the AgGaS to be annealed 2 The wafer is placed in a section of the crucible 4, AgGaS 2Polycrystalline powder is put into carbon-coated boat 7 and is placed on the other end of crucible 4. Vacuum at room temperature to 10 -3 Seal the crucible after Pa. Then put the sealed quartz crucible 4 into an appropriate position in the three-stage annealing furnace. The high temperature zone 3 is raised to 950°C at a rate of 10-30°C / h, and the annealing zone 1 and gradient zone 2 are raised to 830°C and 890°C at corresponding heating rates. Maintain gradient zone 2 temperature linearly with position. After the temperature rise is completed, enter the constant temperature stage, keep the temperature of the furnace body constant and continue for 100h for crystal annealing. After the annealing is completed, the temperature in the high temperature zone 3 is lowered to room temperature at a constant ra...

Embodiment 3

[0031] Example 3: CdGeAs 2 single crystal annealing method

[0032] Same as Example 1, the CdGeAs to be annealed 2 Wafer placed on one end of crucible 4, CdGeAs 2 The polycrystalline powder is put into the carbon-coated boat 7 and placed on the other end of the crucible 4, and is vacuumed to 10°C at room temperature. -3 After Pa, the crucible 4 is welded and sealed, and then the sealed quartz crucible 4 is placed in an appropriate position in the three-stage annealing furnace. The high temperature zone 3 is raised to 620°C at a rate of 10-30°C / h, and the annealing zone 1 and gradient zone 2 are raised to 480°C and 550°C at corresponding heating rates, respectively, and the temperature of the gradient zone 2 is kept changing linearly with the position. After the temperature rise is completed, enter the constant temperature stage, keep the temperature of the furnace body constant and continue for 200h to carry out crystal annealing. After the annealing is completed, the temp...

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Abstract

The present invention relates to the field of inorganic compound single crystal annealing modification, and especially to an annealing method for an infrared nonlinear single crystal of a multi-component compound containing easily volatile components. According to the method, a near-stoichiometric polycrystalline material is adopted as annealing atmosphere, and the polycrystalline material volatilization is separated from the single crystal annealing so as to overcome the blindness, wherein the blindness is attempting annealing experiments through change of various annealing parameters in the following cases, the cases comprise that defect type and proportion thereof of the crystal containing easily volatile components are not known; according to the complementation characteristic of the crystal growth and the temperature gradient annealing component volatilization, the temperature of the high temperature zone and the temperature gradient are changed so as to change the proportion of the volatile component and the annealing rate, and achieve the rapid and effective single crystal annealing.

Description

【Technical field】 [0001] The invention relates to the field of inorganic compound single crystal annealing modification, in particular to an annealing method for multi-component infrared nonlinear crystal materials containing volatile components. 【Background technique】 [0002] Multi-component compound single crystal ZnGeP 2 , AgGaS 2 , AgGa 1～x In x Se 2 , AgGaSe 2 , CdGeAs 2 etc. are infrared nonlinear crystal materials with excellent performance. It can use CO 2 Lasers, Nd:YAG lasers, Ti gemstone lasers, Ho, Tm:YAG lasers are used as pump sources to carry out laser experiments such as frequency doubling (SHG) and optical parametric oscillation (OPO) to achieve frequency conversion laser output in the mid- and far-infrared bands. Therefore, these infrared nonlinear crystals have important applications in the fields of atmospheric component detection, infrared medical treatment, and infrared countermeasures. [0003] Such crystals are usually grown as single crysta...

Claims

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Application Information

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IPC IPC(8): C30B33/02
Inventor 王振友吴海信倪友保黄昌保毛明生程旭东
Owner ANHUI INST OF OPTICS & FINE MECHANICS - CHINESE ACAD OF SCI
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