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Method for in-situ growth of potassium dihydrogen phosphate single crystal in environmental scanning electronic microscope

A potassium dihydrogen phosphate single and environmental scanning electron microscope technology, applied in the direction of single crystal growth, crystal growth, single crystal growth, etc., can solve the problem that non-conductive materials cannot be directly observed

Inactive Publication Date: 2009-10-14
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Non-conductive materials cannot be directly observed with conventional SEM

Method used

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  • Method for in-situ growth of potassium dihydrogen phosphate single crystal in environmental scanning electronic microscope
  • Method for in-situ growth of potassium dihydrogen phosphate single crystal in environmental scanning electronic microscope
  • Method for in-situ growth of potassium dihydrogen phosphate single crystal in environmental scanning electronic microscope

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1) fixing potassium dihydrogen phosphate (KDP) polycrystalline powder on the sample stage (11) in the environmental scanning electron microscope sample chamber (7);

[0031] 2) At 2°C, vacuumize the environmental scanning electron microscope sample chamber (7) to 650Pa, so that %, observe the microscopic morphology of KDP polycrystalline powder, such as image 3 as shown in (a);

[0032] 3) Adjust the temperature of the sample stage (11) to -1°C, and keep the pressure of the sample chamber (7) at 650Pa, so that The water vapor in the sample chamber condenses into a liquid state on the sample stage (11), so that the KDP polycrystalline powder is dissolved and observed in situ, such as image 3 as indicated in (b);

[0033] 4) After the KDP polycrystalline powder is completely dissolved, keep the pressure of the sample chamber (7) constant at 650Pa, and adjust the temperature to 1.5°C so that And keep it for 3 hours, so that KDP grows in the form of single crystal, a...

Embodiment 2

[0036] 1) fixing the KDP polycrystalline powder on the sample stage (11) in the environmental scanning electron microscope sample chamber (7);

[0037] 2) At 2.1°C, the environmental scanning electron microscope sample chamber (7) is evacuated to 400Pa, so that Observe the microscopic morphology of KDP polycrystalline powder, such as Figure 4 as shown in (a);

[0038] 3) Adjust the temperature of the sample stage (11) to 1°C, and increase the pressure of the sample chamber to 670Pa, so that The water vapor in the sample chamber condenses into a liquid state on the sample stage, so that the KDP polycrystalline powder is dissolved and observed in situ, such as Figure 4 as indicated in (b);

[0039] 4) After the KDP polycrystalline powder is dissolved, keep the temperature of the sample stage (11) at 1°C, and adjust the pressure of the sample chamber (7) to 600Pa, so that And keep it for 66 minutes, so that KDP grows in the form of single crystal, and observe the morph...

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Abstract

The invention relates to a method for in-situ growth of potassium dihydrogen phosphate (KDP) single crystal in an environmental scanning electronic microscope (ESEM), belonging to the field of material discipline. The invention applies controllable vacuum environment and temperature changing condition of the ESEM and in-situ grows KDP single crystal and simultaneously in-situ observes the process of dissolving and growing of the KDP. The method prepares the KDP single crystal by the KDP polycrystal powder through controlling water-vapor pressure, relative moisture and the temperature of a sample platform in an ESEM sample chamber; the pressure for dissolving the KDP polycrystal powder is 600 to 670Pa, the temperature is minus 1 to 1 DEG C, and Phi is approximately equal to 100 percent; the pressure for growing the KDP single crystal is 600 to 650Pa, the temperature is 1 to 2.2 DEG C, and Phi is approximately equal to 91 percent to 95 percent. The method is also applicable to grow other water-soluble crystals, and provides methods and conditions for basic problems of dynamically studying microcosmic appearance characteristics and growth mechanism of the water-soluble crystals and the influence of moisture environment to the water-soluble crystals and the like.

Description

technical field [0001] The present invention relates to a kind of in-situ growth potassium dihydrogen phosphate (KH 2 PO 4 , KDP) single crystal, and a method to observe the crystal growth process in situ. technical background [0002] Potassium dihydrogen phosphate (KDP) single crystal has excellent piezoelectric, ferroelectric and electro-optic physical properties, such as high UV transmittance, damage threshold, birefringence coefficient and electro-optic coefficient. KDP is highly valued in high-power laser system technology, and is widely used in various industries, such as making Q switches in two, three, and four frequency doubling devices of Nd:YAG lasers. [0003] KDP is a water-soluble crystal, which is usually prepared by a solution method, that is, the crystal is grown by a solution cooling method under atmospheric pressure. The period of growing large KDP crystals by solution method is long. The initial temperature of crystal growth is 50-60°C, and the cryst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/14C30B7/00C30B30/00
Inventor 吉元张隐奇卫斌王丽
Owner BEIJING UNIV OF TECH
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