Preparation method and application of dipotassium tetradiphosphate strontium crystal

A technology of dipotassium strontium tetrametaphosphate and crystal, which is applied in crystal growth, chemical instruments and methods, single crystal growth and other directions, and can solve problems such as the preparation of dipotassium strontium tetrametaphosphate crystals that have not yet been found.

Inactive Publication Date: 2017-08-18
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, no reports about the preparation and use of stront

Method used

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  • Preparation method and application of dipotassium tetradiphosphate strontium crystal
  • Preparation method and application of dipotassium tetradiphosphate strontium crystal
  • Preparation method and application of dipotassium tetradiphosphate strontium crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1——Growing strontium dipotassium tetrametaphosphate crystals in a melt by the Kyropoulos method

[0024] 117.48g (0.85mol) K 2 CO 3 , 125.49g (0.85mol) SrCO 3 and 391.10 g (3.4 mol) NH 4 h 2 PO 4 After grinding and mixing evenly (the molar ratio is K:Sr:P=2:1:4), slowly raise the temperature in the range of 150-300°C to release a large amount of CO produced by the reaction. 2 , NH 3 and H 2 O gas, followed by pre-firing at 400°C for 10 hours. Then put the obtained sample into a Φ60mm×60mm open platinum crucible, put the crucible into a crystal growth furnace, heat up to 900°C to melt the sample, and keep the temperature for 48h to fully escape the gas remaining in the melt to make The melt was homogeneous, and the melt was then cooled to a temperature 2°C above the crystallization temperature. The seed crystal is fixed on the seed crystal rod, introduced into the furnace from the small hole on the top of the growth furnace, and the seed crystal is broug...

Embodiment 2

[0025] Example 2——Growing strontium dipotassium tetrametaphosphate crystals in the melt by pulling method

[0026] 132.24g (1.12mol) KPO 3 and 137.51g (0.56mol) Sr(PO 3 ) 2 After grinding and mixing uniformly (the molar ratio is K:Sr:P=2:1:4), sintering at 600°C for 24 hours. Then put the obtained sample into a Φ60mm×40mm open platinum crucible, put the crucible into the crystal growth pulling furnace, heat up to 800°C to melt the sample, and keep the temperature for 3h to make the melt homogeneous, and then cool down the melt to a temperature 5°C above the crystallization temperature. The seed crystal is fixed on the seed crystal rod, introduced into the furnace through the small hole at the top, and the seed crystal is brought into contact with the liquid surface of the melt to start crystal growth. The seed crystal is rotated at a speed of 30 rpm, and the seed crystal rod is pulled at a rate of 0.5 mm / hour. At the end of the crystal growth, the crystal is removed from ...

Embodiment 3

[0028] The crystal of strontium dipotassium tetrametaphosphate prepared in Example 1 is analyzed by single crystal X-ray diffraction structure, as can be seen: the prepared crystal chemical formula is K 2 SrP4 o 12 ; Its crystallographic structure belongs to the tetragonal crystal system, I-4 space group, and the unit cell parameters are Z=2, the unit cell volume is The anionic group in the structure is formed by the phosphorus-oxygen tetrahedron sharing its two oxygen vertices with each other [P 4 o 12 ] 4- cyclic anion. Carry out powder X-ray diffraction test to the prepared strontium dipotassium tetrametaphosphate crystal, and its diffraction spectrum is as follows figure 1 shown.

[0029] Carry out DSC-TG analysis to the prepared strontium dipotassium tetrametaphosphate crystal, the result is as follows figure 2 shown. It can be seen from the figure that the melting point of the crystal is about 701°C, and there is no obvious thermal weight loss below 900°C, tha...

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Abstract

The invention relates to a preparation method of dipotassium tetradiphosphate strontium crystal. The method comprises the steps of burdening a compound containing K, Sr and P at the molar ratio of 2:1:1 and mixing evenly, carrying out pre-sintering and sintering, heating the mixture in a crucible until melting, and keeping a constant temperature higher than a melting point temperature for 1-50h to prepare a melt; cooling the melt to the temperature which is 1-5 DEG C higher than the melting point and growing the dipotassium tetradiphosphate strontium crystal in the melt by adopting a kyropoulos method or a czochralski method. The crystal can be used for preparing a nonlinear optical device, the nonlinear optical device comprises a device, and the device comprises at least one dipotassium tetradiphosphate strontium crystal.

Description

technical field [0001] The invention relates to a preparation method and application of strontium dipotassium tetrametaphosphate crystal. Background technique [0002] The so-called nonlinear optical crystal refers to a type of crystal that can produce nonlinear optical effects, which can change the frequency of the laser, including frequency multiplication, sum frequency, difference frequency, optical parametric oscillation and amplification. Lasers can be frequency converted through nonlinear optical devices, thereby extending the wavelength of the laser and broadening the application range of the laser. Therefore, nonlinear optical crystals have great applications in the field of laser technology. [0003] At present, after decades of hard work by scientists from various countries, some nonlinear optical crystals have been applied in practice, such as: BBO, LBO, KTP, and other crystals. However, there are still shortcomings in the application of crystals of these materi...

Claims

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Application Information

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IPC IPC(8): C30B29/14C30B15/00C30B17/00
CPCC30B29/14C30B15/00C30B17/00
Inventor 孙同庆王策孔勇发刘宏德刘士国许京军
Owner NANKAI UNIV
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