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Compound rubidium-lead-phosphorus-oxygen and rubidium-lead-phosphorus-oxygen optical crystal, preparation method and use

A technology of optical crystals and compounds, applied in chemical instruments and methods, phosphorus compounds, crystal growth, etc., can solve the problems of high price, serious layered growth habit, and long growth cycle.

Active Publication Date: 2018-03-23
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the crystal growth technology of these materials has become increasingly mature, there are still obvious shortcomings: such as crystal deliquescence, long growth cycle, serious layered growth habit and expensive price, etc.

Method used

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  • Compound rubidium-lead-phosphorus-oxygen and rubidium-lead-phosphorus-oxygen optical crystal, preparation method and use
  • Compound rubidium-lead-phosphorus-oxygen and rubidium-lead-phosphorus-oxygen optical crystal, preparation method and use
  • Compound rubidium-lead-phosphorus-oxygen and rubidium-lead-phosphorus-oxygen optical crystal, preparation method and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] According to the reaction formula: (1) Rb 2 CO 3 +2PbO+2(NH 4 )H 2 PO 4 →2RbPbPO 4 +CO 2 ↑+2NH 3 ↑+3H 2 O ↑ Synthesis of RbPbPO 4 compound;

[0041] Rb 2 CO 3 , PbO, (NH 4 )H 2 PO 4 Weigh the raw materials with a molar ratio of 1:2:2 and put them into a mortar, mix and carefully grind them, then put them into a corundum crucible with an opening of Φ100mm×100mm, put them into a muffle furnace, raise the temperature slowly to 400°C, and keep the temperature constant for 12 hours , take out the crucible after cooling, grind the sample evenly, and then put it in the crucible, raise the temperature of the muffle furnace to 800°C, keep the temperature for 48 hours, take out the sample, put it into a mortar and grind it carefully to obtain a single-phase multi-phase compound of rubidium lead phosphorus oxide Crystal powder, and then X-ray analysis of the polycrystalline powder, the obtained X-ray spectrum and RbPbPO 4 The X-ray spectra of single crystals ground ...

Embodiment 2

[0048] According to the reaction formula: (2) Rb 2 CO 3 +2PbCO 3 +2(NH 4 )H 2 PO 4 →2RbPbPO 4 +3CO 2 ↑+2NH 3 ↑+3H 2 O ↑ Preparation of RbPbPO 4 compound;

[0049] Rb 2 CO 3 , PbCO 3 , (NH 4 )H 2 PO 4 Weigh the raw materials directly at a molar ratio of 1:2:2, mix them with the flux PbO at a molar ratio of 1:2, put them into an open platinum crucible of Φ80mm×80mm, and heat them at a heating rate of 80°C / h to 980°C, constant temperature for 30 hours, to obtain a rubidium-lead-phosphorus-oxygen mixed melt;

[0050] Lower the temperature of the mixed melt to 930°C. At this time, quickly extend the seed rod under the liquid surface, slowly lower the temperature to 850°C at a rate of 2°C / h, lift the seed rod out of the liquid surface, and the seed rod will There are aggregates, and then the temperature is lowered to room temperature at a rate of 50°C / h to obtain RbPbPO 4 seed crystal;

[0051] Crystal growth in the compound melt: the obtained rubidium-lead-phosph...

Embodiment 3

[0055] According to the reaction formula: (3) Rb 2 CO 3 +2Pb(NO 3 ) 2 +2(NH 4 )H 2 PO 4 →2RbPbPO 4 +CO 2 ↑+4NO 2 ↑+O 2 ↑+2NH 3 ↑+3H 2 O ↑ synthetic RbPbPO4 compound;

[0056] Rb 2 CO 3 , Pb(NO 3 ) 2 , (NH 4 )H 2 PO 4 Put it into a mortar with a molar ratio of 1:2:2, mix and grind it carefully, then put it into a corundum crucible with an opening of Φ100mm×100mm, put it into a muffle furnace, slowly raise the temperature to 400°C, keep the temperature for 12 hours, and after cooling Take out the crucible, grind the sample evenly, then place it in the crucible, raise the temperature of the muffle furnace to 800°C, keep the temperature for 48 hours, take out the sample, put it into a mortar and grind it carefully to obtain a single-phase polycrystalline powder of rubidium lead phosphorus oxide compound, Carry out X-ray analysis to this polycrystalline powder again, gained X-ray spectrogram and RbPbPO 4 The X-ray spectra of single crystals ground into powders a...

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PUM

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Abstract

The invention relates to a compound rubidium-lead-phosphorus-oxygen and rubidium-lead-phosphorus-oxygen optical crystal and its preparation method and application. The chemical formula of the compound rubidium-lead-phosphorus-oxygen is RbPbPO4, the molecular weight is 387.63, it belongs to the orthorhombic crystal system, the space group is Pnma, and the crystal The cell parameters are a=7.635(4)Å, b=5.750(3)Å, c=10.151(6)Å, V=445.6(4)Å3, Z=4. The rubidium-lead-phosphorus-oxygen compound was obtained by the solid-state reaction method. Then, the crystal is grown by the high-temperature melt method of the compound, and the rubidium-lead-phosphorus-oxygen optical crystal can be obtained. Its light transmission band is between 254nm and 2600nm. The crystal has moderate mechanical hardness and is easy to cut and polish. It is suitable for making detectors, aircraft, hoods, window materials in fairings, lenses or periscopes in microscopes and telescopes, Optical devices such as prisms that change the direction of light in binocular telescopes, spectrometers and other instruments.

Description

technical field [0001] The invention relates to a preparation method and application of a compound rubidium-lead-phosphorus-oxygen and rubidium-lead-phosphorus-oxygen optical crystal. The chemical formula of the compound is RbPbPO 4 . Background technique [0002] Due to their rich structural chemistry and their potential applications in optics, catalysis, magnetism, fuel, and bone medicine, inorganic phosphates have become a hot topic of research. Phosphorus atoms pass through sp 3 Hybridization bonds with oxygen atoms to form a rigid PO 4 tetrahedral group. PO 4 Tetrahedral groups can form polyanion groups of different configurations by sharing oxygen atoms, so that phosphate compounds have rich structural configurations. At the same time, due to its rigidity, chemical corrosion resistance and thermal stability, phosphate has some excellent properties, so it has been widely used. For example, KDP, DKDP, KTP, and ADP have been widely used due to their excellent nonlin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/14C30B15/00C01B25/45
Inventor 潘世烈黄生世韩健
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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