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Compound boron rubidium sulfate, boron rubidium sulfate crystal and preparation method thereof

A technology of rubidium borosulfate and compound, which is applied in the field of compound rubidium borosulfate and rubidium borosulfate crystals and its preparation, and can solve the problems that single crystal growth of rubidium borosulfate is rarely reported.

Active Publication Date: 2013-07-17
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

So far, there are few reports on the growth of functional materials rubidium borosulfate and large-sized single crystals of rubidium borosulfate with both boronyl and sulfuryl groups

Method used

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  • Compound boron rubidium sulfate, boron rubidium sulfate crystal and preparation method thereof

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Experimental program
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Embodiment 1

[0034] According to the reaction formula: 5Rb 2 SO 4 +3(NH 4 ) 2 SO 4 +2H 3 BO 3 →2Rb 5 BS 4 o 16 +6NH 3 ↑+6H 2 O ↑ adopt solid phase reaction method to synthesize Rb 5 BS 4 o 16 compound;

[0035] a. Rb 2 SO 4 , (NH 4 ) 2 SO 4 and H 3 BO 3 Put it into a mortar with a molar ratio of 5:3:2, 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 500°C, keep the temperature constant for 48 hours, take out the sample, put it into a mortar and grind carefully to obtain a single-phase polycrystalline powder of rubidium borosulfate compound, and then Carry out X-ray analysis to this polycrystalline powder, gained X-ray spectrogram and Rb 5 BS 4 o 16 The X-ray spectra of sing...

Embodiment 2

[0042] According to the reaction formula: 5Rb 2 CO 3 +8(NH 4 ) 2 SO 4 +2H 3 BO 3 →2Rb 5 BS 4 o 16 +16NH 3 ↑+11H 2 O↑+5CO 2 ↑ Synthesis of Rb 5 BS 4 o 16 compound;

[0043] a. Rb 2 CO 3 , (NH 4 ) 2 SO 4 and H 3 BO 3 Put it into a mortar with a molar ratio of 5:8:2, mix it carefully and grind it carefully, then put it into a corundum crucible with an opening of Φ100mm×100mm, put it into a muffle furnace, raise the temperature slowly to 400°C, keep the temperature constant for 12 hours, take it out after cooling Crucible, grind the sample evenly, and then put it in the crucible, raise the temperature of the muffle furnace to 500 ° C, take out the sample after 48 hours of constant temperature, put it into a mortar and grind carefully to obtain a single-phase polycrystalline powder of rubidium borosulfate compound, and then The polycrystalline powder is subjected to X-ray analysis, and the obtained X-ray spectrum is consistent with that of Rb 5 BS 4 o 16 Th...

Embodiment 3

[0050] According to the reaction formula: 5Rb 2 O+8(NH 4 ) 2 SO 4 +B 2 o 3 →2Rb 5 BS 4 o 16 +16NH 3 ↑+8H 2 O ↑ synthesis of Rb 5 BS 4 o 16 compound;

[0051] Rb 2 O, (NH 4 ) 2 SO 4 and H 3 BO 3 Weigh the raw materials directly according to the molar ratio of 5:8:1, and combine the weighed raw materials with the flux PbO-H 3 BO 3 Mixing at a molar ratio of 1:4, where PbO and H 3 BO 3The molar ratio is 1:3, put it into an open platinum crucible of Φ80mm×80mm, heat it to 480°C at a temperature increase rate of 1°C / h, and keep the temperature for 12 hours to obtain rubidium borosulfate Rb 5 BS 4 o 16 mixed melt;

[0052] Lower the temperature of the mixed melt to 440°C, quickly extend the seed rod under the liquid surface, slowly lower the temperature by 30°C at a rate of 1°C / h, lift the seed rod out of the liquid surface, there will be aggregates on the seed rod, Then lower the temperature to room temperature at a rate of 10°C / h to obtain rubidium borosu...

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Abstract

The invention relates to a compound boron rubidium sulfate, a boron rubidium sulfate crystal and a preparation method thereof. The chemical formula of the compound is Rb5BS4O16, the molecular weight is 822.40, the chemical formula of the compound boron rubidium sulfate crystal is Rb5BS4O16, the molecular weight is 822.40, the compound boron rubidium sulfate crystal belongs to a tetragonal system, the space group is P43212, the cell parameters are as follows: a is equal to 10.148(4) A0, c is equal to 16.689(14) A0, Z is equal to 4, V is equal to 1718.8(17) A3, the boron rubidium sulfate compound is prepared by a solid reaction process, the compound is used for growing crystal through a flux growth method to obtain the boron rubidium sulfate crystal, the prepared crystal has a large dimension of at least centimeter level, and the crystal has the advantages of wide transmission waveband, fast preparation speed, simplicity in operation, short growth period, good mechanical property and easiness for processing, and the like.

Description

technical field [0001] The invention relates to a compound rubidium borosulfate and rubidium borosulfate crystal and a preparation method. Background technique [0002] The in-depth research in the field of optoelectronics and the continuous development of new materials make optoelectronic crystals play an extremely important role and have huge potential applications in many fields. These studies and applications put forward higher physical and chemical requirements for optoelectronic crystals, making people explore optoelectronic crystal materials with multifunctional groups. [0003] Having both boroxy and sulfoxy groups in one crystal could make it a functional material with new properties. So far, there have been few reports on the growth of functional materials rubidium borosulfate and large-sized single crystals of rubidium borosulfate with both boronoxy and sulfoxy groups. Therefore, there is a need for a method for synthesizing rubidium borosulfate and growing larg...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/24C30B9/12C30B17/00
Inventor 潘世烈董凌云
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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