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Compound trirubidium 9-hydroxytrichloroheptaborate, birefringent crystal of trirubidium 9-hydroxytrichloroheptaborate and preparation method and application of birefringent crystal

A technology of hydroxytrichloroheptaboric acid and birefringent crystals, applied in chemical instruments and methods, boron compounds, crystal growth, etc., can solve the birefringence of quartz crystals that can only be used in Rochester prisms and cannot be directly used in the ultraviolet region minor issues

Pending Publication Date: 2022-07-29
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

Take MgF 2 For example, its transmission range is 110-8500nm, it is a good crystal material for deep ultraviolet, but its birefringence is too small, it is not suitable for making Glan prism, it can only be used for Luo Hungarian prism, and the separation angle of light speed is small, the size of the period is large, and it is inconvenient to use; the birefringence of quartz crystal is also small, and the same problem exists; YVO 4 The crystal is also an artificially prepared birefringent crystal, and due to the YVO 4 The melting point is high, and the iridium crucible must be used for pulling growth, and the growth atmosphere is a weak oxygen atmosphere, so there is a problem of price change of yttrium element during growth, which reduces the quality of the crystal, making it difficult to obtain high-quality crystals and its penetration. The range is 400-5000nm, it cannot be directly used in the ultraviolet region
Calcite in natural form is a birefringent crystal that is widely used, but its impurity content is relatively high. Ordinary crystals can only be used in the band above 350nm. It is difficult to obtain ultraviolet optical grade calcite crystals, and its use band cannot reach the deep ultraviolet region ( <250nm)
Rutile also mainly exists in natural form, and it is difficult to synthesize artificially, and it is small in size, high in hardness, and difficult to process
Several borate birefringent crystals have been reported in recent years: the high-temperature phase BaB 2 o 4 The transmission range of the crystal is 189-3500nm, and the birefringence is relatively large, but the crystal has phase transition, which is easy to crack during the crystal growth process, which affects the yield and utilization of the crystal.

Method used

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  • Compound trirubidium 9-hydroxytrichloroheptaborate, birefringent crystal of trirubidium 9-hydroxytrichloroheptaborate and preparation method and application of birefringent crystal
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  • Compound trirubidium 9-hydroxytrichloroheptaborate, birefringent crystal of trirubidium 9-hydroxytrichloroheptaborate and preparation method and application of birefringent crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Preparing Compounds:

[0042] According to the reaction formula: 3RbCl+7H 3 BO 3 =Rb 3 [B(OH) 3 ][B 3 O 3 (OH) 3 ] 2 Cl 3 +6H 2 O synthesis compound Rb 3 [B(OH) 3 ][B 3 O 3 (OH) 3 ] 2 Cl 3 :

[0043] RbCl and H were combined in a molar ratio of rubidium:boron of 3:7 3 BO 3 Weigh it into a mortar, add 5mL of deionized water and grind it carefully, then put it into a 100mL open glass beaker, put it into a magnetic heating stirrer, slowly heat it up to 80 °C, and keep it at a constant temperature for 1 hour. After the sample is dried Take it out, and fully grind it to obtain a single-phase polycrystalline powder of trirubidium nonahydroxytrichloroheptaborate compound, put it into a mortar and grind for X-ray analysis, the obtained X-ray spectrum and Rb 3 [B(OH) 3 ][B 3 O 3 (OH) 3 ] 2 Cl 3 The X-ray spectra obtained from the single crystal structure are consistent.

Embodiment 2

[0045] Preparing Compounds:

[0046] According to the reaction formula: 3RbOH+7H 3 BO 3 +3HCl=Rb 3 [B(OH) 3 ][B 3 O 3 (OH) 3 ] 2 Cl 3 +9H 2 O synthesis compound Rb 3 [B(OH) 3 ][B 3 O 3 (OH) 3 ] 2 Cl 3 :

[0047] According to the molar ratio of rubidium:boron:chlorine 3:7:3, RbOH, H 3 BO 3 and HCl were weighed into a mortar, and 5 mL of deionized water was added to grind carefully, then put into a 100 mL corundum crucible, placed in a magnetic heating stirrer, slowly heated to 85 ° C, and kept at a constant temperature for 1 hour, after the sample was dried Take it out, and fully grind it to obtain a single-phase polycrystalline powder of trirubidium nonahydroxytrichloroheptaborate compound, put it into a mortar and grind for X-ray analysis, the obtained X-ray spectrum and Rb 3 [B(OH) 3 ][B 3 O 3 (OH) 3 ] 2 Cl 3 The X-ray spectra obtained from the single crystal structure are consistent.

Embodiment 3

[0049] Preparing Compounds:

[0050] According to the reaction formula: 3Rb 2 O+14H 3 BO 3 +6HCl=2Rb 3 [B(OH) 3 ][B 3 O 3 (OH) 3 ] 2 Cl 3 +15H 2 O synthesis compound Rb 3 [B(OH)3 ][B 3 O 3 (OH) 3 ] 2 Cl 3 :

[0051] According to the molar ratio of rubidium:boron:chlorine 3:7:3, Rb 2 O, H 3 BO 3 Weigh and HCl into a mortar and add 5mL of deionized water to grind carefully, then put it into a 100mL open glass beaker, put it in a water bath, slowly heat up to 80 °C, keep the temperature for 1.5 hours, and take out the sample after drying. , and fully ground to obtain a single-phase polycrystalline powder of trirubidium nonahydroxytrichloroheptaborate compound, which was put into a mortar and ground for X-ray analysis, and the obtained X-ray spectrum and Rb 3 [B(OH) 3 ][B 3 O 3 (OH) 3 ] 2 Cl 3 The X-ray spectra obtained from the single crystal structure are consistent.

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Abstract

The invention relates to a compound trirubidium 9-hydroxytrichloroheptaborate, a birefringent crystal of the trirubidium 9-hydroxytrichloroheptaborate and a preparation method and application of the birefringent crystal of the trirubidium 9-hydroxytrichloroheptaborate, the molecular formula of the compound is Rb3 [B (OH) 3] [B3O3 (OH) 3] 2Cl3, the molecular weight of the compound is 687.50, and the compound is prepared by adopting a mild solvent evaporation method. The chemical formula of the crystal is Rb3 [B (OH) 3] [B3O3 (OH) 3] 2Cl3, the molecular weight is 687.50, the crystal belongs to a hexagonal system, the space group is P63 / m, the cell parameters a are equal to 13.7234 (9), b is equal to 13.7234 (9), c is equal to 6.5167 (5), V is equal to 1062.87 (16) 3, Z is equal to 2, the crystal is grown by adopting a room temperature solution method or a hydrothermal method, the ultraviolet transmission cut-off edge of the crystal is 180 nm, and the birefringence is about 0.120 (532 nm). The nonahydroxy trichloro rubidium heptaborate birefringent crystal disclosed by the invention is moderate in mechanical hardness and easy to grow, cut, polish and store; the high birefringence is realized; the method has important application in the fields of optics and communication, and can be used for manufacturing polarization beam splitting prisms, phase delay devices, electro-optical modulators and the like.

Description

technical field [0001] The invention relates to a compound trirubidium nonahydroxytrichloroheptaborate and trirubidium nonahydroxytrichloroheptaborate birefringent crystal, preparation method and application, in particular to a compound whose molecular formula is Rb for visible light-deep ultraviolet waveband 3 [B(OH) 3 ][B 3 O 3 (OH) 3 ] 2 Cl 3 A birefringent crystal of trirubidium nonahydroxytrichloroheptaborate. Background technique [0002] Birefringence refers to the phenomenon that a beam of light is projected onto the surface of a crystal to produce two beams of refracted light. The fundamental reason for this phenomenon is the anisotropy of the crystal material. When light propagates in an optically heterogeneous homogeneous body (such as a crystal other than a cubic system), in addition to a few special directions (along the optical axis), its vibration characteristics will be changed, and it will be decomposed into two electric field vector vibration directio...

Claims

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Application Information

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IPC IPC(8): C30B29/12C01B35/00C30B7/04C30B7/10C30B7/14
CPCC30B29/12C30B7/04C30B7/10C30B7/14C01B35/00C01P2002/72
Inventor 潘世烈焦佳豪张敏
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI