Alkali metal borate compounds, single-crystal and preparation method thereof

A boroaluminate compound and a technology of boroaluminate, applied in chemical instruments and methods, single crystal growth, single crystal growth, etc., can solve problems such as difficulty in obtaining large-size high-quality single crystals, difficulty in crystal growth, etc., and achieve easy Processing and preservation, moderate hardness, good mechanical properties

Inactive Publication Date: 2008-06-04
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] K has been found in boroaluminate compounds 2 al 2 B 2 o 7 (KABO) crystal, BaAl 2 B 2 o 7 (BABO) crystals ("Two new nonlinear optical crystals: BaAl 2 B 2 o 7 and KAl 2 B 2 o 7 , SPIE, Vol.3556, 21, 1998", BaAlBO 3 f 2 (BABF) crystals ("Japanese Journal of Applied Physics" 241(10B): 1131, 2002), etc., they all have nonlinear optical effects, but crystal growth is difficult, and it is difficult to obtain large-size high-quality single crystals

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Preparation of NaBa 4 al 2 B 8 o 18 Cl 3 compound.

[0041] Adopt solid phase reaction method, reaction equation is as follows:

[0042] NaCl+BaCl 2 +3BaCO 3 +Al 2 o 3 +8H 3 BO 3 =NaBa 4 al 2 B 8 o 18 Cl 3 +3CO 2 +12H 2 O↑

[0043] The dosage of the above reagents: NaCl: 0.05mol; BaCl 2 : 0.05mol; BaCO 3 : 0.15mol; Al 2 o 3 : 0.05mol; H 3 BO 3 : 0.40mol.

[0044] The specific operation steps are: weigh the reagents according to the above dosage, mix them in a mortar and grind them thoroughly, then put them into a Φ50mm×50mm open platinum crucible, compact them, put them into a muffle furnace, and slowly rise to 750°C, the heating rate is 5°C / hour, constant temperature for 10 hours, take out the crucible after cooling, at this time the sample is loose, take out the sample and grind it again, then put it in the crucible for compaction, in the muffle furnace at 800 ℃ sintering for 96 hours, at this time the sample shrank into a block. At this tim...

Embodiment 2

[0046] Preparation of KBa 4 al 2 B 8 o 18 Cl 3 compound.

[0047] Adopt solid phase reaction method, reaction equation is as follows:

[0048] KCl+BaCl 2 +3Ba(OH) 2 +Al 2 o 3 +4B 2 o 3 = KBa 4 al 2 B 8 o 18 Cl 3 +3H 2 O↑

[0049] The dosage of the above reagents: KCl: 0.05mol; BaCl 2 : 0.05mol; Ba(OH) 2 : 0.15mol; Al 2 o 3 : 0.05mol; B 2 o 3 : 0.20mol.

[0050] The specific operation steps are: weigh the reagents according to the above dosage, mix them in a mortar and grind them thoroughly, then put them into a Φ50mm×50mm open platinum crucible, compact them, put them into a muffle furnace, and slowly rise to 750°C, the heating rate is 10°C / hour, constant temperature for 20 hours, take out the crucible after cooling, at this time the sample is loose, take out the sample and re-grind and mix, then put it in the crucible for compaction, in the muffle furnace at 810 ℃ sintering for 72 hours, at which time the sample shrank into a block. At this point, ta...

Embodiment 3

[0052] Preparation of RbBa 4 al 2 B 8 o 18 Cl 3 compound.

[0053] Adopt solid phase reaction method, reaction equation is as follows:

[0054] RbCl+BaCl 2 2H 2 O+3BaCO 3 +2Al(OH) 3 +4B 2 o 3 =

[0055] RbB 4 al 2 B 8 o 18 Cl 3 +5H 2 O↑+3CO 2 ↑

[0056] The dosage of the above reagents: RbCl: 0.05mol; BaCl 2 2H 2 O: 0.05mol; BaCO 3 : 0.15mol; Al(OH) 3 : 0.10mol; B 2 o 3 : 0.20mol.

[0057]The specific operation steps are: weigh the reagents according to the above dosage, mix them in a mortar and grind them thoroughly, then put them into a Φ50mm×50mm open platinum crucible, compact them, put them into a muffle furnace, and slowly rise to 750°C, the heating rate is 15°C / hour, constant temperature for 30 hours, take out the crucible after cooling, at this time the sample is loose, take out the sample and re-grind and mix, then put it in the crucible for compaction, in the muffle furnace at 820 ℃ sintering for 48 hours, at this time the sample shrank int...

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PUM

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Abstract

The invention provides an alkali metal boro-ahuminate compound and a monocrystal and a preparation method thereof, wherein the molecular formulas of the alkali metal boro-ahuminate compound and the monocrystal thereof are the MBa4Al2B8O18Cl3 in which the M is Na and the K is Rb or Cs and which belongs to the tetragonal system, the space group is P4<2>nm without center of symmetry; the preparation of the compound is that the compound materials containing M, Ba, Al, B, O and Cl elements is evenly mixed according to the mol ratio of the M, Ba, Al, B, O and Cl elements of 1:4:2:8:18:3, and is heated for making the solid phase reaction, getting the compound; the preparation of the monocrystal is that the alkali metal boro-ahuminate is made based on the flux growth method, the fluxing agent is the lithium fluoride, the sodium fluoride or the lithium chloride; the mol ratio between the alkali metal boro-ahuminate and the fluxing agent is 1:6 to 15; the second harmonic generation of the made compound powder nearly doubles the DKP; the crystal has relative wide transmission wave band, proper hardness and good mechanical performance and is uneasy for break and deliquescence and easy to process and store.

Description

technical field [0001] The invention belongs to the field of compounds and their single crystals and preparation methods, in particular to an alkali metal boroaluminate compound and its single crystal and its preparation method; the chemical formula of the alkali metal boroaluminate compound and its single crystal is MBa 4 Al 2 B 8 o 18 Cl 3 , where M is an alkali metal Na, K, Rb or Cs. technical background [0002] In modern laser technology, the laser wavelengths that can be directly obtained by using laser crystals are limited, and there are still blank bands in the ultraviolet to infrared spectral regions. Nonlinear optical crystals have attracted much attention because they can effectively broaden the wavelength range of lasers. Here, nonlinear optical crystals refer to crystals with nonlinear optical effects. Nonlinear optical effects refer to effects such as frequency doubling, sum frequency, difference frequency, optical parametric oscillation or amplification. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/10
Inventor 吴以成张书峰李云阁傅佩珍
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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