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Preparation method of millimeter-scale tubular R'xR1-xAl3(BO3)4 crystals

An xr1-xal3, millimeter-level technology, applied in the field of macroscopic tubular crystal preparation, can solve problems such as non-reporting

Inactive Publication Date: 2012-10-17
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

These two types of crystals can be grown into centimeter-scale bulk crystals by the commonly used flux method. However, R′ with tubular structure has not been reported yet. x R 1-x Al 3 (BO 3 ) 4 the crystal

Method used

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  • Preparation method of millimeter-scale tubular R'xR1-xAl3(BO3)4 crystals
  • Preparation method of millimeter-scale tubular R'xR1-xAl3(BO3)4 crystals
  • Preparation method of millimeter-scale tubular R'xR1-xAl3(BO3)4 crystals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Example 1: Spontaneous Crystallization Preparation of Millimeter-scale Tubular R' x R 1-x al 3 (BO 3 ) 4 the crystal

[0044] Take YAl 3 (BO 3 ) 4 powder, high purity B 2 o 3 As raw material, according to the molar ratio of YAl 3 (BO 3 ) 4 :B 2 o 3 =1:25 ingredients (at this time R=Y; x=0) weigh 33.76g YAl 3 (BO 3 ) 4 Powder, 144.77g B 2 o 3 After grinding and mixing the weighed raw materials evenly, put them into an open platinum crucible of φ60mm×50mm, melt them in a muffle furnace at 1150°C, and after cooling to room temperature, put the above platinum crucible into a crystal growth furnace and heat up to 1200°C to completely melt the material in the crucible into a high-temperature solution, keep at this temperature for 8 hours to fully homogenize the high-temperature solution; then cool down at a rate of 1.5°C / h to spontaneously nucleate and grow; wait until the temperature drops to 900°C When the temperature is lowered to room temperature at a r...

Embodiment 2

[0047] Example 2: Spontaneous Crystallization Preparation of Millimeter-scale Tubular R' x R 1-x al 3 (BO 3 ) 4 the crystal

[0048] Take YAl 3 (BO 3 ) 4 powder, high-purity B 2 o 3 and analytically pure Li 2 O, Na2 O is the raw material, according to the molar ratio of YAl 3 (BO 3 ) 4 :B 2 o 3 : Li 2 O:Na 2 O=1:5:1:1 ingredients (R=Y; x=0), weigh 101.28g YAl 3 (BO 3 ) 4 Powder, 87.02g B 2 o 3 , 7.47g Li 2 O, 15.50g Na 2 O; After grinding and mixing the weighed raw materials evenly, put them into an open platinum crucible of φ60mm×50mm, melt them in a muffle furnace at 1180°C, and after cooling to room temperature, put the above platinum crucible into a crystal growth furnace and heat up To 1160°C, the material in the crucible is completely melted into a high-temperature solution, and kept at this temperature for 20 hours to fully homogenize the high-temperature solution; then the temperature is lowered at a rate of 0.5°C / h to spontaneously nucleate and ...

Embodiment 3

[0051] Example 3: Spontaneous Crystallization Preparation of Millimeter-scale Tubular R' x R 1-x Al 3 (BO 3 ) 4 the crystal

[0052] YbAl 3 (BO 3 ) 4 powder, high-purity B 2 o 3 and analytically pure SrC 2 o 4 .H 2 O is the raw material, according to the molar ratio YbAl 3 (BO 3 ) 4 :B 2 o 3 : SrC 2 o 4 .H 2 O=1:5:1 ingredients (R=Yb; x=0), weigh 122.31g YbAl 3 (BO 3 ) 4 Powder, 87.02g B 2 o 3 , 48.42g SrC 2 o 4 .H 2 O, the molar ratio of YbAl in the growth system 3 (BO 3 ) 4 :B 2 o 3 : SrO=1:5:1; after grinding and mixing the weighed raw materials evenly, put them into an open platinum crucible of φ60mm×50mm, melt them in a muffle furnace at 1250°C, and after cooling to room temperature, put the above platinum crucible Put it into a crystal growth furnace, raise the temperature to 1160°C, completely melt the material in the crucible into a high-temperature solution, and keep it at this temperature for 24 hours to fully homogenize the high-tempe...

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Abstract

A preparation method of millimeter-scale tubular R'xR1-xAl3(BO3)4 crystals comprises the following steps of: mixing a R'xR1-xAl3(BO3)4 compound or a raw material which makes up the compound with B containing a B compound and MPhiO according to the mol ratio of 1:2-50:0-6, placing into a muffle furnace of 1150-1250 DEG C for fusing, cooling to room temperature to obtain a raw material for crystal growth, placing the raw material for crystal growth into a heating furnace, heating until it is completely fused so as to obtain a high-temperature solution, standing at constant temperature or stirring to homogenize the high-temperature solution, cooling to room temperature at 0.1-5 DEG C / h, cooling to room temperature at 10-60 DEG C / h to obtain a millimeter-scale tubular R'xR1-xAl3(BO3)4 solid crystal substance, and boiling by the use of an acid solution to obtain the millimeter-scale tubular R'xR1-xAl3(BO3)4 crystals. The method provided by the invention can be used to obtain macroscopic hollow hexagonal-prism tubular crystals, belongs to spontaneous nucleation growth, and is simple and high-efficient.

Description

technical field [0001] The invention relates to a method for preparing macroscopic tubular crystals, in particular to a millimeter-scale tubular R' x R 1-x Al 3 (BO 3 ) 4 A method for preparing nonlinear optical crystals and laser self-frequency doubling crystals. Background technique [0002] In recent years, one-dimensional tubular hollow structures have been widely concerned in the field of nanometer and micrometer. Since the discovery of carbon nanotubes, various nanometer or microtubes have been synthesized, such as boron nitride (BN), boron carbide ( BC), and zinc oxide ZnO nanotubes that have attracted much attention. The objects of research are often the field emission, light absorption, gas adsorption, catalytic activity, magnetic properties, conductivity, etc. of nanotubes. At the same time, nanotubes also have potential applications in the fields of interface materials and medical biology. However, the preparation of tubular crystals has always been limited ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/22C30B7/08
Inventor 胡章贵曹自立余雪松岳银超
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI