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Czochralski growing method of magnesium aluminate spinel crystal doped with transition metal ions

A transition metal, magnesium-aluminum spinel technology, applied in the direction of crystal growth, single crystal growth, single crystal growth, etc., can solve the problems of poor crystal quality, difficult to use, small diameter, etc., to achieve high-quality results

Active Publication Date: 2014-08-27
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2006 and 2008, AnisJouinia .etc and P. Lombard .etc grew Mn:MgAl by micro pull-down method respectively 2 o 4 and Ti:MgAl 2 o 4 Crystal (see J.Cryst. Growth 293 (2006) 517 and J.Cryst. Growth, 311(2009) 899); in 2004 and 2005, Ayana Tomita .etc and TokushiSatoa .etc grew Mn:MgAl by floating zone method 2 o 4 and Ti:MgAl 2 o 4 crystals (see J.Lumin. 109 (2004) 19 and J.Lumin. 114 (2005) 155); in 1990 and 1997, l. E. Bausa.etc and N.V. Kuleshova.etc used the flame method to grow Ti: MgAl 2 o 4 and Ni:MgAl 2 o 4 Crystal (see J. appl. Phys. 68(1990) 457 and J. Lumin. 71 (1997) 265); in 1968, D. L. Wood .etc obtained Cr:MgAl by molten salt method 2 o 4 Crystal (see J. Chem. Phys. 48 (1968) 5255), studies have shown that these doped magnesium aluminum spinel crystals are promising laser materials in the visible light band, but the quality of crystals grown by these methods is poor, and the crystals inside There are defects such as inclusions and internal cores, or the shape of the crystal is long and small in diameter, which is difficult to meet the needs of practical use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A method for growing magnesium-aluminum spinel crystals doped with transition group metal ions, the specific steps of which are as follows:

[0026] (1) Preparation of Cr 3+ The doping concentration is 0.05at% magnesium aluminum spinel single crystal, let Cr 3+ The effective segregation coefficient is k, and TM=Cr 2 o 3 , x=0.0005, using MgAl 2 o 4 Polycrystalline and Cr 2 o 3 Powder as raw material, according to Cr 2 o3 :MgAl 2 o 4 =0.0005 / k :(1-0.0005 / k ) ratio to weigh the ingredients;

[0027] (2) Put the initial raw material for crystal growth into the iridium crucible, and place the MgAl in the direction 2 o 4 Install the seed crystal on the seed crystal rod, close the furnace door, evacuate to below 10Pa, set the heating program to heat up the molten material;

[0028] (3) After the raw materials in the pot are completely melted, keep it for a period of time, and carry out crystal growth at a speed of 10r / min and a pulling speed of 1.2mm / h.

[0...

Embodiment 2

[0031] A method for growing magnesium-aluminum spinel crystals doped with transition group metal ions, the specific steps of which are as follows:

[0032] (1) Preparation of Ti 3+ The doping concentration is 0.05at% magnesium aluminum spinel single crystal, let Ti 3+ The effective segregation coefficient is k, and TM=Ti 2 o 3 , x=0.0005, using MgAl 2 o 4 Polycrystalline and Ti 2 o 3 Powder as raw material, according to Ti 2 o 3 :MgAl 2 o 4 =0.0005 / k :(1-0.0005 / k ) ratio to weigh the ingredients;

[0033] (2) Put the initial raw material for crystal growth into the iridium crucible, and place the MgAl in the direction 2 o 4 Install the seed crystal on the seed crystal rod, close the furnace door, evacuate to below 10Pa, set the heating program to heat up the molten material;

[0034] (3) After the raw materials in the pot are completely melted, keep it for a period of time, and carry out crystal growth at a speed of 12r / min and a pulling speed of 1.5mm / h.

...

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PUM

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Abstract

The invention discloses a growing method of a magnesium aluminate spinel crystal doped with transition metal ions. The molecular formula of the crystal can be expressed as TM2xMgAl2(1-x)O4 and Tm'yMg1-yAl2O4 (TM=Ti<3+>, Cr<3+>, Fe<3+> and Ni<3+>; TM'=Mn<2+>, V<2+> and Co<2+>, 0<x<1, and 0<y<1). The growing method is characterized in that MgAl2O4 polycrystalline raw materials synthesized with the flame method and transition metal oxides prepared according to the proportional concentration are placed in an iridium crucible and sufficiently heated to be molten, the magnesium aluminate spinel crystal or the doped magnesium aluminate spinel crystal is adopted as a seed crystal, and crystal growth is conducted with the Czochralski method. According to the method, the crystal with the large size and high quality can be obtained and be expected to be applied to the fields of micromachining, laser medicine, laser chemistry, laser printing, military application, underwater communication and axis isotope separation.

Description

technical field [0001] The invention relates to a growth method of magnesium-aluminum spinel crystals doped with transition group metal ions, and belongs to the technical field of crystal growth. Background technique [0002] At present, the fields of microprocessing, laser medical treatment, laser chemistry, laser printing, military application, underwater communication and axial isotope separation urgently require the development of solid-state lasers to short wavelengths. Magnesia-aluminum spinel single crystal doped with transition metal ions is expected to become a short-wavelength laser material and has attracted widespread attention in the world. in MgAl 2 o 4 Incorporation of transition metal ions such as Cr 3+ , Ti 3+ etc., due to the interaction between the spinel crystal field and the dopant ions, the energy state of the ions is split and changed, so that the activated ions generate the energy level structure of the short-wavelength laser output in the crystal...

Claims

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Application Information

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IPC IPC(8): C30B29/22C30B15/00
Inventor 孙贵花张庆礼殷绍唐孙敦陆刘文鹏罗建乔王小飞谷长江
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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