Preparation method of transforming yttrium aluminum garnet doped ceramic into single crystal

A technology of yttrium aluminum garnet and single crystal, which is applied in the field of single crystal preparation by non-melting method, can solve the problems of uneven composition and low doping, achieve uniform composition, high doping concentration, and increase controllability Effect

Inactive Publication Date: 2014-05-28
SOUTH WEST INST OF TECHN PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to solve the problems in the above-mentioned prior art, and provide a kind of doped yttrium aluminum garnet with simple operation, strong controllability, short production cycle, low cost (no need for iridium crucible), and uniform composition. Solid-state crystal growth method to solve the problems of low doping and uneven composition in the prior art

Method used

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  • Preparation method of transforming yttrium aluminum garnet doped ceramic into single crystal
  • Preparation method of transforming yttrium aluminum garnet doped ceramic into single crystal
  • Preparation method of transforming yttrium aluminum garnet doped ceramic into single crystal

Examples

Experimental program
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Effect test

Embodiment 1

[0036] Neodymium nitrate hexahydrate (Nd(NO 3 ) 3 ·6H 2 O), yttrium nitrate hexahydrate (Y(NO 3 ) 3 ·6H 2 O), aluminum ammonium sulfate dodecahydrate (NH 4 Al(SO 4 ) 2 12H 2 O) Feedstock, ammonium bicarbonate (NH 4 HCO 3 ) as a precipitant, and the coprecipitation method was used to synthesize Nd 0.06 Y 2.94 Al 5 o 12 The precursor was calcined at 900°C for 2 hours to synthesize highly active and highly dispersed Nd with an average particle size of 20 nm 0.06 Y 2.94 Al 5 o 12 Nano powder. Using 0.14% SiO by powder weight 2 As a sintering aid, it is mixed in Nd by ball milling method 0.06 Y 2.94 Al 5 o 12 Among the powder raw materials, the ball milling medium is high-purity agate balls, and the ball milling solvent is alcohol. The total volume of powder: the volume of agate balls: the volume of alcohol = 1:2:4. After ball milling for 48 hours, the Nd 0.06 Y 2.94 Al 5 o 12 The slurry was poured into a glass flask, and then dried in an oven at 80° C. f...

Embodiment 2

[0042] Erbium nitrate hexahydrate (Er(NO 3 ) 3 ·6H 2 O), yttrium nitrate hexahydrate (Y(NO 3 ) 3 ·6H 2 O), aluminum ammonium sulfate dodecahydrate (NH 4 Al(SO 4 ) 2 12H 2 O) Feedstock, ammonium bicarbonate (NH 4 HCO 3 ) as a precipitant, and the co-precipitation method was used to synthesize Er 0.6 Y 2.4 Al 5 o 12 The precursor was calcined at 1100°C for 2 hours to synthesize highly active and highly dispersed Er with an average particle size of 55 nm. 0.6 Y 2.4 Al 5 o 12 Nano powder; use 0.14% SiO by powder weight 2 and 0.08% MgO as a sintering aid, and mixed in Er 0.6 Y 2.4 Al 5 o 12 Among the powder raw materials, the ball milling medium is high-purity agate balls, and the ball milling solvent is alcohol. The total volume of powder: the volume of agate balls: the volume of alcohol = 1:2:5. After 36 hours of ball milling, the Er 0.6 Y 2.4 Al 5 o 12 The slurry was poured into a glass flask, and then dried in an oven at 80° C. for 120 hours. After th...

Embodiment 3

[0048] With cerium nitrate hexahydrate (Ce(NO 3 ) 3 ·6H 2 O), yttrium nitrate hexahydrate (Y(NO 3 ) 3 ·6H 2 O), aluminum ammonium sulfate dodecahydrate (NH 4 Al(SO 4 ) 2 12H 2 O) Feedstock, ammonium bicarbonate (NH 4 HCO 3 ) as the precipitating agent, the Ce was synthesized by co-precipitation method 0.09 Y 2.91 Al 5 o 12The precursor was calcined at 1300°C for 4 hours to synthesize highly active and highly dispersed Ce with an average particle size of 200 nm 0.09 Y 2.91 Al 5 o 12 Nano powder; use 0.14% SiO by powder weight 2 , 0.08%MgO, and 0.78%LiF are used as sintering aids, and they are mixed in Ce by ball milling 0.09 Y 2.91 Al 5 o 12 Among the powder raw materials, the ball milling medium is high-purity agate balls, and the ball milling solvent is alcohol. The total volume of powder: the volume of agate balls: the volume of alcohol = 1:2:5. After ball milling for 24 hours, the YAG slurry was poured into a glass flask, and then dried in an oven at 8...

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Abstract

The invention provides a preparation method for transforming yttrium aluminum garnet doped ceramic into a single crystal. The method aims at providing a solid-state crystal growth method with strong controllability and uniform yttrium aluminum garnet doped crystal components. The method is realized through the following technical scheme: at least one of silicon dioxide, magnesium oxide and lithium fluoride is added in nanometer yttrium aluminum garnet doped ceramic powder according to 0.2% to 1% of powder weight to serve as a sintering additive and then the sintering additive takes alcohol as a medium ball mill with an agate ball; heating is carried out under flow oxygen atmosphere at a temperature of 600 to 800 DEG C, the powder is placed into a stainless steel grinding tool again to form a ceramic biscuit in a dry-pressed manner, furthermore, cold isostatic pressing is carried out on the ceramic biscuit, and heat preservation is implemented under the vacuum degree higher than 10-3 Pa and the temperature being greater than 1550 DEG C to obtain the doped yttrium aluminum garnet ceramic; a yttrium aluminum garnet crystal and the doped yttrium aluminum garnet ceramic are in a light glue combination to form a complex, and an argon treatment is carried out for 20 hours at the temperature higher than 1600 DEG C and the high pressure of 0 to 300 MPa; the heat preservation is carried out on a yttrium aluminum garnet doped single crystal for 100 hours under hydrogen, oxygen or air atmosphere at a temperature higher than 1200 DEG C.

Description

technical field [0001] The invention belongs to the field of single crystal preparation by a non-melting method, in particular to a solid-state crystal growth preparation method of doped yttrium aluminum garnet single crystal. Background technique [0002] Rare earth doped yttrium aluminum garnet (chemical formula is Re x Y 3-x Al 5 o 12 , referred to as Re:YAG) belongs to the cubic crystal system, has no birefringence effect, has the advantages of high melting point, good mechanical and thermal conductivity, and can maintain stable optical properties under long-term optical pump radiation conditions. Its single crystal has become the most important One of the solid-state laser materials. It can be used for material processing, laser breeding, laser medical treatment, laser information storage, laser communication, laser ranging and target indication, etc. Due to the limitations of the growth and preparation of Re:YAG crystals, it can no longer meet the development need...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/28C30B1/12C30B33/02
Inventor 张伟张志斌邓杰罗辉梁松林
Owner SOUTH WEST INST OF TECHN PHYSICS
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