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A kind of preparation method of rare earth garnet single crystal

The technology of garnet and yttrium iron garnet is applied in the field of preparation of rare earth garnet single crystal, which can solve the problems of deviation of melt composition, low solute content, lower growth temperature, etc., so as to avoid the deviation of single crystal composition, Overcome the effect of severe component deviation

Active Publication Date: 2021-11-05
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The use of these fluxes greatly reduces the growth temperature, but due to the low content of the solute itself, the melt composition will gradually deviate from the established composition as the growth time prolongs.

Method used

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  • A kind of preparation method of rare earth garnet single crystal

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Comparison scheme
Effect test

Embodiment 1

[0023] A preparation method of rare earth garnet single crystal adopts multi-layer thickening method, comprising the following steps:

[0024] (1) Preparation of polycrystalline material: according to the crystal molecular formula Y (2.9-x) Yb x Bi 0.1 Fe 5 o 12 , where x=0.2, according to the molar ratio, respectively weigh Y with a purity ≥99.99% 2 o 3 、 Bi 2 o 3 , Yb 2 o 3 and Fe2O3 raw material, namely Yb 2 o 3 : Bi 2 o 3 :Y 2 o 3 :Fe 2 o 3 =0.2:0.1:2.7:5 Weigh 500g, place the weighed raw materials in an agate mortar and grind them thoroughly for 2 hours to obtain a mixed powder raw material; place the mixed powder raw material at a temperature of 1100°C Pre-fired for 12 hours, then ground for 2 hours to obtain YIG polycrystalline material;

[0025] (2) Add flux: add PbO-B in the YIG polycrystalline material that obtains in step (1) 2 o 3 Composite flux, wherein the mass ratio is YIG polycrystalline material: Fe2O3: PbO: B2O3 = 1.68:5.44:90.81:2.07, and...

Embodiment 2

[0033] A preparation method of rare earth garnet single crystal adopts multi-layer thickening method, comprising the following steps:

[0034] (1) Preparation of polycrystalline material: according to the crystal molecular formula Y (2.9-x) T mx Bi 0.1 Fe 5 o 12 , where x=0.35, according to the molar ratio, respectively weigh Y with a purity ≥99.99% 2 o 3 、 Bi 2 o 3 、Tm 2 o 3 and Fe 2 o 3 Raw material, ie Tm 2 o 3 : Bi 2 o 3 :Y 2 o 3 :Fe 2 o 3 =0.35:0.1:2.55:5 Weigh 500g, place the weighed various raw materials in an agate mortar and grind them fully for 2.5h to uniformity to obtain the mixed powder raw materials; and place the mixed powder raw materials at a temperature of 1300 Pre-fire at ℃ for 12 hours, then grind for 2 hours to obtain YIG polycrystalline material;

[0035] (2) Add flux: add PbO-B in the YIG polycrystalline material that obtains in step (1) 2 o 3 Composite flux, wherein the mass ratio is YIG polycrystalline material: Fe 2 o 3 :PbO:B ...

Embodiment 3

[0043] A preparation method of rare earth garnet single crystal adopts multi-layer thickening method, comprising the following steps:

[0044] (1) Preparation of polycrystalline material: according to the crystal molecular formula Y (2.9-x) Ho x Bi 0.1 Fe 5 o 12 , where x=0.4, respectively weigh Y with a purity ≥99.99% according to the molar ratio 2 o 3 、 Bi 2 o 3 , Ho2O3 and Fe2O3 raw materials, namely Ho 2 o 3 : Bi 2 o 3 :Y 2 o 3 :Fe 2 o 3 =0.4:0.1:2.5:5 Weigh 500g, place the weighed raw materials in an agate mortar and grind them thoroughly for 3 hours to obtain a mixed powder raw material; place the mixed powder raw material at a temperature of 1400°C Pre-fired for 12 hours, then ground for 2 hours to obtain YIG polycrystalline material;

[0045] (2) Add flux: add PbO-B in the YIG polycrystalline material that obtains in step (1) 2 o 3 Composite flux, wherein the mass ratio is YIG polycrystalline material: Fe2O3: PbO: B2O3 = 1.56:5.02:91.29:2.13, and plac...

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Abstract

The invention discloses a method for preparing a rare earth garnet single crystal, comprising the following steps: according to the crystal molecular formula Y （2.9‑x） Re x Bi 0.1 Fe 5 o 12 , where x=0.2~0.4, accurately weigh the raw materials, mix, sinter, and grind to obtain the polycrystalline material; add PbO composite flux to the polycrystalline material, ball mill, briquetting; clean the seed crystal; crystal growth, the seed crystal slowly Immerse in a high-temperature solution that is close to supersaturation, grow briefly, and then lift off the liquid surface to complete the initial growth; supplement the solute according to the theoretically calculated consumption to make it supersaturated again, repeat the above steps, and perform the secondary growth of the crystal; Repeat many times The above steps obtain the target crystal. The present invention adopts the mode of growth-replenishing solute-re-growth-replenishing solute to carry out crystal growth, realizes precise control of crystal growth and quality, and obtains rare earth garnet single crystal with smooth surface and no cracks; through multi-layer thickening The thickness of the rare earth garnet single crystal prepared by this method can reach more than 100 μm, which is suitable for the application of magneto-optic and microwave devices.

Description

technical field [0001] The invention relates to the technical field of crystal growth, in particular to a method for preparing a rare earth garnet single crystal. Background technique [0002] Rare earth garnet crystal is a kind of functional material with excellent microwave, magneto-optical and magnetic garnet structure. It is widely used in various optical devices, magneto-optical devices and microwave devices. It is a key material in the field of optical communication. Among them, the yttrium iron garnet crystal (Y 3 Fe 5 o 12 ), referred to as YIG, is the representative of this type of magneto-optic crystal. Typically, non-reciprocal optical isolators must be used to avoid the impact of reflected light on the light source. YIG is the core material of the optical isolator. It has very low light absorption loss in the near-infrared region and has become an indispensable high-tech material for optical communication. [0003] The oxide raw material for growing garnet s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/28C30B15/00C30B33/02
CPCC30B15/00C30B29/28C30B33/02
Inventor 徐家跃王昂申慧田甜蒋颖穗封鹏
Owner SHANGHAI INST OF TECH
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