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Preparation method of large-size yttrium iron garnet single crystal

A technology of yttrium iron garnet and large size is applied in the field of large size yttrium iron garnet single crystal material and its preparation, and can solve the problems of poor uniformity, small size of yttrium iron garnet single crystal and the like

Pending Publication Date: 2022-03-08
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims to find a preparation process that can realize the growth of large-sized yttrium-iron garnet single crystals, so as to solve the problems of small size and poor uniformity in growing yttrium-iron garnet single crystals by the molten salt method, and provide large-sized yttrium-iron garnet single crystals. Iron garnet single crystal growth provides a new idea

Method used

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  • Preparation method of large-size yttrium iron garnet single crystal
  • Preparation method of large-size yttrium iron garnet single crystal
  • Preparation method of large-size yttrium iron garnet single crystal

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Embodiment 1 uses the top seed method to grow large-size yttrium iron garnet crystals:

[0041] The initial raw material Y 2 o 3 , Fe 2 o 3 And the composite flux is weighed according to the stoichiometric ratio to obtain the initial mixture, and the mass fraction of the composite flux in the mixed raw material is 73.78%. Among them, the composite flux includes Z1 component PbF 2 , Z2 component B 2 o 3 and Z3 component Bi 2 o 3 , and the molar ratio of component Z1, component Z2, and component Z3 is 6:2:1.

[0042] The initial mixture was thoroughly mixed in a mixer for 24 hours, and the obtained mixed raw material was loaded into a platinum crucible, and placed in a crystal growth furnace at 1050° C. for 48 hours to form the raw material. Use yttrium-iron garnet seed crystals to find the supersaturation temperature of the melt, introduce formal seed crystals at 990°C, and then slowly cool down to grow; the crystal rotation rate is 30rpm, and the cooling rate i...

Embodiment 2

[0043] Embodiment 2 uses the top seed method to grow large-size yttrium iron garnet crystals:

[0044] The initial raw material Y 2 o 3 , Fe 2 o 3 And the composite flux is weighed according to the stoichiometric ratio to obtain the initial mixture, and the mass fraction of the composite flux in the mixed raw material is 68.25%. Among them, the composite flux includes Z1 component PbF 2 , Z2 component B 2 o 3 and Z3 component Bi 2 o 3 , and the molar ratio of component Z1, component Z2, and component Z3 is 4:2:1.

[0045] The initial mixture was thoroughly mixed in a mixer for 24 hours, and the obtained mixed raw material was loaded into a platinum crucible, and placed in a crystal growth furnace at 1100° C. for 48 hours to form the raw material. Use yttrium-iron garnet seed crystals to find the supersaturation temperature of the melt, introduce formal seed crystals at the supersaturation temperature of 1040°C, and then slowly cool down and grow; the crystal rotation ...

Embodiment 3

[0046] Embodiment 3 The yttrium iron garnet single crystal obtained in embodiment 1 is subjected to structure and performance tests:

[0047] (a) Cut the crystal into a small piece and grind it into a powder for XRD powder diffraction test. The powder diffraction spectrum of yttrium-iron garnet single crystal shows that the room temperature is a typical garnet-type structure, which belongs to the cubic crystal system (see figure 2 ).

[0048] (b) Slicing the obtained yttrium iron garnet single crystal according to (110) or (211) direction, followed by fine polishing on both sides. The transmittance was measured with a UV-Vis-NIR spectrophotometer (Lambda950). The transmittance spectrum shows that the transmittance is as high as 76.24% in the 1200-2300nm band (see image 3 ).

[0049] (c) slice the obtained yttrium iron garnet single crystal according to (110) or (211) direction, then perform double-sided polishing and gold-plated electrodes. The prepared samples were use...

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Abstract

The invention discloses a preparation method of a large-size yttrium iron garnet single crystal. The preparation method comprises the following steps: 1) obtaining a mixed raw material containing yttrium oxide, iron oxide and a composite fluxing agent; the composite fluxing agent contains Bi2O3; and 2) growing through a top seed crystal method to obtain the yttrium iron garnet single crystal material. The crystal has excellent magnetic properties and stable physicochemical properties, is a core material of isolators, circulators, phase shifters and filters, and has a wide application market in the field of 5G communication. According to the preparation method, the growth temperature of the crystal is greatly reduced through the composite fluxing agent containing Bi2O3, the large-size yttrium iron garnet single crystal with the size of 50mm * 42mm * 11mm and the weight of 74.72 g is obtained, the crystal is good in uniformity and free of cracks and inclusions, and the quality of the crystal completely meets the application of microwave and magneto-optical devices.

Description

technical field [0001] The invention relates to a large-size yttrium iron garnet single crystal material and a preparation method thereof, belonging to the field of crystal growth and functional materials. Background technique [0002] Garnet ferrite single crystal is the core material of microwave and magneto-optical devices, and has a wide range of application markets in aerospace, electronic information, mobile communication and other fields. Microwave and magneto-optical ferrite devices mainly involve devices such as isolators, circulators, phase shifters, filters, etc. The most important features are non-reciprocal transmission, ferromagnetic resonance, and electrical controllability. The key core device for the isolation, phase shifting, switching, modulation, amplification and other functions of microwave transmission in the system. With the improvement of application requirements, the development of high power, high temperature stability, and low loss materials has ...

Claims

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Application Information

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IPC IPC(8): C30B9/12C30B29/28
CPCC30B9/12C30B29/28
Inventor 龙西法杨晓明苏榕冰何超王祖建
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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