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A kind of preparation method of ytterbium doped bismuth iridate pyrochlore polycrystalline material

A polycrystalline material and pyrochlore technology, which is applied in the field of preparation of pyrochlore polycrystalline materials, can solve the problems of complex preparation process, compound heterophase, low preparation efficiency, etc. Efficient effect

Active Publication Date: 2022-02-01
HEFEI UNIV
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  • Abstract
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Problems solved by technology

[0004] The purpose of the present invention is in order to overcome prior art existence in traditional high-temperature solid state reaction IrO 2 The steam is easy to volatilize, causing the stoichiometric ratio to be mismatched, resulting in the compound phase; at the same time, the preparation process of the pyrochlore polycrystalline sample in the prior art is complicated and the preparation efficiency is low. During the grinding process of the raw material, it is easy to overflow or carry out of the material, resulting in a mismatch of the stoichiometric ratio, causing the compound to produce an impurity phase, and the problem of waste of raw materials, providing a Yb 3+ A method for preparing bismuth iridate-doped pyrochlore polycrystalline material, the method has the advantages of high preparation efficiency, and the raw material is not easy to overflow or carry out the material during the grinding process

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  • A kind of preparation method of ytterbium doped bismuth iridate pyrochlore polycrystalline material
  • A kind of preparation method of ytterbium doped bismuth iridate pyrochlore polycrystalline material
  • A kind of preparation method of ytterbium doped bismuth iridate pyrochlore polycrystalline material

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preparation example Construction

[0034] Yb described in the present invention 3+ The preparation method of doped bismuth iridate pyrochlore polycrystalline material comprises the following steps:

[0035] (1) Change Yb 2 o 3 Powder, Bi 2 o 3 Powder and IrO 2 The first calcination after powder mixing;

[0036] (2) Grinding the mixture calcined for the first time in step (1) and pressing it into a disc, and calcining for the second time;

[0037] (3) Grinding the mixture calcined for the second time in step (2) and pressing it into a disc, and calcining for the third time to obtain Bi 2-x Yb x Ir 2 o 7 Crystal, where 0≤x≤1.5.

[0038] The present invention adopts Yb 2 o 3 Powder, Bi 2 o 3 Powder and IrO 2 Powder blending, three calcinations and two grinding and tableting to prepare Bi 2-x Yb x Ir 2 o 7 crystals. The preparation process of the method is simple, but the preparation efficiency is high.

[0039] In the method of the present invention, in step (1), Yb 2 o 3 Powder, Bi 2 o 3 ...

Embodiment 1

[0058] (1) Change Yb 2 o 3 Powder, Bi 2 o 3 Powder and IrO 2 After the powder is mixed, the first calcination is carried out in a horse-boiling furnace, wherein, Yb 2 o 3 Powder, Bi 2 o 3 Powder and IrO 2 The mass ratio of the powder is 1:1.5:4, the first calcination process is: the temperature in the horse boiling furnace is raised from room temperature to 973.15K, the heating rate is 5K / min, calcined at 973.15K for 12 hours, and then cooled to 473.15K, The cooling rate is 3K / min, and finally cool down to room temperature with the furnace;

[0059] (2) After the mixture calcined for the first time in step (1) is ground with a grinding rod, it is pressed into a disc with a diameter of 1.5cm and a thickness of 1mm with a tablet press under a pressure of 6Mpa for 5 minutes. Carry out the second calcination in the middle, the second calcination process is: the temperature in the horse boiling furnace is warmed up from room temperature to 1223.15K, the heating rate is 3K / ...

Embodiment 2

[0063] (1) Change Yb 2 o 3 Powder, Bi 2 o 3 Powder and IrO 2 After the powder is mixed, the first calcination is carried out in a horse-boiling furnace, wherein, Yb 2 o 3 Powder, Bi 2 o 3 Powder and IrO 2 The mass ratio of the powder is 1:3.5:5, the first calcination process is: the temperature in the horse boiling furnace is raised from room temperature to 950K, the heating rate is 4K / min, calcined at 950K for 14 hours, and then cooled to 473.15K, the cooling rate 2K / min, and finally cooled down to room temperature with the furnace;

[0064] (2) After the mixture calcined for the first time in step (1) is ground with a grinding rod, it is pressed into a disc with a diameter of 1.4cm and a thickness of 1.2mm with a tablet press under a pressure of 8Mpa for 6 minutes. Carry out calcining for the second time in the horse boiling furnace, the second calcining process is: the temperature in the horse boiling furnace is warming up to 1200K by room temperature, and the heat...

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Abstract

The invention relates to the technical field of preparation of pyrochlore polycrystalline materials, and discloses a Yb 3+ A preparation method of doped bismuth iridate pyrochlore polycrystalline material. The method includes the following steps: (1) Yb 2 O 3 Powder, Bi 2 O 3 Powder and IrO 2 After the powder is mixed, the first calcination is carried out; (2) the mixture after the first calcination in the step (1) is ground and pressed into a disk, and the second calcination is carried out; (3) the second calcination in the step (2) is carried out. The calcined mixture is ground and pressed into discs, and calcined for the third time to obtain Bi 2‑x Yb x Ir 2 O 7 crystal, where 0≤x≤1.5. The preparation process of the method is simple, but the preparation efficiency is high. At the same time, the invention solves the problems of material overflow or carry-out during the grinding process by grinding with a grinding rod, resulting in mismatch of stoichiometric ratios, resulting in the generation of impurity phases of compounds, and waste of raw materials.

Description

technical field [0001] The invention relates to the technical field of preparation of pyrochlore polycrystalline materials, in particular to a kind of ytterbium (Yb 3+ ) preparation method of bismuth iridate pyrochlore polycrystalline material. Background technique [0002] Ytterbium (Yb) is one of the important rare earth magnetic elements, and its electronic configuration is 4f 14 6s 2 , in the trivalent lanthanide rare earth elements Yb 3+ has a smaller ionic radius, which is Yb 3+ The magnetic moment is 4.5μ B . Use Yb 3+ Doping bismuth iridate (Bi 2 Ir 2 o 7 ) to obtain the pyrochlore-structured polycrystalline material Bi 2-x Yb x Ir 2 o 7 (0≤x≤1.5), can effectively reduce the lattice constant, and at the same time, the increase of Yb-doped components can lead to stronger Yb-Ir antiferromagnetic exchange, so that the compound has enhanced antiferromagnetic (AFM) properties . On the other hand, the reduced radius of the A site leads to a reduced Ir-O-Ir...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/22C30B28/02B02C19/08
CPCC30B29/22C30B28/02B02C19/08
Inventor 丰远边健刘慧高先和程玮方保龙王梦雅
Owner HEFEI UNIV
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