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Preparation method of new phosphate composite ceramic solidified body material

The technology of composite ceramic and solidified body is applied in the preparation of new phosphate composite ceramic solidified body and the solidification treatment of high radioactive nuclear waste, which can solve the problems of long preparation cycle and shorten the preparation cycle, so as to save the energy consumption of the mill and shorten the The effect of preparation cycle and shortening of fine grinding time

Active Publication Date: 2022-05-13
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are currently no relevant reports on the application of NZP-monazite composite ceramics in the field of nuclide solidification at home and abroad.
[0004] The purpose of the present invention is to provide a new phosphate composite ceramic solidified body that can simultaneously solidify multiple radionuclides, and to provide a simple, efficient and energy-saving preparation method for the current ceramic solidified body with long preparation period and complicated procedures. , realizing the integration of synthesis and sintering, greatly shortening the preparation cycle, and the obtained solidified body has high density, good mechanical properties and excellent chemical stability

Method used

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  • Preparation method of new phosphate composite ceramic solidified body material
  • Preparation method of new phosphate composite ceramic solidified body material
  • Preparation method of new phosphate composite ceramic solidified body material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A 0.5 B 2 (PO 4 ) 3 -(Ln,An)PO 4 The general formula of the chemical composition of the type phosphate composite ceramic solidified body is (1-x)Sr 0.5 Ti 2 (PO 4 ) 3 -xNdPO 4 , wherein x is 0.0001; its preparation process comprises the following steps:

[0041] (1) Ingredients: TiO 2 , NH 4 h 2 PO 4 , Sr(NO 3 ) 2 、Nd 2 o 3 As the raw material, according to the stoichiometric ratio of the cured body, such as Figure 4 shown;

[0042] (2) Mixing and pre-sintering treatment: After mixing each raw material with a ball mill for 4 hours, pre-sinter at 600°C for 8 hours in a muffle furnace;

[0043] (3) Add 1wt% ZnO to the calcined powder as a sintering aid, and use a planetary ball mill to mill again for 24 hours for mechanical activation;

[0044] (4) Molding and molding: the obtained powder is granulated and shaped, and isostatically pressed under a pressure of 200MPa, and then the molded green body is kept at 700°C for 1 hour in a muffle furnace for moldi...

Embodiment 2

[0047] A 0.5 B 2 (PO 4 ) 3 -(Ln,An)PO 4 The general formula of the chemical composition of the type phosphate composite ceramic solidified body is (1-x)Sr 0.5 Ti 2 (PO 4 ) 3 -xNdPO 4 , wherein x is 0.2; its preparation process comprises the following steps:

[0048] (1) Ingredients: TiO 2 , NH 4 h 2 PO 4 , Sr(NO 3 ) 2 、Nd 2 o 3 As the raw material, according to the stoichiometric ratio of the cured body, such as Figure 5 shown;

[0049] (2) Mixing and pre-sintering treatment: After mixing each raw material with a ball mill for 4 hours, pre-sinter at 600°C for 8 hours in a muffle furnace;

[0050] (3) Add 1wt% ZnO to the calcined powder as a sintering aid, and use a planetary ball mill to mill again for 24 hours for mechanical activation;

[0051] (4) Molding and molding: the obtained powder is granulated and shaped, and isostatically pressed under a pressure of 200MPa, and then the molded green body is kept at 700°C for 1 hour in a muffle furnace for moldin...

Embodiment 3

[0054] The chemical composition of a NZP type-monazite type phosphate composite ceramic solidified body is (1-x)Sr 0.5 Ti 2 (PO 4 ) 3 -xNdPO 4 , x is 0.4; Its preparation process comprises the following steps:

[0055] (1) Ingredients: TiO 2 , NH 4 h 2 PO 4 , Sr(NO 3 ) 2 、Nd 2 o 3 As the raw material, according to the stoichiometric ratio of the cured body, such as Image 6 shown;

[0056] (2) Mixing and pre-sintering treatment: After mixing each raw material with a ball mill for 4 hours, pre-sinter at 600°C for 8 hours in a muffle furnace;

[0057] (3) Add 1wt% ZnO to the calcined powder as a sintering aid, and use a planetary ball mill to mill again for 24 hours for mechanical activation;

[0058] (4) Molding and molding: the obtained powder is granulated and shaped, and isostatically pressed under a pressure of 200MPa, and then the molded green body is kept at 700°C for 1 hour in a muffle furnace for molding;

[0059] (5) Sintering: The green body is placed i...

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Abstract

The invention discloses a method for preparing a novel phosphate composite ceramic solidified body material, which comprises the following steps: mixing raw materials, pre-sintering to obtain a precursor, adding sintering aids to the precursor, mechanically activating, molding, and sintering to obtain A new type of phosphate composite ceramic solidified body material; wherein, the phosphorus source in the raw material is ammonium dihydrogen phosphate or phosphorus pentoxide; the raw material of A, B, Ln, An elements in the raw material is nitrate, metal alkoxide or oxide One; A is +1 or +2 valence element, B is +4 valence element, Ln is +3 or +4 valence lanthanide, An is +3 or +4 valence actinide. The NZP type ceramics and the monazite ceramics in the novel phosphate composite ceramic solidified body prepared by the invention are all solidified body materials with excellent chemical stability, so the phosphate composite ceramic solidified body has a large waste holding capacity and good stability.

Description

technical field [0001] The invention belongs to the field of novel composite ceramic materials, and relates to a preparation method of a novel phosphate composite ceramic solidified body, which is especially suitable for the solidification treatment of high-radioactive nuclear waste containing multiple fission and (sub)actinide radionuclides. Background technique [0002] High Level Liquid Waste (HLLW) is the raffinate produced by the separation and recovery of U and Pu during the reprocessing process of spent fuel. Not only U and Pu remain in HLLW, but also minor actinide nuclides (Np, Am, Cm) and hundreds of isotopes of more than 30 elements including fissionable nuclides such as Sr and Cs. HLLW not only has strong radiotoxicity, but also has complex nuclide components and multiple characteristics (fission and actinide nuclides with different valence states and ionic radii), making it difficult to handle and dispose of. For the treatment of HLLW, it is currently recognize...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/447C04B35/50
CPCC04B35/447C04B35/50C04B2235/443C04B2235/48C04B2235/3206C04B2235/3284C04B2235/3281C04B2235/666
Inventor 王军霞王进冯硕詹磊杨世源谭宏斌
Owner SOUTHWEAT UNIV OF SCI & TECH
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