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Preparation method of novel phosphate composite ceramic solidified body material

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

Active Publication Date: 2020-01-31
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 novel phosphate composite ceramic solidified body material
  • Preparation method of novel phosphate composite ceramic solidified body material
  • Preparation method of novel 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 Figure 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 ...

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Abstract

The invention discloses a preparation method of a novel phosphate composite ceramic solidified body material, which comprises the following steps: mixing raw materials, presintering to obtain a precursor, adding a sintering aid into the precursor, and carrying out mechanical activation, molding and sintering to obtain the novel phosphate composite ceramic solidified body material; wherein a phosphorus source in the raw materials is ammonium dihydrogen phosphate or phosphorus pentoxide; the raw materials of elements A, B, Ln and An in the raw materials are one selected from nitrate, metal alkoxide or oxide; A is a +1 or +2 valent element, B is a +4 valent element, Ln is a +3 or +4 valent lanthanide, and An is a +3 or +4 valent actinide. The NZP type ceramic and the monazite ceramic in the novel phosphate composite ceramic solidified body prepared by the invention are solidified body materials with excellent chemical stability, so that the phosphate composite ceramic solidified body is large in waste packaging capacity and good in 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 Applications(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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