CN105801108B - A kind of preparation method of three-dimensional open-framework lithium matrix body tritium increment agent material - Google Patents

A kind of preparation method of three-dimensional open-framework lithium matrix body tritium increment agent material Download PDF

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CN105801108B
CN105801108B CN201610141152.2A CN201610141152A CN105801108B CN 105801108 B CN105801108 B CN 105801108B CN 201610141152 A CN201610141152 A CN 201610141152A CN 105801108 B CN105801108 B CN 105801108B
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tritium
ceramic
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increment
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CN105801108A (en
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张迎春
王朝富
向茂乔
张云
刘辉
刘淑雅
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University of Science and Technology Beijing USTB
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
    • C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
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    • C04B38/0003—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof containing continuous channels, e.g. of the "dead-end" type or obtained by pushing bars in the green ceramic product
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Abstract

A kind of preparation method of three-dimensional open-framework lithium matrix body tritium increment agent material, is used for the solid-state tritium increment online and offline production tritium of covering, belongs to tritium proliferating agent Material Field.Steps are as follows：(1), prepared by slurry：In Li2TiO3Or Li4SiO4Organic monomer mixing and ball milling is added in powder, prepares the ceramic slurry of good dispersion.(2), body preparation：Initiator is added in slurry, injection porosity is in 32%~40% three-dimensional organic material skeleton die, and gel solidification obtains ceramic body.(3), block is sintered：It is warming up to 800 DEG C~1200 DEG C in Muffle furnace, keeps the temperature 2h~4h, furnace cooling obtains three-dimensional open-framework lithium-based ceramic block.Block materials prepared by this method have the characteristics that the controlled diameter in regular good mechanical property, duct, porosity and hole.Line style organic matter using different-diameter and quantity regulates and controls aperture and porosity size respectively, and prepares the equipment of the block and simple for process, can efficiently produce in batches.

Description

A kind of preparation method of three-dimensional open-framework lithium matrix body tritium increment agent material
Technical field
The invention belongs to ceramic material fields, are related to the preparation method of porous ceramics block, especially a kind of poly- for core Become the preparation of three-dimensional open-framework ceramic block in heap tritium-breeding material.
Background technology
Lithium-based ceramic (Li2TiO3、Li4SiO4) there is higher lithium ion density, excellent chemical stability, lower Reactivity has a series of excellent properties such as good compatibility with structural material.This ceramic material can be used as structure and function Material is widely used in new energy materials field, be considered as during solid-state tritium rises in value agent material comprehensive performance it is good, most before One of the material on way.
In current solid-state tritium proliferating agent, there is spherical proliferating agent large specific surface area, easy to loading and unloading, transport facility, lithium to hold The advantages that easily recycling, being conducive to thermal stress relaxation and prevent irradiation from cracking.Therefore, spherical increase generally is selected in fusion reactor design It is worth agent.But the compression strength of bead is low, is easily broken；Gap is small between ball and ball, is unfavorable for the release and diffusion of tritium；Production effect Rate is low, is unfavorable for mass production.Currently, in tritium increment Material Field, research both domestic and external focuses mostly in the life for improving bead It is seldom to the research of three-dimensional open-framework block in production. art parameter and equipment.The present invention is by exploring the molding difficulty of ceramics Point has successfully prepared three-dimensional open-framework solid-state tritium increment lithium-based ceramic block.
Invention content
The present invention to be solved it is a key issue that the solid-state tritium prepared rises in value ceramic block channel diameter 0.2~ 2mm, porosity are 32~40%, and prepared ceramic block spatially has three-dimensional open-framework.Compared to ceramic microsphere, With higher mechanical performance, compression strength, porosity, can efficiently produce in batches.
The technical scheme is that：
The preparation method of a kind of three-dimensional open-framework lithium matrix body tritium increment agent material, it is characterised in that the step of preparation It is：
(1) preparation of solid-state tritium proliferating agent lithium Quito hole ceramic slurry：(1) Li is weighed2TiO3Or Li4SiO4Powder is added The quality such as 8%~15% monomeric acrylamide of powder quality score, 1%~3% crosslinking agent methylene-bisacrylamide, powder Deionized water, 2~8h of ball milling obtain the ceramic slurry of good dispersion.
(2) molding of green body：0.1%~1wt% initiator ammonium persulfates, stirring will be added in slurry in step (1) Poured into after uniformly in the organic framework structured silica gel mould of three-dimensional that pre-designed porosity is 32%~40%, 40 DEG C~ Gel solidification forms ceramic body in 80 DEG C, this green compact is then carried out temperature and humidity control drying.
(3) it is sintered：The dry ceramic body of above-mentioned steps (2) is sintered, heating rate is 1~2 DEG C/min, 400~600 DEG C of 3~6h of heat preservation, then be warming up to 900~1100 DEG C with 1~2 DEG C/min, keep the temperature 2-4h, then furnace cooling, i.e., Obtain three-dimensional open-framework solid-state tritium increment lithium-based ceramic block.
In the step (2), a diameter of 0.2~2mm in duct in solid-state tritium proliferating agent lithium base porous ceramics.
The present invention compared with prior art possessed by advantage：
(1) present invention process flow is simple, easy to operate, efficient, can produce in batches, and it is raw to solve ceramic microsphere batch Produce difficult problem.
(2) three-dimensional open-framework tritium increment lithium-based ceramic pore size and controlled porosity.Compared with ceramic bead, more have Conducive to the diffusion and release of tritium.
(3) contact area is big compared with ceramic microsphere at work for three-dimensional open-framework tritium increment lithium-based ceramic block, thus has Have higher compression strength, it is possible to prevente effectively from bead load it is excessive and the problem of lead to its rupture.
Specific implementation mode：
Embodiment 1：
(1) at room temperature, Li is weighed2TiO3、Li4SiO4It is mono- that 60g deionized waters, 6g is added in ceramic powder 60g in powder Body acrylamide, 1g crosslinking agent methylene-bisacrylamides, choose the proportioning steel ball of appropriate granularity, are positioned over ball milling in ball grinder 2~8h is prepared into the ceramic slurry of good dispersion.
(2) slurry after ball milling is taken out, the bubble being further reduced in solution is vacuumized, mass fraction, which is added, is It is organic to pour into the three-dimensional that designed porosity is 32%~40% after stirring by 10% APS initiator 10ml In material skeleton structure silica gel mould.
(3) mold equipped with slurry is put into 50~80 DEG C of baking oven 2 hours, ceramic green is obtained after gel sets Base places into dry in climatic chamber, drying condition：25 DEG C of temperature, starting relative humidity 90%, per hour reduce by 10% to Relative humidity is 50%, is kept for two hours.48h is dried in the natural environment.Then in Muffle kiln roasting, firing system used Degree is：2 DEG C/min of heating rate keeps the temperature two hours when rising to 500 DEG C, then is warming up to 1150 DEG C with 2 DEG C/min, keeps the temperature 4h, Then it cools to room temperature with the furnace, obtains three-dimensional open-framework solid-state tritium increment Li2TiO3、Li4SiO4Ceramic block.
Embodiment 2：
(1) at room temperature, ionized water 120g is removed, ceramic powder Li is weighed2TiO3、Li4SiO4, ceramic powder addition is The 50% of deionized water quality, is placed in ball grinder, in 2 hours of planetary ball mill ball milling.
(2) slurry is taken out, is vacuumized to eliminate the bubble in solution.It is then placed in oil bath magnetic stirring apparatus, it will Temperature rises to 80~120 DEG C, and 6g agar powders is taken to be added in solution, then oil bath temperature is reduced to 90 DEG C, will after stirring a period of time It is in 32~40% three-dimensional organic material skeleton structure molds that slurry, which injects porosity,.
(3) mold equipped with slurry is placed in gel in 40~80 DEG C and obtains ceramic green, placed into climatic chamber It is dry, drying condition：25 DEG C of temperature, starting relative humidity 90%, it is 50% to reduce by 10% per hour to relative humidity, keeps two A hour.Then 48h is dried in the natural environment and obtains ceramic body, and dried ceramic body is put into Muffle furnace and is carried out Firing, heating rate are 2 DEG C/min, and 2~6h is kept the temperature at 400 DEG C, then rise to 1150 DEG C with identical heating rate, heat preservation 2~4 It a hour, cools to room temperature with the furnace, obtains three-dimensional open-framework Li2TiO3And Li4SiO4Ceramic block.

Claims (1)

1. a kind of preparation method of three-dimensional open-framework lithium matrix body tritium increment agent material, it is characterised in that the step of preparation is：
(1) preparation of solid-state tritium proliferating agent lithium Quito hole ceramic slurry：Weigh Li2TiO3Or Li4SiO4Powder quality is added in powder 8%~15% monomeric acrylamide of score, 1%~3% crosslinking agent methylene-bisacrylamide and with the quality such as powder go from Sub- water, 2~8h of ball milling obtain the ceramic slurry of good dispersion；
(2) molding of ceramic body：Initiator ammonium persulfate will be added in ceramic slurry in step (1), is poured after stirring evenly Entering in the pre-designed organic framework structured silica gel mould of three-dimensional, gel solidification forms ceramic body in 40 DEG C~80 DEG C, Then this green compact is subjected to temperature and humidity control drying；
(3) it is sintered：The dry ceramic body of above-mentioned steps (2) is sintered, is kept the temperature, then furnace cooling is to get to three-dimensional Pore passage structure solid-state tritium increment lithium-based ceramic block；
In the step (2), the addition of initiator ammonium persulfate is 0.1%~1wt% of ceramic slurry, three-dimensional organic backbone Structure silica gel mould porosity is 32%~40%；
In the step (2), a diameter of 0.2~2mm in duct in solid-state tritium proliferating agent lithium base porous ceramics；
Sintering condition is described in the step (3)：Heating rate is 1~2 DEG C/min, and 3~6h is kept the temperature at 400~600 DEG C, then 900~1100 DEG C are warming up to 1~2 DEG C/min, keeps the temperature 2-4h.
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CN109859858A (en) * 2019-02-01 2019-06-07 中国工程物理研究院核物理与化学研究所 A kind of foam type tritium multiplication agent and preparation method thereof
CN110292906B (en) * 2019-07-30 2020-08-28 华中科技大学 Wet grinding modified lithium silicate, preparation method thereof and application of wet grinding modified lithium silicate as adsorbent
CN112174195A (en) * 2020-09-28 2021-01-05 中科院过程工程研究所南京绿色制造产业创新研究院 Carbon-coated lithium titanate tritium proliferation agent and preparation method and preparation device system thereof
CN113929488A (en) * 2021-09-30 2022-01-14 华中科技大学 Lithium ceramic tritium propagation agent with curved pore path structure and preparation method thereof

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