CN105801108A - Preparation method of three-dimensional open-framework structure lithium base block tritium value-added agent material - Google Patents

Preparation method of three-dimensional open-framework structure lithium base block tritium value-added agent material Download PDF

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CN105801108A
CN105801108A CN201610141152.2A CN201610141152A CN105801108A CN 105801108 A CN105801108 A CN 105801108A CN 201610141152 A CN201610141152 A CN 201610141152A CN 105801108 A CN105801108 A CN 105801108A
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tritium
preparation
block
framework
dimensional open
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CN105801108B (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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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/624—Sol-gel processing
    • C—CHEMISTRY; METALLURGY
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • 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
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21B—FUSION REACTORS
    • G21B1/00—Thermonuclear fusion reactors
    • G21B1/11—Details
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
    • C04B2235/3203—Lithium oxide or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/448—Sulphates or sulphites
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/10—Nuclear fusion reactors

Abstract

The invention discloses a preparation method of a three-dimensional open-framework structure lithium base block tritium value-added agent material, and belongs to the field of tritium value-added agent materials. The three-dimensional open-framework structure lithium base block tritium value-added agent material is used for solid state tritium value-added cladding on-line and off-line tritium production. The preparation method comprises the steps that 1, a sizing agent is prepared, particularly, an organic monomer is added into Li2TiO3 or Li4SiO4 powder for mixing and ball mixing, and a ceramic sizing agent with good dispersity is prepared; 2, a blank is prepared, particularly, an initiator is introduced into the sizing agent, and the sizing agent mixed with the added initiator is injected into a three-dimensional organic material framework die with the porosity of 32%-40%, gel solidification is performed, and the ceramic blank is obtained; 3, a block is sintered, particularly, the temperature in a muffle furnace is increased to 800-1200 DEG C and kept for 2-4 h, furnace cooling is performed, and the three-dimensional open-framework structure lithium base block is obtained. The block material prepared through the method has the advantages that mechanical property is good, pore rules are orderly, and porosity and the hole diameter are controllable. Different amounts of linear organic matter with different diameters are adopted for adjusting the hole diameter and the porosity, the preparation equipment and technology of the block are simple, and efficient batch production can be achieved.

Description

A kind of preparation method of three-dimensional open-framework lithio block tritium proliferating agent material
Technical field
The invention belongs to ceramic material field, the preparation method relating to porous ceramics block, particularly a kind of for the preparation of three-dimensional open-framework ceramic block in nuclear fusion stack tritium-breeding material.
Background technology
Lithium-based ceramic (Li2TiO3、Li4SiO4) there is higher lithium ion density, excellent chemical stability, relatively low reactivity and structural material have a series of excellent properties such as the good compatibility.This ceramic material can be widely used in new energy materials field as 26S Proteasome Structure and Function material, in solid-state tritium proliferating agent material be considered as combination property well, one of the material of most future.
In current solid-state tritium proliferating agent, spherical proliferating agent has that specific surface area is big, easy to loading and unloading, transport is convenient, lithium easily reclaims, is conducive to thermal stress lax and prevents the advantages such as irradiation cracking.Therefore, the spherical proliferating agent of general selection in fusion reactor designs.But the comprcssive strength of bead is low, be easily broken；Between ball and ball, space is little, is unfavorable for release and the diffusion of tritium；Production efficiency is low, is unfavorable for mass production.At present, at tritium increment Material Field, research both domestic and external focuses mostly on the processing parameter improving bead and equipment, and the research of three-dimensional open-framework block is little.The present invention, by exploring the difficult point of pottery molding, has successfully prepared three-dimensional open-framework solid-state tritium increment lithium-based ceramic block.
Summary of the invention
The present invention to solve it is a key issue that the solid-state tritium increment ceramic block channel diameter prepared is at 0.2～2mm, and porosity is 32～40%, and prepared ceramic block spatially has three-dimensional open-framework.Compared to ceramic microsphere, to have higher mechanical performance, comprcssive strength, porosity, can produce in batches efficiently.
The technical scheme is that
The preparation method of a kind of three-dimensional open-framework lithio block tritium proliferating agent material, it is characterised in that the step of preparation is:
(1) preparation of solid-state tritium proliferating agent lithio porous ceramics slurry: (1) weighs Li2TiO3Or Li4SiO4Powder body, adds the deionized water of the quality such as powder quality mark 8%～15% monomeric acrylamide, 1%～3% cross-linking agent methylene-bisacrylamide, powder body, ball milling 2～8h, obtains the ceramic size of good dispersion.
(2) molding of base substrate: 0.1%～1wt% initiator ammonium persulfate will be added in the slurry in step (1), pour in the organic framework structured silica gel mould of three-dimensional that pre-designed porosity is 32%～40% after stirring, in 40 DEG C～80 DEG C, gel solidification forms ceramic body, then these green compact is carried out temperature and humidity control and dries.
(3) sintering: the ceramic body that above-mentioned steps (2) is dry is sintered, heating rate is 1～2 DEG C/min, it is incubated 3～6h at 400～600 DEG C, it is warming up to 900～1100 DEG C again with 1～2 DEG C/min, insulation 2-4h, then furnace cooling, namely obtains three-dimensional open-framework solid-state tritium increment lithium-based ceramic block.
In described step (2), in solid-state tritium proliferating agent lithio porous ceramics, the diameter in duct is 0.2～2mm.
The present invention is have the advantage that compared with prior art:
(1) present invention process flow process is simple, easily operates, and efficiency is high, it is possible to batch production, the problem solving ceramic microsphere batch production difficulty.
(2) three-dimensional open-framework tritium increment lithium-based ceramic pore size and controlled porosity.Compared with ceramic bead, it is more beneficial for diffusion and the release of tritium.
(3) three-dimensional open-framework tritium increment lithium-based ceramic block operationally contact area is big compared with ceramic microsphere, thus has higher comprcssive strength, it is possible to the problem being prevented effectively from bead overcharge and causing it to break.
Detailed description of the invention:
Embodiment 1:
(1), under room temperature, Li is weighed2TiO3、Li4SiO4Ceramic powder 60g, adds 60g deionized water, 6g monomeric acrylamide, 1g cross-linking agent methylene-bisacrylamide in powder body, chooses the proportioning steel ball of suitable granularity, be positioned in ball grinder ball milling 2～8h prepared composition and dissipate the ceramic size that property is good.
(2) slurry after ball milling is taken out, its evacuation is reduced further the bubble in solution, add the APS initiator 10ml that mass fraction is 10%, pour into after stirring in the three-dimensional organic material framing structure silica gel mould that the porosity designed is 32%～40%.
(3) will be equipped with the mould of slurry to put in the baking oven of 50～80 DEG C 2 hours, after gel sets, obtain ceramic green, place in climatic chamber dry, drying condition: temperature 25 DEG C, starting relative humidity 90%, reducing by 10% to relative humidity per hour is 50%, keeps two hours.Dry 48h in natural environment.Then burning till in Muffle furnace, calcining system used is: 2 DEG C/min of heating rate, rises to insulation two hours when 500 DEG C, then is warming up to 1150 DEG C with 2 DEG C/min, is incubated 4h, then cools to room temperature with the furnace, obtains three-dimensional open-framework solid-state tritium increment Li2TiO3、Li4SiO4Ceramic block.
Embodiment 2:
(1) under room temperature, remove ionized water 120g, weigh ceramic powder Li2TiO3、Li4SiO4, ceramic powder addition was the 50% of deionized water quality, is placed in ball grinder, planetary ball mill ball milling 2 hours.
(2) slurry is taken out, by its evacuation to eliminate the bubble in solution.Being then placed in oil bath magnetic stirring apparatus, temperature rises to 80～120 DEG C, take 6g agar powder and add in solution, then oil bath temperature is reduced to 90 DEG C, it is in 32～40% three-dimensional organic material framing structure moulds that slurry injected after stirring a period of time porosity.
(3) will be equipped with the mould of slurry to be placed in 40～80 DEG C gel and obtain ceramic green, place in climatic chamber dry, drying condition: temperature 25 DEG C, starting relative humidity 90%, reducing by 10% to relative humidity per hour is 50%, keeps two hours.Then in natural environment, dry 48h obtains ceramic body, dried ceramic body is put in Muffle furnace and burns till, heating rate is 2 DEG C/min, it is incubated 2～6h at 400 DEG C, then 1150 DEG C are risen to identical heating rate, it is incubated 2～4 hours, cools to room temperature with the furnace, obtain three-dimensional open-framework Li2TiO3And Li4SiO4Ceramic block.

Claims (4)

1. the preparation method of a three-dimensional open-framework lithio block tritium proliferating agent material, it is characterised in that the step of preparation is:
(1) preparation of solid-state tritium proliferating agent lithio porous ceramics slurry: weigh Li2TiO3Or Li4SiO4Powder body, add powder quality mark 8%～15% monomeric acrylamide, 1%～3% cross-linking agent methylene-bisacrylamide and and the deionized water of the quality such as powder body, ball milling 2～8h, obtain the ceramic size of good dispersion；
(2) molding of ceramic body: initiator ammonium persulfate will be added in the ceramic size in step (1), pour in the organic framework structured silica gel mould of pre-designed three-dimensional after stirring, in 40 DEG C～80 DEG C, gel solidification forms ceramic body, then these green compact is carried out temperature and humidity control and dries；
(3) sintering: the ceramic body that above-mentioned steps (2) is dry is sintered, is incubated, then furnace cooling, namely obtain three-dimensional open-framework solid-state tritium increment lithium-based ceramic block.
2. the preparation method of three-dimensional open-framework lithio block tritium proliferating agent material according to claim 1, it is characterized in that, in described step (2), the addition of initiator ammonium persulfate is 0.1%～1wt% of ceramic size, and three-dimensional organic framework structured silica gel mould porosity is 32%～40%.
3. the preparation method of three-dimensional open-framework lithio block tritium proliferating agent material according to claim 1, it is characterised in that in described step (2), in solid-state tritium proliferating agent lithio porous ceramics, the diameter in duct is 0.2～2mm.
4. the preparation method of three-dimensional open-framework lithio block tritium proliferating agent material according to claim 1, it is characterized in that, sintering condition described in described step (3) is: heating rate is 1～2 DEG C/min, it is incubated 3～6h at 400～600 DEG C, it is warming up to 900～1100 DEG C with 1～2 DEG C/min again, is incubated 2-4h.
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Cited By (4)

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Publication number Priority date Publication date Assignee Title
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
CN110292906A (en) * 2019-07-30 2019-10-01 华中科技大学 Modified lithium metasilicate of wet grinding and preparation method thereof and the application 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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CN101301677A (en) * 2008-06-03 2008-11-12 西安交通大学 Method for quickly and precisely casting complex parts
CN101510450A (en) * 2009-03-31 2009-08-19 北京科技大学 Method for preparing ceramic tritium proliferation agent in fusion stack cladding
CN102731111A (en) * 2012-07-05 2012-10-17 北京科技大学 Novel preparation method of ceramic microspheres

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN110292906A (en) * 2019-07-30 2019-10-01 华中科技大学 Modified lithium metasilicate of wet grinding and preparation method thereof and the application as adsorbent
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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