CN104209053A - Preparation method of lithium silicate microsphere through melting, atomizing, and forming - Google Patents
Preparation method of lithium silicate microsphere through melting, atomizing, and forming Download PDFInfo
- Publication number
- CN104209053A CN104209053A CN201310205766.9A CN201310205766A CN104209053A CN 104209053 A CN104209053 A CN 104209053A CN 201310205766 A CN201310205766 A CN 201310205766A CN 104209053 A CN104209053 A CN 104209053A
- Authority
- CN
- China
- Prior art keywords
- lithium metasilicate
- microballoon
- lithium
- lithium silicate
- melting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Primary Cells (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention relates to a preparation method of a tritium breeding agent material for fusion reactor tritium production blanket, and specifically discloses a preparation method of a lithium silicate microsphere through melting, atomizing, and forming. The method comprises the following steps: (1) adding raw materials for preparing lithium silicate powder into a platinum crucible; (2) heating the platinum crucible by a temperature-control program to make the raw materials carry out reactions completely, keeping on heating until the lithium silicate powder is completely melt; (3) blowing the melt lithium silicate liquid to form multiple small liquid drops, curing the small lithium silicate drops into lithium silicate microspheres; (4) sieving the obtained lithium silicate microspheres; (5) carrying out an annealing treatment on the lithium silicate microspheres. The lithium silicate microsphere obtained through the provided preparation method has the advantages of high surface density, good spherical degree, and smooth surface.
Description
Technical field
The invention belongs to a kind of method preparing the tritium multiplication agent material producing tritium covering as fusion reactor, be specifically related to a kind of molding method for preparing of lithium metasilicate microballoon.
Background technology
In the face of the problem that mankind's energy shortage and environment go from bad to worse, clean, safety, reproducible fusion energy receive much concern.Nuclear fusion energy is that resource is unlimited, the desirable energy of clean and safe, is one of approach finally solving mankind energy problem.Deuterium and tritium realize the basic fusion fuel of two kinds of fusion reaction, deuterium is at the content comparatively horn of plenty of occurring in nature, but tritium is at occurring in nature content very rare (in air insufficient total amount 1 kilogram), tritium must be realized by the tritium propagation covering of fusion reactor and control oneself (both a tritium participates in fusion reaction and produces a neutron, and this neutron is absorbed generation tritium again by the lithium of breeding in covering to be continued to participate in fusion reaction).In order to maintain the continual and steady operation of fusion reactor, need to produce in tritium covering at fusion reactor to carry out tritium propagation, with the tritium of supplementary burnup.Tritium multiplication agent generally adopts the material containing lithium, can be divided into liquid tritium multiplication agent and solid-state tritium multiplication agent two kinds with the form of material.Liquid multiplication agent can also heat-carrying while product tritium, and can process continuously, and its tritium breeding ratio is comparatively large, but there is the weak points such as MHD effect, chemism are large, large to the corrosivity of structural material, the extraction difficulty of tritium.The chemical stability of solid-state tritium multiplication agent is good, can use at higher temperatures and tritium extracts easily.
Current International Thermonuclear heap (ITER) each participant prioritizing selection adopts the design of solid-state tritium multiplication agent covering to control oneself to realize tritium, and just adopts the ternary lithium ceramic containing lithium as product tritium material in this blanket design.Compare discovery by relevant performance data, the multiplication agent materials such as lithium metasilicate, lithium titanate and lithium zirconate have good combination property, become the candidate materials that fusion reactor produces tritium covering tritium multiplication agent.Because lithium metasilicate has, lithium atom density is high, good with the compatibility of structural material and beryllium thereof, calorifics, chemistry, machinery, irradiation behaviour good, tritium rate of release large, tritium hold-up is low and tritium extracts the advantages such as easy, and thus lithium metasilicate is the tritium multiplication agent material of ITER each side prioritizing selection.
Due to the handling of spherical multiplication agent easily, have to have between larger surface area, bead that more duct, permeability are good, the diffusion that is conducive to tritium and release.Therefore, solid-state tritium multiplication agent material generally adopts spheric granules.At present, have techniques such as adopting polymerization forming method, freeze forming method, wet method to prepare tritium multiplication agent microballoon, but the lithium metasilicate microballoon apparent density of preparation low, close that porosity is high, sphericity is low, rough surface, easily efflorescence blocking put forward the weak points such as tritium pipeline.
Summary of the invention
The object of the present invention is to provide a kind of atomized molten molding method for preparing of lithium metasilicate microballoon, lithium metasilicate microballoon apparent density prepared by the method be high, good sphericity, smooth surface.
Realize the technical scheme of the object of the invention: a kind of atomized molten molding method for preparing of lithium metasilicate microballoon, the method comprises the following steps:
(1) lithium metasilicate powder raw materials is joined in platinum crucible;
(2) adopt temperature programmed control mode of heating to heat to platinum crucible, melting process mesosilicic acid powder for lithium raw materials fully reacts, and by lithium metasilicate powder body melting to liquid;
(3) the lithium metasilicate liquid of melting is dispelled into droplet, lithium metasilicate droplet is solidified into lithium metasilicate microballoon;
(4) the lithium metasilicate microballoon obtained in above-mentioned steps (3) is sieved;
(5) annealing in process is carried out to lithium metasilicate microballoon.
The raw materials of lithium metasilicate powder is adopted in described step (1) to be one in the mixture of lithium carbonate and silica or the mixture of lithium hydroxide and silica.
Adopt the concrete steps of temperature programmed control mode of heating as follows in described step (2):
1., when temperature is less than 500 DEG C, the rate of heat addition is 10 DEG C/min;
2. temperature is within the scope of 500 DEG C ~ 900 DEG C, and the rate of heat addition is 5 DEG C/min;
3. temperature is greater than 900 DEG C when being less than or equal to 1250 DEG C, and the rate of heat addition is 10 DEG C/min.
Lithium metasilicate powder is adopted directly to join in platinum crucible as raw material in described step (1).
Adopt direct mode of heating in described step (2), the rate of heat addition is 10 DEG C/min.
In described step (3), the lithium metasilicate liquid of melting is dispelled into droplet, the concrete grammar that lithium metasilicate droplet is solidified into lithium metasilicate microballoon comprises the following steps: open mozzle end plug, the lithium metasilicate liquid runs down mozzle of melting flows out under gravity, under the effect of the gases at high pressure of atomizer ejection, melting lithium metasilicate liquid is dispelled into droplet, and lithium metasilicate droplet is solidified into lithium metasilicate microballoon in decline process under surface tension effects.
In described step (5) to lithium metasilicate microballoon 1050 DEG C, under vacuum environment insulation within two hours, carry out annealing in process.
Advantageous Effects of the present invention is: this preparation method's moulding process of the present invention is simple, the parameter affecting microballoon shaping is few, the impurity element of microballoon is mainly derived from raw material and platinum crucible, and the platinum element introduced is the catalyst being beneficial to tritium release, thus avoid some preparation methods need add adhesive introduce impurity, ensure that the purity of microballoon, reduce the introducing of long-lived radioactivity element.The microspherulite diameter utilizing the present invention to prepare is controlled, microballoon relative density be greater than 95% solid density, close porosity and be less than 5%, sphericity is greater than 0.95, smooth surface.Solid material in preparation method of the present invention is the solid reaction raw material preparing lithium metasilicate microballoon, also can be suitable for lithium metasilicate powder.
Accompanying drawing explanation
Fig. 1 is the structural representation of the atomized molten shaped device of a kind of lithium metasilicate microballoon provided by the present invention.
In figure: 1. platinum crucible, 2. mozzle, 3. atomizer, 4. mozzle end plug, 5. induction heating apparatus, 6. collector.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in further detail.
The atomized molten molding method for preparing of a kind of lithium metasilicate microballoon provided by the present invention, comprises the following steps:
(1) lithium metasilicate powder raw materials is joined in platinum crucible 1
The raw materials of lithium metasilicate powder is the one in the mixture of lithium carbonate and silica or the mixture of lithium hydroxide and silica.
Lithium metasilicate raw powder's production technology: lithium carbonate and silica are mixed according to the proportioning that mol ratio is 4:1.Or lithium hydroxide and silica are mixed according to the proportioning that silicon mol ratio is 4:1.
This step also can adopt lithium metasilicate powder directly to join in platinum crucible 1 as raw material.
(2) adopt temperature programmed control mode of heating to heat to platinum crucible 1, melting process mesosilicic acid powder for lithium raw materials fully reacts, and by lithium metasilicate powder body melting to liquid
When the one in employing silica lithium carbonate and the mixture of silica or the mixture of lithium hydroxide and silica prepares lithium metasilicate powder, adopt the concrete steps of temperature programmed control mode of heating as follows:
1., when temperature is less than 500 DEG C, the rate of heat addition is 10 DEG C/min.
2. temperature is within the scope of 500 DEG C ~ 900 DEG C, and the rate of heat addition is 5 DEG C/min; Namely adopt the mode slowly heated up, ensure that lithium carbonate and silica fully react and generate lithium metasilicate powder, or ensure that lithium hydroxide and silica fully react and generate lithium metasilicate powder.
3. temperature is greater than 900 DEG C when being less than or equal to 1250 DEG C, and the rate of heat addition is 10 DEG C/min; Namely adopt the mode be rapidly heated, when temperature reaches the fusing point 1250 DEG C of lithium metasilicate, lithium metasilicate powder body melting is liquid.
When adopting lithium metasilicate powder directly to join in platinum crucible as raw material, adopt direct mode of heating, the rate of heat addition is 10 DEG C/min.When temperature reaches the fusing point 1250 DEG C of lithium metasilicate, lithium metasilicate powder body melting is liquid.
(3) the lithium metasilicate liquid of melting is dispelled into droplet, lithium metasilicate droplet is solidified into lithium metasilicate microballoon
1. atomizer 3 adjustments of gas pressure is opened between 0.2-0.3Mpa scope;
2. the mozzle 2 that has of platinum crucible 1 nested inside, open the mozzle end plug 4 made by platinum bar in mozzle 2 lower part outlet, the lithium metasilicate liquid runs down mozzle 2 of melting flows out under gravity, the outlet of atomizer 3 is positioned at mozzle 2 and exports bottom, under the effect of the gases at high pressure of atomizer 3 ejection, melting lithium metasilicate liquid is dispelled into droplet, and lithium metasilicate droplet is solidified into lithium metasilicate microballoon in decline process under surface tension effects.
Open the induction heating apparatus 5 at mozzle 2 place simultaneously, prevent remaining lithium metasilicate melt liquid condensation from blocking mozzle 2;
(4) the lithium metasilicate microballoon obtained in above-mentioned steps (3) is sieved
The lithium metasilicate microballoon obtained in above-mentioned steps (3) falls in collector 6, adopts model selecting machine that aspherical particle is removed, then sieves out by the lithium metasilicate microballoon of particle diameter within the scope of 0.1mm ~ 1.2mm by pulp classifier.
(5) annealing in process is carried out to lithium metasilicate microballoon
Lithium metasilicate drop can remain a large amount of stress in quick cooling procedure, and these internal stress can cause the generation of some crackles, and develops along crystal boundary.In order to improve the mechanical strength of microballoon, need to the lithium metasilicate microballoon obtained in above-mentioned steps (5) 1050 DEG C, under vacuum environment insulation within two hours, carry out annealing in process.
In conjunction with the accompanying drawings and embodiments the present invention is explained in detail above, but the present invention is not limited to above-described embodiment, in the ken that those of ordinary skill in the art possess, various change can also be made under the prerequisite not departing from present inventive concept.The content be not described in detail in the present invention all can adopt prior art.
Claims (7)
1. an atomized molten molding method for preparing for lithium metasilicate microballoon, is characterized in that: the method comprises the following steps:
(1) lithium metasilicate powder raw materials is joined in platinum crucible (1);
(2) adopt temperature programmed control mode of heating to platinum crucible (1) heating, melting process mesosilicic acid powder for lithium raw materials fully reacts, and by lithium metasilicate powder body melting to liquid;
(3) the lithium metasilicate liquid of melting is dispelled into droplet, lithium metasilicate droplet is solidified into lithium metasilicate microballoon;
(4) the lithium metasilicate microballoon obtained in above-mentioned steps (3) is sieved;
(5) annealing in process is carried out to lithium metasilicate microballoon.
2. the atomized molten molding method for preparing of a kind of lithium metasilicate microballoon as claimed in claim 1, is characterized in that: adopt in described step (1) raw materials of lithium metasilicate powder to be one in the mixture of lithium carbonate and silica or the mixture of lithium hydroxide and silica.
3. the atomized molten molding method for preparing of a kind of lithium metasilicate microballoon as claimed in claim 2, is characterized in that: adopt the concrete steps of temperature programmed control mode of heating as follows in described step (2):
1., when temperature is less than 500 DEG C, the rate of heat addition is 10 DEG C/min;
2. temperature is within the scope of 500 DEG C ~ 900 DEG C, and the rate of heat addition is 5 DEG C/min;
3. temperature is greater than 900 DEG C when being less than or equal to 1250 DEG C, and the rate of heat addition is 10 DEG C/min.
4. the atomized molten molding method for preparing of a kind of lithium metasilicate microballoon as claimed in claim 1, is characterized in that: adopt lithium metasilicate powder directly to join in platinum crucible (1) as raw material in described step (1).
5. the atomized molten molding method for preparing of a kind of lithium metasilicate microballoon as claimed in claim 4, is characterized in that: adopt direct mode of heating in described step (2), the rate of heat addition is 10 DEG C/min.
6. the atomized molten molding method for preparing of a kind of lithium metasilicate microballoon according to any one of claim 1 to 5, it is characterized in that: in described step (3), the lithium metasilicate liquid of melting is dispelled into droplet, the concrete grammar that lithium metasilicate droplet is solidified into lithium metasilicate microballoon comprises the following steps: open mozzle end plug (4), the lithium metasilicate liquid runs down mozzle (2) of melting flows out under gravity, under the effect of the gases at high pressure sprayed at atomizer (3), melting lithium metasilicate liquid is dispelled into droplet, lithium metasilicate droplet is solidified into lithium metasilicate microballoon in decline process under surface tension effects.
7. the atomized molten molding method for preparing of a kind of lithium metasilicate microballoon according to any one of claim 1 to 5, is characterized in that: in described step (5) to lithium metasilicate microballoon 1050 DEG C, under vacuum environment insulation within two hours, carry out annealing in process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310205766.9A CN104209053A (en) | 2013-05-29 | 2013-05-29 | Preparation method of lithium silicate microsphere through melting, atomizing, and forming |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310205766.9A CN104209053A (en) | 2013-05-29 | 2013-05-29 | Preparation method of lithium silicate microsphere through melting, atomizing, and forming |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104209053A true CN104209053A (en) | 2014-12-17 |
Family
ID=52091196
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310205766.9A Pending CN104209053A (en) | 2013-05-29 | 2013-05-29 | Preparation method of lithium silicate microsphere through melting, atomizing, and forming |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104209053A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105645421A (en) * | 2015-12-30 | 2016-06-08 | 浙江工业大学 | Mesoporous hollow lithium silicate microspheres as well as preparation and application of mesoporous hollow lithium silicate microspheres |
| CN107824122A (en) * | 2017-12-07 | 2018-03-23 | 中国工程物理研究院核物理与化学研究所 | A kind of multiplication agent ceramic bead molten atomizing prilling granulator and method |
| CN113368517A (en) * | 2021-06-10 | 2021-09-10 | 盘星新型合金材料(常州)有限公司 | Atomizing spray plate, spherical silicon boride ceramic powder, and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010089931A1 (en) * | 2009-02-04 | 2010-08-12 | 独立行政法人産業技術総合研究所 | Method for producing lithium silicate compound |
| CN102241516A (en) * | 2010-05-13 | 2011-11-16 | 中国科学院上海硅酸盐研究所 | Method for preparing Li4SiO4 ceramic powder by water-based sol-gel process |
-
2013
- 2013-05-29 CN CN201310205766.9A patent/CN104209053A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010089931A1 (en) * | 2009-02-04 | 2010-08-12 | 独立行政法人産業技術総合研究所 | Method for producing lithium silicate compound |
| CN102241516A (en) * | 2010-05-13 | 2011-11-16 | 中国科学院上海硅酸盐研究所 | Method for preparing Li4SiO4 ceramic powder by water-based sol-gel process |
Non-Patent Citations (3)
| Title |
|---|
| HUA TANG 等: "Influence of Heat Treatment on Lithium Orthosilicate Pebble", 《ADVANCED MATERIALS RESEARCH》, vol. 624, 27 December 2012 (2012-12-27) * |
| MATTHIAS H.H. KOLB等: "Enhanced fabrication process for lithium orthosilicate pebbles as breeding material", 《FUSION ENGINEERING AND DESIGN》, 21 February 2011 (2011-02-21) * |
| Y.J.FENG等: "Fabrication and characterization of LiSiO4 pebbles by melt spraying method", 《FUSION ENGINEERING AND DESIGH》, 3 March 2012 (2012-03-03) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105645421A (en) * | 2015-12-30 | 2016-06-08 | 浙江工业大学 | Mesoporous hollow lithium silicate microspheres as well as preparation and application of mesoporous hollow lithium silicate microspheres |
| CN107824122A (en) * | 2017-12-07 | 2018-03-23 | 中国工程物理研究院核物理与化学研究所 | A kind of multiplication agent ceramic bead molten atomizing prilling granulator and method |
| CN107824122B (en) * | 2017-12-07 | 2020-07-31 | 中国工程物理研究院核物理与化学研究所 | Proliferant ceramic pellet melting and spraying granulation device and method |
| CN113368517A (en) * | 2021-06-10 | 2021-09-10 | 盘星新型合金材料(常州)有限公司 | Atomizing spray plate, spherical silicon boride ceramic powder, and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106971765B (en) | A kind of preparation process of high TRISO content inertia base dispersion fuel pellet | |
| CN105289433B (en) | A kind of method of prepare with scale transition metal oxide porous microsphere | |
| CN105081337B (en) | Method and device for preparing fine spherical metal powder through high-frequency supersonic plasma gas | |
| CN111548137B (en) | Ceramic precursor slurry and 3D printing reaction forming method of porous ceramic piece | |
| CN104575626A (en) | Tracing microsphere for pebble bed high-temperature gas-cooled reactor | |
| CN104209053A (en) | Preparation method of lithium silicate microsphere through melting, atomizing, and forming | |
| CN1937097A (en) | Technology for making nuclear fuel element core by external gelatinization method | |
| CN108751975A (en) | The preparation method of tritium proliferation ceramic bead in a kind of fusion reactor solid blanket | |
| CN107274936A (en) | A kind of fast preparation method of the enhanced uranium dioxide nuclear fuel of beryllium oxide | |
| CN110893468A (en) | Method and device for preparing spherical metal powder by combined atomization | |
| CN108565442A (en) | A kind of preparation method of the compound sulfide material of nucleocapsid | |
| CN102020268A (en) | Hollow carbon sphere and preparation method thereof | |
| CN102259837B (en) | Particle used for hydrogen production and preparation method thereof | |
| CN105860105A (en) | Preparation method of polyamide 6 powder for laser sintering | |
| CN102672189A (en) | Preparation method of spherical tungsten powder | |
| CN106630615B (en) | A method of hollow glass micropearl is manufactured using cullet | |
| CN102194532A (en) | Preparation method of compound powder of boron carbide and carbon | |
| CN105568032B (en) | A kind of injection molding through-hole foamed metal and preparation method thereof | |
| CN103708419B (en) | Method for preparing of high-activity LiH microspheres through wet process | |
| CN103252499B (en) | The preparation facilities that ferrum-based catalyst aerosolization is shaped and preparation technology | |
| CN107134299B (en) | A kind of preparation method of the ceramic microsphere of thorium base carbide and/or thorium base oxycarbide | |
| CN106495093B (en) | A kind of reversible hydrogen manufacturing system of high-performance lithium borohydride-magnesium hydride and hydrogen production process | |
| CN104496487B (en) | Double-layer ceramic microsphere of nucleocapsid structure and preparation method thereof | |
| Lo Frano et al. | Feasibility study of a new fabrication method for the Li4SiO4 pebbles | |
| CN103964488A (en) | Method for preparing micro or nano copper oxide powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20141217 |