CN103183509A - Lithium titanate ceramic ball tritium propagation material and preparation method thereof - Google Patents
Lithium titanate ceramic ball tritium propagation material and preparation method thereof Download PDFInfo
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- CN103183509A CN103183509A CN2013101343748A CN201310134374A CN103183509A CN 103183509 A CN103183509 A CN 103183509A CN 2013101343748 A CN2013101343748 A CN 2013101343748A CN 201310134374 A CN201310134374 A CN 201310134374A CN 103183509 A CN103183509 A CN 103183509A
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- ceramic balls
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- lithium titanate
- tritium
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Abstract
The invention belongs to the technical field of nuclear energy, and particularly relates to a lithium titanate ceramic tritium propagation material and a preparation method thereof. Ceramic balls are prepared by adopting an isostatic pressing method and have higher density in comparison with the ceramic balls formed by adopting rotation molding, wet-process dewatering molding and wet-process TiO2 molding. As the ceramic balls prepared by other methods are formed under the condition of inexistence of external pressure, the compactness of the components of the ceramic balls prepared by other methods is not as good as that of the components of the ceramic balls prepared by the isostatic pressing method. Simultaneously, carbon dioxide in the structure is released in a sintering process, so that the density of the balls is low; according to the preparation method, firstly powder is prepared and is completely reacted, so that the carbon dioxide is released, and when the ceramic balls are sintered in the second step, the few carbon dioxide is released, so that the prepared lithium titanate ceramic balls have high density. In addition, if the density of the ceramic balls needs to be continuously increased, the pressure of the isostatic pressing can also be increased, so that the density of the obtained ceramic balls is increased.
Description
Technical field
The invention belongs to the nuclear energy technology field, particularly a kind of lithium titanate Ceramic Balls tritium-breeding material and preparation method thereof.
Background technology
Solid tritium propagation clad material is one of critical material of commercial nuclear fusion stack, and its technology of preparing and thermal technology's physical property have directly determined the interior behavior research of the heap of covering, is the necessary basis of carrying out design and development tritium propagation covering.
Magnetic confinement nuclear fusion can be one of choice of technology of the human following STRATEGIES OF SUSTAINABLE DEVELOPMENT energy, according to present international magnetic confinement fusion technology development situation prediction, with the tokamak fusion reactor be the magnetic confinement nuclear fusion heap commercial technology of sign very likely first three made substantial progress in 10 years in 21st century, opportunity of cleaning nuclear fusion energy technology of developing potential alternative fossil energy is ripe.
Tritium is artificial nucleic and consumes in the deuterium-tritium body fusion reaction, in order to keep the continual and steady operation of fusion reactor, need carry out tritium production and propagation in the fusion reactor covering, to replenish the tritium of burnup.
The kind of solid product tritium material is more, and the correlative study work of having carried out at present mainly concentrates on Li
2O, Li
2ZrO
3, LiAlO
2, Li
2TiO
3, Li
2SiO
3, Li
4SiO
4On tritium performance, mechanical property and the thermal characteristics etc. several tritium multiplication agents.At present, Li
4SiO
4And Li
2TiO
3Become the preferred material that Europe and Japanese fusion reactor produce tritium covering tritium multiplication agent respectively.From the design of cladding structure, multiplication agent is made microballoon, if single size distributes, its closestpacking filling ratio in covering also has only 67%, considers that the grating of different diameter microballoon is filled, maximum loading level is 80%.The preparation method comprises that mainly Japan is at Li
2TiO
3The rotational forming of exploitation, wet method dehydration moulding, wet method TiO
2The addition moulding, the extrusion moulding in Europe, heating reunion moulding and the moulding of fusion spray thing etc.
Summary of the invention
At the prior art deficiency, the invention provides a kind of lithium titanate Ceramic Balls tritium-breeding material and preparation method thereof.
A kind of preparation method of lithium titanate Ceramic Balls tritium-breeding material, its concrete steps are as follows:
(1) Quilonum Retard and titanium oxide and excessive dehydrated alcohol are mixed, wherein the molar ratio of Quilonum Retard and titanium oxide is 1.1～1.2;
(2) mixed solution that step (1) is obtained uses zirconia ball as abrading-ball, and batch mixing is 4～5 hours on ball crusher;
(3) compound that step (2) is obtained is dried in baking oven, and temperature is set at 80～90 ℃, and drying time is 8～12 hours;
(4) compound and crucible are all put into sintering oven, set heating curve, sintering oven is steadily heated up, compound is carried out sintering; Be warmed up to 500～600 ℃ through two hours, be incubated 3 hours, and then with two hours time, be warmed up to 900 ℃～1000 ℃, be incubated 24 hours; Reaction equation is: Li
2CO
3+ TiO
2=Li
2TiO
3+ CO
2↑;
(5) compound behind the sintering that step (4) is obtained adds excessive dehydrated alcohol again, pours into again in the abrasive dust jar, uses the zirconia ceramics ball, mixes 4 hours at ball crusher;
(6) compound that step (5) is obtained is dried in baking oven, and temperature is set at 80～90 ℃, and drying time is 8～12 hours;
(7) compound after step (6) oven dry is pulverized, sieved;
(8) the compound powder of step (7) gained is packed in the rubber mold, on isostatic pressing machine, rubber mold is pressurizeed, institute's plus-pressure is 100～200 MPa;
(9) Ceramic Balls of gained behind step static pressure such as (8) is carried out sintering in High Temperature Furnaces Heating Apparatus, the sintering temperature is 1200 ~ 1350 ℃, and soaking time is 5～8 hours, namely obtains a kind of lithium titanate Ceramic Balls tritium-breeding material.
A kind of lithium titanate Ceramic Balls tritium-breeding material, the molecular formula of described lithium titanate Ceramic Balls tritium-breeding material is Li
2TiO
3, its density is not less than 3.061 g/cm
3, namely be not less than β-Li
2TiO
3Theoretical density 89.2%, its thermal conductivity is 1.8～2.0 W/mK.
Beneficial effect of the present invention is:
The method of static pressure such as employing of the present invention prepares Ceramic Balls, than rotational forming, wet method dehydration moulding, wet method TiO
2It is high that the density of addition moulding is wanted.The Ceramic Balls of other method preparation all is that the compactness of its composition is just not as waiting method of static pressure at the situation compacted under that does not have external pressure.Structure is in sintering process simultaneously, also to discharge carbonic acid gas, make the density of ball lower, and in the present invention, at first having prepared powder, these powders are complete reaction, discharged carbonic acid gas, in second step when carrying out the Ceramic Balls sintering, the carbonic acid gas of release seldom, this makes that also prepared lithium titanate Ceramic Balls density is higher.In addition, if want to continue to improve the density of Ceramic Balls, can also improve the pressure that waits static pressure, the Ceramic Balls density of Huo Deing can increase like this.The lithium titanate material of the present invention's preparation is better than the Ceramic Balls density of existing method preparation, and thermal conductivity is also higher, is more suitable for using as the covering bred material in fusion reactor.
Description of drawings
Fig. 1 is the XRD figure of the prepared lithium titanate Ceramic Balls tritium-breeding material of embodiment 1.
Embodiment
The invention provides a kind of lithium titanate Ceramic Balls tritium-breeding material and preparation method thereof, the present invention will be further described below in conjunction with the drawings and specific embodiments.
Embodiment 1
(1) Quilonum Retard 0.11 mol, titanium oxide 0.1 mol and 100 ml ethanol are mixed; Mixed solution uses zirconia ball as abrading-ball, and batch mixing is 4 hours on ball crusher.Under 80 ℃ of temperature, use oven for drying 4 hours.
(2) compound sintering in sintering oven.Be warmed up to 600 ℃ in two hours, be incubated 3 hours, be warmed up to 900 ℃ with two hours again, be incubated 24 hours.Naturally cooling then.After the taking-up, use zirconia ball to carry out abrasive dust at ball mill, ground 4 hours, sieve.
(3) ceramic powder is packed in the rubber mold, on isostatic pressing machine, rubber mold is pressurizeed, institute's plus-pressure is 150 MPa.
(4) Ceramic Balls behind the static pressure such as grade is carried out sintering in High Temperature Furnaces Heating Apparatus, sintering temperature is 1200 ~ 1350 ℃, and soaking time is 5～8 hours.After the insulation, the material furnace cooling, to be cooled after room temperature, Ceramic Balls is taken out.
Material is tested through XRD, and the material structure of preparation is Li
2TiO
3, through the XPS test, contain Li in the lithium titanate material
+
Claims (2)
1. the preparation method of a lithium titanate Ceramic Balls tritium-breeding material is characterized in that concrete steps are as follows:
(1) Quilonum Retard and titanium oxide and excessive dehydrated alcohol are mixed, wherein the molar ratio of Quilonum Retard and titanium oxide is 1.1～1.2;
(2) mixed solution that step (1) is obtained uses zirconia ball as abrading-ball, and batch mixing is 4～5 hours on ball crusher;
(3) compound that step (2) is obtained is dried in baking oven, and temperature is set at 80～90 ℃, and drying time is 8～12 hours;
(4) compound and crucible are all put into sintering oven, set heating curve, sintering oven is steadily heated up, compound is carried out sintering; Be warmed up to 500～600 ℃ through two hours, be incubated 3 hours, and then with two hours time, be warmed up to 900 ℃～1000 ℃, be incubated 24 hours; Reaction equation is: Li
2CO
3+ TiO
2=Li
2TiO
3+ CO
2↑;
(5) compound behind the sintering that step (4) is obtained adds excessive dehydrated alcohol again, pours into again in the abrasive dust jar, uses the zirconia ceramics ball, mixes 4 hours at ball crusher;
(6) compound that step (5) is obtained is dried in baking oven, and temperature is set at 80～90 ℃, and drying time is 8～12 hours;
(7) compound after step (6) oven dry is pulverized, sieved;
(8) the compound powder of step (7) gained is packed in the rubber mold, on isostatic pressing machine, rubber mold is pressurizeed, institute's plus-pressure is 100～200 MPa;
(9) Ceramic Balls of gained behind step static pressure such as (8) is carried out sintering in High Temperature Furnaces Heating Apparatus, sintering temperature is 1200 ~ 1350 ℃, and soaking time is 5～8 hours, namely obtains a kind of lithium titanate Ceramic Balls tritium-breeding material.
2. lithium titanate Ceramic Balls tritium-breeding material, it is characterized in that: the molecular formula of described lithium titanate Ceramic Balls tritium-breeding material is Li
2TiO
3, its density is not less than 3.061 g/cm
3, namely be not less than β-Li
2TiO
3Theoretical density 89.2%, its thermal conductivity is 1.8～2.0 W/mK.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101343748A CN103183509A (en) | 2013-04-17 | 2013-04-17 | Lithium titanate ceramic ball tritium propagation material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101343748A CN103183509A (en) | 2013-04-17 | 2013-04-17 | Lithium titanate ceramic ball tritium propagation material and preparation method thereof |
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| CN103183509A true CN103183509A (en) | 2013-07-03 |
Family
ID=48674994
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|---|---|---|---|
| CN2013101343748A Pending CN103183509A (en) | 2013-04-17 | 2013-04-17 | Lithium titanate ceramic ball tritium propagation material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103854706A (en) * | 2014-03-25 | 2014-06-11 | 中国人民解放军陆军军官学院 | Preparation method of fusion reactor cladding neutrons and tritium breeding agent beryllium acid lithium pellets |
| CN104828859A (en) * | 2015-04-20 | 2015-08-12 | 陕西科技大学 | Subcritical preparation method for super-uniform submicron beta-Li2TiO3 powder |
| CN107256724A (en) * | 2017-06-09 | 2017-10-17 | 山东东佳集团股份有限公司 | Tritium breeds the preparation method of ceramic material metatitanic acid lithium |
| 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 |
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| CN201317125Y (en) * | 2008-12-16 | 2009-09-30 | 淄博华创精细陶瓷有限公司 | Novel isostatic pressing shaping die |
| CN102354748A (en) * | 2011-09-30 | 2012-02-15 | 苏州大学 | Anode material for lithium ion battery and preparation method thereof |
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2013
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103854706A (en) * | 2014-03-25 | 2014-06-11 | 中国人民解放军陆军军官学院 | Preparation method of fusion reactor cladding neutrons and tritium breeding agent beryllium acid lithium pellets |
| CN103854706B (en) * | 2014-03-25 | 2017-02-08 | 中国人民解放军陆军军官学院 | Preparation method of fusion reactor cladding neutrons and tritium breeding agent beryllium acid lithium pellets |
| CN104828859A (en) * | 2015-04-20 | 2015-08-12 | 陕西科技大学 | Subcritical preparation method for super-uniform submicron beta-Li2TiO3 powder |
| CN107256724A (en) * | 2017-06-09 | 2017-10-17 | 山东东佳集团股份有限公司 | Tritium breeds the preparation method of ceramic material metatitanic acid lithium |
| CN107256724B (en) * | 2017-06-09 | 2018-12-11 | 山东东佳集团股份有限公司 | The preparation method of tritium proliferation ceramic material metatitanic acid lithium |
| 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 |
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Application publication date: 20130703 |