CN103172372B - Lithium zirconate ceramic ball tritium breeding material and preparation method thereof - Google Patents
Lithium zirconate ceramic ball tritium breeding material and preparation method thereof Download PDFInfo
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- CN103172372B CN103172372B CN201310134204.XA CN201310134204A CN103172372B CN 103172372 B CN103172372 B CN 103172372B CN 201310134204 A CN201310134204 A CN 201310134204A CN 103172372 B CN103172372 B CN 103172372B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 38
- 239000000463 material Substances 0.000 title claims abstract description 25
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 18
- 238000009395 breeding Methods 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910052722 tritium Inorganic materials 0.000 title abstract description 13
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 title abstract description 12
- 230000001488 breeding effect Effects 0.000 title abstract 2
- 238000005245 sintering Methods 0.000 claims abstract description 21
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000462 isostatic pressing Methods 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 150000001875 compounds Chemical class 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000003068 static effect Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 239000000428 dust Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 17
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 9
- 238000000465 moulding Methods 0.000 abstract description 6
- 230000018044 dehydration Effects 0.000 abstract description 3
- 238000006297 dehydration reaction Methods 0.000 abstract description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract 3
- 239000001569 carbon dioxide Substances 0.000 abstract 3
- 238000005056 compaction Methods 0.000 abstract 1
- 238000001175 rotational moulding Methods 0.000 abstract 1
- 230000004927 fusion Effects 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 8
- 235000011089 carbon dioxide Nutrition 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 229910010093 LiAlO Inorganic materials 0.000 description 1
- 230000003542 behavioural effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to the technical field of nuclear energy and particularly relates to a lithium zirconate ceramic ball tritium breeding material and a preparation method thereof. According to the preparation method disclosed by the invention, an isostatic pressing method is adopted for preparing ceramic balls, and the density is higher than those prepared by rotational molding, wet process dehydration molding and wet process ZrO2 addition molding. The ceramic balls prepared by other methods are molded under the situation that external pressure does not exist, and the degree of compaction of components is lower than that of the isostatic pressing method. Simultaneously, the structure can release carbon dioxide during the sintering process, and the density of the balls is lower; and however, in the preparation method disclosed by the invention, powder is firstly prepared and can realize full reaction and release the carbon dioxide, and when the sintering of the ceramic balls is performed in the second step, the released carbon dioxide is very little, and the density of the prepared lithium zirconate ceramic balls is higher. In addition, if the density of the ceramic balls needs to be improved continuously, the pressure for isostatic pressing can be improved, and then the density of the obtained ceramic balls can be increased.
Description
Technical field
The invention belongs to nuclear energy technology field, particularly a kind of lithium zirconate 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 behavioral study 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 strategic energy of human future Sustainable development, according to the current situation prediction of current international magnetic confinement fusion technology, very likely in 21st century, first three makes substantial progress magnetic confinement nuclear fusion heap commercial technology taking Tokamak Fusion Reactor as mark for 10 years, develops the ripe of the clean nuclear fusion energy technology of potential alternative fossil energy.
Tritium is artificial nucleic and consumes in deuterium-tritium body fusion reaction, in order to maintain the continual and steady operation of fusion reactor, need in fusion reactor blanket, carry out tritium production and propagation, to supplement 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
4in tritium performance, mechanical property and thermal characteristics etc. several tritium multiplication agents.At present, Li
4siO
4and Li
2tiO
3become respectively the preferred material that Europe and Japanese fusion reactor produce tritium covering tritium multiplication agent.From the design of cladding structure, multiplication agent is made to microballoon, if single size distributes, its closestpacking filling ratio in covering also only has 67%, considers that the grating of different diameter microballoon is filled, maximum loading level is 80%.Preparation method mainly comprises that Japan is for Li
2tiO
3rotational forming, wet method dehydration forming, the wet method TiO of exploitation
2addition moulding, extrusion moulding, heating reunion moulding and the moulding of melting spray thing etc. in Europe.And Li
2zrO
3also be a kind of tritium-breeding material, current preparation method is mainly sol-gel method.The efficiency that this method is prepared ball is high, but in ball sintering process, breakage rate is also high, wastes more serious.
Summary of the invention
For prior art deficiency, the invention provides a kind of lithium zirconate Ceramic Balls tritium-breeding material and preparation method thereof.
A preparation method for lithium zirconate Ceramic Balls tritium-breeding material, its concrete steps are as follows:
(1) Quilonum Retard and zirconium white and excessive dehydrated alcohol are mixed, wherein Quilonum Retard and zirconic molar ratio are 1.1～1.2;
(2) mixed solution step (1) being obtained uses zirconia ceramics ball as abrading-ball, batch mixing 4～5 hours on ball crusher;
(3) compound step (2) being obtained is dried in baking oven, and Temperature Setting is 80～90 DEG C, 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 to sintering; Be warmed up to 500～600 DEG C through two hours, be incubated 3 hours, and then with two hours, be warmed up to 900 DEG C～1000 DEG C, be incubated 24 hours; Reaction equation is: Li
2cO
3+ ZrO
2=Li
2zrO
3+ CO
2↑;
(5) compound after sintering step (4) being obtained rejoins excessive dehydrated alcohol, again pours in abrasive dust tank, uses zirconia ceramics ball as abrading-ball, mixes 4 hours on ball crusher;
(6) compound step (5) being obtained is dried in baking oven, and Temperature Setting is 80～90 DEG C, and drying time is 8～12 hours;
(7) compound after step (6) is dried is pulverized, sieved;
(8) the compound powder of step (7) gained is packed in rubber mold, on isostatic pressing machine, rubber mold is pressurizeed, institute's plus-pressure is 100～200 MPa;
(9) Ceramic Balls of gained after the static pressure such as step (8) is carried out to sintering in High Temperature Furnaces Heating Apparatus, sintering temperature is 1200 ~ 1350 DEG C, and soaking time is 5～8 hours, obtains a kind of lithium zirconate Ceramic Balls tritium-breeding material.
A kind of lithium zirconate Ceramic Balls tritium-breeding material, the molecular formula of described lithium zirconate Ceramic Balls tritium-breeding material is Li
2zrO
3, its density is not less than 4.01 g/cm
3, be not less than β-Li
2zrO
3theoretical density 96.55%, its thermal conductivity is 1.2～2.2 W/mK.
Beneficial effect of the present invention is:
The method of the static pressure such as employing of the present invention is prepared Ceramic Balls, than rotational forming, wet method dehydration forming, wet method ZrO
2it is high that the density of addition moulding is wanted.Ceramic Balls prepared by other method, is all there is no the situation compacted under of external pressure, and the compactness of its composition is just not as waiting method of static pressure.Structure is in sintering process simultaneously, also to discharge carbonic acid gas, make the density of ball lower, and in the present invention, first prepared powder, complete reaction of these powders, discharge carbonic acid gas, in the time that second step carries out Ceramic Balls sintering, the carbonic acid gas of release is little, and this also makes prepared lithium zirconate Ceramic Balls density higher.In addition, if want to continue to improve the density of Ceramic Balls, the pressure that waits static pressure can also be improved, the Ceramic Balls density obtaining like this can increase.The Ceramic Balls density that lithium zirconate material prepared by the present invention is prepared than existing method is better, and thermal conductivity is also higher, is more suitable for using as covering bred material in fusion reactor.
Brief description of the drawings
Fig. 1 is the XRD figure of the prepared lithium zirconate Ceramic Balls tritium-breeding material of embodiment 1.
Embodiment
The invention provides a kind of lithium zirconate Ceramic Balls tritium-breeding material and preparation method thereof, below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Embodiment 1
(1) Quilonum Retard 0.11 mol, zirconium white 0.1 mol, 100 ml ethanol are mixed; Mixed solution uses zirconia ceramics ball as abrading-ball, batch mixing 4 hours on ball crusher.At 80 DEG C of temperature, use oven for drying 4 hours.
(2) compound sintering in sintering oven.Within two hours, be warmed up to 600 DEG C, be incubated 3 hours, then be warmed up to 900 DEG C with two hours, be incubated 24 hours.Then naturally cooling.After taking-up, on ball mill, use zirconia ceramics ball to carry out abrasive dust, grind 4 hours, sieve.
(3) ceramic powder is packed in rubber mold, on isostatic pressing machine, rubber mold is pressurizeed, institute's plus-pressure is 150 MPa.
(4) waiting Ceramic Balls after static pressure to carry out sintering in High Temperature Furnaces Heating Apparatus, sintering temperature is 1200 ~ 1350 DEG C, and soaking time is 5～8 hours.After insulation, 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
2zrO
3, through XPS test, in lithium zirconate material, contain Li+.
Claims (1)
1. a preparation method for lithium zirconate Ceramic Balls tritium-breeding material, is characterized in that: the molecular formula of described lithium zirconate Ceramic Balls tritium-breeding material is Li
2zrO
3, its density is not less than 4.01g/cm
3, be not less than β-Li
2zrO
3theoretical density 96.55%, its thermal conductivity is 1.2～2.2W/mK;
Described preparation method's concrete steps are as follows:
(1) Quilonum Retard and zirconium white and excessive dehydrated alcohol are mixed, wherein Quilonum Retard and zirconic molar ratio are 1.1～1.2;
(2) mixed solution step (1) being obtained uses zirconia ceramics ball as abrading-ball, batch mixing 4～5 hours on ball crusher;
(3) compound step (2) being obtained is dried in baking oven, and Temperature Setting is 80～90 DEG C, 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 to sintering; Be warmed up to 500～600 DEG C through two hours, be incubated 3 hours, and then with two hours, be warmed up to 900 DEG C～1000 DEG C, be incubated 24 hours; Reaction equation is: Li
2cO
3+ ZrO
2=Li
2zrO
3+ CO
2↑;
(5) compound after sintering step (4) being obtained rejoins excessive dehydrated alcohol, again pours in abrasive dust tank, uses zirconia ceramics ball as abrading-ball, mixes 4 hours on ball crusher;
(6) compound step (5) being obtained is dried in baking oven, and Temperature Setting is 80～90 DEG C, and drying time is 8～12 hours;
(7) compound after step (6) is dried is pulverized, sieved;
(8) the compound powder of step (7) gained is packed in rubber mold, on isostatic pressing machine, rubber mold is pressurizeed, institute's plus-pressure is 100～200MPa;
(9) Ceramic Balls of gained after the static pressure such as step (8) is carried out to sintering in High Temperature Furnaces Heating Apparatus, sintering temperature is 1200～1350 DEG C, and soaking time is 5～8 hours, obtains a kind of lithium zirconate Ceramic Balls tritium-breeding material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310134204.XA CN103172372B (en) | 2013-04-17 | 2013-04-17 | Lithium zirconate ceramic ball tritium breeding material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310134204.XA CN103172372B (en) | 2013-04-17 | 2013-04-17 | Lithium zirconate ceramic ball tritium breeding material and preparation method thereof |
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|---|---|
| CN103172372A CN103172372A (en) | 2013-06-26 |
| CN103172372B true CN103172372B (en) | 2014-11-26 |
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| CN201310134204.XA Expired - Fee Related CN103172372B (en) | 2013-04-17 | 2013-04-17 | Lithium zirconate ceramic ball tritium breeding material and preparation method thereof |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101214977A (en) * | 2007-01-05 | 2008-07-09 | 北京理工大学 | Preparation method of lithium zirconate material for absorbing carbon dioxide at high temperature |
| 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 |
-
2013
- 2013-04-17 CN CN201310134204.XA patent/CN103172372B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101214977A (en) * | 2007-01-05 | 2008-07-09 | 北京理工大学 | Preparation method of lithium zirconate material for absorbing carbon dioxide at high temperature |
| 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 |
Non-Patent Citations (8)
| Title |
|---|
| CHHCSBTBM中固体氚陶瓷增殖剂微球研究进展;陈晓军等;《核聚变与等离子体物理》;20060930;第26卷(第3期);第215页 * |
| Experimantal evidence for tritium release-controlling processes in lithium silicates;Wbreitung等;《Journal of Nuclear Materials》;19911231;全文 * |
| Wbreitung等.Experimantal evidence for tritium release-controlling processes in lithium silicates.《Journal of Nuclear Materials》.1991,全文. * |
| 固体氚增殖剂的制备及性能综述;朱德琼等;《材料导报》;20080930;第22卷(第9期);第73页 * |
| 朱德琼等.固体氚增殖剂的制备及性能综述.《材料导报》.2008,第22卷(第9期),第73页. * |
| 溶胶-凝胶法制备锆酸锂陶瓷微球;王和义等;《高技术通讯》;19970831(第8期);全文 * |
| 王和义等.溶胶-凝胶法制备锆酸锂陶瓷微球.《高技术通讯》.1997,(第8期),全文. * |
| 陈晓军等.CHHCSBTBM中固体氚陶瓷增殖剂微球研究进展.《核聚变与等离子体物理》.2006,第26卷(第3期),第215页. * |
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| CN103172372A (en) | 2013-06-26 |
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