CN104140259A - Method for quickly manufacturing Li2TiO3 tritium breeding small balls - Google Patents
Method for quickly manufacturing Li2TiO3 tritium breeding small balls Download PDFInfo
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- CN104140259A CN104140259A CN201410369142.5A CN201410369142A CN104140259A CN 104140259 A CN104140259 A CN 104140259A CN 201410369142 A CN201410369142 A CN 201410369142A CN 104140259 A CN104140259 A CN 104140259A
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- powder
- tio
- dimensional model
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Links
- 238000000034 method Methods 0.000 title claims abstract description 25
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 title claims abstract description 20
- 229910052722 tritium Inorganic materials 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title abstract description 7
- 229910007848 Li2TiO3 Inorganic materials 0.000 title abstract 5
- 238000009395 breeding Methods 0.000 title abstract 3
- 230000001488 breeding effect Effects 0.000 title abstract 3
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 20
- 238000010146 3D printing Methods 0.000 claims abstract description 17
- 238000012545 processing Methods 0.000 claims abstract description 15
- 239000011230 binding agent Substances 0.000 claims abstract description 9
- 239000011812 mixed powder Substances 0.000 claims abstract description 8
- 239000011324 bead Substances 0.000 claims description 72
- 238000002360 preparation method Methods 0.000 claims description 16
- 239000000853 adhesive Substances 0.000 claims description 10
- 230000001070 adhesive effect Effects 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 5
- 239000004677 Nylon Substances 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- 239000003822 epoxy resin Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 229920001778 nylon Polymers 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- 238000000280 densification Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000012360 testing method Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000004927 fusion Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000013081 microcrystal Substances 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000007926 Craterellus fallax Nutrition 0.000 description 1
- 240000007175 Datura inoxia Species 0.000 description 1
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910052805 deuterium Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002641 lithium Chemical group 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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- Powder Metallurgy (AREA)
Abstract
The invention provides a method for quickly manufacturing Li2TiO3 tritium breeding small balls. The method comprises the following steps that (1) Li2TiO3 powder and binder powder are mixed to form mixed powder; (2) a small ball three-dimensional model is established in a computer and is stored in the format of STL; (3) the mixed powder obtained in the step (1) is transferred into 3D printing equipment, the small ball three-dimensional model in the format of STL is introduced into a system of the 3D printing equipment; (4) technological parameters are set and the 3D printing equipment is started to obtain small ball entities; (5) the small ball entities are placed into a cold isostatic press to be compacted; (6) binder removal processing is conducted on the small ball entities; (7) the small ball entities are sintered in a sintering furnace. The Li2TiO3 small balls manufactured through the method are high in degree of sphericity, compactness and crushing strength, and large-scale and mechanical production of the Li2TiO3 tritium breeding small balls can be realized.
Description
Technical field
The present invention relates to 3D and print field, particularly a kind of 3D of utilization printing technique is prepared Li fast
2tiO
3the method of tritium propagation bead.
Background technology
Along with society and economic development, the demand of the energy is increased day by day.For the final energy problem that solves, people have turned to nucleosynthesis by sight.Fusion reaction is compared with fission reaction, and the radiation causing in reaction process is less, compares with sun power with wind energy, and its energy density is larger.Therefore, nucleosynthesis is undoubtedly optimal green high-efficient production capacity mode.Comprise in the world that seven countries of China and unit have jointly signed ITER and be designed for research and realize nucleosynthesis generating in November, 2006.The starting material of fusion reaction are two kinds of isotropic substance deuteriums and the tritiums of hydrogen, and deuterium can extract from seawater, and resource is compared with horn of plenty.Tritium be the high-energy neutron that produces by nucleosynthesis after suitable slowing down, bombardment tritium multiplication agent (
6li,
7li) constantly produce tritium gas, to realize controlling oneself of tritium.
Be rich in
6the lithium-based ceramic Li of Li
2tiO
3, there is higher lithium atom density, low reactivity, excellent chemical stability and good tritium release performance, be considered to one of solid tritium multiplication agent of tool future, receive domestic and international investigator's concern.Due to microspheroidal tritium multiplication agent, there is the features such as convenient filling, easy recovery, and there is larger specific surface area, good permeability, be conducive to diffusion and the release of tritium, therefore, prepare the emphasis that the uniform tritium propagation of high sphericity, high-compactness, size distribution bead becomes research.
Li
2tiO
3the preparation method of bead has multiple, is conventionally divided into mechanical process and wet method, and at present, studying more is wet processing.The primary process of wet method is by Li
2tiO
3powder and binding agent are mixed into ceramic size, then splash in solidifying agent by needle tubing, utilize the surface tension of drop to form bead, then obtain ceramic bead after binder removal sintering.Through continuous research with improve, adopt that wet method can obtain that footpath is little, any surface finish, bead that sphericity is higher.
But wet method is to operator and the requirement of needle tubing bore is high, bead balling ratio is not high, experimental repeatability is poor, bead size distribution is wide, is difficult to realize automatization, the production in enormous quantities of bead.Therefore, seek a kind of stable high Li that changes fast and automatically
2tiO
3ceramic bead preparation method has important scientific meaning and practical value.
Summary of the invention
The object of the present invention is to provide quick preparation Li
2tiO
3the method of tritium propagation bead, the Li of preparation
2tiO
3bead has high sphericity, high-compactness and high crushing strength, can realize Li
2tiO
3extensive, the mechanization production of tritium propagation bead.
A kind of quick preparation Li
2tiO
3the method of tritium propagation bead, comprises the following steps:
(1) by Li
2tiO
3powder and adhesive powder mixed preparing mixed powder, in mixed powder, the weight percentage of each composition is respectively: Li
2tiO
3powder 70～90wt%, adhesive powder 10～30wt%;
(2) in computer, set up bead three-dimensional model, the diameter of single bead three-dimensional model is 1～10mm, and the number of bead three-dimensional model is set as 1～1000, and saves as STL form;
(3) mixed powder in step (1) is transferred in 3D printing device, and the bead three-dimensional model of STL form is imported in the system of 3D printing device;
(4) set processing parameter and open 3D printing device, the processing parameter of 3D printing device is as follows: laser power 10～50W, and lasing beam diameter 100～300 μ m, sweep span 100～300 μ m, scanning speed 1000～3000mm/s, obtains bead entity;
(5) the bead entity of step (4) gained is put into cold isostatic press densification, the pressure applying to bead entity is 100～600MPa, and the dwell time is 20～60min;
(6) the bead entity of processing through step (5) is moved in resistance furnace and carries out binder removal processing, at 250～700 ℃ of temperature, be incubated 1～2h;
(7) the bead entity of processing through step (6) is carried out to sintering in sintering oven, sintering temperature is 600～1000 ℃, and soaking time is 1.5～3h.
As preferably, the material that described adhesive powder is selected is epoxy resin, stearic acid or nylon.
Technique effect of the present invention is embodied in:
The present invention is applied to Li by 3D printing technique
2tiO
3the preparation of bead.According to set up different models in computer, can one time to produce tens to thousands of beads, realized Li
2tiO
3efficient, controlled preparation.Whole preparation process is completed by 3D printing device, is conducive to Li
2tiO
3stable and the mass production of bead.The Li preparing by this method
2tiO
3the density of bead is higher, and size distribution is even, and crystal grain is tiny, and crystal grain and intergranule exist a fixed gap, be conducive to tritium gas by bead internal divergence to surface.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention;
Fig. 2 is 3D print procedure schematic diagram of the present invention;
Fig. 3 (a), (b) are respectively three-dimensional model diagram and the laser sintered procedure chart of embodiment 1;
Fig. 4 is the SEM figure of the sample of embodiment 1 preparation;
Fig. 5 is that the sample density of embodiment 2 preparations is with the Changing Pattern figure of sintering temperature;
Fig. 6 is the SEM figure of the sample of embodiment 2 preparations;
Fig. 7 is the SEM figure of the sample of embodiment 3 preparations.
Embodiment
Embodiment 1:
By the Li of 25g
2tiO
3the adhesive powder of powder and 2.78g evenly mixes (adhesive powder select material be epoxy resin, stearic acid or nylon), be laid on 3D printing device worktable, then by bead three-dimensional model (diameter 4mm, STL form) import in the system of 3D printing device, set equipment parameters (laser power: 20W, lasing beam diameter: 200 μ m, sweep span: 200 μ m, scanning speed: 2000mm/s), start successively scanning.The bead entity obtaining is transferred in cold isostatic press, and applying pressure is 300MPa, and pressurize 30min obtains comparatively fine and close bead entity.Then bead entity is moved in resistance furnace and carries out binder removal processing, after cooling, sintering in High Temperature Furnaces Heating Apparatus, sintering temperature is 850 ℃, soaking time is 2h, obtains Li
2tiO
3bead entity.
Fig. 2 is the process schematic diagram that 3D of the present invention prints bead entity, and 3D prints bead entity and completed by computer controlled automatic.
Fig. 3 (a), (b) are respectively three-dimensional model diagram and the laser sintered procedure chart of embodiment 1.As can be seen from Figure 3 the method for, printing by 3D can realize Li easily and fast
2tiO
3the preparation of bead.
The density of measuring bead entity prepared by this embodiment through Archimedes's drainage is 90%; The crushing strength of testing bead entity prepared by this example by universal testing machine is 36N.
Fig. 4 is the SEM photo of the bead entity prepared in embodiment.Therefrom can find out Li
2tiO
3bead size of microcrystal is little, be about 1 μ m, and hole is less, comparatively fine and close.
Embodiment 2:
By the Li of 25g
2tiO
3the adhesive powder of powder and 6.25g evenly mixes (adhesive powder select material be epoxy resin, stearic acid or nylon), be laid on 3D printing device worktable, then by bead three-dimensional model (diameter 4mm, STL form) import in system, set equipment parameters (laser power: 20W, lasing beam diameter: 200 μ m, sweep span: 200 μ m, scanning speed: 2000mm/s), start successively scanning.The bead entity obtaining is transferred in cold isostatic press, and applying pressure is 300MPa, and pressurize 30min obtains comparatively fine and close bead entity.Then bead entity is moved in resistance furnace and carries out binder removal processing, after cooling, sintering in High Temperature Furnaces Heating Apparatus, sintering temperature is 650～950 ℃, soaking time is 2h, obtains Li
2tiO
3bead entity.
Through Archimedes's drainage, measure in this embodiment, when sintering temperature is 850 ℃, the density of the bead entity of preparation is 83.3%; The crushing strength of testing bead entity prepared by this example by universal testing machine is 28N.
Fig. 5 prepares the density of bead entity with the Changing Pattern of sintering temperature in example, can find out, when sintering temperature is increased to 850 ℃ by 650 ℃, density obviously improves; Continue after rising sintering temperature to 950 ℃, the density of bead entity changes not obvious.So in this embodiment, the optimal sintering temperature of bead entity is 850 ℃.
Fig. 6 prepares the SEM photo of bead entity in this example, as can be seen from the figure, and Li
2tiO
3crystal grain is tiny evenly, and size of microcrystal is about 1 μ m left and right, and crystal grain and intergranule exist a fixed gap.
Embodiment 3:
By the Li of 25g
2tiO
3the epoxy powder of powder and 10.7g evenly mixes, be laid on 3D printing device worktable, then by bead three-dimensional model (diameter 4mm, STL form) import in system, set equipment parameters (laser power: 20W, lasing beam diameter: 200 μ m, sweep span: 200 μ m, scanning speed: 2000mm/s), start successively scanning.The bead entity obtaining is transferred in cold isostatic press, and applying pressure is 300MPa, and pressurize 30min obtains comparatively fine and close bead entity.Then bead entity is moved in resistance furnace and carries out binder removal processing, after cooling, sintering in High Temperature Furnaces Heating Apparatus, sintering temperature is 850 ℃, soaking time is 2h, obtains Li
2tiO
3bead entity.
The density of measuring bead entity prepared by this embodiment through Archimedes's drainage is 78.1%; The crushing strength of testing bead entity prepared by this example by universal testing machine is 17N.
Fig. 7 is the SEM photo of preparing bead entity in example, as can be seen from the figure, and the Li preparing under this embodiment
2tiO
3the space of bead entity is more, Li
2tiO
3crystal grain is tiny, and particle diameter is about 500nm, is a kind of typical porous nanocrystalline pottery.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (2)
1. prepare fast Li for one kind
2tiO
3the method of tritium propagation bead, is characterized in that: comprise the following steps:
(1) by Li
2tiO
3powder and adhesive powder mixed preparing mixed powder, in mixed powder, the weight percentage of each composition is respectively: Li
2tiO
3powder 70～90wt%, adhesive powder 10～30wt%;
(2) in computer, set up bead three-dimensional model, the diameter of single bead three-dimensional model is 1～10mm, and the number of bead three-dimensional model is set as 1～1000, and saves as STL form;
(3) mixed powder in step (1) is transferred in 3D printing device, and the bead three-dimensional model of STL form is imported in the system of 3D printing device;
(4) set processing parameter and open 3D printing device, the processing parameter of 3D printing device is as follows: laser power 10～50W, and lasing beam diameter 100～300 μ m, sweep span 100～300 μ m, scanning speed 1000～3000mm/s, obtains bead entity;
(5) the bead entity of step (4) gained is put into cold isostatic press densification, the pressure applying to bead entity is 100～600MPa, and the dwell time is 20～60min;
(6) the bead entity of processing through step (5) is moved in resistance furnace and carries out binder removal processing, at 250～700 ℃ of temperature, be incubated 1～2h;
(7) the bead entity of processing through step (6) is carried out to sintering in sintering oven, sintering temperature is 600～1000 ℃, and soaking time is 1.5～3h.
2. a kind of quick preparation Li according to claim 1
2tiO
3the method of tritium propagation bead, is characterized in that: the material that described adhesive powder is selected is epoxy resin, stearic acid or nylon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410369142.5A CN104140259B (en) | 2014-07-30 | 2014-07-30 | One prepares Li fast 2tiO 3the method of tritium propagation bead |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410369142.5A CN104140259B (en) | 2014-07-30 | 2014-07-30 | One prepares Li fast 2tiO 3the method of tritium propagation bead |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104140259A true CN104140259A (en) | 2014-11-12 |
| CN104140259B CN104140259B (en) | 2016-01-13 |
Family
ID=51849612
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410369142.5A Expired - Fee Related CN104140259B (en) | 2014-07-30 | 2014-07-30 | One prepares Li fast 2tiO 3the method of tritium propagation bead |
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|---|---|
| CN (1) | CN104140259B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104526838A (en) * | 2014-12-30 | 2015-04-22 | 宁波伏尔肯机械密封件制造有限公司 | Method for 3D ceramic printing forming |
| CN104609867A (en) * | 2015-02-15 | 2015-05-13 | 上海材料研究所 | Densifying method for selective laser sintered ceramic parts |
| CN105130402A (en) * | 2015-06-30 | 2015-12-09 | 成都新柯力化工科技有限公司 | Nanometer ceramic material used for 3D printing and 3D printing molding method thereof |
| JP2017127998A (en) * | 2016-01-18 | 2017-07-27 | 国立研究開発法人産業技術総合研究所 | Powder for molding |
| JP2017127999A (en) * | 2016-01-18 | 2017-07-27 | 国立研究開発法人産業技術総合研究所 | Method for manufacturing molded object |
| CN107140953A (en) * | 2017-04-18 | 2017-09-08 | 华中科技大学 | A kind of method that quick extrusion prepares ceramic microsphere |
| 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 |
| CN110148478A (en) * | 2019-06-10 | 2019-08-20 | 中国科学院合肥物质科学研究院 | A kind of fusion reactor solid-state water cooling covering production tritium multiplication agent-neutron multiplication agent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731111A (en) * | 2012-07-05 | 2012-10-17 | 北京科技大学 | Novel preparation method of ceramic microspheres |
| CN103817767A (en) * | 2014-03-14 | 2014-05-28 | 邓湘凌 | Method for manufacturing ceramic products with 3D printing technology |
-
2014
- 2014-07-30 CN CN201410369142.5A patent/CN104140259B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731111A (en) * | 2012-07-05 | 2012-10-17 | 北京科技大学 | Novel preparation method of ceramic microspheres |
| CN103817767A (en) * | 2014-03-14 | 2014-05-28 | 邓湘凌 | Method for manufacturing ceramic products with 3D printing technology |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104526838A (en) * | 2014-12-30 | 2015-04-22 | 宁波伏尔肯机械密封件制造有限公司 | Method for 3D ceramic printing forming |
| CN104526838B (en) * | 2014-12-30 | 2017-01-11 | 宁波伏尔肯陶瓷科技有限公司 | Method for 3D ceramic printing forming |
| CN104609867A (en) * | 2015-02-15 | 2015-05-13 | 上海材料研究所 | Densifying method for selective laser sintered ceramic parts |
| CN104609867B (en) * | 2015-02-15 | 2016-10-26 | 上海材料研究所 | A kind of method for densifying of selective laser sintering ceramic member |
| CN105130402A (en) * | 2015-06-30 | 2015-12-09 | 成都新柯力化工科技有限公司 | Nanometer ceramic material used for 3D printing and 3D printing molding method thereof |
| CN105130402B (en) * | 2015-06-30 | 2017-06-06 | 哈尔滨理工大学 | A kind of nano ceramic material and its 3D printing forming method for 3D printing |
| JP2017127998A (en) * | 2016-01-18 | 2017-07-27 | 国立研究開発法人産業技術総合研究所 | Powder for molding |
| JP2017127999A (en) * | 2016-01-18 | 2017-07-27 | 国立研究開発法人産業技術総合研究所 | Method for manufacturing molded object |
| CN107140953A (en) * | 2017-04-18 | 2017-09-08 | 华中科技大学 | A kind of method that quick extrusion prepares ceramic microsphere |
| CN107140953B (en) * | 2017-04-18 | 2019-11-22 | 华中科技大学 | A kind of method that quick extrusion prepares ceramic microsphere |
| 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 |
| CN110148478A (en) * | 2019-06-10 | 2019-08-20 | 中国科学院合肥物质科学研究院 | A kind of fusion reactor solid-state water cooling covering production tritium multiplication agent-neutron multiplication agent |
| CN110148478B (en) * | 2019-06-10 | 2021-01-01 | 中国科学院合肥物质科学研究院 | Fusion reactor solid-state water-cooled cladding tritium production breeder-neutron multiplier |
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| Publication number | Publication date |
|---|---|
| CN104140259B (en) | 2016-01-13 |
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