CN104140259B - One prepares Li fast 2tiO 3the method of tritium propagation bead - Google Patents
One prepares Li fast 2tiO 3the method of tritium propagation bead Download PDFInfo
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- CN104140259B CN104140259B CN201410369142.5A CN201410369142A CN104140259B CN 104140259 B CN104140259 B CN 104140259B CN 201410369142 A CN201410369142 A CN 201410369142A CN 104140259 B CN104140259 B CN 104140259B
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- bead
- entity
- tio
- powder
- printing device
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- 239000011324 bead Substances 0.000 title claims abstract description 82
- 238000000034 method Methods 0.000 title claims abstract description 29
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 title claims abstract description 21
- 229910052722 tritium Inorganic materials 0.000 title claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000010146 3D printing Methods 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 15
- 239000000853 adhesive Substances 0.000 claims abstract description 11
- 230000001070 adhesive effect Effects 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 9
- 239000011230 binding agent Substances 0.000 claims abstract description 8
- 239000011812 mixed powder Substances 0.000 claims abstract description 8
- 238000012545 processing Methods 0.000 claims abstract description 6
- 238000000280 densification Methods 0.000 claims abstract description 3
- 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
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 description 8
- 239000013078 crystal Substances 0.000 description 6
- 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
- 238000010586 diagram 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
- 238000002156 mixing Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000013081 microcrystal Substances 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
- 230000015572 biosynthetic process Effects 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
- 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
- 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
- 239000013535 sea water Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- Powder Metallurgy (AREA)
Abstract
The invention provides one and prepare Li fast
2tiO
3the method of tritium propagation bead, comprises the following steps: (1) is by Li
2tiO
3powder and adhesive powder are mixed to form mixed powder; (2) set up bead three-dimensional model in a computer, and save 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, obtaining bead entity; (5) bead entity is put into cold isostatic press densification; (6) bead entity is carried out binder removal process; (7) bead entity is sintered in sintering oven.Li prepared by the present invention
2tiO
3bead has high sphericity, high-compactness, high crushing strength, and can realize Li
2tiO
3extensive, the mechanization production of tritium propagation bead.
Description
Technical field
The present invention relates to 3D printing field, particularly one utilizes 3D printing technique to prepare 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.In order to finally solve energy problem, sight has been turned to nucleosynthesis by people.Fusion reaction is compared with fission reaction, and the radiation caused in reaction process is less, compares with sun power with wind energy, and its energy density is larger.Therefore, nucleosynthesis optimal green high-efficient production capacity mode beyond doubt.Comprise in the world in November, 2006 China seven countries and unit jointly signed ITER be designed for research and realize nucleosynthesis generating.The starting material of fusion reaction are two kinds of isotropic substance deuteriums and the tritium of hydrogen, and deuterium can extract from seawater, and resource is horn of plenty comparatively.Tritium be then the high-energy neutron that produced by nucleosynthesis after suitable slowing down, bombardment tritium multiplication agent (
6li,
7li) constantly tritium gas is produced, to realize controlling oneself of tritium.
Be rich in
6the lithium-based ceramic Li of Li
2tiO
3, have higher lithium atom density, low reactivity, excellent chemical stability and good tritium release performance, one of solid tritium multiplication agent being considered to most future, receives the concern of domestic and international investigator.There is due to microspheroidal tritium multiplication agent the features such as convenient filling, easily recovery, and there is larger specific surface area, good permeability, be conducive to diffusion and the release of tritium, therefore, prepare high sphericity, high-compactness, even particle size distribution tritium propagation bead become the emphasis of research.
Li
2tiO
3the preparation method of bead has multiple, is usually 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 are added dropwise in solidifying agent by needle tubing, utilize the surface tension of drop to form bead, then obtain ceramic bead after binder removal sintering.Through constantly research and improvement, adopt wet method can obtain the bead that footpath is little, any surface finish, sphericity are 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 the automatization, the production in enormous quantities that realize bead.Therefore, seek a kind of stablizing and change high Li 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 and prepare Li fast
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.
One prepares Li fast
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) set up bead three-dimensional model in a computer, 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, lasing beam diameter 100 ~ 300 μm, sweep span 100 ~ 300 μm, 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 applied to bead entity is 100 ~ 600MPa, and the dwell time is 20 ~ 60min;
(6) carry out binder removal process by the bead entity processed through step (5) immigration resistance furnace, at 250 ~ 700 DEG C of temperature, be incubated 1 ~ 2h;
(7) sintered in sintering oven by the bead entity processed through step (6), sintering temperature is 600 ~ 1000 DEG C, 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:
3D printing technique is applied to Li by the present invention
2tiO
3the preparation of bead.According to setting up different models in computer, can one time to produce tens to thousands of beads, achieve Li
2tiO
3efficient, controlled synthesis.Whole preparation process is completed by 3D printing device, is conducive to Li
2tiO
3stable and the mass production of bead.By Li prepared by this method
2tiO
3the density of bead is higher, even particle size distribution, and crystal grain is tiny, and there is a fixed gap between crystal grain and crystal grain, is conducive to tritium gas by bead internal divergence to surface.
Accompanying drawing explanation
Fig. 1 is present invention process schematic flow sheet;
Fig. 2 is 3D print procedure schematic diagram of the present invention;
Fig. 3 (a), (b) are respectively the three-dimensional model diagram of embodiment 1 and laser sintered procedure chart;
Fig. 4 is the SEM figure of sample prepared by embodiment 1;
Fig. 5 is the Changing Pattern figure of sample density with sintering temperature of embodiment 2 preparation;
Fig. 6 is the SEM figure of sample prepared by embodiment 2;
Fig. 7 is the SEM figure of sample prepared by embodiment 3.
Embodiment
Embodiment 1:
By the Li of 25g
2tiO
3the adhesive powder Homogeneous phase mixing of powder and 2.78g (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 μm, sweep span: 200 μm, scanning speed: 2000mm/s), start successively to scan.Transfer in cold isostatic press by the bead entity obtained, applying pressure is 300MPa, pressurize 30min, obtains comparatively fine and close bead entity.Then moved in resistance furnace by bead entity and carry out binder removal process, after cooling, sinter in High Temperature Furnaces Heating Apparatus, sintering temperature is 850 DEG C, and soaking time is 2h, obtains Li
2tiO
3bead entity.
Fig. 2 is the process schematic 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 the three-dimensional model diagram of embodiment 1 and laser sintered procedure chart.As can be seen from Figure 3, the method printed by 3D can realize Li easily and fast
2tiO
3the preparation of bead.
The density measuring bead entity prepared by this embodiment through Archimedes's drainage is 90%; The crushing strength being tested 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 μm, and hole is less, comparatively fine and close.
Embodiment 2:
By the Li of 25g
2tiO
3the adhesive powder Homogeneous phase mixing of powder and 6.25g (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 μm, sweep span: 200 μm, scanning speed: 2000mm/s), start successively to scan.Transfer in cold isostatic press by the bead entity obtained, applying pressure is 300MPa, pressurize 30min, obtains comparatively fine and close bead entity.Then moved in resistance furnace by bead entity and carry out binder removal process, after cooling, sinter in High Temperature Furnaces Heating Apparatus, sintering temperature is 650 ~ 950 DEG C, and soaking time is 2h, obtains Li
2tiO
3bead entity.
Measure in this embodiment through Archimedes's drainage, when sintering temperature is 850 DEG C, the density of the bead entity of preparation is 83.3%; The crushing strength being tested bead entity prepared by this example by universal testing machine is 28N.
Fig. 5 is the Changing Pattern of density with sintering temperature preparing bead entity in example, can find out, when sintering temperature is increased to 850 DEG C by 650 DEG C, density significantly improves; After continuing to raise sintering temperature to 950 DEG C, the density change of bead entity is not obvious.So in this embodiment, the optimal sintering temperature of bead entity is 850 DEG C.
Fig. 6 is the SEM photo preparing bead entity in this example, as can be seen from the figure, and Li
2tiO
3uniform small grains, size of microcrystal is about about 1 μm, there is a fixed gap between crystal grain and crystal grain.
Embodiment 3:
By the Li of 25g
2tiO
3the epoxy powder Homogeneous phase mixing of powder and 10.7g, 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 μm, sweep span: 200 μm, scanning speed: 2000mm/s), start successively to scan.Transfer in cold isostatic press by the bead entity obtained, applying pressure is 300MPa, pressurize 30min, obtains comparatively fine and close bead entity.Then moved in resistance furnace by bead entity and carry out binder removal process, after cooling, sinter in High Temperature Furnaces Heating Apparatus, sintering temperature is 850 DEG C, and soaking time is 2h, obtains Li
2tiO
3bead entity.
The density measuring bead entity prepared by this embodiment through Archimedes's drainage is 78.1%; The crushing strength being tested bead entity prepared by this example by universal testing machine is 17N.
Fig. 7 is the SEM photo preparing bead entity in example, as can be seen from the figure, and the Li prepared 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 amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. prepare Li fast 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) set up bead three-dimensional model in a computer, 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, lasing beam diameter 100 ~ 300 μm, sweep span 100 ~ 300 μm, 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 applied to bead entity is 100 ~ 600MPa, and the dwell time is 20 ~ 60min;
(6) carry out binder removal process by the bead entity processed through step (5) immigration resistance furnace, at 250 ~ 700 DEG C of temperature, be incubated 1 ~ 2h;
(7) sintered in sintering oven by the bead entity processed through step (6), sintering temperature is 600 ~ 1000 DEG C, and soaking time is 1.5 ~ 3h.
2. one according to claim 1 prepares Li fast
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.
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|---|---|---|---|
| CN201410369142.5A CN104140259B (en) | 2014-07-30 | 2014-07-30 | One prepares Li fast 2tiO 3the method of tritium propagation bead |
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| 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 |
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|---|---|
| CN104140259A CN104140259A (en) | 2014-11-12 |
| CN104140259B true CN104140259B (en) | 2016-01-13 |
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|---|---|---|---|
| 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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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| 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 |
| JP6664650B2 (en) * | 2016-01-18 | 2020-03-13 | 国立研究開発法人産業技術総合研究所 | Manufacturing method of molded object |
| JP6699824B2 (en) * | 2016-01-18 | 2020-05-27 | 国立研究開発法人産業技術総合研究所 | Modeling powder |
| CN107140953B (en) * | 2017-04-18 | 2019-11-22 | 华中科技大学 | A kind of method that quick extrusion prepares ceramic microsphere |
| 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 |
| 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 |
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 |
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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 |
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