CN104593630B - Directional solidifying preparation method of lotus-shaped porous aluminum - Google Patents
Directional solidifying preparation method of lotus-shaped porous aluminum Download PDFInfo
- Publication number
- CN104593630B CN104593630B CN201510030049.6A CN201510030049A CN104593630B CN 104593630 B CN104593630 B CN 104593630B CN 201510030049 A CN201510030049 A CN 201510030049A CN 104593630 B CN104593630 B CN 104593630B
- Authority
- CN
- China
- Prior art keywords
- aluminum
- vacuum
- open
- porous aluminum
- crucible
- 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.)
- Expired - Fee Related
Links
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a directional solidifying preparation method of lotus-shaped porous aluminum. The directional solidifying preparation method comprises the following steps: adding electrolytic aluminum with the purity higher than 99.9% into a vacuum directional solidifying furnace, closing a furnace door, locking a furnace door safety lock, starting a vacuum pump, carrying out vacuumizing until the pressure is below 10＜-1＞Pa, switching on a circulating cooling water valve, and heating electrolytic aluminum to 680-750 DEG C until electrolytic aluminum is completely molten; shutting down a vacuum system, supplying hydrogen or mixed gas of hydrogen and argon until reaching a preset pressure, and after maintaining the temperature for a period of time, carrying out downward draw-casting, so as to prepare lotus-shaped porous aluminum. The porosity of openings of porous aluminum is 30%-70%, the average diameter of air holes is 0.2mm-1.0mm, and the air holes can be uniformly or directionally positioned. The lotus-shaped porous aluminum can be widely applied to the fields of aviation, aerospace, automobiles, information, buildings, military, nuclear energy and the like.
Description
Technical field
The invention belongs to non-ferrous metal metal technical field of new material preparation, especially relate to the directional solidifying method for preparing of a kind of Rhizoma Nelumbinis shape porous aluminum.
Background technology
In recent years, along with each field is to environment-protecting clean, the demand of the green material such as energy-efficient, new material, new technique constantly occur.Metal polyporous material is constantly expanded as the structural material of excellent performance and functional material, its application, from solid-
Liquid-
Between gas
High efficiency filter and be separated to surface combustion, fuel cell, pipe of energy-saving heat, from noise elimination, antidetonation to Superlight, metal polyporous material has become the new engineering material of a kind of excellent performance having function and structure double attribute concurrently, is widely used in the industry such as metallurgical machinery, petrochemical industry, energy environment protection, defence and military, nuclear technology and bio-pharmaceuticals.
At present, the preparation method of porous metals mainly has gas-blowing foaming method, solid blowing agent method, infiltration casting, solvent casting method, spray deposition, powder metallurgic method, slurry foaming, vapour deposition process and electrodeposition process.All there is pore size size and the shortcoming such as be difficult to control at distribution and all hook degree of metallic matrix Cao in gas-blowing foaming method and solid blowing agent method；Porous material prepared by infiltration casting and solvent casting method, its porosity can only be maintained in narrower range,
And its production cost is higher；Spray deposition and powder metallurgic method prepare porous material, and production cost is higher, it is difficult to form industrialization.
Metal-
Gas eutectic freezing method is Ukraine scientist Shapovalov
In 1993
Nian Qi application the U.S. and European patent in propose, afterwards the U.S. and Japan in succession carried out relevant metal/
The research of gas eutectic solidifying process.Porous material prepared by the method, structure is that cylindrical air holes rules orientation is arranged in metallic matrix, and this technique is considered as the important advance producing porous material, and its porosity, aperture are easily controlled, and technique is simple, and cost is relatively low.Compared with porous material prepared by traditional method, the porous material produced by this technique has that the density of material of identical material is low, specific modulus and the advantage such as specific strength height, medium and small, the good heat conductivity of stress collection.
Summary of the invention
It is an object of the invention to propose the directional solidifying method for preparing of a kind of preparation technology Rhizoma Nelumbinis simple, lower-cost shape porous aluminum, it utilize metal-
Porous aluminum material prepared by gas eutectic freezing method have rule oriented loose structure, porosity and aperture be easily controlled, tensile strength, compressive strength and the excellent advantage of heat conductivility.
The object of the present invention is achieved like this:
A kind of Rhizoma Nelumbinis shape porous
The directional solidifying method for preparing of aluminum, feature is: comprise the following steps:
(1
) it is 99.9% by purity
After above electrolytic aluminium cleaning remove impurity, 200
DEG C holding furnace toasts 2 ~ 4 h
Fully degasification, is placed with melting kettle and insulation crucible in vacuum oriented consolidation furnace, is put in vacuum oriented consolidation furnace by electrolytic aluminium subsequently, close the fire door of vacuum oriented consolidation furnace, lock fire door safety lock, open vacuum pump, be evacuated to 10-1Pa
Below；
(2
) open chiller and be passed through cooling circulating water, open the heating power supply of the induction coil of melting kettle outer layer heating, electrified regulation, electrolytic aluminium is heated to 680 ~ 750
DEG C, after the electrolytic aluminium in melting kettle all melts, close vacuum system, obtain aluminum liquid；
(3
) high pressure hydrogen or hydrogen are filled with in vacuum oriented consolidation furnace with argon gaseous mixture, pressure limit is 0.5 ~ 10.0MPa
, heat-insulation pressure keeping is 10 ~ 30
Minute；
(4
) graphite heater being incubated crucible outer layer is heated, it is ensured that the temperature in cast preincubation crucible is on aluminum liquid fusing point；
(5
) press control bar, aluminum liquid good for refine in melting kettle is poured in the insulation crucible of good heat insulation, after liquid level is completely steady, open the trailer system of vacuum oriented consolidation furnace, by the downward cast of draw bar, directional solidification speed is 1 ~ 10mm/min
, after the whole directional solidification of aluminum melt in insulation crucible, close power supply；
(6
) when the temperature being incubated in crucible is reduced to room temperature, open vent valve, lay down furnace gas, to open bell, take out sample, close circulating water cooling system, obtain Rhizoma Nelumbinis shape porous aluminum, the open porosity of porous aluminum is 30 ~ 70
%, pore average pore size are 0.2 ~ 1.0mm
, hole can realize being uniformly distributed or aligning.
The purity of described hydrogen and argon is 99.99%
。
Melting mode of heating is Frequency Induction Heating.
The invention have the advantages that
(1
) porous aluminum prepared has Lotus-type Structure, and porosity and aperture are easily controlled；
(2
) porous aluminum prepared has excellent tensile strength and compressive strength；
(3
) compared with the porous aluminum material using traditional method to prepare, the method technological operation is simple, production efficiency is high, and production cost is low.
This porous aluminum can be applicable to the heat radiations such as computer chip, high-power electronic device and photoelectric device, can be widely applied to the fields such as Aeronautics and Astronautics, automobile, information, building, military affairs and nuclear energy.
Accompanying drawing explanation
Fig. 1
It is the vacuum oriented consolidation furnace schematic diagram that uses of the present invention, 1.
Melting kettle；2.
Vacuum oriented consolidation furnace；3.
Aluminum liquid；4.
Pressure gauge；5.
Hydrogen；6.
Insulation crucible；7.
Chiller；8.
Porous metals；9.
Trailer system；10.
Draw bar.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.It should be noted that, the accompanying drawing of the present invention all uses the non-accurate ratio simplified very much, only in order to convenient, the distinct aid illustration present invention.
Embodiment 1
:
By 2kg
Purity is 99.9%
After above electrolytic aluminium cleaning remove impurity, 200
DEG C holding furnace toasts 2 ~ 4 h
Fully degasification, is placed with melting kettle and insulation crucible in vacuum oriented consolidation furnace, is put in vacuum oriented consolidation furnace by electrolytic aluminium subsequently, close the fire door of vacuum oriented consolidation furnace, lock fire door safety lock, open vacuum pump, be evacuated to 10-1Pa
Below；Open cooling circulating water, open the heating power supply of the induction coil of melting kettle outer layer heating, electrified regulation, electrolytic aluminium is heated to 680
DEG C, after the electrolytic aluminium in melting kettle all melts, close vacuum system, be filled with purity and be 99.99%
Hydrogen 0.5MPa
, heat-insulation pressure keeping 15
Minute；The graphite heater of insulation crucible outer layer is heated, it is ensured that the temperature in cast preincubation crucible is on aluminum liquid fusing point；Press control bar, pours in the insulation crucible of good heat insulation by aluminum liquid good for refine in melting kettle, after liquid level is completely steady, opens the trailer system of vacuum oriented consolidation furnace, and by the downward cast of draw bar, directional solidification speed is 1mm/min
, start directional solidification.After the whole directional solidification of aluminum melt in insulation crucible, close power supply.When temperature is reduced to room temperature in insulation crucible, opens vent valve, lay down furnace gas, open bell, close circulating water cooling system, take out sample, obtain Rhizoma Nelumbinis shape porous aluminum.
The open porosity of porous aluminum is 35.6
%, pore average pore size is 0.21mm
, hole can realize being uniformly distributed or aligning.
Embodiment 2
:
By 2kg
Purity is 99.9%
After above electrolytic aluminium cleaning remove impurity, 200
DEG C holding furnace toasts 2 ~ 4 h
Fully degasification, is placed with melting kettle and insulation crucible in vacuum oriented consolidation furnace, is put in vacuum oriented consolidation furnace by electrolytic aluminium subsequently, close the fire door of vacuum oriented consolidation furnace, lock fire door safety lock, open vacuum pump, be evacuated to 10-1Pa
Below；Open cooling circulating water, open the heating power supply of the induction coil of melting kettle outer layer heating, electrified regulation, electrolytic aluminium is heated to 700
DEG C, after the electrolytic aluminium in melting kettle all melts, close vacuum system, be filled with purity and be 99.99%
Hydrogen 1.0MPa
, heat-insulation pressure keeping 20
Minute；The graphite heater of insulation crucible outer layer is heated, it is ensured that the temperature in cast preincubation crucible is on aluminum liquid fusing point；Press control bar, pours in the insulation crucible of good heat insulation by aluminum liquid good for refine in melting kettle, after liquid level is completely steady, opens the trailer system of vacuum oriented consolidation furnace, and by the downward cast of draw bar, directional solidification speed is 5mm/min
, start directional solidification.After the whole directional solidification of aluminum melt in insulation crucible, close power supply.When temperature is reduced to room temperature in insulation crucible, opens vent valve, lay down furnace gas, open bell, close circulating water cooling system, take out sample, obtain Rhizoma Nelumbinis shape porous aluminum.
The open porosity of porous aluminum is 43.2
%, pore average pore size is 0.32mm
, hole can realize being uniformly distributed or aligning.
Embodiment 3
:
By 2kg
Purity is 99.9%
After above electrolytic aluminium cleaning remove impurity, 200
DEG C holding furnace toasts 2 ~ 4 h
Fully degasification, is placed with melting kettle and insulation crucible in vacuum oriented consolidation furnace, is put in vacuum oriented consolidation furnace by electrolytic aluminium subsequently, close the fire door of vacuum oriented consolidation furnace, lock fire door safety lock, open vacuum pump, be evacuated to 10-3Pa
Below；Open cooling circulating water, open the heating power supply of the induction coil of melting kettle outer layer heating, electrified regulation, electrolytic aluminium is heated to 720
DEG C, after the electrolytic aluminium in melting kettle all melts, close vacuum system, be filled with purity and be 99.99%
Hydrogen 5.0MPa
, heat-insulation pressure keeping 20
Minute；The graphite heater of insulation crucible outer layer is heated, it is ensured that the temperature in cast preincubation crucible is on aluminum liquid fusing point；Press control bar, pours in the insulation crucible of good heat insulation by aluminum liquid good for refine in melting kettle, after liquid level is completely steady, opens the trailer system of vacuum oriented consolidation furnace, and by the downward cast of draw bar, directional solidification speed is 7mm/min
, start directional solidification.After the whole directional solidification of aluminum melt in insulation crucible, close power supply.When temperature is reduced to room temperature in insulation crucible, opens vent valve, lay down furnace gas, open bell, close circulating water cooling system, take out sample, obtain Rhizoma Nelumbinis shape porous aluminum.
The open porosity of porous aluminum is 55.8
%, pore average pore size is 0.53mm
, hole can realize being uniformly distributed or aligning.
Embodiment 4
:
By 2kg
Purity is 99.9%
After above electrolytic aluminium cleaning remove impurity, 200
DEG C holding furnace toasts 2 ~ 4 h
Fully degasification, is placed with melting kettle and insulation crucible in vacuum oriented consolidation furnace, is put in vacuum oriented consolidation furnace by electrolytic aluminium subsequently, close the fire door of vacuum oriented consolidation furnace, lock fire door safety lock, open vacuum pump, be evacuated to 10-1Pa
Below；Open cooling circulating water, open the heating power supply of the induction coil of melting kettle outer layer heating, electrified regulation, electrolytic aluminium is heated to 750
DEG C, after the electrolytic aluminium in melting kettle all melts, close vacuum system, be filled with purity and be 99.99%
Hydrogen 0.5MPa
With argon 0.5MPa
, heat-insulation pressure keeping 20
Minute；The graphite heater of insulation crucible outer layer is heated, it is ensured that the temperature in cast preincubation crucible is on aluminum liquid fusing point；Press control bar, pours in the insulation crucible of good heat insulation by aluminum liquid good for refine in melting kettle, after liquid level is completely steady, opens the trailer system of vacuum oriented consolidation furnace, and by the downward cast of draw bar, directional solidification speed is 10mm/min
, start directional solidification.After the whole directional solidification of aluminum melt in insulation crucible, close power supply.When temperature is reduced to room temperature in insulation crucible, opens vent valve, lay down furnace gas, open bell, close circulating water cooling system, take out sample, obtain Rhizoma Nelumbinis shape porous aluminum.
The open porosity of porous aluminum is 62.4
%, pore average pore size is 0.68mm
。
Embodiment 5
:
By 2kg
Purity is 99.9%
After above electrolytic aluminium cleaning remove impurity, 200
DEG C holding furnace toasts 2 ~ 4 h
Fully degasification, is placed with melting kettle and insulation crucible in vacuum oriented consolidation furnace, is put in vacuum oriented consolidation furnace by electrolytic aluminium subsequently, close the fire door of vacuum oriented consolidation furnace, lock fire door safety lock, open vacuum pump, be evacuated to 10-1Pa
Below；Open cooling circulating water, open the heating power supply of the induction coil of melting kettle outer layer heating, electrified regulation, electrolytic aluminium is heated to 720
DEG C, after the electrolytic aluminium in melting kettle all melts, close vacuum system, be filled with purity and be 99.99%
Hydrogen 1MPa
With argon 0.5MPa
, heat-insulation pressure keeping 20
Minute；The graphite heater of insulation crucible outer layer is heated, it is ensured that the temperature in cast preincubation crucible is on aluminum liquid fusing point；Press control bar, pours in the insulation crucible of good heat insulation by aluminum liquid good for refine in melting kettle, after liquid level is completely steady, opens the trailer system of vacuum oriented consolidation furnace, and by the downward cast of draw bar, directional solidification speed is 5mm/min
, start directional solidification.After the whole directional solidification of aluminum melt in insulation crucible, close power supply.When temperature is reduced to room temperature in insulation crucible, opens vent valve, lay down furnace gas, open bell, close circulating water cooling system, take out sample, obtain Rhizoma Nelumbinis shape porous aluminum.
The open porosity of porous aluminum is 68.5
%, pore average pore size is 0.84mm
。
Claims (2)
1. the directional solidifying method for preparing of a Rhizoma Nelumbinis shape porous aluminum, it is characterised in that: described preparation method comprises the following steps:
(1) after the electrolytic aluminium that purity is more than 99.9% being cleared up remove impurity, 2 ~ 4 abundant degasification of h are toasted in 200 DEG C of holding furnaces, melting kettle and insulation crucible it is placed with in vacuum oriented consolidation furnace, subsequently electrolytic aluminium is put in vacuum oriented consolidation furnace, close the fire door of vacuum oriented consolidation furnace, locking fire door safety lock, opens vacuum pump, is evacuated to below 10-1Pa；
(2) open chiller and be passed through cooling circulating water, open the heating power supply of the induction coil of melting kettle outer layer heating, electrified regulation, electrolytic aluminium is heated to 680 ~ 750 DEG C, after the electrolytic aluminium in melting kettle all melts, close vacuum system, obtain aluminum liquid；
(3) high pressure hydrogen or hydrogen being filled with in vacuum oriented consolidation furnace with argon gaseous mixture, pressure limit is 0.5 ~ 10.0MPa, and heat-insulation pressure keeping is 10 ~ 30 minutes；
(4) graphite heater of insulation crucible outer layer is heated, it is ensured that the temperature in cast preincubation crucible is on aluminum liquid fusing point；
(5) press control bar, aluminum liquid good for refine in melting kettle is poured in the insulation crucible of good heat insulation, after liquid level is completely steady, open the trailer system of vacuum oriented consolidation furnace, by the downward cast of draw bar, directional solidification speed is 1 ~ 10mm/min, after the whole directional solidification of aluminum melt in insulation crucible, closes power supply；
(6) when the temperature being incubated in crucible is reduced to room temperature, open vent valve, lay down furnace gas, open bell, take out sample, close circulating water cooling system, obtain Rhizoma Nelumbinis shape porous aluminum, the open porosity of porous aluminum is 30 ~ 70%, pore average pore size is 0.2 ~ 1.0mm, and hole can realize being uniformly distributed or aligning.
The directional solidifying method for preparing of Rhizoma Nelumbinis shape porous aluminum the most according to claim 1, it is characterised in that: the purity of described hydrogen and argon is 99.99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510030049.6A CN104593630B (en) | 2015-01-22 | 2015-01-22 | Directional solidifying preparation method of lotus-shaped porous aluminum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510030049.6A CN104593630B (en) | 2015-01-22 | 2015-01-22 | Directional solidifying preparation method of lotus-shaped porous aluminum |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104593630A CN104593630A (en) | 2015-05-06 |
| CN104593630B true CN104593630B (en) | 2017-01-11 |
Family
ID=53119680
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510030049.6A Expired - Fee Related CN104593630B (en) | 2015-01-22 | 2015-01-22 | Directional solidifying preparation method of lotus-shaped porous aluminum |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104593630B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105039770B (en) * | 2015-06-30 | 2017-03-29 | 西安理工大学 | A kind of method that utilization directional solidification technique prepares porous metal material |
| FR3063921B1 (en) | 2017-03-16 | 2022-07-29 | Office National Detudes Et De Rech Aerospatiales Onera | SINTERED METALLIC MATERIAL WITH ORIENTATED POROSITY COMPRISING AT LEAST ONE FERROMAGNETIC PART AND METHOD OF MANUFACTURING |
| CN107876714B (en) * | 2017-10-25 | 2019-04-30 | 刘宗蒲 | A kind of preparation method of high efficiency and heat radiation metal material |
| CN109028949B (en) * | 2018-08-13 | 2019-12-03 | 岳阳联创热能设备有限公司 | A kind of dedicated smelting furnace |
| CN116024444B (en) * | 2022-12-28 | 2024-04-26 | 付亚波 | High-strength high-conductivity high-elasticity titanium bronze alloy, preparation method thereof and vacuum melting solidification device |
| CN116397156A (en) * | 2023-04-12 | 2023-07-07 | 昆明理工大学 | Preparation method of secondary composite porous steel-based material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5181549A (en) * | 1991-04-29 | 1993-01-26 | Dmk Tek, Inc. | Method for manufacturing porous articles |
| CN101173332A (en) * | 2007-11-21 | 2008-05-07 | 大连华乌科技转化有限公司 | Method for producing polyporous material based on solid/gas eutectic directional solidification |
| CN103240405A (en) * | 2013-05-13 | 2013-08-14 | 北京科技大学 | In-situ reaction precipitation manufacture device and process of lotus-root-shaped porous metal material |
-
2015
- 2015-01-22 CN CN201510030049.6A patent/CN104593630B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5181549A (en) * | 1991-04-29 | 1993-01-26 | Dmk Tek, Inc. | Method for manufacturing porous articles |
| CN101173332A (en) * | 2007-11-21 | 2008-05-07 | 大连华乌科技转化有限公司 | Method for producing polyporous material based on solid/gas eutectic directional solidification |
| CN103240405A (en) * | 2013-05-13 | 2013-08-14 | 北京科技大学 | In-situ reaction precipitation manufacture device and process of lotus-root-shaped porous metal material |
Non-Patent Citations (1)
| Title |
|---|
| "Al-H系定向凝固制备多孔Al";张华伟;《金属学报》;20070131;第43卷(第1期);第11页-12页、表1 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104593630A (en) | 2015-05-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104593630B (en) | Directional solidifying preparation method of lotus-shaped porous aluminum | |
| CN108486400B (en) | Metal-based hollow sphere composite foam material and preparation method thereof | |
| CN103895285B (en) | High strength stratiform Al based ceramic metal composite and preparation method thereof | |
| CN103922746B (en) | Methods for preparing compact silicon nitride ceramic material and compact special-shaped silicon nitride ceramic material by virtue of aqueous tape casting | |
| CN103252448B (en) | A kind of thin-wall high-strength mold shell preparation method manufactured for single crystal blade | |
| CN102226296B (en) | Efficient directional solidification impurity-removing technology by utilizing polycrystalline silicon ingot production furnace | |
| CN103695815B (en) | Device and method for separate preheating and one-step infiltration extrusion forming of magnesium-based composite | |
| CN104046877B (en) | Orienting stephanoporate SiC-Cu matrix material used for electronic packaging and preparation method | |
| CN105903969B (en) | A kind of porous copper material and preparation method thereof with oriented laminated hole | |
| CN104744047A (en) | Method for preparing silicon nitride crucible through reactive sintering | |
| CN105039770A (en) | Method for utilizing directional solidification technique to prepare porous metal materials | |
| CN102808090A (en) | Device and method for preparing ultrahigh-purity metal magnesium from industrial pure magnesium | |
| CN103924293B (en) | A kind of bottom strengthens refrigerating unit and method of cooling thereof | |
| CN103182509A (en) | Preparation method of porous capillary core for loop heat pipe | |
| CN105057668A (en) | Sintering method of stainless steel fibre felt | |
| CN100584974C (en) | Prepare the method for porous material based on solid/solid/gas eutectic directional solidification | |
| CN103240405B (en) | In-situ reaction precipitation manufacture device and process of lotus-root-shaped porous metal material | |
| CN104403694A (en) | Liquid-state continuous slag discharge device and slag discharge method of fixed bed gasification furnace | |
| CN112899513A (en) | Foamed aluminum with open-close hole coexisting structure and preparation method thereof | |
| CN203065635U (en) | Bottom enhanced cooling device | |
| CN203200177U (en) | Narrow inductive coupling CVD (Chemical Vapor Deposition) densifying tool for preparing crucible made of carbon/carbon composite material and chemical vapor deposition furnace | |
| CN106007519A (en) | Preparation method of compound carbon fiber heat-insulation material | |
| CN104988342A (en) | Zirconium alloy melting and casting method | |
| CN106222500B (en) | A kind of aluminum matrix composite and preparation method | |
| CN103436753B (en) | The alterant of silumin alloy melt and utilize the silumin preparation method of this alterant |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170111 Termination date: 20220122 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |