CN106637214A - Method for improving intrinsic melting point by using negative curvature of surface - Google Patents
Method for improving intrinsic melting point by using negative curvature of surface Download PDFInfo
- Publication number
- CN106637214A CN106637214A CN201611247064.7A CN201611247064A CN106637214A CN 106637214 A CN106637214 A CN 106637214A CN 201611247064 A CN201611247064 A CN 201611247064A CN 106637214 A CN106637214 A CN 106637214A
- Authority
- CN
- China
- Prior art keywords
- fusing point
- melting point
- intrinsic
- negative
- solid material
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/44—Compositions for etching metallic material from a metallic material substrate of different composition
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/24—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The invention discloses a method for improving an intrinsic melting point by using negative curvature of a surface. An area of which one of principal curvatures is negative and the absolute value of the curvature is smaller than 1 micron is firstly prepared on the outer surface or the inner surface of a metal, or a metal oxide, or a polymer or a high polymer material through dealloying, etching, partial component evaporation, chemical vapor reaction, an electrochemical method and a hydrothermal method; the ratio of the superficial area of the negative curvature in the total superficial area is not smaller than 80%; and then the obtained material with the negative curvature on the surface is heated to a conventional melting point of the material, and the unmelted part is the final product. The intrinsic melting point of the obtained product is higher than the conventional melting point of the subordinate material. The method is simple, high in repeatability and high in universality and novel idea and strategy are provided for expanding high-temperature application of the material.
Description
Technical field
The present invention is that, with regard to lifting material melts melting point method, more particularly to one kind lifts material using surface negative cruvature
The method of intrinsic fusing point.
Background technology
Fusing refers to phase in version of the material by solid-state to liquid, is a kind of common phenomenon in nature, is also that material exists
The phenomenon that must take into when being used in human society, the productive life for being also widely used for human society.So far, remove
By adding doped chemical in material or changing the external environment condition that material is located --- for example embed or be mounted to Gao Rong
In point matrix, apply the methods such as pressure, moment impact, laser irradiation to be lifted outside material melts temperature, only minority oxide
The intrinsic fusing point of itself can be obtained because the viscosity of its melt is high or its oxide-containing chemical key is extremely strong to rise, other materials
The intrinsic fusing point rise phenomenon of itself is undiscovered.Also, human society has been accepted as reduction with size, material itself
Intrinsic fusing point can be reduced.
For a long time, human society needs to use solid matter in hot environment, such as in Aero-Space engine
Need to use high temperature alloy, heat-insulated ceramic material etc., need to use resistant to elevated temperatures catalyst of energy etc. in chemical industry, such as
It is such.Therefore, the mankind are earnestly seeking the resistant to elevated temperatures solid matter of energy always.If the mankind can lift existing material itself
Intrinsic fusing point, that will significantly lift the industrial development of human society.Based on this, a kind of surface negative cruvature of development lifts thing
The method of the intrinsic fusing point of matter, is the core concept of present patent application.
The content of the invention
The purpose of the present invention, is to solve the mankind earnestly to seek resistant to elevated temperatures solid matter material always, there is provided one kind is not
Need to adulterate extraneous element, vary without external environment condition, the method that the intrinsic fusing point of material is lifted using surface negative cruvature.
The present invention is achieved by following technical solution：
The present invention is using the method for de- alloy, etching, fractions evaporation or chemical gas phase reaction in solid appearing surface
Or prepare on inner surface one of principal curvatures to bear, the curvature absolute value is less than 1 micron of region, the surface area institute of the negative cruvature
The ratio for accounting for total surface area is not less than 80%.The material can be metal, metal oxide, polymer or macromolecule.The mistake
Journey can be de- alloy, etching, fractions evaporation, chemical gas phase reaction.Then possess being somebody's turn to do for surface negative cruvature by what is obtained
Block material is heated to the conventional melting point of the material, and remaining part is final product.The intrinsic fusing point of the product is higher than its affiliated thing
The conventional melting point of matter.
Fusing point is typically referred to, and at one atm, the form of block material is by the temperature that Solid State Transformation is liquid.Such as
The fusing point of gold, typically refers to 1064 DEG C, and we are referred to as conventional melting point this fusing point.With surface negative cruvature form material
Fusing point has exceeded the fusing point of block, and this is to realize lifting fusing point phenomenon truly for the first time.In order to avoid with
Conventional melting point is obscured, we term it intrinsic fusing point.
The method that a kind of use surface negative cruvature lifts the intrinsic fusing point of material, with following steps：
(1) one block of solid material with fusing point is taken, it is anti-using de- alloy, etching, fractions evaporation, chemical gaseous phase
Answer, electrochemical method and hydro-thermal method prepare one of principal curvatures for negative, the curvature absolute value on its outer surface or inner surface
Region less than 1 micron, and the surface area of negative cruvature accounts for the ratio of the total surface area of the solid material and is not less than 80%；
(2) solid material obtained in step (1) is heated to the conventional melting point of the solid material, unfused part is eventually
Product.The intrinsic fusing point (its outer surface or inner surface have fusing point during negative cruvature) of the end-product is normal higher than its affiliated material
Rule fusing point.
The solid material with fusing point of the step (1) is metal, metal oxide, polymer or macromolecule material
Material.
The preparation process is simple of the present invention, repeatable strong, universality are high, and the intrinsic fusing point of handled rear material can be higher than
Its original conventional melting point, has expanded application of the material in hot environment.
Description of the drawings
Fig. 1 is the nano-porous gold structure that scanning transmission electron microscope (STEM) three-dimensionalreconstruction of embodiment 1 goes out；
Fig. 2 be the nano-porous gold structure that scanning transmission electron microscope (STEM) three-dimensionalreconstruction of embodiment 1 goes out hole wall in it is double
The distribution map of curved surface (bright grey), concave surface (light gray) and convex surface (Dark grey)；
Fig. 3 be embodiment 1 in room temperature, 1064 DEG C (golden conventional melting point) be incubated 10 minutes, 1151 DEG C insulation 10 minutes after
The transmission electron microscope bright field image of the nano-porous gold of shooting and its electron diffraction pattern；
Fig. 4 is the scanning electron microscopic picture of the nano-porous silver structure of embodiment 2；
Fig. 5 is the transmission electron microscope picture of the nano-porous silver structure of embodiment 2.
Specific embodiment
The present invention is further illustrated by specific examples below.What embodiment was merely exemplary, and it is non-limiting
's.
Embodiment 1
Original material species is electrum.
(1) method for corroding electrum by nitric acid sloughs the silver element (de- alloy approach) in alloy, obtains nanometer
Porous gold (Fig. 1).The surface of this cellular structure includes convex surface, three kinds of configurations of surface (Fig. 2) of concave surface and hyperboloid, its composition
Ratio successively 75%, 8%, 17%.Two principal curvatures of wherein convex surface are positive camber, and concave surface is negative cruvature, hyperboloid
Then for one positive one negative.Hyperboloid and concave surface are the surface comprising negative cruvature, and curvature absolute value is about 0.05nm-1, its ratio
Sum is 83%, meets the condition for lifting the intrinsic fusing point of material.
(2) nano-porous gold to preparing in (1) is heated.When temperature rise to 1064 DEG C of the conventional melting point of gold with
And when 1151 DEG C (Fig. 3), the nano-porous gold for still having subregion maintains porous form, while the sharp keen spot in electron diffraction pattern
Point shows that its crystal habit is maintained, it was demonstrated that the intrinsic fusing point in this region has been enhanced at least 87 DEG C.
Fig. 1 is the nano-porous gold structure that scanning transmission electron microscope (STEM) three-dimensionalreconstruction of embodiment 1 goes out.
Fig. 2 be the nano-porous gold structure that scanning transmission electron microscope (STEM) three-dimensionalreconstruction of embodiment 1 goes out hole wall in it is double
The distribution map of curved surface (bright grey), concave surface (light gray) and convex surface (Dark grey).
Fig. 3 A are the transmission electron microscope pictures and its electron diffraction pattern of the nano-porous gold that embodiment 1 shoots in room temperature.By
It can be seen that this structure original state is crystal in figure.
Fig. 3 B are the transmission electron microscopes of the nano-porous gold that embodiment 1 shoots after the insulation 10 minutes of 1064 DEG C of golden conventional melting point
Picture and its electron diffraction pattern.As can be seen from Figure this structure still keeps crystal state.
Fig. 3 C are transmission electron microscope picture and its electricity of the embodiment 1 in 1151 DEG C of nano-porous golds shot after being incubated 10 minutes
Sub- diffraction spectra.As can be seen from Figure this structure still keeps crystal state, it was demonstrated that its intrinsic fusing point has been enhanced at least 87 DEG C.
Embodiment 2
Original material species is aerdentalloy.
The method (de- alloy approach) of the aluminium element in aerdentalloy is sloughed by hcl corrosion, nano-porous silver is obtained
(Fig. 3 and Fig. 4).The surface curvature distribution of the material meets the condition for lifting the intrinsic fusing point of material.It is warming up to the conventional melting point of silver
962 DEG C, still there is part nano-porous silver unfused, it was demonstrated that the intrinsic fusing point of this part nano-porous silver melts higher than the routine of silver
Point.
Fig. 4 is the scanning electron microscopic picture of the nano-porous silver structure of embodiment 2.As can be seen from Figure this structure has big face
Product negative cruvature is present.
Fig. 5 is the transmission electron microscope picture of the nano-porous silver structure of embodiment 2.As can be seen from Figure this structure has big face
Product negative cruvature is present.
Embodiment 3
Original material species is carborundum.
At a high temperature of 1000 DEG C, with chlorine or ratio 2 are more than：1 chlorine-hydrogen gas mixture processes carborundum table
Face can slough surface element silicon, obtain porous diamond lattic structure crystal carbon.The surface curvature distribution of the material meets lifting material
The condition of intrinsic fusing point.
Embodiment 4
Original material species is calcium chloride fused salt.
Electrochemically obtain nanoporous titanium directly by the titanium oxide reduction of microballoon form in calcium chloride fused salt.
The surface curvature distribution of the material meets the condition for lifting the intrinsic fusing point of material.
Embodiment 5
Material category is nanoporous cerium oxide.
Nanoporous cerium oxide nano-rod is prepared with hydro-thermal method, the pass surface comprising a large amount of negative cruvature surfaces is obtained.Should
The surface curvature distribution of material meets the condition for lifting the intrinsic fusing point of material.
Some embodiments of the present invention described in detail above, but, the present invention is not limited in above-mentioned embodiment
Detail, the present invention range of the technology design in, various simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy is no longer separately illustrated.
Additionally, can also be combined between a variety of embodiments of the present invention, as long as it is without prejudice to this
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (2)
1. the method that a kind of use surface negative cruvature lifts the intrinsic fusing point of material, with following steps：
(1) one block of solid material with fusing point is taken, using de- alloy, etching, fractions evaporation, chemical gas phase reaction, electricity
Chemical method and hydro-thermal method prepare one of principal curvatures on its outer surface or inner surface and are less than 1 for negative, the curvature absolute value
The region of micron, and the surface area of negative cruvature accounts for the ratio of the total surface area of the solid material and is not less than 80%.
(2) solid material obtained in step (1) is heated to the conventional melting point of the solid material, unfused part is whole product
Thing；Conventional melting point of the intrinsic fusing point of the end-product higher than its affiliated material.
2. the method that a kind of use surface negative cruvature according to claim 1 lifts the intrinsic fusing point of material, it is characterised in that institute
The solid material with fusing point for stating step (1) is metal, metal oxide, polymer or macromolecular material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611247064.7A CN106637214B (en) | 2016-12-29 | 2016-12-29 | A method of the intrinsic fusing point of substance is promoted with surface negative cruvature |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611247064.7A CN106637214B (en) | 2016-12-29 | 2016-12-29 | A method of the intrinsic fusing point of substance is promoted with surface negative cruvature |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106637214A true CN106637214A (en) | 2017-05-10 |
| CN106637214B CN106637214B (en) | 2019-04-16 |
Family
ID=58836843
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611247064.7A Expired - Fee Related CN106637214B (en) | 2016-12-29 | 2016-12-29 | A method of the intrinsic fusing point of substance is promoted with surface negative cruvature |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106637214B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107475544A (en) * | 2017-08-29 | 2017-12-15 | 天津理工大学 | A kind of method that glassy metal is prepared under the condition of high temperature |
| CN111254308A (en) * | 2020-01-21 | 2020-06-09 | 天津理工大学 | Method for improving high-temperature stability of metal twin crystal |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004059428A (en) * | 2002-07-29 | 2004-02-26 | Samsung Sdi Co Ltd | Carbon nanotube for fuel cell, method of manufacturing the same and fuel cell using the same |
| CN103803644A (en) * | 2012-11-14 | 2014-05-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for controlling product crystal form and morphology of titanium-based nanometer material |
| CN102745747B (en) * | 2011-12-14 | 2014-07-30 | 江苏大学 | Preparation method for rod-like Sc2W3O12 negative thermal expansion material |
| CN103985850A (en) * | 2014-05-20 | 2014-08-13 | 武汉纺织大学 | Method for preparing vanadium pentoxide/conductive substrate composite electrode material |
| CN104386757A (en) * | 2014-10-21 | 2015-03-04 | 天津师范大学 | One-dimensional bismuth ferrite nanotube as well as preparation method and application thereof |
| CN104953117A (en) * | 2015-04-30 | 2015-09-30 | 常州大学 | Lithium ion battery negative material and preparation method thereof |
| CN105018770A (en) * | 2014-04-30 | 2015-11-04 | 中国科学院金属研究所 | Method for preparing porous metal material and application thereof |
| CN105047949A (en) * | 2015-06-09 | 2015-11-11 | 昆山艾可芬能源科技有限公司 | Preparation method of fuel cell nano electrode material |
| TW201625406A (en) * | 2015-01-05 | 2016-07-16 | Univ Nat Yunlin Sci & Tech | Method for preparing thorn-like zinc oxide/carbon nano tube composite material for concentrating, capturing, and sensing light |
-
2016
- 2016-12-29 CN CN201611247064.7A patent/CN106637214B/en not_active Expired - Fee Related
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004059428A (en) * | 2002-07-29 | 2004-02-26 | Samsung Sdi Co Ltd | Carbon nanotube for fuel cell, method of manufacturing the same and fuel cell using the same |
| CN102745747B (en) * | 2011-12-14 | 2014-07-30 | 江苏大学 | Preparation method for rod-like Sc2W3O12 negative thermal expansion material |
| CN103803644A (en) * | 2012-11-14 | 2014-05-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for controlling product crystal form and morphology of titanium-based nanometer material |
| CN105018770A (en) * | 2014-04-30 | 2015-11-04 | 中国科学院金属研究所 | Method for preparing porous metal material and application thereof |
| CN103985850A (en) * | 2014-05-20 | 2014-08-13 | 武汉纺织大学 | Method for preparing vanadium pentoxide/conductive substrate composite electrode material |
| CN104386757A (en) * | 2014-10-21 | 2015-03-04 | 天津师范大学 | One-dimensional bismuth ferrite nanotube as well as preparation method and application thereof |
| TW201625406A (en) * | 2015-01-05 | 2016-07-16 | Univ Nat Yunlin Sci & Tech | Method for preparing thorn-like zinc oxide/carbon nano tube composite material for concentrating, capturing, and sensing light |
| CN104953117A (en) * | 2015-04-30 | 2015-09-30 | 常州大学 | Lithium ion battery negative material and preparation method thereof |
| CN105047949A (en) * | 2015-06-09 | 2015-11-11 | 昆山艾可芬能源科技有限公司 | Preparation method of fuel cell nano electrode material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107475544A (en) * | 2017-08-29 | 2017-12-15 | 天津理工大学 | A kind of method that glassy metal is prepared under the condition of high temperature |
| CN111254308A (en) * | 2020-01-21 | 2020-06-09 | 天津理工大学 | Method for improving high-temperature stability of metal twin crystal |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106637214B (en) | 2019-04-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Cheng et al. | Characterization of plasma electrolytic oxidation coatings on Zircaloy-4 formed in different electrolytes with AC current regime | |
| Ruffino et al. | Novel approach to the fabrication of Au/silica core–shell nanostructures based on nanosecond laser irradiation of thin Au films on Si | |
| Ni et al. | Effects of inclination angle on surface roughness and corrosion properties of selective laser melted 316L stainless steel | |
| CN105543587A (en) | Ultrahigh-strength nano-crystalline Al-Mg aluminum alloy material and preparation method thereof | |
| CN106637214A (en) | Method for improving intrinsic melting point by using negative curvature of surface | |
| Riesch et al. | Tensile behaviour of drawn tungsten wire used in tungsten fibre-reinforced tungsten composites | |
| CN108779538A (en) | High-strength F e-Cr-Ni-Al multiphases stainless steel and its manufacturing method | |
| Shan et al. | A protective ceramic coating to improve oxidation and thermal shock resistance on CrMn alloy at elevated temperatures | |
| US20080085421A1 (en) | Surface-Treated Light Alloy Member and Method for Manufacturing Same | |
| Wen et al. | Design and characterization of SMAT-MAO composite coating and its influence on the fatigue property of 2024 Al alloy | |
| Adibpour et al. | Microstructural and tribological properties of A356 based surface hybrid composite produced by friction stir processing | |
| US20160221078A1 (en) | Aluminum-based porous body and method for manufacturing same | |
| KR102261029B1 (en) | Nickel-based super alloy for diffusion bonding and method for diffusion bonding using the same | |
| Zheng et al. | Microstructure and mechanical properties of Mg-Gd-Y-Zn-Zr alloy by cyclic expansion-extrusion with an asymmetrical extrusion cavity (CEE-AEC) | |
| Chen et al. | The microstructure and texture of Mo–La2O3 alloys with high transverse ductility | |
| US10233558B2 (en) | Method for manufacturing a part coated with a protective coating | |
| CN104854253A (en) | Cermet thermal spray powder, roller for molten metal plating bath, article in molten metal plating bath | |
| Li et al. | Effect of annealing temperature on microstructure and mechanical properties in oxide dispersion strengthened Fe-14Cr alloys prepared by spark plasma sintering | |
| CN107739856B (en) | A kind of preparation method of Ti-Y alloy block nano material | |
| Wixtrom et al. | Electrochemical polishing applications and EIS of a vitamin B4-based ionic liquid | |
| Zhu et al. | Nanoinstabilities of Cu2O porous nanostructured films as driven by nanocurvature effect and thermal activation effect | |
| Zhang et al. | The fracture and merging of W nanofibers under low-energy He ion irradiations at an elevated temperature | |
| Fan et al. | Effect of different annealing temperatures on microstructures and properties of Cu–Sn Alloy | |
| Dong et al. | Influence of cyclic non-isothermal heat treatment on microstructure, mechanical property and corrosion behavior of Al–Zn–Mg alloy | |
| Lu et al. | Dendritic boundary corrosion of AA2198 weld using fiber laser welding with Al–Cu filler wire |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for 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: 20190416 Termination date: 20191229 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |