CN103806042A - Preparation method for carbon fiber electroplating iron-nickel alloy - Google Patents
Preparation method for carbon fiber electroplating iron-nickel alloy Download PDFInfo
- Publication number
- CN103806042A CN103806042A CN201410027011.9A CN201410027011A CN103806042A CN 103806042 A CN103806042 A CN 103806042A CN 201410027011 A CN201410027011 A CN 201410027011A CN 103806042 A CN103806042 A CN 103806042A
- Authority
- CN
- China
- Prior art keywords
- carbon fiber
- parts
- electroplating
- preparation
- weight
- 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
Images
Abstract
The invention belongs to the technical field of electroplating, and relates to a preparation method for a carbon fiber electroplating iron-nickel alloy. The preparation method comprises the following steps of performing degumming oxidation treatment on a carbon fiber bundle; preparing an electroplating solution, namely weighing 60 to 90 parts by weight of NiSO4.6H2O, 10 to 30 parts by weight of NiCl2.6H2O, 60 to 80 parts by weight of FeSO4.7HO, 15 to 20 parts by weight of C6H5Na3O7.2H2O, 1 to 3 parts by weight of C7H5NO3S and 10 to 30 parts by weight of H3BO3 respectively, dissolving the components in a proper amount of ultrapure water, weighing 0.1 to 0.3 part by weight of C6H5NaO2S, dissolving C6H5NaO2S in a small amount of ultrapure water, uniformly mixing the two solutions, and controlling the pH value to be 3 to 4.5; performing electroplating treatment on the surfaces of carbon fibers. According to the method, the magnetism of the electroplated carbon fibers can be improved by controlling the magnetism.
Description
Technical field
The invention belongs to electroplating technology field, relate to a kind of on carbon fiber surface the preparation method of electroplating iron-nickel alloy.
Background technology
Along with electronic product becomes more and more popular, in offering convenience to our life, its hazards of electromagnetic radiation causing is also increasing.Therefore, eliminating electromagnetic shielding pollutes extremely important to improving human life quality.Compare traditional metal shield materials, carbon fiber has light weight, high ratio modulus, antifatigue, high strength and good conductivity advantage, therefore carbon fiber is carried out to surface metalation modification, and with resin matrix compound be prepared into matrix material have proportion little, can produce continuously, comprehensive shielded effective outstanding advantage, therefore in electronic product, have broad application prospects.
The metallized method of material surface mainly contains electrochemical plating, electroless plating method, ion sputtering method, vacuum vapour deposition etc. at present.Wherein electrochemical plating and electroless plating method are all applicable to the metallization of carbon fiber surface, but electrochemical plating production efficiency is high, process stabilizing, and little to the burden of environment, the therefore surface metalation of very suitable carbon fiber.Carbon fiber surface nickel plating can obviously improve its conductivity, makes to have good electromagnetic wave shielding by the matrix material of its filling, but can not give carbon fiber magnetic, is subject to certain limitation during therefore for wide-band electromagnetic shielding field.
Iron-nickel alloy is a kind of low frequency soft magnetic materials in low-intensity magnetic field with high magnetic permeability and low-coercivity, by controlling thermal treatment process and smelting technology, can realize the regulation and control of alloy composition, phase composite and magnetic, but the report of so far there are no carbon fiber surface electroplating iron-nickel alloy.Obviously, based on the premium properties of above fiber and iron-nickel alloy, had superiority and combined, can be prepared high performance electromagnetic shielding material.
Summary of the invention
The object of the invention is to overcome the above-mentioned deficiency of prior art, provide a kind of by the control to magnetic, can improve the magnetic methods of the carbon fiber after plating.The method has the advantages that technique is simple, workable, binding force of cladding material is good.By preparing iron-nickel alloy at carbon fiber surface, the iron-nickel alloy magnetic obtaining can reach 15～25emu/g, makes the conjugated fibre of its filling have good electromagnetism over-all properties, is expected to obtain in wide-band electromagnetic shielding field application.Concrete preparation technology is as follows: the carbon fiber surface oxide treatment of removing photoresist, the control of surface activation process and electroplating iron-nickel technique thereof.The iron-nickel alloy coating bright in color obtaining, is evenly distributed, and thickness can be controlled in 1um left and right, almost there is no the phenomenon of evil mind.
The invention provides a kind of preparation method of carbon fiber electroplating iron-nickel alloy, concrete completing steps is as follows:
A preparation method for carbon fiber electroplating iron-nickel alloy, comprises the following steps:
(1) carbon fiber bundle that is 7-8um by the filament diameter oxide treatment of removing photoresist;
(2) preparation electroplate liquid: according to weight proportion, take respectively the NiSO of 60～90 parts
46H
2o, the NiCl of 10～30 parts
26H
2o, the FeSO of 60～80 parts
47HO, the C of 15～20 parts
6h
5na
3o
72H
2o, the C of 1～3 part
7h
5nO
3the H of S and 10～30 parts
3bO
3, be dissolved in appropriate ultrapure water, stir at ambient temperature, then take the C of 0.1～0.3 part
6h
5naO
2s is dissolved in a small amount of ultrapure water, stirs, and subsequently above-mentioned two kinds of solution is mixed, and at room temperature stirs, and controls pH value between 3～4.5;
(3) electroplating iron-nickel technique
The electroplate liquid that step (2) is prepared is placed in 50～70 ℃ of water-baths, cross 30min after temperature-stable, the carbon fiber bundle of processing through step (1) is connected into circuit as negative electrode, nickel plate is as anode, connect after good circuit, regulating YIN and YANG pole span is from being 5～15cm, regulate D.C. regulated power supply, electric current is remained between 50～300mA, voltage is between 0.5～3V, after electroplating 5～60min, use washed with de-ionized water fiber surface 2～3 times, then in the vacuum drying oven of 30～80 ℃, after dry 4～10h, take out, complete the plating at carbon fiber surface.
Wherein, the treatment process of step (1) is preferably as follows: by described carbon fiber bundle, first in acetone, soak 24h, the calcination oxidation of removing photoresist in retort furnace again, retort furnace calcination condition is: temperature is 300～600 ℃, time keeps temperature rise rate scope between 2～10 ℃/min within being controlled at 30～90min under air atmosphere, after insulation finishes, be down to room temperature with stove.
Feature of the present invention and beneficial effect: cost is low, nontoxic, technique is simple, workable, can realize continuously and producing, improve binding force of cladding material, and the performances such as the thickness of its iron-nickel alloy, composition and magnetic are all adjustable, can obtain the shielding material of electromagnetism high comprehensive performance, be a kind of electroplating technology of promoting the use of, and can expand the use range of carbon fiber.
Accompanying drawing explanation
Carbon fiber electrically plating iron nickel alloy surfaces shape appearance figure in Fig. 1 example 1.
The XRD analysis figure of carbon fiber electroplating iron-nickel alloy in Fig. 2 example 1.
The magnetic hysteresis loop figure of carbon fiber electroplating iron-nickel alloy in Fig. 3 example 1.
Carbon fiber electroplating iron-nickel alloy EDS analysis chart in Fig. 4 example 2.
The magnetic hysteresis loop figure of carbon fiber electroplating iron-nickel alloy in Fig. 5 example 2.
Embodiment:
Below in conjunction with drawings and Examples, the present invention will be described.
Example 1
(1) the 4K(mass of fibers that oxidizing process is 7-8um by filament diameter that removes photoresist is 4000 carbon fiber monofilament) carbon fiber, first in acetone, soak 24h, then the calcination oxidation of removing photoresist in retort furnace.The condition of removing photoresist: 400 ℃ of temperature, soaking time 30min, heat-up rate is 2 ℃/min, is down to room temperature takes out after insulation finishes with stove.
(2) configuration of electroplate liquid, according to weight proportion, first takes respectively the NiSO of 90g
46H
2the NiCl of O, 15g
26H
2the FeSO of O, 50g
47H
2the C of O, 17.5g
6h
5na
3o
72H
2the C of O, 1.5g
7h
5nO
3the H of S (asccharin) and 20g
3bO
3be dissolved in the ultrapure water of 400mL, stir at ambient temperature, then take the C of 0.2g
6h
5naO
2s (benzene sulfinic acid sodium salt) is dissolved in the ultrapure water of 50mL, stirs with glass stick, subsequently above-mentioned two kinds of solution is mixed, and at room temperature stirs 10min with glass stick, then uses the volumetric flask constant volume of 500mL, and pH value is 3.7.
(3) plating solution that electroplating iron-nickel technique prepares step (2) is placed in the water-bath of 55 ℃, cross 30min after temperature-stable, the carbon fiber of processing through step (1) is intercepted to a branch of of 7cm length and be connected into circuit as negative electrode, nickel plate is as anode (overall specification 60 × 70mm, the specification that immerses plating solution liquid level is 60 × 65mm), connect after good circuit, regulating YIN and YANG pole span is from being 6cm.Regulate D.C. regulated power supply, make electric current remain on 100mA, voltage is 1.2V, electroplates after 15min, uses washed with de-ionized water fiber surface 2～3 times, then in the vacuum drying oven of 40 ℃, after dry 6h, takes out, and completes the plating at carbon fiber surface.As shown in Figure 1, as shown in Figure 2, the magnetic hysteresis loop after its plating as shown in Figure 3 in the XRD figure analysis of its iron-nickel alloy obtaining for its microscopic appearance figure.
Example 2
(1) the 4K(mass of fibers that oxidizing process is 7-8um by filament diameter that removes photoresist is 4000 carbon fiber monofilament) carbon fiber, first in acetone, soak 24h, then the calcination oxidation of removing photoresist in retort furnace.The condition of removing photoresist: 400 ℃ of temperature, soaking time 30min, heat-up rate is 3～4 ℃/min, is down to room temperature takes out after insulation finishes with stove.
(2) configuration of electroplate liquid, according to weight proportion, first takes respectively the NiSO of 80g
46H
2the NiCl of O, 15g
26H
2the FeSO of O, 40g
47H
2the C of O, 17.5g
6h
5na
3o
72H
2the C of O, 1.5g
7h
5nO
3the H of S (asccharin) and 20g
3bO
3be dissolved in 400mL ultrapure water, stir at ambient temperature, then take the C of 0.2g
6h
5naO
2s (benzene sulfinic acid sodium salt) is dissolved in the ultrapure water of 50mL, stirs with glass stick, subsequently above-mentioned two kinds of solution is mixed, and at room temperature glass stick stirs 10min, then uses the volumetric flask constant volume of 500mL, and pH value is 3.
(3) plating solution that electroplating iron-nickel technique prepares step (2) is placed in the water-bath of 55 ℃, cross 30min after temperature-stable, the carbon fiber of processing through step (1) is intercepted to a branch of of 6.2cm length and be connected into circuit as negative electrode, nickel plate is as anode (overall specification 60 × 70mm, the specification that immerses plating solution liquid level is 60 × 60mm), connect after good circuit, regulating YIN and YANG pole span is from being 8cm.Regulate D.C. regulated power supply, make electric current remain on 100mA, voltage is 0.8V, electroplate after 10min, use washed with de-ionized water fiber surface 2～3 times, then in the vacuum drying oven of 40 ℃, after dry 6h, take out, complete the plating at carbon fiber surface, as shown in Figure 4, iron nickel mass ratio reaches Fe:Ni=8.86:91.14 in energy spectrum analysis after its plating, and mol ratio is Fe:Ni=9.28:90.27; Magnetic hysteresis loop after its plating as shown in Figure 5.
Claims (2)
1. a preparation method for carbon fiber electroplating iron-nickel alloy, comprises the following steps:
(1) carbon fiber bundle that is 7-8um by the filament diameter oxide treatment of removing photoresist;
(2) preparation electroplate liquid: according to weight proportion, take respectively the NiSO of 60～90 parts
46H
2o, the NiCl of 10～30 parts
26H
2o, the FeSO of 60～80 parts
47HO, the C of 15～20 parts
6h
5na
3o
72H
2o, the C of 1～3 part
7h
5nO
3the H of S and 10～30 parts
3bO
3, be dissolved in appropriate ultrapure water, stir at ambient temperature, then take the C of 0.1～0.3 part
6h
5naO
2s is dissolved in a small amount of ultrapure water, stirs, and subsequently above-mentioned two kinds of solution is mixed, and at room temperature stirs, and controls pH value between 3～4.5;
(3) electroplating iron-nickel technique
The electroplate liquid that step (2) is prepared is placed in 50～70 ℃ of water-baths, cross 30min after temperature-stable, the carbon fiber bundle of processing through step (1) is connected into circuit as negative electrode, nickel plate is as anode, connect after good circuit, regulating YIN and YANG pole span is from being 5～15cm, regulate D.C. regulated power supply, electric current is remained between 50～300mA, voltage is between 0.5～3V, after electroplating 5～60min, use washed with de-ionized water fiber surface 2～3 times, then in the vacuum drying oven of 30～80 ℃, after dry 4～10h, take out, complete the plating at carbon fiber surface.
2. the preparation method of carbon fiber electroplating iron-nickel alloy according to claim 1, it is characterized in that, the treatment process of step (1) is as follows: by described carbon fiber bundle, first in acetone, soak 24h, the calcination oxidation of removing photoresist in retort furnace again, retort furnace calcination condition is: temperature is 300～600 ℃, within the time is controlled at 30～90min, under air atmosphere, keep temperature rise rate scope between 2～10 ℃/min, after insulation finishes, be down to room temperature with stove.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410027011.9A CN103806042B (en) | 2014-01-20 | 2014-01-20 | The preparation method of carbon fiber electroplating iron-nickel alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410027011.9A CN103806042B (en) | 2014-01-20 | 2014-01-20 | The preparation method of carbon fiber electroplating iron-nickel alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103806042A true CN103806042A (en) | 2014-05-21 |
| CN103806042B CN103806042B (en) | 2016-04-20 |
Family
ID=50703408
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410027011.9A Expired - Fee Related CN103806042B (en) | 2014-01-20 | 2014-01-20 | The preparation method of carbon fiber electroplating iron-nickel alloy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103806042B (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104480698A (en) * | 2014-11-24 | 2015-04-01 | 天津大学 | Method for preparing permalloy-coated carbon fiber employing two-step electrodeposition method |
| CN105908493A (en) * | 2016-04-19 | 2016-08-31 | 郑州四维特种材料有限责任公司 | Metal modified carbon fiber, preparation method and application thereof |
| CN106968004A (en) * | 2017-03-29 | 2017-07-21 | 浙江东尼电子股份有限公司 | A kind of electroplating process of magnetic material |
| CN107541758A (en) * | 2017-08-01 | 2018-01-05 | 昆明理工大学 | A kind of method in carbon-based material surface Electrodeposition Bath of Iron nickel alloy coating |
| CN107746505A (en) * | 2017-10-17 | 2018-03-02 | 中南大学 | A kind of coat carbon fiber reinforced ABS/PP electromagnetic shielding composite materials and preparation method thereof |
| CN110724990A (en) * | 2019-09-23 | 2020-01-24 | 中国地质大学（武汉） | Electrosilvering carbon fiber electrode and preparation method thereof |
| US10576335B2 (en) | 2017-07-20 | 2020-03-03 | Taylor Made Golf Company, Inc. | Golf club including composite material with color coated fibers and methods of making the same |
| CN113622009A (en) * | 2021-08-03 | 2021-11-09 | 安徽省吉祥纺织工程先进技术研究院 | Electroplating treatment process of carbon fiber-based high-performance fabric |
| CN113668020A (en) * | 2021-08-03 | 2021-11-19 | 安徽三宝棉纺针织投资有限公司 | Preparation method of carbon fiber fabric electroplating solution |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5827997A (en) * | 1994-09-30 | 1998-10-27 | Chung; Deborah D. L. | Metal filaments for electromagnetic interference shielding |
| US20100074834A1 (en) * | 2008-09-22 | 2010-03-25 | Samsung Electronics Co., Ltd. | Apparatus and method for surface-treating carbon fiber by resistive heating |
| CN101886330A (en) * | 2010-06-10 | 2010-11-17 | 天津大学 | Fe-Co magnetic alloy plated carbon fiber, preparation method and application thereof |
| WO2010139052A1 (en) * | 2009-06-02 | 2010-12-09 | Integran Technologies, Inc. | Metal-coated polymer article of high durability and vacuum and/or pressure integrity |
| US20110160037A1 (en) * | 2009-12-30 | 2011-06-30 | Cheil Industries Inc. | Carbon Nanofiber-Metal Composite and Method for Preparing the Same |
| CN102154816A (en) * | 2011-01-20 | 2011-08-17 | 天津市飞荣达科技有限公司 | FeCo alloy/CuO double-plating magnetic carbon fiber and preparation method and application |
-
2014
- 2014-01-20 CN CN201410027011.9A patent/CN103806042B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5827997A (en) * | 1994-09-30 | 1998-10-27 | Chung; Deborah D. L. | Metal filaments for electromagnetic interference shielding |
| US20100074834A1 (en) * | 2008-09-22 | 2010-03-25 | Samsung Electronics Co., Ltd. | Apparatus and method for surface-treating carbon fiber by resistive heating |
| WO2010139052A1 (en) * | 2009-06-02 | 2010-12-09 | Integran Technologies, Inc. | Metal-coated polymer article of high durability and vacuum and/or pressure integrity |
| US20110160037A1 (en) * | 2009-12-30 | 2011-06-30 | Cheil Industries Inc. | Carbon Nanofiber-Metal Composite and Method for Preparing the Same |
| CN101886330A (en) * | 2010-06-10 | 2010-11-17 | 天津大学 | Fe-Co magnetic alloy plated carbon fiber, preparation method and application thereof |
| CN102154816A (en) * | 2011-01-20 | 2011-08-17 | 天津市飞荣达科技有限公司 | FeCo alloy/CuO double-plating magnetic carbon fiber and preparation method and application |
Non-Patent Citations (2)
| Title |
|---|
| KI-YEON PARK ET AL: "Microwave absorbing hybrid composites containing Ni–Fe coated carbon nanofibers prepared by electroless plating", 《COMPOSITES: PART A》 * |
| ZHOU HAI-HUI ET AL: "Catalytic graphitization of PAN-based carbon fibers with electrodeposited Ni-Fe alloy", 《TRANSACTIONS OF NONFERROUS METALS SOCIETY OF CHINA》 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104480698A (en) * | 2014-11-24 | 2015-04-01 | 天津大学 | Method for preparing permalloy-coated carbon fiber employing two-step electrodeposition method |
| CN105908493A (en) * | 2016-04-19 | 2016-08-31 | 郑州四维特种材料有限责任公司 | Metal modified carbon fiber, preparation method and application thereof |
| CN106968004A (en) * | 2017-03-29 | 2017-07-21 | 浙江东尼电子股份有限公司 | A kind of electroplating process of magnetic material |
| US10576335B2 (en) | 2017-07-20 | 2020-03-03 | Taylor Made Golf Company, Inc. | Golf club including composite material with color coated fibers and methods of making the same |
| US11752403B2 (en) | 2017-07-20 | 2023-09-12 | Taylor Made Golf Company, Inc. | Golf club including composite material with color coated fibers and methods of making the same |
| US11213726B2 (en) | 2017-07-20 | 2022-01-04 | Taylor Made Golf Company, Inc. | Golf club including composite material with color coated fibers and methods of making the same |
| CN107541758A (en) * | 2017-08-01 | 2018-01-05 | 昆明理工大学 | A kind of method in carbon-based material surface Electrodeposition Bath of Iron nickel alloy coating |
| CN107746505B (en) * | 2017-10-17 | 2020-09-08 | 中南大学 | Coating carbon fiber reinforced ABS/PP electromagnetic shielding composite material and preparation method thereof |
| CN107746505A (en) * | 2017-10-17 | 2018-03-02 | 中南大学 | A kind of coat carbon fiber reinforced ABS/PP electromagnetic shielding composite materials and preparation method thereof |
| CN110724990B (en) * | 2019-09-23 | 2020-09-04 | 中国地质大学（武汉） | Electrosilvering carbon fiber electrode and preparation method thereof |
| CN110724990A (en) * | 2019-09-23 | 2020-01-24 | 中国地质大学（武汉） | Electrosilvering carbon fiber electrode and preparation method thereof |
| CN113622009A (en) * | 2021-08-03 | 2021-11-09 | 安徽省吉祥纺织工程先进技术研究院 | Electroplating treatment process of carbon fiber-based high-performance fabric |
| CN113668020A (en) * | 2021-08-03 | 2021-11-19 | 安徽三宝棉纺针织投资有限公司 | Preparation method of carbon fiber fabric electroplating solution |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103806042B (en) | 2016-04-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103806042B (en) | The preparation method of carbon fiber electroplating iron-nickel alloy | |
| CN105810915B (en) | A kind of preparation of order mesoporous carbon ball composite material of the embedding sulphur of graphene coated and the application as lithium sulfur battery anode material | |
| CN103247777B (en) | Cobaltosic oxide multi-shell hollow sphere cathode material for lithium ion battery and preparation method thereof | |
| CN106033813B (en) | A method of anode material of lithium-ion battery is prepared using sodium alginate as carbon source | |
| CN203096163U (en) | Adjusting device for uniformly coating for magnetic field | |
| CN108134093A (en) | A kind of carbon nanotube paper-metal or alloy composite current collector and preparation method thereof | |
| CN108878828A (en) | Carbon-coated nickelic tertiary cathode material of one kind and preparation method thereof | |
| CN108933251A (en) | A kind of biomass carbon/ferric oxide composite material and preparation method thereof | |
| CN105932236B (en) | A kind of coating modification method of lithium ion battery electrode material | |
| CN105682442A (en) | Preparation method for light-weight graphite fiber foam nickel electromagnetic shielding material | |
| CN100353594C (en) | Metal oxide electrode material for producing adulterant utilizing electro-deposition-heat treatment technology | |
| CN103866364B (en) | The magnetospheric preparation method of stainless steel fibre Surface Fe nickel alloy | |
| CN105789579A (en) | Bionic synthesizing method of lithium ion cell anode material FeO4/Fe2O3/Fe/C | |
| CN103274385A (en) | Lithium ion battery cathode material carbon microsphere and preparation method thereof | |
| CN108893762B (en) | Electrodeposition method of Ni-63 radioactive sheet source | |
| CN102628214A (en) | Carbon fiber composite material with ZnO layer electrolytically deposited on surface as well as preparation method and application thereof | |
| CN104600259B (en) | Lithium battery negative electrode material with lamellar structure and preparation method of lithium battery negative electrode material | |
| CN104480698A (en) | Method for preparing permalloy-coated carbon fiber employing two-step electrodeposition method | |
| CN107394171B (en) | Preparation method of lithium nickel manganese oxide | |
| CN108777289A (en) | A kind of preprocess method of stable water-retaining type lead carbon battery negative material | |
| CN108091881A (en) | A kind of preparation method of carbon film-M collectors | |
| CN114804218A (en) | Microwave absorbing material with multilevel heterostructure and preparation method thereof | |
| CN103726087A (en) | Method of pulse electrodeposition on nickel coating by carbon fiber preform | |
| CN105048020B (en) | A kind of method that lithium doping cobalt ferrite material is prepared by raw material of waste lithium cell | |
| CN106960950A (en) | Tertiary cathode material method of modifying |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160420 Termination date: 20220120 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |