CN105118382A - Graphene layer, membrane material, method for preparing membrane material, and flexible display device - Google Patents
Graphene layer, membrane material, method for preparing membrane material, and flexible display device Download PDFInfo
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- CN105118382A CN105118382A CN201510541659.2A CN201510541659A CN105118382A CN 105118382 A CN105118382 A CN 105118382A CN 201510541659 A CN201510541659 A CN 201510541659A CN 105118382 A CN105118382 A CN 105118382A
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- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
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- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
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- G09F9/301—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements flexible foldable or roll-able electronic displays, e.g. thin LCD, OLED
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Abstract
The invention relates to the field of electronic materials and discloses a graphene layer. The graphene layer comprises a graphene membrane and an organic insulating membrane adhering to the surface of one side of the graphene membrane, wherein a hydrogen bond can be formed between the graphene membrane and the organic insulating membrane, and the organic insulating membrane is polyethylene, polyvinylidene difluoride, polytetrafluoroethylene or acrylic resin. The invention further discloses a membrane material composed of the graphene layer and a polyimide substrate and a method for preparing the membrane material. On one hand, the hydrogen bond can be formed by the organic insulating membrane and the graphene membrane in the follow-up photolithography technique, and connection is tight; on the other hand, the organic insulating membrane can also be tightly connected with polyimide, so that adhesion between graphene and polyimide is effectively strengthened by means of the organic insulating membrane. The membrane material composed of the graphene membrane, the organic insulating membrane and the polyimide substrate is high in adhesion performance, and the graphene membrane does not fall off easily. The membrane material can be applied to a display device.
Description
Technical field
The present invention relates to field of electronic devices, particularly a kind of graphene layer, film material, its preparation method and flexible display device.
Background technology
In recent years, Flexible Displays achieved develop rapidly.For flexible display device, high-quality substrate is most important.For Graphene, Graphene has the electric charge degree of excursion of high compared with silicon 100 times, the current density of high compared with copper 100 times, outstanding heat conductivity and chemical resistance structure, not only can realize the application of number of chemical sexual function, also have the feature such as flexibility and retractility, available simple method carries out synthesizing and printing.Graphene not only can be used as the equivalent material of current material, also can be applicable to the material of time generation transistor and electrode member, therefore enjoys and attract attention widely.
Polyimide (PI) has the excellent advantage such as mechanical property, stable performance, withstand high temperatures, no matter as structured material or as functional material, all has huge application prospect.Because PI film is high-temperature electric heating membrane, can reach 250 DEG C by bearing temperature for a long time, therefore, in photolithographic patterning Graphene process, be that basement membrane extremely has advantage with PI.Before photolithographic patterning Graphene, first will prepare Graphene in polyimide base film, method is:
1, vapour deposition (CVD) method is utilized to prepare graphene film on copper film or nickel film;
2, immerse in acid solution, by soaking away copper film or nickel film at the described copper film with graphene film or nickel film;
3, copper film or nickel film are corroded completely, only remaining graphene film swims in acid solution surface, polyimide film is placed in acid solution, graphene film and polyimide film are attached together naturally with intermolecular force, pick up, graphene film is adsorbed on polyimide film.
After obtaining being adsorbed in the graphene film on polyimide film, then by graphene film through photolithographic patterning process, so that make drive electrode and induction electrode etc.
But PI basement membrane adhesion property is poor, in photolithographic patterning process, very easily there is situation about coming off from PI basement membrane in Graphene, seriously governs the application of Graphene in display device.
Summary of the invention
The invention provides a kind of graphene layer, film material, its preparation method and flexible display device, described film material can by organic insulating film by Graphene and polyimide matrix compact siro spinning technology, improve the adhesiveness between Graphene and polyimide, ensure Graphene difficult drop-off.
The invention provides a kind of graphene layer, comprise graphene film and the organic insulating film adhering to described graphene film one side surface;
Hydrogen bond can be formed between described graphene film and organic insulating film;
Described organic insulating film is tygon, polyvinylidene fluoride, teflon or acrylic type resin.
The invention provides a kind of film material, comprise the graphene layer described in polyimide substrate and technique scheme, described polyimide substrate adheres to the organic insulating film in described graphene layer and is connected.
The invention provides a kind of preparation method of film material, comprise the following steps:
(A) adopt vapour deposition process to be deposited on by Graphene on Cu film or Ni film, through modification, obtain the graphene film with hydroxyl;
(B) described with the graphene film of hydroxyl applying one deck organic insulating film and solidifying;
(C) coating polyimide film on described organic insulating film, and carry out ultra-violet curing, obtain intermediate;
(D) described intermediate is immersed in acid solution, removes Cu film or Ni film, obtain film material;
Described organic insulating film is tygon, polyvinylidene fluoride, teflon or acrylic type resin.
Preferably, in described step (A), the method for described modification is:
Graphene and alcohols and gold chloride are reacted, then through electro-deposition, obtains the graphene film with hydroxyl.
Preferably, in described step (B), the pre-rotating speed of described coating is 300 ~ 500rpm/5 ~ 10sec, and main rotating speed is 600 ~ 1200rpm/15 ~ 30sec; The temperature of described solidification is 200 ~ 250 DEG C, and the time of described solidification is 30 ~ 60 minutes.
Preferably, in described step (C), the pre-rotating speed of described coating is 300 ~ 500rpm/5 ~ 10sec, and main rotating speed is 600 ~ 1200rpm/15 ~ 30sec.
Preferably, also comprise predrying after described coating, predrying temperature is 90 ~ 120 DEG C, and the pre-dried time is 120 ~ 150 seconds.
Preferably, in described step (C), the irradiation transfer rate of described ultra-violet curing is 0.8 ~ 1.6m/min, and the irradiation time of described ultra-violet curing is 2 ~ 8 seconds.
Preferably, in described step (C), the bake out temperature after described ultra-violet curing is 200 ~ 250 DEG C, and drying time is 30 ~ 60min.
Present invention also offers a kind of flexible display device, comprise the film material that described in film material described in technique scheme or technique scheme prepared by method.
Compared with prior art, graphene layer of the present invention comprises graphene film and adheres to the organic insulating film of described graphene film one side surface; Hydrogen bond can be formed between described graphene film and organic insulating film; Described organic insulating film is tygon, polyvinylidene fluoride, teflon or acrylic type resin.On the one hand, organic insulating film can form hydrogen bond with graphene film in subsequent optical carving technology, connects closely; On the other hand, organic insulating film can also form compact siro spinning technology with polyimide, and therefore, organic insulating film effectively improves the adhesion property of Graphene and polyimide.The film material that graphene film, organic insulating film and polyimide substrate are formed, adhesion property is good, graphene film difficult drop-off.
Accompanying drawing explanation
Fig. 1 is the structural representation of film material of the present invention;
Fig. 2 is the preparation flow figure of film material of the present invention;
Fig. 3 is the principle schematic that acrylic type resin and graphene layer form hydrogen bond in photolithographic.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
The embodiment of the invention discloses a kind of graphene layer, comprise graphene film and the organic insulating film adhering to described graphene film one side surface;
Hydrogen bond can be formed between described graphene film and organic insulating film;
Described organic insulating film is tygon, polyvinylidene fluoride, teflon or acrylic type resin.
According to the present invention, described graphene layer comprises graphene film and organic insulating film.Described graphene film with modification group, can and organic insulating film between form hydrogen bond, described modification group is preferably hydroxyl.
The preparation method of described graphene film is preferably:
Graphene and alcohols and gold chloride are reacted, then through electro-deposition, obtains the graphene film with hydroxyl.
In the preparation method of described Graphene, first, Graphene, alcohols and gold chloride are obtained by reacting the Graphene with carboxyl; With the Graphene of carboxyl through electro-deposition, obtain the graphene film with hydroxyl.For the condition of described reaction, according to the condition of existing Graphene modification doping.
By said method, doping forms the Graphene possessing labile functional groups, reduces the sheet resistance of Graphene on the one hand; Form active function groups by doping on the one hand, be beneficial to and react with its organic insulation rete, improve adhesiveness.
Described organic insulating film is tygon, polyvinylidene fluoride, teflon or acrylic type resin.Gather the group such as base, double bond with epoxy in described organic insulating film, when follow-up photoetching, can with graphene film with modification group (as hydroxyl) form hydrogen bond.This hydrogen bond effectively improves the sticking problem of organic insulating film and graphene film, and both combine closely.
The embodiment of the invention discloses a kind of film material, comprise the graphene layer described in polyimide substrate and technique scheme, described polyimide substrate adheres to the organic insulating film in described graphene layer and is connected.
In the present invention, described film material comprises polyimide substrate, organic insulating film and graphene film.Described polyimide substrate adheres to the organic insulating film in described graphene layer and is connected, and graphene film adheres to organic insulating film and is connected, and namely organic insulating film is being between graphene film and polyimide substrate.Because described organic insulating film and polyimide have similar character, therefore organic insulating film and polyimide substrate have good connectivity.And organic insulating film can form hydrogen bond with graphene film in subsequent optical carving technology, and hydrogen bond effectively improves the sticking problem of organic insulating film and graphene film, and both combine closely.The character of comprehensive two aspects, organic insulating film effectively improves the adhesion property of Graphene and polyimide, and film material of the present invention has better integraty, and Graphene not easily comes off in follow-up lithographic patterning process.
Fig. 1 is the structural representation of film material of the present invention, and in Fig. 1,1 is graphene film, and 2 is organic insulating film, and 3 is polyimide substrate.
The embodiment of the invention also discloses a kind of preparation method of film material, comprise the following steps:
(A) adopt vapour deposition process to be deposited on by Graphene on Cu film or Ni film, through modification, obtain the graphene film with hydroxyl;
(B) described with the graphene film of hydroxyl applying one deck organic insulating film and solidifying;
(C) coating polyimide film on described organic insulating film, and carry out ultra-violet curing, obtain intermediate;
(D) described intermediate is immersed in acid solution, removes Cu film or Ni film, obtain film material;
Described organic insulating film is tygon, polyvinylidene fluoride, teflon or acrylic type resin.
According to the present invention, first adopt vapour deposition process to be deposited on by Graphene on the surface of Cu film or Ni film side, through modification, obtain the graphene film with hydroxyl.Described vapour deposition process is namely: using carbon compounds such as methane as carbon source, pyrolytic, becomes Graphene at Cu film or the superficial growth of Ni film.Ni etc. is had to the metal of higher molten carbon amounts.The carbon atom that carbon source cracking produces infiltrates when high temperature, when temperature reduces, separates out nucleation, grow up into Graphene from Ni film.Cu etc. is had to the metal of lower molten carbon amounts, under high temperature, gaseous carbon source cracking Formed atomic adsorption, in surface, grows into Graphene island, then two dimension merging of growing up obtains Graphene.Described carbon source can be hydro carbons, as methane, ethene, acetylene etc.For described vapour deposition process temperature used, pressure and reaction time, those skilled in the art can implement according to known conditions.
The method of described modification is preferably:
Graphene and film alcohols and gold chloride are reacted, then through electro-deposition, obtains the graphene film with hydroxyl.
Reaction process is:
In the method for described modification, first, Graphene, alcohols and gold chloride are obtained by reacting the Graphene with carboxyl; With the Graphene of carboxyl through electro-deposition, obtain the graphene film with hydroxyl.For the condition of described reaction, according to the condition of existing Graphene modification doping.
According to the present invention, after obtaining the graphene film with hydroxyl, described with the graphene film of hydroxyl applying one deck organic insulating film and solidifying.Described organic insulating film is tygon, polyvinylidene fluoride, teflon or acrylic type resin.Described coating is carried out preferably by the automatic double surface gluer of litho machine.Being specially of described coating: by the tygon of melting, polyvinylidene fluoride, teflon or acrylic type resin, is spin-coated on by the automatic double surface gluer of litho machine on the surface of Cu film or the other side of Ni film.The pre-rotating speed of described coating is 300 ~ 500rpm/5 ~ 10sec, and main rotating speed is 600 ~ 1200rpm/15 ~ 30sec.The temperature of described solidification is preferably 200 ~ 250 DEG C, and the time of described solidification is preferably 30 ~ 60 minutes.By solidification, add the hardness of organic insulating film and improve the transmitance of organic insulating film.
According to the present invention, after forming organic insulating film, coating polyimide film on described organic insulating film, and carry out ultra-violet curing, obtain intermediate.Described coating is specially: by the polyimide of melting, by the automatic double surface gluer spin coating of litho machine.In coating, it is 300 ~ 500rpm/5 ~ 10sec that the rotating speed of gluing is preferably pre-rotating speed, and main rotating speed is 600 ~ 1200rpm/15 ~ 30sec.Prerotation makes resin uniform spreading, and main turning makes resin be thinned to desired thickness.After coating, predrying temperature is preferably 90 ~ 120 DEG C, and the pre-dried time is preferably 120 ~ 150 seconds.The irradiation transfer rate of described ultra-violet curing is preferably 0.8 ~ 1.6m/min.The irradiation time of described ultra-violet curing is preferably 2 ~ 8 seconds.Bake out temperature after described ultra-violet curing is preferably 200 ~ 250 DEG C, and drying time is preferably 30 ~ 60min.
According to the present invention, after obtaining described intermediate, described intermediate is immersed in acid solution, removes Cu film or Ni film, obtain film material.The pH value of described acid solution is 1 ~ 3, be preferably inorganic acids, can be in nitric acid, phosphoric acid and sulfuric acid one or more.Being understandable that, about the acidic materials comprised in acid solution are not limited in above-mentioned cited kind, can also be other acidic materials known to those skilled in the art, and above-mentioned cited kind is only wherein comparatively conventional and important kind.The time of described immersion is preferably 25 ~ 45 minutes, is preferably 30 ~ 35 minutes, until Cu film or Ni film are removed clean.By the immersion of acid solution.Not only can remove Cu film or Ni film, the sheet resistance of graphene film can also be reduced.
Fig. 2 is the preparation flow figure of film material of the present invention, and in Fig. 2, graphene is graphene film, and Cu is copper film, and OC is organic insulating film, and PI is polyimide substrate.
Present invention also offers a kind of flexible display device, the film material that described in the film material described in technique scheme or technique scheme prepared by method.
Graphene layer of the present invention comprises graphene film and adheres to the organic insulating film of described graphene film one side surface; Hydrogen bond can be formed between described graphene film and organic insulating film; Described organic insulating film is tygon, polyvinylidene fluoride, teflon or acrylic type resin.On the one hand, organic insulating film can form hydrogen bond with graphene film in subsequent optical carving technology, connects closely; On the other hand, organic insulating film can also form compact siro spinning technology with polyimide, and therefore, organic insulating film effectively improves the adhesion property of Graphene and polyimide.The film material that graphene film, organic insulating film and polyimide substrate are formed, adhesion property is good, graphene film difficult drop-off.
In order to understand the present invention further, be described in detail to graphene layer provided by the invention, rete, its preparation method and flexible display device below in conjunction with embodiment, protection scope of the present invention is not limited by the following examples.
Embodiment 1
(A) reference literature YuQK, JaureguiLA, WuW, etal.Controlandcharacterizationofindividualgrainsandgrai nboundariesingraphenegrownbychemicalvapourdeposition.Nat Mater, 2011, the vapour deposition process that 10:443 – 449 records, is deposited on Graphene on Cu film or Ni film.
By Graphene, butanols and gold chloride under the phosphoric acid buffer liquid system of pH=9, under ambient temperature, react more than 30min, under agitation, adopt the electro-deposition of cyclic voltammetry one step to prepare compound substance, obtain the graphene film with hydroxyl.
(B) by the acrylic type resin of melting, be spin-coated on the graphene film with hydroxyl by the automatic double surface gluer of litho machine, pre-rotating speed (making resin uniform spreading) 300rpm/10sec, main rotating speed 600/15sec (making resin be thinned to desired thickness), solidifies 45 minutes under 200 DEG C of conditions.
(C) by the polyimide of melting, by the automatic double surface gluer spin coating of litho machine, the pre-rotating speed of gluing is 500rpm/10sec, and main rotating speed is 1200rpm/30sec.After coating, under 100 DEG C of conditions predrying 120 seconds.Then be cured (i=365nm, g=408nm, h=436nm) under ultraviolet light conditions, the irradiation transfer rate of ultra-violet curing is 1.2m/min, and the irradiation time of ultra-violet curing is 5 seconds.Finally dry 30 minutes under 230 DEG C of conditions, obtain intermediate.
(D) described intermediate is immersed in pH value be 2 nitric acid and phosphoric acid mix acid liquor in, soak 30 minutes, remove Cu film or Ni film, obtain film material.
100 blocks of film materials method described in embodiment 1 prepared carry out photolithographic patterning development, and coming off of graphene film does not appear in the film material of 95%.
Acrylic type resin and graphene layer form hydrogen bond in photolithographic, and principle as shown in Figure 3.Fig. 3 is the principle schematic that acrylic type resin and graphene layer form hydrogen bond in photolithographic.
Be the graphene film of substrate with polyimide by existing method preparation, the photolithographic patterning development of Progressive symmetric erythrokeratodermia, more than 85% all there is coming off of Graphene.
Embodiment 2
(A) reference literature YuQK, JaureguiLA, WuW, etal.Controlandcharacterizationofindividualgrainsandgrai nboundariesingraphenegrownbychemicalvapourdeposition.Nat Mater, 2011, the vapour deposition process that 10:443 – 449 records, is deposited on Graphene on Cu film.
By Graphene, butanols and gold chloride under the phosphoric acid buffer liquid system of pH=9, under ambient temperature, react more than 30min, under agitation, adopt the electro-deposition of cyclic voltammetry one step to prepare compound substance, obtain the Graphene with carboxyl.
(B) by the tygon of melting, be spin-coated on the graphene film with hydroxyl by the automatic double surface gluer of litho machine, gluing transfers Spincoatnig to: pre-rotating speed (making resin uniform spreading) 500rpm/10sec, main rotating speed 1200rpm/30sec (making resin be thinned to desired thickness), solidifies 45 minutes under 230 DEG C of conditions.
(C) by the polyimide of melting, by the automatic double surface gluer spin coating of litho machine, the pre-rotating speed of gluing is 400rpm/10sec, and main rotating speed is 1100rpm/30sec.After coating, under 120 DEG C of conditions predrying 130 seconds.Then be cured (i=365nm, g=408nm, h=436nm) under ultraviolet light conditions, the irradiation transfer rate of ultra-violet curing is 1.6m/min, and the irradiation time of ultra-violet curing is 4 seconds.Finally dry 50 minutes under 250 DEG C of conditions, obtain intermediate.
(D) described intermediate is immersed in pH value be 1 nitric acid and phosphoric acid mix acid liquor in, soak 25 minutes, remove Cu film, obtain film material.
100 blocks of film materials method described in embodiment 1 prepared carry out photolithographic patterning development, and coming off of graphene film does not appear in the film material of 95%.
Embodiment 3
(A) reference literature YuQK, JaureguiLA, WuW, etal.Controlandcharacterizationofindividualgrainsandgrai nboundariesingraphenegrownbychemicalvapourdeposition.Nat Mater, 2011, the vapour deposition process that 10:443 – 449 records, is deposited on Graphene on Cu film.
By Graphene, amylalcohol and gold chloride under the phosphoric acid buffer liquid system of pH=9, under ambient temperature, react more than 30min, under agitation, adopt the electro-deposition of cyclic voltammetry one step to prepare compound substance, obtain the Graphene with carboxyl.
(B) by the teflon of melting, be spin-coated on the graphene film with hydroxyl by the automatic double surface gluer of litho machine, gluing transfers Spincoatnig to: pre-rotating speed (making resin uniform spreading) 500rpm/5sec, main rotating speed 1000rpm/15sec (making resin be thinned to desired thickness), solidifies 50 minutes under 230 DEG C of conditions.
(C) by the polyimide of melting, by the automatic double surface gluer spin coating of litho machine, the pre-rotating speed of gluing is 450rpm/10sec, and main rotating speed is 1000rpm/30sec.After coating, under 120 DEG C of conditions predrying 140 seconds.Then be cured (i=365nm, g=408nm, h=436nm) under ultraviolet light conditions, the irradiation transfer rate of ultra-violet curing is 1.6m/min, and the irradiation time of ultra-violet curing is 8 seconds.Finally dry 60 minutes under 200 DEG C of conditions, obtain intermediate.
(D) described intermediate is immersed in pH value be 3 nitric acid and phosphoric acid mix acid liquor in, soak 30 minutes, remove Cu film, obtain film material.
100 blocks of film materials method described in embodiment 3 prepared carry out photolithographic patterning development, and coming off of graphene film does not appear in the film material of 95%.
Be the graphene film of substrate with polyimide by existing method preparation, the photolithographic patterning development of Progressive symmetric erythrokeratodermia, more than 85% all there is coming off of Graphene.
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. a graphene layer, comprises graphene film and the organic insulating film adhering to described graphene film one side surface;
Hydrogen bond can be formed between described graphene film and organic insulating film;
Described organic insulating film is tygon, polyvinylidene fluoride, teflon or acrylic type resin.
2. a film material, comprises polyimide substrate and graphene layer according to claim 1, and described polyimide substrate adheres to the organic insulating film in described graphene layer and is connected.
3. a preparation method for film material, comprises the following steps:
(A) adopt vapour deposition process to be deposited on by Graphene on Cu film or Ni film, through modification, obtain the graphene film with hydroxyl;
(B) described with the graphene film of hydroxyl applying one deck organic insulating film and solidifying;
(C) coating polyimide film on described organic insulating film, and carry out ultra-violet curing, obtain intermediate;
(D) described intermediate is immersed in acid solution, removes Cu film or Ni film, obtain film material;
Described organic insulating film is tygon, polyvinylidene fluoride, teflon or acrylic type resin.
4. preparation method according to claim 3, is characterized in that, in described step (A), the method for described modification is:
Graphene and alcohols and gold chloride are reacted, then through electro-deposition, obtains the graphene film with hydroxyl.
5. preparation method according to claim 4, is characterized in that, in described step (B), the pre-rotating speed of described coating is 300 ~ 500rpm/5 ~ 10sec, and main rotating speed is 600 ~ 1200rpm/15 ~ 30sec; The temperature of described solidification is 200 ~ 250 DEG C, and the time of described solidification is 30 ~ 60 minutes.
6. the preparation method according to claim 3 ~ 5 any one, is characterized in that, in described step (C), the pre-rotating speed of described coating is 300 ~ 500rpm/5 ~ 10sec, and main rotating speed is 600 ~ 1200rpm/15 ~ 30sec.
7. preparation method according to claim 6, is characterized in that, in described step (C), also comprises predrying after described coating, and predrying temperature is 90 ~ 120 DEG C, and the pre-dried time is 120 ~ 150 seconds.
8. preparation method according to claim 7, is characterized in that, in described step (C), the irradiation transfer rate of described ultra-violet curing is 0.8 ~ 1.6m/min, and the irradiation time of described ultra-violet curing is 2 ~ 8 seconds.
9. the preparation method according to claim 7 ~ 8 any one, is characterized in that, in described step (C), the bake out temperature after described ultra-violet curing is 200 ~ 250 DEG C, and drying time is 30 ~ 60min.
10. a flexible display device, is characterized in that, comprises the film material that described in film material according to claim 2 or claim 3 ~ 9 any one prepared by method.
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| CN105118382B (en) | 2019-04-09 |
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