CN104332390B - A kind of patterned Graphene preparation method, array base palte and display device - Google Patents
A kind of patterned Graphene preparation method, array base palte and display device Download PDFInfo
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- CN104332390B CN104332390B CN201410433335.2A CN201410433335A CN104332390B CN 104332390 B CN104332390 B CN 104332390B CN 201410433335 A CN201410433335 A CN 201410433335A CN 104332390 B CN104332390 B CN 104332390B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/322—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to modify their internal properties, e.g. to produce internal imperfections
Abstract
The embodiments of the invention provide a kind of patterned Graphene preparation method, array base palte and display device, belong to electrode material field, to solve the problem of sheet resistance is changed greatly during photoetching process fabricating patterned graphene.The patterned Graphene preparation method, including：It will be patterned into graphene and be placed in immersion in acid etching liquid, to reduce the sheet resistance of the patterned Graphene.The present invention is available in the method for photoetching process fabricating patterned graphene.
Description
Technical field
The present invention relates to electrode material field, more particularly to a kind of patterned Graphene preparation method, array base palte and
Display device.
Background technology
Graphene is a kind of by the tightly packed carbonaceous new material into bi-dimensional cellular shape structure of single layer of carbon atom.Theory hair
It is existing：Graphene has 200,000cm2/ Vs mobility, 100 times are higher by than silicon, and its electric conductivity can compare favourably with copper, light transmission
Rate is up to 97.7%, far above conductive film, while graphene has high flexibility, can be used as the replacement material of current material
Material, can also be applied to the material of time generation transistor and electrode member, therefore get most of the attention.
The existing method patterned to graphene is roughly divided into two kinds, and one kind is photoetching process, and another is laser
Direct write method.Compared to photoetching process, there is advantages below to graphene pattern by the way of laser direct-writing：Technique is simple, complete
Cheng Wuxu chemistry consumptive material and during being patterned due to being not introduced into other reagents so that mixing in graphene film layer
Miscellaneous group will not react and cause graphene sheet resistance to change, but this method make obtained patterned Graphene due to
Not enough become more meticulous and the production cycle be longer, production efficiency is far away from photoetching process, it is impossible to the inferior position produced in enormous quantities so that
Graphene can only be patterned using photoetching process at this stage.
But inventor has found in actual production, is used during being patterned using photoetching process to graphene
Developer solution, stripper graphene film sheet resistance that making can all obtained dramatically increase, prevent it from being satisfied with actual demand.Institute
So that how obtaining low sheet resistance of graphene thin film will be important topic that those skilled in the art are faced.
The content of the invention
The embodiments of the invention provide a kind of patterned Graphene preparation method, array base palte and display device, to solve
The problem of certainly sheet resistance is changed greatly during photoetching process fabricating patterned graphene.
To reach above-mentioned purpose, embodiments of the invention are adopted the following technical scheme that：
A kind of patterned Graphene preparation method, including：
It will be patterned into graphene and be placed in immersion in acid etching liquid, to reduce the side of the patterned Graphene after immersion
Resistance.
Optionally, the initial sheet resistance of sheet resistance≤graphene of the patterned Graphene after the immersion.
Optionally, the pH of the acid etching liquid is 1-3.
Optionally, the patterned Graphene is placed in acid etching liquid and soaked 100-140 seconds.
Optionally, the acid etching liquid includes heavy metal inorganic acids and one kind or many in nonmetallic inorganic acids
Kind.
Further, the heavy metal inorganic acids include the one or more in gold chloride and chloroplatinic acid.
Further, the nonmetallic inorganic acids includes the one or more in nitric acid, phosphoric acid and sulfuric acid.
Optionally, it is placed in the graphene that will be patterned into acid etching liquid before immersion, in addition to：
The substrate of glass for having graphene to docile carries out photoetching process, to be formed with photoresist figure on the glass substrate
Case；
Dry etching is carried out to the substrate of glass for being formed with photoetching agent pattern, glue pattern covers are not photo-etched to remove
Graphene；
After dry etching is finished, the photoresist removed in substrate of glass is peeled off, to obtain the patterned Graphene.
Optionally, the graphene is bilayer graphene or three layer graphenes.
Optionally, the graphene is for doped graphene or undoped with graphene.
Optionally, before the glass substrate for having graphene to docile carries out photoetching process, still further comprise：
The graphene is transferred in polyethylene terephthalate film, then with high temperature gummed tape by its docile in glass
In glass substrate.
A kind of array base palte, including obtained patterned Graphene is made by above-mentioned technical proposal.A kind of display device, bag
The array base palte provided by above-mentioned technical proposal is provided.
, should the embodiments of the invention provide a kind of preparation method of patterned Graphene, array base palte and display device
Method is soaked using acid etching liquid to patterned Graphene, is made in the acid ion and graphene film layer in etching liquid
Doped ions chemically react, with graphene film layer surface again doped with electrically active metal ion group so that
Making the electro-chemical activity of graphene film layer surface becomes active, and this can not only significantly reduce the side of photolithographic patterning rear graphene
Resistance, can also obtain the patterned Graphene become more meticulous, be that the volume production of graphene lays the foundation.
Brief description of the drawings
The flow chart for the patterned Graphene preparation method that Fig. 1 is provided by the embodiment of the present invention；
Fig. 2 is that existing laser straight literary style is entered from method provided by the present invention with regard to identical graphene raw material under different line widths
Comparison diagram obtained by row patterning.
Embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below in conjunction with accompanying drawing, it is clear that retouched
The embodiment stated is only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, sheet
The every other embodiment that field those of ordinary skill is obtained under the premise of creative work is not made, belongs to the present invention
The scope of protection.
Patterned Graphene preparation method provided in an embodiment of the present invention, array base palte and display device are carried out below
It is described in detail.
The embodiments of the invention provide a kind of patterned Graphene preparation method, including：It will be patterned into graphene and be placed in acid
Property etching liquid in soak, with reduce immersion after the patterned Graphene sheet resistance.
Single-layer graphene is larger due to sheet resistance, it is impossible to be satisfied with actual demand, it is usually the case that acquired stone
Black alkene is generally the graphene of redeposited second layer or more layer after single-layer graphene doping.In the method, with double-layer graphite
Illustrated exemplified by alkene, but it is understood that, graphene used in the present invention is not limited to bilayer, can also be many
Layer, will be described in detail in the examples below for the contents of the section by such as three layers.
Graphene used in the present embodiment is doped graphene, and it is in photoetching process patterning process successively through overexposure, aobvious
After the steps such as shadow, etching, stripping, because the effect of developer solution, stripper causes the sheet resistance of graphene film layer increased, cause
The patterned Graphene sheet resistance obtained by usual photolithography is larger, it is impossible to be used in actual production.So, after the above procedure
Continue with acid etching liquid to soak patterned Graphene, by the acid ion in etching liquid and graphene film layer
Doped ions the chemical reaction such as occur complexing, exchange, graphene film layer surface again doped with electrically active metal from
Subbase group so that the electro-chemical activity of graphene film layer surface becomes active, so as to reduce the side of photolithographic patterning graphene
Resistance.
The embodiments of the invention provide a kind of patterned Graphene preparation method, this method is using acid etching liquid to pattern
Graphite alkene soaks, and the acid ion in etching liquid is chemically reacted with the Doped ions in graphene film layer, in graphite
Alkene film surface is again doped with electrically active metal ion group so that the electro-chemical activity of graphene film layer surface becomes
Vivaciously, this can not only significantly reduce the sheet resistance of photolithographic patterning rear graphene, can also obtain the patterned Graphene become more meticulous,
Laid the foundation for the volume production of graphene.
In another embodiment of the invention, sheet resistance≤graphene of the patterned Graphene after the immersion is first
Beginning sheet resistance.Wherein, the initial sheet resistance of graphene for raw material graphene original sheet resistance (refer in the present embodiment used in not
Begin participating in the sheet resistance of the bilayer graphene of reaction).Obtained pattern graphite can will be made by the immersion of acid etching liquid
The sheet resistance of alkene returns to original sheet resistance or smaller than it of graphene, so that the conduction of the patterned Graphene preferably improved
Property.
In another embodiment of the invention, the pH of the acid etching liquid is 1-3.In the present embodiment, soaking step
Used in etching liquid integrally in acidity, the acidity should be generally maintained as highly acid, about 1-3 or so, in actual production,
Although in immersion, etching liquid reacts with graphene can constantly reduce the pH of etching liquid, should not depart from above-mentioned pH scopes,
The acid ion in etching liquid is influenceed to be reacted with the Doped ions in graphene film layer to avoid acid too late, so that shadow
Ring the sheet resistance of the patterned Graphene obtained after immersion.
In another embodiment of the present invention, the patterned Graphene is placed in acid etching liquid and soaks 100-140
Second.In the present embodiment, 100-140 seconds can be anti-with patterned Graphene to patterned Graphene immersion beneficial to acid etching liquid
Should be complete, in this process, due to being doped with metal ion group into patterned Graphene, equivalent to patterned Graphene
Carry out secondary doping so that the electro-chemical activity of graphene film layer surface becomes active, so as to reduce photolithographic patterning graphite
The sheet resistance of alkene.Meanwhile, substantially needed in actual production, in soaking step by 4-5 acid infusion unit, and pass through above-mentioned acid
Property etch unit be probably also required to 100-140 seconds, further, preferably soak 140 seconds, this also just with patterned Graphene and acid
Property the etching liquid reaction completely required time it is unanimous on the whole, so as to further be laid the foundation for the volume production of graphene.
In further embodiment of the present invention, the acid etching liquid may include heavy metal inorganic acids and nonmetallic nothing
One or more in machine acids.A variety of acidic materials can be included in acid etching liquid, to be provided well for soaking step
Adulterate environment, further to be doped offer advantage again after photolithographic patterning.In one embodiment of this invention, institute
Stating heavy metal inorganic acids may include the one or more in gold chloride and chloroplatinic acid；In one embodiment of this invention, it is described
Nonmetallic inorganic acids may include the one or more in nitric acid, phosphoric acid and sulfuric acid；Further, being preferable to carry out in the present invention
In example, the nonmetallic inorganic acid is nitric acid and the mixed liquor of phosphoric acid, so as to preferably be and patterned Graphene
Learn reaction and advantage is provided.It is understood that on being not limited in about the acidic materials included in acid etching liquid
Cited species is stated, other acidic materials known to those skilled in the art are can also be, above-mentioned cited species is only
Wherein more commonly use and important species.
In another embodiment of the invention, as shown in figure 1, being placed in the graphene that will be patterned into acid etching liquid
Before immersion, it may also include：The substrate of glass for having graphene to docile carries out photoetching process, to be formed on the glass substrate
There is photoetching agent pattern；Dry etching is carried out to the substrate of glass for being formed with photoetching agent pattern, glue figure is not photo-etched to remove
The graphene of case covering；After dry etching is finished, the photoresist removed in substrate of glass is peeled off, to obtain the pattern fossil
Black alkene.In further embodiment of the present invention, before the glass substrate for having graphene to docile carries out photoetching process,
It may also include：The graphene is transferred in polyethylene terephthalate film (PET), then pasted with high temperature gummed tape
Clothes are on the glass substrate.It is understood that being this area skill about the method patterned using photoetching process to graphene
The conventional method that art personnel are understood, is no longer described in detail herein, certainly, and those skilled in the art can also enter to above-mentioned usual photolithography
Row modification, carries out patterning to graphene using the photoetching process obtained by modification and is intended to be included within the scope of the present invention.
In another embodiment of the invention, the graphene can be bilayer graphene or three layer graphenes.Need exist for
Illustrate, the sheet resistance of single-layer graphene is larger, be unfavorable for actual demand, and multilayer (more than three layers) graphene due into
Occurring that technique is bad during film, so in embodiments of the present invention use bilayer graphene or three layer graphenes more more.Wherein, by
Actual demand can be more met in the sheet resistance of bilayer graphene, and film forming procedure is relatively simple compared to three layer graphene processes, so
Bilayer graphene is preferably used in the present embodiment.
In further embodiment of the present invention, the graphene is for doped graphene or undoped with graphene.In this reality
The graphene applied used in example is doped graphene, because single-layer graphene sheet resistance is larger, in order to reduce its sheet resistance, so obtaining
Once adulterated more than the graphene obtained.But need exist for stressing, in embodiments of the present invention, the graphite
Alkene can also be that undoped with graphene, it is longer that this is primarily due to graphene cycle of being adulterated after film forming, to straight undoped with graphene
Tap into row it is photolithographic patterning after be doped again with method provided by the present invention, the sheet resistance of graphene can not only be reduced,
The doping step after graphene film forming can be also reduced, film forming period is reduced, production cost is saved.
The embodiment of the present invention additionally provides a kind of array base palte, including is made by the preparation method that above-described embodiment is provided
Obtained patterned Graphene.Because the patterning of the patterned Graphene is fine, and after being soaked through acid etching liquid, sheet resistance
It is also obtained and significantly decreases, so when applying it in the array base palte that the embodiment of the present invention is provided, can be further
Effectively improve the performance of array base palte.
The embodiment of the present invention additionally provides a kind of display device, including the array base palte provided by above-described embodiment.
Include the array base palte for being provided with the patterned Graphene that the embodiment of the present invention is provided in the display device.Due to the pattern
The patterning of graphite alkene is fine, and after being soaked through acid etching liquid, sheet resistance, which is also obtained, to be significantly decreased, and is being applied
When in the display device provided to the embodiment of the present invention, the performance of display device can be further effectively improved.
Below in conjunction with specific embodiment, the invention will be further described, but the present invention is not limited to following examples.
First, graphene is transferred on PET film, then with high temperature gummed tape by its docile on the glass substrate；
Then, the graphene film layer that test docile is finished respectively is only carrying out developing process and only peeled off (strip)
Graphene film sheet resistance change after technique.
After this step, 200 Ω of graphene film layer sheet resistance change ＜/ is measured after developing process is only carried out, meets stone
Black alkene film sheet resistance qualitative change；Graphene film sheet resistance is measured after strip techniques are only carried out to change greatly, and is changed by 200 Ω/
For 1800 Ω/.
Thus analysis strip techniques are the principal element that graphene sheet resistance changes, wherein, strip liquid and graphene it is anti-
Answer mechanism as follows：
Strip liquid constituent is hydroxyethyl piperazine (a), butyl (b), N-METHYLFORMAMIDE (c), its chemistry
Structure is respectively：
Wherein, the aobvious alkalescence of hydroxyethyl piperazine, the aobvious neutrality of butyl, N-METHYLFORMAMIDE.Strip mixes liquid and integrally shown
Existing alkalescence.
Using strip liquid when being peeled off under conditions of 40 DEG C to doped graphene duplicature, its reaction mechanism is as follows:
Now, with electrically active graphene film complex reaction, hydroxyl and metal formation metal complex occur for strip liquid
Thing, and depart from graphene film so that the free charge of graphene membrane surface drastically reduces even up to saturation, electric property drop
Low, sheet resistance change greatly (graphene film sheet resistance increased dramatically to K Ω ranks), or even is changed into being similar to insulator performance.
Because the graphene film layer sheet resistance after obtained stripping is changed greatly, production requirement can not be satisfied with, so with
It is soaked under the conditions of proper temperature (room temperature) using acid etching liquid afterwards, in this step, acid etching liquid and stone
The reaction mechanism of black alkene film layer is as follows：
Now, with a large amount of acid ions in acid etching liquid the chemical reactions such as be complexed, exchange occur for graphene film layer, with
Adulterate electrically active metal ion group again in graphene membrane surface so that the electro-chemical activity of graphene membrane surface becomes
Vivaciously, the initial sheet resistance for finally making sheet resistance return to graphene film is even less than initial sheet resistance.It will randomly select below above-mentioned each
9 differences in processing step determine the sheet resistance of graphene film layer, wherein, sample 1 and sample 2 are the graphite for having neither part nor lot in reaction
Alkene, specific test data is shown in Table 1：
Table 1 chooses the sheet resistance value for the graphene film layer that 9 differences are determined in each processing step
Can analyze and draw from test result, it is photolithographic patterning during developer solution, stripper can all increase graphene film
Sheet resistance, and during wet etching after patterning, because graphene film layer and acid etching liquid react, make pattern
The sheet resistance of graphite alkene is effectively reduced, i.e., the initial sheet resistance of graphene is 330.5 Ω/ in above table, and in wet etching
The sheet resistance of the patterned Graphene obtained afterwards is 273.6 Ω/, and the sheet resistance not only returns to initial sheet resistance, even lower.Enter one
Step, it will thus provide be applied to photolithographic method (b) with regard to identical graphite with provided by the present invention by existing laser straight literary style (a)
In different line widths, (wherein, laser straight literary style at 20 μm, 30 μm, 100 μm and provided by the present invention is applied to alkene raw material successively
Photolithographic method is at 5 μm) under patterned obtained by comparison diagram (referring to Fig. 2), can more clearly be found out by Fig. 2,
More fine pattern can be obtained under narrower line width by method provided by the present invention.
Obviously, above-described embodiment is only intended to clearly illustrate example, and the not restriction to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change thus extended out or
Change the protection domain still in the invention.
Claims (11)
1. a kind of patterned Graphene preparation method, it is characterised in that including：
Graphene is transferred in polyethylene terephthalate film, then with high temperature gummed tape by its docile in substrate of glass
On；
The substrate of glass for having graphene to docile carries out photoetching process, to be formed with photoetching agent pattern on the glass substrate；
Dry etching is carried out to the substrate of glass for being formed with photoetching agent pattern, to remove the stone for not being photo-etched glue pattern covers
Black alkene；
After dry etching is finished, the photoresist removed in substrate of glass is peeled off, to obtain patterned Graphene；
The patterned Graphene is placed in acid etching liquid and soaked, to reduce the side of the patterned Graphene after immersion
Hinder and obtain the patterned Graphene become more meticulous.
2. according to the method described in claim 1, it is characterised in that the sheet resistance of the patterned Graphene after the immersion≤
The initial sheet resistance of graphene.
3. according to the method described in claim 1, it is characterised in that the pH of the acid etching liquid is 1-3.
4. according to the method described in claim 1, it is characterised in that the patterned Graphene is placed in acid etching liquid and soaked
Bubble 100-140 seconds.
5. according to the method described in claim 1, it is characterised in that the acid etching liquid includes heavy metal inorganic acids and non-
One or more in metal inorganic acids.
6. method according to claim 5, it is characterised in that the heavy metal inorganic acids include gold chloride and chloroplatinic acid
In one or more.
7. method according to claim 5, it is characterised in that the nonmetallic inorganic acids includes nitric acid, phosphoric acid and sulphur
One or more in acid.
8. according to the method described in claim 1, it is characterised in that the graphene is bilayer graphene or three layer graphenes.
9. according to the method described in claim 1, it is characterised in that the graphene is for doped graphene or undoped with graphite
Alkene.
10. a kind of array base palte, it is characterised in that make obtained pattern including such as any one of claim 1-9 methods describeds
Graphite alkene.
11. a kind of display device, it is characterised in that including array base palte as claimed in claim 10.
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| CN104934551B (en) * | 2015-05-14 | 2017-07-28 | 京东方科技集团股份有限公司 | A kind of flexible electrode layer and preparation method thereof, display base plate, display device |
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| CN102180463A (en) * | 2011-02-21 | 2011-09-14 | 电子科技大学 | Method for reducing sheet resistance of graphene thin film |
| CN102435647A (en) * | 2011-10-24 | 2012-05-02 | 北京大学 | Method for detecting heavy metal by utilizing molecular device based on graphene electrode |
| CN102655146A (en) * | 2012-02-27 | 2012-09-05 | 京东方科技集团股份有限公司 | Array substrate, array substrate preparation method and display device |
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