CN106128947B - A kind of lithographic method of multi-layer graphene - Google Patents
A kind of lithographic method of multi-layer graphene Download PDFInfo
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- CN106128947B CN106128947B CN201610515119.1A CN201610515119A CN106128947B CN 106128947 B CN106128947 B CN 106128947B CN 201610515119 A CN201610515119 A CN 201610515119A CN 106128947 B CN106128947 B CN 106128947B
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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
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30604—Chemical etching
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
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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
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/3065—Plasma etching; Reactive-ion etching
Abstract
The invention discloses a kind of lithographic methods of multi-layer graphene, comprising: then A, the external coating photoresist in multi-layer graphene are exposed processing to photoresist, are then cleaned using developer solution to photoresist；B, according to the difference of etching depth, in the etching buffer of the corresponding position brushing different-thickness of photoresist；C, multi-layer graphene is put into reaction chamber, chamber vacuumizes；Ethane is injected into reaction chamber, then reaction chamber is heated, and opens radio-frequency power supply, and first time etching is carried out to the surface of multi-layer graphene；D, the multi-layer graphene by etching for the first time is cleaned with deionized water, then natural air drying；E, multi-layer graphene is immersed in acid etching liquid, carries out second and etches；F, multi-layer graphene photoresist remained on surface is purged using stripper.The present invention can solve the deficiencies in the prior art, realize the accurate control for etching process.
Description
Technical field
The present invention relates to grapheme material technical field, especially a kind of lithographic method of multi-layer graphene.
Background technique
Graphene is one of physics and the primary study object in materialogy field in recent years.It is that stringent two dimension is brilliant
Body, it is being bonded by sp2 hydbridized carbon atoms and have hexagonal lattice honeycomb two-dimensional structure.Graphene has very strong toughness, breaks
200 times more taller than best steel of resistance to spalling.Graphene most potential application at present is the substitute as silicon, and manufacture is super
Micro-transistors, for producing following supercomputer.Replace silicon with graphene, the speed of service of computer processor will
Fast hundreds times.In order to which the semiconductor circuit for replacing silicon wafer is made, need to perform etching processing on the surface of graphene.Chinese invention
101996853 B of patent CN discloses the method that a kind of pair of graphite or graphene carry out anisotropic etching, and realizing size can
It controls and there is the processing of the graphene at atomically flating edge to cut out and pattern.But this method be unable to accurately control it is more
The longitudinal etching depth and lateral etching width of layer graphene, produce influence for the industrial application of graphene.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of lithographic methods of multi-layer graphene, are able to solve the prior art
Deficiency, realize the accurate control for etching process.
In order to solve the above technical problems, the technical solution used in the present invention is as follows.
A kind of lithographic method of multi-layer graphene, comprising the following steps:
A, in the external coating photoresist of multi-layer graphene, processing then is exposed to photoresist, then using development
Liquid cleans photoresist；
B, according to the difference of etching depth, in the etching buffer of the corresponding position brushing different-thickness of photoresist；
C, multi-layer graphene is put into reaction chamber, chamber vacuumizes；Ethane is injected into reaction chamber, then to anti-
It answers chamber to be heated, and opens radio-frequency power supply, first time etching is carried out to the surface of multi-layer graphene；Reaction chamber room pressure
It is maintained at 0.1~0.2Torr, reaction temperature is controlled at 170~245 DEG C, and the flow of ethane is maintained at 100~150sccm, radio frequency
Power is maintained at 600~800W；
D, the multi-layer graphene by etching for the first time is cleaned with deionized water, then natural air drying；
E, multi-layer graphene is immersed in acid etching liquid, carries out second and etches；The temperature control of acid etching liquid exists
50~65 DEG C；
F, multi-layer graphene photoresist remained on surface is purged using stripper.
Preferably, photoresist includes the component of following mass fraction,
10~15 parts of diazonium naphthoquinone sulphonate, 5~7 parts of nitrobenzyl sulfonate esters, 20~25 parts of 2- methoxyl group cyanogen
Benzene, 10~15 parts of n-ethylethylenediamine, 10~20 parts of decahydronaphthalene-beta naphthal, 3~5 parts of polybutylene terephthalate
Ester, 4~6 parts of polyvinyl alcohol resin, 7~10 parts of 1,8- naphthalic anhydride and 2~3 parts of 4- chlorphenyl diethyl phosphate.
Preferably, stripper includes following component,
3- amino -1- the propyl alcohol of 6~10wt%, the 1,3-Dimethyl-2-imidazolidinone of 8~12wt%, 3~7wt%
Alkyl carbamate, the triethylene glycol monobutyl base ether of 5~10wt%, the 4- methoxybenzyl isocyanates of 15~20wt%, 6~
The 3 of 8wt%, the acetone of 5,5- tri-methyl hexanoic acids, 5~10wt%, surplus are water.
Preferably, etching buffer includes the component of following mass fraction,
3~5 parts of 4- amino-n-butyl alcohol, 7~12 parts of pentaerythrite, 1~2 part of 3,5- dinitro-methyl benzoate,
5~10 parts of dibenzyl sulfoxide, 5~7 parts of 3- cyclohexene -1- carboxylate methyl ester and 15~20 parts of dimethyl terephthalate (DMT).
Preferably, acid etching liquid includes following component,
The hydrofluoric acid of 2~3wt%, the phosphoric acid of 12~15wt%, the ammonium persulfate of 4~6wt%, 1.2~2wt% N- ammonia
Ehtylethanolamine, the ethylenediamine tetra-acetic acid of 2.5~5wt%, the Diisopropyl malonate of 6~10wt%, 4~5wt% 4- bromine
The isopropanol of Tolueneisothiocyanate, 20~25wt% between methyl oxinane, 5~10wt%, surplus are water.
Preferably, selectively brushing and protecting on by the multi-layer graphene of etching for the first time before carrying out step E
Coating is protected, protective coating includes the component of following mass fraction,
8~10 parts of 5- amino isophthalic acid, 12~15 parts of methyl ethyl carbonate, 6~8 parts of tripropylene glycol list first
The chloro- 2- nitrophenol of ether, 3~7 parts of 2,3,4- trimethoxy-benzonitrile, 2~5 parts of 4-, 15~18 parts of 3,3,5- tri-
Methyl cyclohexanol, 10~15 parts of N, N- dibenzyl hydroxylamine, 5~10 parts of ten dihydroxystearic acids, 10~20 parts of silicone oil.
Brought beneficial effect is by adopting the above technical scheme: the present invention by the thickness of etching buffer and it is equal from
Cooperation between the control of daughter realizes longitudinal etching depth using etching buffer for the buffer function of etching process
Accurate control.After longitudinal etching, further carved by using gap of the acid etching liquid to first time etching
Erosion.Since first time etches the exposed area that the exposed area of the gap formed horizontally is far longer than gap bottom, pass through
Adjustment to acid etching liquid component, weakens the reaction rate of etching liquid and etching surface, so as to realize lateral etching
While, reduce the influence that longitudinal etching depth is formed by for first time etching to the greatest extent.
In addition, photoresist used in the present invention, which passes through, is added 1,8- naphthalic anhydride and 4- chlorphenyl diethyl phosphate,
It can be in being finally peeled away technique, with 3 in stripper, 5,5- tri-methyl hexanoic acids generate quickly dissolution reaction, so as to
So that stripper is formed the decomposition release effect of speed to photoresist inside, reduces the residual quantity of photoresist.
Protective coating can inhibit corrasion of the acid etching liquid for graphene.Pass through the protection of brushing different-thickness
Coating, may be implemented the etching effect of the different depth of etching surface, so that it is a variety of to form ladder-like, matte shape, Openworks shape etc.
Etched shape.
Specific embodiment
Embodiment 1
A kind of lithographic method of multi-layer graphene, comprising the following steps:
A, in the external coating photoresist of multi-layer graphene, processing then is exposed to photoresist, then using development
Liquid cleans photoresist；
B, entire multi-layer graphene surface is equally divided into two parts, the thickness that etching buffer is brushed by first part is kept
120~150nm is maintained in the thickness of 70~100nm, second part brushing etching buffer；
C, multi-layer graphene is put into reaction chamber, chamber vacuumizes；Ethane is injected into reaction chamber, then to anti-
It answers chamber to be heated, and opens radio-frequency power supply, first time etching is carried out to the surface of multi-layer graphene；Reaction chamber room pressure
It is maintained at 0.12Torr, reaction temperature is controlled at 180 DEG C, and the flow of ethane is maintained at 125sccm, and radio-frequency power supply power is maintained at
600W；Reaction time is 4min；
D, the multi-layer graphene by etching for the first time is cleaned with deionized water, then natural air drying；
E, multi-layer graphene is immersed in acid etching liquid, carries out second and etches；The temperature control of acid etching liquid exists
55℃；Reaction time controls in 80s；
F, multi-layer graphene photoresist remained on surface is purged using stripper.
Photoresist includes the component of following mass fraction,
12 parts of diazonium naphthoquinone sulphonate, 6 parts of nitrobenzyl sulfonate esters, 24 parts of 2- methoxyl group benzonitrile, 10 parts of N-
Ethylethylenediamine, 15 parts of decahydronaphthalene-beta naphthal, 5 parts of polybutylene terephthalate (PBT), 6 parts of polyvinyl alcohol resin, 8
The 1,8- naphthalic anhydride and 3 parts of 4- chlorphenyl diethyl phosphate of part.
Stripper includes following component,
3- amino -1- the propyl alcohol of 8.7wt%, the 1,3-Dimethyl-2-imidazolidinone of 11wt%, 5wt% carbamic acid
Arrcostab, the triethylene glycol monobutyl base ether of 8wt%, the 4- methoxybenzyl isocyanates of 16wt%, 7wt% 3,5,5- trimethyl
The acetone of caproic acid, 6wt%, surplus are water.
Etching buffer includes the component of following mass fraction,
4 parts of 4- amino-n-butyl alcohol, 10 parts of pentaerythrite, 1 part of 3,5- dinitro-methyl benzoate, 6 parts of dibenzyl
Base sulfoxide, 6 parts of 3- cyclohexene -1- carboxylate methyl ester and 18 parts of dimethyl terephthalate (DMT).
Acid etching liquid includes following component,
The hydrofluoric acid of 2.4wt%, the phosphoric acid of 14wt%, the ammonium persulfate of 5wt%, 1.8wt% N- aminoethyl ethanolamine,
Between the ethylenediamine tetra-acetic acid of 4.5wt%, the Diisopropyl malonate of 9wt%, the 4- bromomethyl oxinane of 5wt%, 9wt%
The isopropanol of Tolueneisothiocyanate, 21wt%, surplus are water.
Before carrying out step E, the brushing protective coating on by the multi-layer graphene of etching for the first time, described in step B
First part brush with a thickness of 30~50nm, with a thickness of 70~100nm, protective coating includes following quality for second part brushing
The component of number,
9 parts of 5- amino isophthalic acid, 13 parts of methyl ethyl carbonate, 7 parts of Tripropylene glycol monomethyl Ether, the 2,3 of 4 parts,
The chloro- 2- nitrophenol of 4- trimethoxy-benzonitrile, 3 parts of 4-, 16 parts of 3,3,5- cyclonol, 11 parts of N, N- bis-
Benzyl hydroxylamine, 6 parts of ten dihydroxystearic acids, 15 parts of silicone oil.
Observation is amplified to the multi-layer graphene sample that etching finishes, average longitudinal depth of first part is 78nm,
Average longitudinal depth of second part is 51nm.The lateral etching face of first part is in apparent matte shape, the cross of second part
It is in apparent Openworks shape to etched surface.
Above-mentioned technical process is repeated using the PR1-2000A photoresist of U.S. Futurre, finally for finished surface photoetching
The residual quantity of glue is measured, as a result as follows:
| Test group | Residual quantity (mg) |
| Photoresist in embodiment 1 | 0.0012 |
| PR1-2000A photoresist | 0.0070 |
Embodiment 2
The present embodiment improves on the basis of embodiment 1, mainly improves to the etching technics of step C.
In step C,
Multi-layer graphene is put into reaction chamber, chamber vacuumizes；Ethane is injected into reaction chamber, then to reaction
Chamber is heated, and opens radio-frequency power supply, carries out first time etching to the surface of multi-layer graphene；Reaction chamber room pressure is protected
It holds in 0.15Torr, reaction temperature is controlled at 190 DEG C, and the flow of ethane is maintained at 115sccm, and radio-frequency power supply power is maintained at
650W；Reaction time is 45s；Then the flow of ethane is improved to 150sccm, add flow be 20sccm helium and
Flow is the nitrogen of 15sccm, and reaction chamber room pressure is increased in 0.18Torr, and reaction temperature is controlled at 210 DEG C, reaction
Between be 110s.
By the way that etching process is decomposed into two stages, quickly dividing for etching buffer after being ionized using mixed gas
Solution effect, accelerates the speed of etching, and do not find obvious shortcoming in etching surface.
It is magnified into crossing, average longitudinal depth of multi-layer graphene first part is 73nm, and the average of second part is indulged
It is 58nm to depth.
The power of step C in embodiment 1 is enlarged to 800W, ethane flow is enlarged to 140sccm, by 1min's
Etching amplifies observation to etching surface, and the defects of every etching groove number is 3~5.Thus it demonstrates in embodiment 1
Etching technics is not suitable for quickly etching.
Embodiment 3
The present embodiment improves on the basis of embodiment 1.Mainly the ingredient of protective coating is improved.
Protective coating includes the component of following mass fraction,
9 parts of 5- amino isophthalic acid, 13 parts of methyl ethyl carbonate, 7 parts of Tripropylene glycol monomethyl Ether, the 2,3 of 4 parts,
The chloro- 2- nitrophenol of 4- trimethoxy-benzonitrile, 3 parts of 4-, 16 parts of 3,3,5- cyclonol, 11 parts of N, N- bis-
Benzyl hydroxylamine, 6 parts of ten dihydroxystearic acids, 15 parts of silicone oil and 9 parts of 3- amino-4-methoxyacetanilide.
Multi-layer graphene external coating protective coating with a thickness of 10~15nm, then carry out step E's and step F
Technical process.Flannelette made of this technique and manufactured flannelette in embodiment 1 are compared, as a result as follows:
| Test group | The uniformity (%) |
| Embodiment 1 | 65.3 |
| Embodiment 3 | 81.5 |
It, can be with the 4- bromomethyl oxinane in acid etching liquid by the way that 3- amino-4-methoxyacetanilide is added
Form a complex compound with Tolueneisothiocyanate, in the thinner thickness of protective coating, can be improved protective coating fall off it is equal
Evenness, thus be acid etching liquid for etching surface the corrasion uniformity improve, improve the uniformity of flannelette.
Foregoing description is only proposed as the enforceable technical solution of the present invention, not as to the single of its technical solution itself
Restrictive condition.
Claims (6)
1. a kind of lithographic method of multi-layer graphene, it is characterised in that the following steps are included:
A, in the external coating photoresist of multi-layer graphene, processing then is exposed to photoresist, then uses developer solution pair
Photoresist is cleaned；
B, entire multi-layer graphene surface is equally divided into two parts, the thickness that etching buffer is brushed by first part is maintained at 70
The thickness of~100nm, second part brushing etching buffer are maintained at 120~150nm；
C, multi-layer graphene is put into reaction chamber, chamber vacuumizes；Ethane is injected into reaction chamber, then to reaction chamber
Room is heated, and opens radio-frequency power supply, carries out first time etching to the surface of multi-layer graphene；Reaction chamber room pressure is kept
In 0.1~0.2Torr, reaction temperature is controlled at 170~245 DEG C, and the flow of ethane is maintained at 100~150sccm, radio-frequency power supply
Power is maintained at 600~800W；
D, the multi-layer graphene by etching for the first time is cleaned with deionized water, then natural air drying；
E, multi-layer graphene is immersed in acid etching liquid, carries out second and etches；The temperature control of acid etching liquid 50~
65℃；
F, multi-layer graphene photoresist remained on surface is purged using stripper.
2. the lithographic method of multi-layer graphene according to claim 1, it is characterised in that: photoresist includes following mass parts
Several components,
10~15 parts of diazonium naphthoquinone sulphonate, 5~7 parts of nitrobenzyl sulfonate esters, 20~25 parts of 2- methoxyl group benzonitrile, 10
~15 parts of n-ethylethylenediamine, 10~20 parts of decahydronaphthalene-beta naphthal, 3~5 parts of polybutylene terephthalate (PBT), 4~
6 parts of polyvinyl alcohol resin, 7~10 parts of 1,8- naphthalic anhydride and 2~3 parts of 4- chlorphenyl diethyl phosphate.
3. the lithographic method of multi-layer graphene according to claim 2, it is characterised in that: stripper includes following component,
3- amino -1- the propyl alcohol of 6~10wt%, the 1,3-Dimethyl-2-imidazolidinone of 8~12wt%, 3~7wt% amino
Alkyl formate, the triethylene glycol monobutyl base ether of 5~10wt%, the 4- methoxybenzyl isocyanates of 15~20wt%, 6~
The 3 of 8wt%, the acetone of 5,5- tri-methyl hexanoic acids, 5~10wt%, surplus are water.
4. the lithographic method of multi-layer graphene according to claim 1, it is characterised in that: etching buffer includes following matter
The component of number is measured,
3~5 parts of 4- amino-n-butyl alcohol, 7~12 parts of pentaerythrite, 1~2 part of 3,5- dinitro-methyl benzoate, 5~
10 parts of dibenzyl sulfoxide, 5~7 parts of 3- cyclohexene -1- carboxylate methyl ester and 15~20 parts of dimethyl terephthalate (DMT).
5. the lithographic method of multi-layer graphene according to claim 1, it is characterised in that: acid etching liquid includes with the following group
Part,
The hydrofluoric acid of 2~3wt%, the phosphoric acid of 12~15wt%, the ammonium persulfate of 4~6wt%, 1.2~2wt% N- aminoethyl
Ethanol amine, the ethylenediamine tetra-acetic acid of 2.5~5wt%, the Diisopropyl malonate of 6~10wt%, 4~5wt% 4- bromomethyl
The isopropanol of Tolueneisothiocyanate, 20~25wt% between oxinane, 5~10wt%, surplus are water.
6. the lithographic method of multi-layer graphene according to claim 5, it is characterised in that: before carrying out step E, passing through
Cross for the first time etching multi-layer graphene on selectively brushing protective coating, protective coating include the group of following mass fraction
Part,
8~10 parts of 5- amino isophthalic acid, 12~15 parts of methyl ethyl carbonate, 6~8 parts of Tripropylene glycol monomethyl Ether, 3~
The chloro- 2- nitrophenol of 7 parts of 2,3,4- trimethoxy-benzonitrile, 2~5 parts of 4-, 15~18 parts of 3,3,5- front three basic ring
Hexanol, 10~15 parts of N, N- dibenzyl hydroxylamine, 5~10 parts of ten dihydroxystearic acids, 10~20 parts of silicone oil.
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| CN1870235A (en) * | 2005-05-27 | 2006-11-29 | 三星Sdi株式会社 | Organic tft, method of manufacturing the same and flat panel display device having the same |
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| CN102701144A (en) * | 2012-06-25 | 2012-10-03 | 北京大学 | Method for etching multilayer graphene |
| CN102931055A (en) * | 2012-10-10 | 2013-02-13 | 中国科学院微电子研究所 | Multi-layer graphene thinning method |
| US20140206192A1 (en) * | 2011-07-22 | 2014-07-24 | Research & Business Foundation Sungkyunkwan University | Method for etching atomic layer of graphine |
| WO2015088478A1 (en) * | 2013-12-09 | 2015-06-18 | Empire Technology Development Llc | Graphene etching methods, systems, and composites |
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|---|---|---|---|---|
| CN1870235A (en) * | 2005-05-27 | 2006-11-29 | 三星Sdi株式会社 | Organic tft, method of manufacturing the same and flat panel display device having the same |
| CN101728277A (en) * | 2008-10-24 | 2010-06-09 | 株式会社半导体能源研究所 | Method for manufacturing semiconductor device |
| US20140206192A1 (en) * | 2011-07-22 | 2014-07-24 | Research & Business Foundation Sungkyunkwan University | Method for etching atomic layer of graphine |
| CN102701144A (en) * | 2012-06-25 | 2012-10-03 | 北京大学 | Method for etching multilayer graphene |
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