CN105629682A - Method for removing photoresist from carbon-based thin film surface, and application - Google Patents
Method for removing photoresist from carbon-based thin film surface, and application Download PDFInfo
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- CN105629682A CN105629682A CN201610111722.3A CN201610111722A CN105629682A CN 105629682 A CN105629682 A CN 105629682A CN 201610111722 A CN201610111722 A CN 201610111722A CN 105629682 A CN105629682 A CN 105629682A
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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
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/42—Stripping or agents therefor
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Abstract
The invention discloses a method for removing photoresist from a carbon-based thin film surface, and an application. According to the method, a thin film is irradiated or scanned by a laser beam with relatively high energy; under the irradiation of the laser beam, the laser beam and the photoresist on the surface of a carbon-based material thin film sample are subjected to interaction to enable C-H, C-C bonds in the photoresist molecules to be ruptured to form small molecules and to be endowed with relatively high energy; therefore, the photoresist molecules are subjected to spluttering and transverse movement to break way from the original positions; and meanwhile, the sample surface generates heat due to laser bombardment so as to enable the photoresist molecules to be agglomerated and evaporated. According to the method, the photoresist and other polymer residue on the surface of the carbon-based material thin film sample can be removed without destroying the lattice structures of the material; and in addition, the thin film sample intrinsic characteristics are obtained, so that the electrical property of a device is greatly improved.
Description
Technical field
The present invention proposes a kind of method removing carbon-base film photomask surface glue, can be used for removing the polymkeric substance on carbon-base film surface or the device architecture surface based on this material, in fields such as physics, materialogy, micro-nano electronics, there is application prospect.
Background technology
Carbon-base film comprises Graphene (individual layer, bilayer and multilayer) and graphite etc. Graphene is two-dimensional material the most popular at present, and (under room temperature, the mobility of electronics is 15000cm to have high electron mobility2��V-1��s-1) and thermal conductivity (5000W m-1��K-1)), there is pole high-specific surface area (about 2630cm2��g-1) and physical strength (130GPa). The performance of these excellences becomes the focus in the researchs such as high-speed electronic components, sensor, opto-electronic device. Meanwhile, Graphene has extremely good snappiness so that it is have bigger advantage in flexible electronic device. The research of novel graphite alkene electron device, has huge application prospect by making it in fields such as micro-nano electronics.
Graphene electronic device manufacturing processed to be used photoresist material (PMMA etc.), but, photoresist material and graphenic surface strong adhesion, traditional technology can not remove photoresist material completely, can form the residual of 1��2nm at graphenic surface. Photoresist material residual as scattering center, can strengthen Graphene carrier scattering, reduce its mean free path, significantly reduce graphene carrier mobility, and causes the uncontrollable p-type doping of Graphene. The way solving photoresist material residual at present is, high temperature (more than 100 DEG C) annealing under vacuum or hydrogen/argon gas atmosphere. But, annealing can cause Graphene defect to increase, and changes its electronic property, and Graphene may be made to be oxidized, and causes the doping of P type to increase the weight of.
Summary of the invention
The object of the invention is to propose a kind of method removing carbon-base film photomask surface glue.
The present invention realizes by following technical scheme:
Remove a method for carbon-base film photomask surface glue, comprise the following steps:
(1) the carbon-base film sample with residual photoresist material is chosen;
(2) sample is positioned over below the laser emitting mouth of opticmicroscope of Raman spectrum system (optical maser wavelength can select 514,532 or 633nm etc.). Adjustment film sample position is to, in field of microscope, regulating microscope focus, and focus on film sample surface.
(3) need, with low-yield laser focusing bundle alignment thin film sample, position of removing photoresist, now laser intensity should at below 3mW, to ensure that laser spot is very little, registration.
(4) with the laser beam irradiation of higher-energy or scanning film sample surface certain time, thus photoresist material residual is removed; Superlaser beam intensity is 10��40mW, and the time is within 5s to 10min scope.
The method that the present invention removes carbon-base film photomask surface glue can be applied to the preparation of grapheme transistor.
The technique effect of the present invention is as follows:
The present invention utilizes higher-energy laser beam irradiation or scanning film, when carbon-base film sample irradiates under the laser beam, can interact between laser beam and film sample photomask surface glue, make C-H, C-C bond rupture in photoresist material molecule, form small molecules and there is higher-energy, and make photoresist material molecule sputtering occur and laterally move, depart from home position. Meanwhile, laser bombardment causes sample surfaces to produce heat, makes photoresist material molecule occur to reunite and evaporation.
Method proposed by the invention local, in-situ treatment can need the position removing residual photoresist material, be specially adapted in graphene device to carry out local, original position remove the polymer residues such as photoresist material, other region can not be impacted.
The present invention can remove the polymer residues such as carbon-based material film sample photomask surface glue, and guarantees not destroy material lattice structure, obtains film sample intrinsic characteristic, device electric property is improved greatly; This technology can reduce the contact resistance of device and film sample, such as, before electrode evaporation, film sample needs the position of electrode evaporation do this and removes photoresist material process.
Accompanying drawing explanation
The process remaining photoresist material removed by the single-layer graphene film sample that Fig. 1 is mechanically peel through raman laser. Wherein scheming the AFM graphicerrors of (a) original graphite alkene sample surfaces shape looks, it is sensitive especially to the reflection on particle and border, observes graphenic surface totally smooth; Figure (b) sample surfaces revolve resist coating again acetone remove photoresist after surface topography AFM graphicerrors, it is seen that graphenic surface photoresist material residual is serious; The Raman spectrogram of same position before figure (c) graphite Raman laser removes photoresist and after removing photoresist, the ratio of 2D peak and G peak intensity is about 3/1, and there is no D peak, illustrate that this sample is flawless single-layer graphene, and laser removes photoresist process on Graphene crystalline structure without impact; Figure (d) laser remove photoresist after the AFM graphicerrors of graphenic surface shape looks, it can be seen that the clean non-lithography glue residual through the Graphene position of raman laser process, still remains photoresist material without the position of laser treatment.
Fig. 2 is the sign before and after mechanically peel multi-layer graphene sample raman laser removes photoresist. Wherein, scheme (a) sample surfaces revolve resist coating again acetone remove photoresist after surface topography AFM graphicerrors, it is seen that graphenic surface photoresist material residual is serious. Figure (b) is the graphenic surface shape looks AFM graphicerrors after raman laser removes photoresist material.
Fig. 3 is the sign that CVD Graphene sample raman laser removes photoresist.
Grapheme transistor raceway groove position is carried out raman laser to remove the sign before and after residual photoresist material process by Fig. 4. Wherein scheming (a) is after manufacturing device, the AFM graphicerrors of raceway groove position shape looks, it has been found that photoresist material residual is serious; Figure (b) is the surface topography AFM graphicerrors after raceway groove position raman laser removes photoresist, it is seen that the local residual glue of laser treatment is removed clean.
Fig. 5 is that device channel raman laser removes photoresist the comparison diagram of front and back transfer characteristic curve. Wherein scheming (a) is the device transfer characteristics before laser removes photoresist; Figure (b) is the device transfer characteristics after laser removes photoresist, and device mobility significantly improves after raman laser removes photoresist.
Fig. 6 is that below the reserved electrode of backgate device, graphenic surface laser removes photoresist the sign before and after process. Wherein scheme the AFM graphicerrors that (a) is reserved electrode position graphenic surface shape looks before laser removes photoresist; B () is the AFM graphicerrors after same position raman laser removes photoresist.
Fig. 7 is that backgate device electrode lower position raman laser removes photoresist and do not remove photoresist output characteristic curve comparison diagram, and 1,2 electrodes in figure do not do laser and remove photoresist process; 3,4 electrodes do raman laser and remove photoresist process.
Embodiment
Below by example, the present invention will be further described. It is noted that the object publicizing and implementing example is to help to understand further the present invention, but it will be appreciated by those skilled in the art that: in the spirit and scope not departing from the present invention and claims, various substitutions and modifications are all possible. Accordingly, it is intended that the present invention not be limited to the content disclosed in embodiment, the scope that the scope of protection of present invention defines with claim book is as the criterion.
Embodiment one: peel off single-layer graphene surface removal residual photoresist material
(1) preparation of grapheme material
Utilize mechanically peel method to prepare Graphene, select scotch tape, repeatedly peel off high orientation graphite flakes, and the Graphene on adhesive tape is transferred to target SiO2On/Si substrate, Si is low-resistance silicon, SiO2For thermal oxide growth, thickness is generally 300nm.
(2) sign of grapheme material
Utilizing opticmicroscope, observed shape looks and the color of Graphene by contrast difference, the thickness of preliminary judgement Graphene, roughly estimates the number of plies of Graphene. Raman spectrum is utilized to characterize the Graphene number of plies and quality further. The raman characteristic peak of Graphene has D peak, G peak and 2D peak. Peak according to 2D peak and G peak is by force than I2D/IGJudge the Graphene number of plies, and judge by force graphenic surface defect situation according to peak, D peak. Choose I2D/IG> 2, there is no the sample at obvious D peak, as individual layer and do not have defective Graphene sample simultaneously. Atomic force microscope (AtomicForceMicroscope, AFM) is utilized to characterize Graphene sample surfaces shape looks, it is determined that not remain the original graphite alkene surface topography of photoresist material.
(3) sample is carried out gluing and process of removing photoresist, and characterize
According to traditional technology, with 4000r/min, sample being revolved resist coating, thickness is��280nm, then removes photoresist material with acetone equal solvent. Then with AFM, sample surfaces is characterized, obtain the sample surfaces shape looks having photoresist material to remain.
(4) sample carries out raman laser remove photoresist process.
Sample is positioned over below the laser emitting mouth of Raman spectrum system, with < the low energy laser focusing bundle of 3mW, finds the particular location of pending sample surfaces under the microscope. Graphite Raman spectrogram before removing photoresist with the laser beam collection one of 2mW. Then with the high-energy focusing laser beam irradiation sample surfaces of 10mW, irradiation time is 8 minutes, carries out process of removing photoresist. Graphite Raman spectrogram after removing photoresist with the laser beam collection one of 2mW again, with remove photoresist before spectrum contrast, judge that grapheme material is had not damaged by process of removing photoresist, namely occur with or without D peak.
(5) sign of Graphene sample after removing photoresist
After La Man removes residual photoresist material, it is necessary to whether Experimental Characterization removes photoresist even, complete. Graphenic surface shape looks are again characterized, it is possible to the graphenic surface residual photoresist material that discovery laser beam treatment is crossed is removed, and exposes the shape looks of intrinsic Graphene with AFM; There is no the graphenic surface still photoresist material residual of laser beam treatment.
Embodiment two: peel off multi-layer graphene surface removal residual photoresist material
(1) preparation of grapheme material
Utilize mechanically peel method to prepare Graphene, select scotch tape, repeatedly peel off high orientation graphite flakes, and the Graphene on adhesive tape is transferred to target SiO2On/Si substrate, Si is low-resistance silicon, SiO2For thermal oxide growth, thickness is generally 300nm.
(2) sign of grapheme material
Utilizing opticmicroscope, observed shape looks and the color of Graphene by contrast difference, the thickness of preliminary judgement Graphene, roughly estimates the number of plies of Graphene. Raman spectrum is utilized to characterize the Graphene number of plies and quality further. Choose I2D/IG< 0.6, there is no the sample at obvious D peak, as multilayer and do not have defective Graphene sample simultaneously. AFM is utilized to characterize Graphene sample surfaces shape looks, it is determined that not remain the original graphite alkene surface topography of photoresist material.
(3) sample carries out gluing and process of removing photoresist, and characterizes
According to traditional technology, with 4000r/min, sample being revolved resist coating, thickness is��280nm, then removes photoresist material with acetone equal solvent. Then with AFM, sample surfaces is characterized, obtain the sample surfaces shape looks having photoresist material to remain.
(4) sample carries out raman laser remove photoresist process.
Sample is positioned over below the laser emitting mouth of Raman spectrum system, with < the low energy laser focusing bundle of 3mW, finds the particular location of pending sample surfaces under the microscope. Graphite Raman spectrogram before removing photoresist with the laser beam collection one of 2mW. Then with the high-energy focusing laser beam irradiation sample surfaces of 15mW, irradiation time is 3 minutes, carries out process of removing photoresist. Graphite Raman spectrogram after removing photoresist with the laser beam collection one of 2mW again, with remove photoresist before spectrum contrast, judge that grapheme material is had not damaged by process of removing photoresist, namely occur with or without D peak.
(5) sign of Graphene sample after removing photoresist
After La Man removes residual photoresist material, it is necessary to whether Experimental Characterization removes photoresist even, complete. Graphenic surface shape looks are again characterized, it is possible to the graphenic surface residual photoresist material that discovery laser beam treatment is crossed is removed, and exposes the shape looks of intrinsic Graphene with AFM; There is no the graphenic surface still photoresist material residual of laser beam treatment.
Embodiment three: CVD Graphene sample surfaces removes residual photoresist material
(1) preparation of grapheme material
Copper Foil is put into quartz tube furnace and carries out CVD synthesizing graphite alkene, the wet method transfer method that recycling PMMA is auxiliary, Graphene is transferred to SiO2On/Si substrate, obtain uniform single-layer graphene.
(2) sign of grapheme material
Utilize opticmicroscope, observed shape looks and the color of Graphene by contrast difference. Raman spectrum is utilized to characterize the Graphene number of plies and quality further. Choose I2D/IG> 2, there is no the region at obvious D peak, as individual layer and do not have defective Graphene sample simultaneously. AFM is utilized to characterize Graphene sample surfaces shape looks.
(3) sample carries out raman laser remove photoresist process.
Sample is positioned over below the laser emitting mouth of Raman spectrum system, with < the low energy laser focusing bundle of 3mW, finds the particular location of pending sample surfaces under the microscope. Graphite Raman spectrogram before removing photoresist with the laser beam collection one of 2mW. Then with the high-energy focusing laser beam irradiation sample surfaces of 40mW, irradiation time is 1 minute, carries out process of removing photoresist. Graphite Raman spectrogram after removing photoresist with the laser beam collection one of 2mW again, with remove photoresist before spectrum contrast, judge that grapheme material is had not damaged by process of removing photoresist, namely occur with or without D peak.
(4) sign of Graphene sample after removing photoresist
After La Man removes residual photoresist material, it is necessary to whether Experimental Characterization removes photoresist even, complete. Graphenic surface shape looks are again characterized, it is possible to the graphenic surface residual photoresist material that discovery laser beam treatment is crossed is removed, and exposes the shape looks of intrinsic Graphene with AFM; There is no the graphenic surface still photoresist material residual of laser beam treatment.
Embodiment four: residual photoresist material is removed at grapheme transistor raceway groove position
(1) preparation of grapheme material
Utilize mechanically peel method to prepare Graphene, select scotch tape, repeatedly peel off high orientation graphite flakes, and the Graphene on adhesive tape is transferred to target SiO2On/Si substrate, Si is low-resistance silicon, SiO2For thermal oxide growth, thickness is generally 300nm.
(2) preparation of graphical and source-drain electrode
Pass through micro fabrication, in conjunction with the method for electron beam exposure (EBL) and oxygen plasma etch (ICP), Graphene graphically and is defined source-drain electrode, recycling electron beam evaporation evaporation metal is also peeled off, complete the preparation of source and drain metal electrode, between source-drain electrode, it is the channel region of transistor.
(3) channel region carries out raman laser remove photoresist process
Sample is positioned over below the laser emitting mouth of Raman spectrum system, with < the low energy laser focusing bundle of 3mW, finds the particular location of pending sample surfaces under the microscope. Graphite Raman spectrogram before removing photoresist with the laser beam collection one of 2mW. Then with the high-energy focusing laser beam irradiation sample surfaces of 30mW, irradiation time is 2 minutes, carries out process of removing photoresist. Graphite Raman spectrogram after removing photoresist with the laser beam collection one of 2mW again, with remove photoresist before spectrum contrast, judge that grapheme material is had not damaged by process of removing photoresist, namely occur with or without D peak.
Embodiment five: the reserved electrode area of grapheme transistor removes residual photoresist material
(1) preparation of grapheme material
Copper Foil is put into quartz tube furnace and carries out CVD synthesizing graphite alkene, the wet method transfer method that recycling PMMA is auxiliary, Graphene is transferred to SiO2On/Si substrate, obtain uniform single-layer graphene.
(2) Graphene is graphical
In conjunction with EBL and ICP, Graphene is carried out graphically.
(3) device source-drain electrode is defined
Utilize the Graphene region of electron beam exposure after graphically, expose device source drain electrode, and develop and expose graphenic surface.
(4) sign of the graphenic surface shape looks below electrode is reserved
AFM is utilized to characterize graphenic surface shape looks below reserved electrode, it is possible to observe obvious photoresist material residual.
(5) channel region carries out raman laser remove photoresist process
Sample is positioned over below the laser emitting mouth of Raman spectrum system, with < the low energy laser focusing bundle of 3mW, finds the particular location of pending sample surfaces under the microscope. Graphite Raman spectrogram before removing photoresist with the laser beam collection one of 2mW. Then with the high-energy focusing laser beam irradiation sample surfaces of 30mW, irradiation time is 2 minutes, carries out process of removing photoresist. Graphite Raman spectrogram after removing photoresist with the laser beam collection one of 2mW again, with remove photoresist before spectrum contrast, judge that grapheme material is had not damaged by process of removing photoresist, namely occur with or without D peak.
(6) sign of graphenic surface shape looks after removing photoresist
Utilize AFM characterize graphenic surface remove photoresist after shape looks, with remove photoresist before contrast, it is possible to observe residual photoresist material be removed.
(7) steaming of source and drain metal electrode is plated and is peeled off
Utilize electron beam evaporation evaporation metal and peel off, complete the preparation of source and drain metal electrode
Although the present invention discloses as above with better embodiment, but and it is not used to limit the present invention. Any those of ordinary skill in the art, do not departing from technical solution of the present invention scope situation, all can utilize the Method and Technology content of above-mentioned announcement that technical solution of the present invention is made many possible variations and modification, or be revised as the equivalent embodiment of equivalent variations. Therefore, every content not departing from technical solution of the present invention, the technical spirit of foundation the present invention, to any simple modification made for any of the above embodiments, equivalent variations and modification, all still belongs in the scope of technical solution of the present invention protection.
Claims (4)
1. remove the method for carbon-base film photomask surface glue for one kind, it is characterised in that, comprising:
1) the carbon-base film sample with residual photoresist material is chosen;
2) being positioned over by carbon-base film sample below the laser emitting mouth of opticmicroscope of Raman spectrum system, adjustment carbon-base film sample position is to, in field of microscope, regulating microscope focus, and focus on carbon-base film sample surfaces;
3) being directed at carbon-base film sample with low-yield laser focusing bundle and need position of removing photoresist, now laser intensity should at below 3mW;
4) selecting the laser beam of high-energy, the strength range of laser beam is 10��40mW, with the laser beam irradiation film sample of this high-energy surface, thus removes photoresist material residual.
2. the as claimed in claim 1 method removing carbon-base film photomask surface glue, it is characterised in that, step 2) in optical maser wavelength select 514,532 or 633nm.
3. the as claimed in claim 1 method removing carbon-base film photomask surface glue, it is characterised in that, step 4) in time of irradiating within 5s to 10min scope.
4. the method removing carbon-base film photomask surface glue as claimed in claim 1 is applied to the preparation of grapheme transistor.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106328832A (en) * | 2016-10-27 | 2017-01-11 | 武汉华星光电技术有限公司 | Removal method of anisotropic conductive adhesive film |
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| CN1450413A (en) * | 2002-04-10 | 2003-10-22 | 财团法人激光技术综合研究所 | Photoresist removing method and apparatus thereof |
| CN102074584A (en) * | 2010-12-06 | 2011-05-25 | 复旦大学 | Air-gap grapheme transistor and manufacturing method thereof |
| CN102590309A (en) * | 2012-02-03 | 2012-07-18 | 游学秋 | Manufacture and application method for graphene transistor and biosensor of graphene transistor |
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2016
- 2016-02-29 CN CN201610111722.3A patent/CN105629682A/en active Pending
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| US20020170897A1 (en) * | 2001-05-21 | 2002-11-21 | Hall Frank L. | Methods for preparing ball grid array substrates via use of a laser |
| CN1450413A (en) * | 2002-04-10 | 2003-10-22 | 财团法人激光技术综合研究所 | Photoresist removing method and apparatus thereof |
| CN102074584A (en) * | 2010-12-06 | 2011-05-25 | 复旦大学 | Air-gap grapheme transistor and manufacturing method thereof |
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Application publication date: 20160601 |