CN107117609B - A kind of graphene thinning device with optics in situ detection - Google Patents
A kind of graphene thinning device with optics in situ detection Download PDFInfo
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- CN107117609B CN107117609B CN201710368001.5A CN201710368001A CN107117609B CN 107117609 B CN107117609 B CN 107117609B CN 201710368001 A CN201710368001 A CN 201710368001A CN 107117609 B CN107117609 B CN 107117609B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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Abstract
The present invention relates to a kind of graphene thinning device with optics in situ detection, which, which is equipped with, is thinned optical path unit, excitation light path unit, in situ detection optical path unit, workbench and computer etc..First laser beam being thinned for graphene that optical path unit issues is thinned, the second laser beam that excitation light path unit issues is used to excite the graphene of area to be machined to generate Raman scattering.In situ detection optical path unit collects the Raman scattering signal that graphene generates, and obtains the number of plies and temperature information of area to be machined graphene according to the bias size of the ratio and Raman peak position of the peak Raman scattering signal 2D and G peak intensity.Apparatus of the present invention can carry out local thickness's measurement to the non-uniform graphene sample in part simultaneously and be thinned, device is according to the graphene number of plies of actually measured area to be machined, adjust laser power and thinned time, the thinned number of plies of accurate control graphene, to obtain the graphene film that the number of plies is uniform, controllable.
Description
Technical field
The present invention relates to graphene processing equipment field, dress is thinned in especially a kind of graphene with optics in situ detection
It sets.
Background technique
Graphene is by carbon atom with sp2Hybrid form forms the flat film of honeycomb structure, is a kind of novel two
Tie up material.Graphene has excellent optics, electricity, mechanical property, is the core material of next-generation micro-nano ray machine electrical part.Stone
The preparation method of black alkene is classified by the form of carbon source, can be divided into solid phase method, liquid phase method and vapor phase method, however in graphene device
In part preparation, with the mechanical stripping highly oriented pyrolytic graphite method in solid phase method and the chemical vapour deposition technique in vapor phase method using most
It is extensive.Both methods is each advantageous, and certain shortcoming is also individually present.The graphene quality of mechanical stripping method preparation
Height, but usually only several microns to tens microns of size, low yield is prepared, and thickness is uncontrollable.And chemical vapour deposition technique can
The graphene polycrystal film or grade monocrystal thin films of large area are prepared, yield is high, but the graphene of this method preparation is easy to deposit
In defect, and in uneven thickness or discontinuous phenomenon is easy to appear in wide area.
In graphene device, the number of plies of graphene is the important parameter for determining graphene characteristic.The electronics knot of graphene
Structure, optical property and the number of plies are closely related, and the performance of many graphene photoelectric devices is directly determined by its number of plies.And above-mentioned graphite
Alkene preparation process is difficult to control accurately there is graphene number of plies or the prepared non-uniform problem of graphene number of plies.Therefore
In the preparation process of graphene device, need to carry out the graphene being prepared subsequent be thinned.Graphene number of plies is carried out
Accuracy controlling becomes urgent problem to be solved.
The thinned of graphene needs to carry out the graphene film of atomic-level thickness accurate thickness regulation, this is to mainstream
Semiconductor etching process brings great challenge.Currently, graphene thining method mainly includes following 3 kinds.(1) chemical etching
Method.Document " Science.2011；331 (6021): the lattice structure of top layer graphene 1168 " is destroyed by splash-proofing sputtering metal zinc, so
The graphene layer being destroyed afterwards using diluted hydrochloric acid dissolution metallic zinc and top layer, to realize that the graphene of monoatomic layer precision is carved
Erosion.(2) plasma etching method.Patent " CN102931055B " discloses a kind of stone using plasma etching to any thickness
Black alkene carries out thinned method.(3) laser is thinned.Patent " CN102931055B " disclose it is a kind of using ultrafast laser to graphite
Alkene carries out thinned method, is removed the graphene of certain number of plies from sample using laser, to realize the accurate control of the number of plies
System.Above-mentioned three kinds of methods otherwise graphene sample can only be carried out it is global be thinned, be unable to satisfy heterogeneous sample to part
Non-uniform areas carries out thinned demand；It needs to be measured the number of plies of entire graphene film before being thinned, thus
Obtain the number of plies information of each position of sample, so carry out it is thinned, however it is this first measure that the method that is thinned afterwards needs will measurement
Coordinate when thickness is strictly aligned with thinned coordinate, can be accurately positioned local non-uniform areas and then be realized thinned, practical behaviour
Make very difficult.
Summary of the invention
It is a primary object of the present invention to overcome drawbacks described above in the prior art, a kind of band optics in situ detection is provided,
Graphene can be obtained in real time and is thinned position number of plies information, and graphene can be carried out according to the number of plies information that real-time measurement obtains
Thinned device, the device can also monitor the temperature information of measured point in real time, avoid destroying in thinning process because temperature is excessively high
Graphene.
The present invention adopts the following technical scheme:
A kind of graphene thinning device with optics in situ detection, which is characterized in that including workbench, optical path list is thinned
Member, excitation light path unit, in situ detection optical path unit and computer；The workbench is equipped with vacuum chamber to place graphene；This subtracts
Thin optical path unit is set to above workbench to issue first laser beam realization to graphene and be thinned；Excitation light path unit setting
To issue second laser beam above workbench, and graphene surface is focused on after the second laser beam and first laser beam conjunction beam
Measured point；The in situ detection optical path unit, which is located at below workbench, scatters light with the graphite Raman for collecting measured point generation,
The raman spectral signal of graphene measured point is obtained by spectrum analysis after being filtered；The computer and in situ detection light
Road unit, thinned optical path unit are connected to obtain the number of plies and temperature value of graphene measured point according to spectral signal, and according to quilt
The measuring point number of plies adjusts first laser beam to control the thinned number of plies.
Preferably, the thinned optical path unit include the first laser device being sequentially placed, laser shutter, optical attenuator with
First reflecting mirror；The first laser beam of first laser device transmitting successively passes through laser shutter, optical attenuator and the first reflection
Mirror；The laser shutter and optical attenuator are connected with the computer.
Preferably, the excitation light path unit includes second laser, dichroscope, beam expanding lens and the first focusing objective len；
The second laser is for emitting second laser beam；The dichroscope closes beam for reflected second laser Shu Bingyu first laser beam
To beam expanding lens, which focuses on first laser beam and second laser beam the measured point of the graphene.
Preferably, the second laser is solid state laser, wavelength 532nm, power 200mW.
Preferably, the in situ detection optical path unit includes the second focusing objective len set gradually, the second reflecting mirror, first
Notch filtering light piece, the second notch filtering light piece, condenser lens, fibre-optical splice, optical fiber and spectrometer；Second focusing objective len is located at institute
It states below graphene to collect the Raman diffused light that the graphene is thinned position；Second reflecting mirror is by the graphene of collection
Scatter light reflection, and pass sequentially through the first notch filtering light piece, the second notch filtering light piece filters out first laser beam, second laser respectively
Beam, then by entering fibre-optical splice after condenser lens convergence；Fibre-optical splice is transferred to spectrometer by optical fiber and carries out spectrum analysis
Obtain spectral signal；The computer is connected according to the ratio in judgement graphene at the peak Raman signal 2D and the peak G with the spectrometer
The number of plies, and the temperature value that graphene is thinned region is obtained according to the drift condition at the peak 2D and the peak G.
Preferably, the central wavelength of the second notch filtering light piece is 532nm, halfwidth 10nm, optical density (OD) OD > 5.
Preferably, the central wavelength of the first notch filtering light piece is equal with the central wavelength of the first laser beam, and half
Gao Kuanwei 10nm, optical density (OD) OD > 5.
It preferably, further include three-dimensional precise displacement platform；The three-dimensional precise displacement platform is fixedly connected with the workbench, and by
The computer control drives the working table movement to detect next measured point.
Preferably, the vacuum chamber above and below uses clear quartz window；The first laser beam and the second laser
Beam focuses on the graphene through clear quartz window above；The Raman diffused light that the graphene generates is through following
Clear quartz window outgoing.
It preferably, further include vacuum pump, which is connected with the vacuum chamber to vacuumize.
By the above-mentioned description of this invention it is found that compared with prior art, the invention has the following beneficial effects:
1) can real-time monitoring graphene in situ the number of plies, graphene is thinned and carries out simultaneously with thickness measure, without coordinate pair
Quasi- process, it is easy to operate simple, meet the demand of uneven graphene local reduction；
2) can be according to the graphene number of plies of real-time measurement, by adjusting optical attenuator and laser shutter, accurate control subtracts
Laser power used in thin and time, to accurately control thinned graphene number of plies；
3) temperature change in thinning process can be monitored in real time, prevent in thinning process because temperature it is excessively high caused by graphene sample
The damage of product.
Detailed description of the invention
Fig. 1 is the simplified structure diagram of the specific embodiment of the invention.
Optical path unit, 11- first laser device, 12- laser shutter, 13- optical attenuator, the first reflecting mirror of 14- is thinned in 1-；
2- excitation light path unit, 21- second laser, 22- dichroscope, 23- beam expanding lens, the first focusing objective len of 24-；3- in situ detection
Optical path unit, the second focusing objective len of 31-, the second reflecting mirror of 32-, 33- the first notch filtering light piece, 34- the second notch filtering light piece,
35- condenser lens, 36- fibre-optical splice, 37- optical fiber, 38- spectrometer；4- graphene, 41- vacuum chamber, 42- workbench, 43- tri-
Tie up precision displacement table, 44- vacuum pump.
Specific embodiment
Below by way of specific embodiment, the invention will be further described.
As shown in Figure 1, a kind of graphene thinning device with optics in situ detection, is equipped with and optical path unit 1, exciting light is thinned
Road unit 2, in situ detection optical path unit 3, three-dimensional precise displacement platform 43, workbench 42, vacuum pump 44 and computer.The workbench
42 are equipped with vacuum chamber 41 to place graphene 4, and provide vacuum bad border required for graphene is thinned.Vacuum chamber about 41 two
Face is clear quartz window, and processed graphene is placed on the quartz window in vacuum chamber 41.Processed graphene can be straight
Switch through and move on the quartz window in vacuum chamber 41, be also transferred in transparent substrates, such as substrate of glass, quartz substrate, oxidation
Aluminium substrate etc., then the transparent substrates for being loaded with graphene are placed on the quartz window in vacuum chamber 41.
Workbench 42 is mounted on three-dimensional precise translation stage 43, and three-dimensional precise displacement platform 43 is controlled by computer for driving
Workbench 42 and vacuum chamber 41 are mobile.Vacuum chamber 41 is connected by vacuum pipe with vacuum pump 44, and vacuum pump 44 is by vacuum chamber 41
It is evacuated to low vacuum state, prevents destruction of the oxygen to graphene in graphene thinning process.
The device of the invention using laser graphene is carried out it is thinned, and device can real-time monitoring be thinned graphene a little
Used laser power is thinned by controlling according to graphene thickness and required target thickness that measurement obtains in thickness
And the thinned time, it realizes that the number of plies is controllable and is thinned.The device can also monitor the temperature being thinned a little in real time, adjust laser function in real time
Rate and thinned time avoid causing graphene sample to damage because temperature is excessively high in thinning process.It is specific as follows:
Optical path unit 1 is thinned and is located at 42 top of workbench, for being thinned for graphene, including the first laser set gradually
Device 11, laser shutter 12, optical attenuator 13 and reflecting mirror 14.First laser device 11 is optical fiber picosecond laser device, is issued
First laser beam power is 1W, wavelength 1030nm, pulse recurrence frequency 10KHz, pulsewidth 10ps.The sound of laser shutter 12
It is 1 microsecond between seasonable, opening and closing by laser shutter 12 accurately controls the number for reaching the laser pulse on graphene,
To which graphene number of plies be accurately thinned.Optical attenuator 13 is made of two panels polariscope, passes through first polariscope
Rotation accurate continuous can adjust the power for focusing on the first laser beam on graphene.
Excitation light path unit 2 is located at 42 top of workbench, for exciting the graphene sample being thinned to generate Raman signal,
Including second laser 21, dichroscope 22, beam expanding lens 23 and the first focusing objective len 24 being sequentially placed.Second laser 21 is
The solid state laser of diode-end-pumped, the second laser beam wavelength issued are 532nm, power 200mW.Dichroic
Mirror 22 is long logical dichroscope, and cutoff frequency 650nm, i.e. wavelength are greater than the light of 650nm, can be by dichroscope 22, and wave
The long light for being less than 650nm, is reflected by dichroscope 22.Therefore wavelength is that the first laser beam of 1030nm can pass through binomial Look mirror
22, and the second laser beam that wavelength is 532nm is then reflected by binomial Look mirror 22, to realize first laser beam and second laser
The conjunction beam of beam.The amplification factor of beam expanding lens 23 is 3 times, and the amplification factor of the first focusing objective len is 50 times, numerical aperture 0.7.
After first laser beam is reflected by reflecting mirror 14, successively pass through dichroscope 22, beam expanding lens 23 and the first focusing objective len 24, focuses
Being thinned for graphene is carried out in processed graphene surface.Spot diameter size after focusing is about 2 μm.Second laser beam according to
It is secondary to focus on graphene sample surface with first laser beam after dichroscope 22, beam expanding lens 23, the first focusing objective len 24
Same point excites the graphene sample of focal spot to generate Raman scattering signal.Graphene is contained in the Raman scattering signal
Number of plies information and processing stand temperature information.First laser device 11 and second laser 21 focus on same point, the quilt
Weak points and it is measured as same point, is all the focus point of laser beam.
In situ detection optical path unit 3 is placed in 42 lower section of vacuum chamber 41 and workbench, for real-time in-situ measurement graphene
The number of plies and it is thinned when temperature, including the second focusing objective len 31, the second reflecting mirror 32, the first notch filtering light piece being sequentially placed
33, the second notch filtering light piece 34, condenser lens 35, fibre-optical splice 36, optical fiber 37 and spectrometer 38.Second focusing objective len 31 is used
Light, the times magnification of the second focusing objective len 31 are scattered in the graphite Raman for collecting first laser beam and second laser beam focal spot
Number is 50 times, numerical aperture 0.7.Since first laser beam and second laser beam may pass through graphene into the second conglomeration
Mirror 31, therefore include a large amount of first laser beam and second laser beam in Raman diffused light collected by the second focusing objective len 31.
Light beam collected by second focusing objective len 31 successively passes through the first notch filtering light piece 33 and second after the reflection of the second reflecting mirror 32
Notch filtering light piece 34 is filtered.The central wavelength of first notch filtering light piece is 1030nm, halfwidth 10nm, optical density (OD) OD
=6, it can effectively prevent the transmission of first laser beam.The central wavelength of second notch filtering light piece be 532nm, halfwidth 10nm,
Optical density (OD) OD=6, for preventing passing through for second laser beam.After filtering out first laser beam and second laser beam, collection it is pure
Net graphite Raman scattered signal line focus lens 35 are coupled into fibre-optical splice 36, and by optical fiber 37 be sent to spectrometer 38 into
Row spectrum analysis.The graphite Raman spectral signal that measurement obtains is transmitted to computer by spectrometer 38.
Computer can obtain the number of plies information of the graphene according to the peak 2D of graphite Raman signal and the ratio at the peak G.
According to the number of plies and the set goal number of plies of the graphene that measurement obtains, computer is fast by adjusting optical attenuator 13 and laser
Used laser power and thinned time is thinned in the accurate control graphene of door 12, accurately carries out to graphene thinned.Subtracting
During thin, device can real-time monitoring be thinned the number of plies a little, it is ensured that be thinned after graphene number of plies be the desired number of plies.By
It will lead to the offset at the peak graphene D Yu the peak position G in the variation of temperature value, computer passes through D in monitoring graphene spectral signal
The drift condition at peak and the peak position G can obtain being thinned temperature value a little, so that the temperature value to weak points is supervised in real time
Control, avoids during being thinned due to the excessively high damage for leading to graphene sample of weak points temperature.
First laser beam and second laser beam can pass through upper quartz window and focus on the graphene being thinned, graphene
The exciting light of generation can be emitted by the quartz window of lower part, and be collected by situ detection optical path unit 3, and carry out spectrum point
Analysis.Three-dimensional precise translation stage 43 drives workbench 42 and vacuum chamber 41 to move, so that processed graphene and first swashs
Light beam, second laser beam generate relative motion.After the graphene of some point is thinned to the expected number of plies, D translation platform
Graphene is moved to next point by 43, is carried out the detection of the number of plies and is thinned.Device is according in this way to each of on graphene
Point carries out thickness measure and is thinned, thus obtain that thickness is uniform, the controllable graphene film of the number of plies.
The above is only a specific embodiment of the present invention, but the design concept of the present invention is not limited to this, all to utilize this
Design makes a non-material change to the present invention, and should all belong to behavior that violates the scope of protection of the present invention.
Claims (10)
1. a kind of graphene thinning device with optics in situ detection, which is characterized in that including workbench, be thinned optical path unit,
Excitation light path unit, in situ detection optical path unit and computer；The workbench is equipped with vacuum chamber to place graphene；Light is thinned in this
Road unit is set to above workbench to issue first laser beam realization to graphene and be thinned；The excitation light path unit is set to work
Make above platform to issue second laser beam, the second laser beam is for exciting graphene to generate Raman signal, and the second laser
The measured point of graphene surface is focused on after beam and first laser beam conjunction beam；The in situ detection optical path unit is located at below workbench
Light is scattered to collect the graphite Raman of measured point generation, graphene measured point is obtained by spectrum analysis after being filtered
Raman spectral signal；The computer is connected in situ detection optical path unit, thinned optical path unit to be obtained according to spectral signal
The number of plies and temperature value of graphene measured point, and first laser beam is adjusted to control the thinned number of plies according to the measured point number of plies.
2. a kind of graphene thinning device with optics in situ detection as described in claim 1, it is characterised in that: described to be thinned
Optical path unit includes the first laser device being sequentially placed, laser shutter, optical attenuator and the first reflecting mirror；The first laser device
The first laser beam of transmitting successively passes through laser shutter, optical attenuator and the first reflecting mirror；The laser shutter and optical attenuator
Device is connected with the computer.
3. a kind of graphene thinning device with optics in situ detection as described in claim 1, it is characterised in that: the excitation
Optical path unit includes second laser, dichroscope, beam expanding lens and the first focusing objective len；The second laser is for emitting second
Laser beam；The dichroscope closes beam to beam expanding lens, first focusing objective len for reflected second laser Shu Bingyu first laser beam
First laser beam and second laser beam are focused on to the measured point of the graphene.
4. a kind of graphene thinning device with optics in situ detection as claimed in claim 3, it is characterised in that: described second
Laser is solid state laser, wavelength 532nm, power 200mW.
5. a kind of graphene thinning device with optics in situ detection as described in claim 1, it is characterised in that: the original position
Light path unit includes the second focusing objective len set gradually, the second reflecting mirror, the first notch filtering light piece, the second notch filtering light
Piece, condenser lens, fibre-optical splice, optical fiber and spectrometer；Second focusing objective len is located at below the graphene described to collect
Graphene is thinned the Raman diffused light of position；Second reflecting mirror passes sequentially through the graphene scattering light reflection of collection
First notch filtering light piece, the second notch filtering light piece filter out first laser beam, second laser beam respectively, then are converged by the condenser lens
Enter fibre-optical splice afterwards；Fibre-optical splice is transferred to spectrometer progress spectrum analysis by optical fiber and obtains spectral signal；The calculating
Machine is connected with according to the ratio in judgement graphene number of plies at the peak Raman signal 2D and the peak G with the spectrometer, and according to the peak 2D and the peak G
Drift condition obtains the temperature value that graphene is thinned region.
6. a kind of graphene thinning device with optics in situ detection as claimed in claim 5, it is characterised in that: described second
The central wavelength of notch filtering light piece is 532nm, halfwidth 10nm, optical density (OD) OD > 5.
7. a kind of graphene thinning device with optics in situ detection as claimed in claim 5, it is characterised in that: described first
The central wavelength of notch filtering light piece is equal with the central wavelength of the first laser beam, halfwidth 10nm, optical density (OD) OD > 5.
8. a kind of graphene thinning device with optics in situ detection as described in claim 1, it is characterised in that: further include three
Tie up precision displacement table；The three-dimensional precise displacement platform is fixedly connected with the workbench, and is driven by computer control described
Working table movement is to detect next measured point.
9. a kind of graphene thinning device with optics in situ detection as described in claim 1, it is characterised in that: the vacuum
Chamber above and below uses clear quartz window；The first laser beam and the second laser beam penetrate suprasil window above
Mouth focuses on the graphene；The Raman diffused light that the graphene generates is emitted through following clear quartz window.
10. a kind of graphene thinning device with optics in situ detection as described in claim 1, it is characterised in that: further include
Vacuum pump, the vacuum pump are connected with the vacuum chamber to vacuumize.
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| CN109342484A (en) * | 2018-12-21 | 2019-02-15 | 四川聚创石墨烯科技有限公司 | A kind of doping graphene oxide attribute detection method |
| CN109974775B (en) * | 2019-01-14 | 2022-04-19 | 天元羲王控股有限公司 | Automatic on-line detection equipment and method for graphene production |
| CN112798472A (en) * | 2020-12-24 | 2021-05-14 | 广东工业大学 | Quality online detection method and device for graphene-based composite material production |
| CN113929085B (en) * | 2021-10-26 | 2023-10-10 | 中国科学院上海光学精密机械研究所 | Three-dimensional patterned porous graphene blackbody and preparation method and application thereof |
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| JPH04113649A (en) * | 1990-09-03 | 1992-04-15 | Fujitsu Ltd | Apparatus for manufacturing semiconductor device |
| US20110299720A1 (en) * | 2010-03-18 | 2011-12-08 | The Regents Of The University Of California | Systems and methods for material layer identification through image processing |
| CN102156116A (en) * | 2011-03-11 | 2011-08-17 | 中国科学院半导体研究所 | Graphene sheet intercalation compound preparation method and in situ microRaman representation system |
| CN102492926A (en) * | 2011-12-16 | 2012-06-13 | 东南大学 | Preparation method for grapheme thin film with local monoatomic layer |
| US9234798B2 (en) * | 2013-06-21 | 2016-01-12 | National Chung Cheng University | System and method for detecting number of layers of a few-layer graphene |
| CN104073786A (en) * | 2014-06-11 | 2014-10-01 | 清华大学 | Method for accurately controlling graphene layers |
| JP6457766B2 (en) * | 2014-09-17 | 2019-01-23 | 国立大学法人岩手大学 | Apparatus and method for determining the number of layers in a two-dimensional thin film atomic structure using Raman scattering spectrum of an insulating material |
| CN105460930B (en) * | 2016-01-04 | 2017-05-31 | 河南工程学院 | A kind of regulation and control and the method and device of sign Graphene band gap |
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