CN105762090A - Method of monitoring graphene surface molecule adsorption process - Google Patents
Method of monitoring graphene surface molecule adsorption process Download PDFInfo
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- CN105762090A CN105762090A CN201610137360.5A CN201610137360A CN105762090A CN 105762090 A CN105762090 A CN 105762090A CN 201610137360 A CN201610137360 A CN 201610137360A CN 105762090 A CN105762090 A CN 105762090A
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- graphene
- adsorption process
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- laser
- graphenic surface
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 21
- 238000012544 monitoring process Methods 0.000 title claims abstract description 16
- 238000012546 transfer Methods 0.000 claims abstract description 18
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 239000000523 sample Substances 0.000 claims description 21
- 238000012360 testing method Methods 0.000 claims description 8
- 229920006395 saturated elastomer Polymers 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 4
- 238000001237 Raman spectrum Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 3
- 239000004065 semiconductor Substances 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000007789 gas Substances 0.000 description 21
- 238000013532 laser treatment Methods 0.000 description 10
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000001069 Raman spectroscopy Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000003795 desorption Methods 0.000 description 3
- 230000005669 field effect Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000002390 adhesive tape Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 208000036626 Mental retardation Diseases 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- -1 graphite alkene Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/16—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only elements of Group IV of the Periodic System
- H01L29/1606—Graphene
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/10—Measuring as part of the manufacturing process
- H01L22/14—Measuring as part of the manufacturing process for electrical parameters, e.g. resistance, deep-levels, CV, diffusions by electrical means
Abstract
The invention discloses a method of monitoring a graphene device surface molecule adsorption process, which mainly monitors transfer characteristics of a graphene device, in particular Dirac point points, supervises a graphene surface gas adsorption dynamic process in the device in real time, i.e., a whole process from graphene surface cleaning to molecule saturation adsorption, and more accurately measures time required in the process.
Description
Technical field
The present invention proposes the monitoring method of a kind of graphenic surface gas molecule adsorption process, can be used for the dynamic process of monitor in real time graphene device surface gas Molecular Adsorption under short-term environment, the time that estimation graphene device surface is adsorbed by gas molecule completely, in fields such as chemistry, physics, materialogy, micro-nano electronics, there is application prospect.
Background technology
Graphene is two dimensional surface crystalline material, integrates multiple excellent specific property, has character and the wide application prospects such as good mechanics, electricity.Sensor based on Graphene causes strong concern recently, only Graphene thickness only one carbon atom, and has the specific surface area of super large, it is possible to reach 2630m2/ g, has the gas molecule absorption property of excellence.
The detection that gas molecule is adsorbed by current graphene film changes mainly through the conductance before and after detected gas Molecular Adsorption.Gaseous molecular adsorbate has different the Nomenclature Composition and Structure of Complexes, it is possible to interact in different patterns from Graphene.Graphene is generally in p-type quasiconductor under atmospheric environment, and when it is exposed to other various gases, the response direction of its conductance is probably different.Such as NO2Being adsorbed on graphenic surface (adulterating as one) and can change the electron concentration concentration of Graphene, thus changing the conductance of Graphene, detection conductance change can detect NO2。
Summary of the invention
Present invention aim at providing a kind of method, can real-time dynamic monitoring graphene device surface gas Molecular Adsorption process.
The present invention can be achieved through the following technical solutions:
The monitoring method of a kind of graphenic surface gas molecule adsorption process, comprises the steps:
(1) preparing graphene device sample, this graphene device includes source and drain metal electrode and graphene-channel；
(2) sample is positioned over below the laser emitting mouth of Raman spectrum system optical microscope.Adjust sample position in field of microscope, regulate microscope focus, and focus on graphene-channel surface；
(3) with low-energy focusing laser beam be directed at graphene-channel surface, now laser intensity should at below 3mW, to ensure that laser spot is only small, registration；
(4) with the laser beam irradiation of higher-energy or scanning graphene-channel surface, control laser intensity and time, remove the empty gas and water equimolecular on graphene-channel surface, thus obtaining the graphene-channel surface of cleaning；Superlaser beam intensity is 10～40mW, and the time is within 10min to 5s scope；
(5) after removing graphene-channel surface molecular, the electrology characteristic of rapid in site measurement graphene device sample, namely utilizing probe station or be integrated in the probe station of Raman spectrogrph and the transfer characteristic curve of Semiconductor Parameter Analyzer test graphene device, namely source-drain current is with the change of back gate voltage.At regular intervals, test a transfer characteristic curve, until the transfer characteristic curve of front and back twice does not change.Namely once close laser, namely gas molecule in air starts to be adsorbed onto on the surface of graphene-channel, so that the transfer characteristic of graphene device (I-Vg) curve changes, when I-Vg stablizes, the absorption of graphenic surface gas molecule reaches capacity immediately；By monitoring graphene device I-Vg curve monitoring graphene device surface gas Molecular Adsorption process, and by measuring I-Vg curve stable process, estimate Molecular Adsorption graphenic surface required time.
The technique effect of the present invention is as follows:
(1) present invention can in real time, dynamically monitor graphene device surface gas Molecular Adsorption process.
(2) this technology can for local graphite alkene surface, it is adaptable to monitoring graphene device entirety or local desorption process, and monitoring process does not affect other region of Graphene.
(3) this technology is by instant graphene device transfer characteristic curve of measuring, and monitoring graphenic surface is adsorbed to the saturated overall process of surface adsorption from gas molecule, can comparatively accurately measure the time needed for the saturated absorption of graphene device molecule.
Accompanying drawing explanation
Fig. 1 Graphene backgate field-effect transistor: (a) device surface AFM shape appearance figure, is arranged above device source electrode 1, and lower section is element leakage pole 2；B the Raman spectrogram of graphene-channel 3 correspondence position in () sample, peak is by force than I2D/IG～1.
Fig. 2 is graphene molecules adsorption process monitoring result in embodiment: (a) Graphene backgate field-effect transistor dirac point versus time curve；Before (b) laser treatment, the transfer characteristic curve of device；C, in the different time after () laser treatment, the transfer characteristic curve of device, the curve corresponding to time lengthening is as shown by arrows, it is seen that As time goes on, and transfer characteristic curve is toward moving right；D the 338th minute measured transfer characteristic curve after () graphene device laser treatment, now transfer characteristic curve does not change over time, and namely Molecular Adsorption reaches saturated.
Detailed description of the invention
Below by example, the present invention will be further described.It should be noted that the purpose publicizing and implementing example is in that help is further appreciated by the present invention, but it will be appreciated by those skilled in the art that: in the spirit and scope without departing from the present invention and claims, various substitutions and modifications are all possible.Therefore, the present invention should not be limited to embodiment disclosure of that, and the scope that the scope of protection of present invention defines with claims is as the criterion.
The monitoring method of graphenic surface gas molecule adsorption process provided by the invention, specifically includes following steps:
(1) preparation of grapheme material
Utilize mechanical stripping method to prepare Graphene, select adhesive tape, repeatedly peel off highly oriented 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, method in conjunction with electron beam exposure (EBL) and oxygen plasma etch (ICP), Graphene graphically and is defined source-drain electrode, recycle the method evaporation metal of electron beam evaporation and peel off, complete the preparation of source and drain metal electrode, between source-drain electrode, be the channel region of transistor.
(3) electrical performance testing before backgate device laser treatment
Sample puts sample on room temperature probe station, and tests the transfer characteristic curve of Graphene backgate field-effect transistor with Semiconductor Parameter Analyzer, and namely source-drain current is with the change curve (I-Vg) of back gate voltage.
(4) channel region is carried out laser treatment, make graphenic surface Gas desorption
Sample is positioned over below the laser emitting mouth of Raman spectrum system, with < mental retardation of 2mW focuses on laser beam, finds the particular location of pending sample surfaces under the microscope.With the graphite Raman spectrogram before the laser beam acquisition process of 2mW.Then with high-energy focusing laser beam irradiation sample surfaces a period of time of 30mW, Gas desorption is made.Open the graphite Raman spectrogram after process with the laser beam collection of 2mW again, contrast with processing front spectrum, it is judged that grapheme material is had not damaged by processing procedure, namely occurs with or without D peak.
(5) electrical performance testing after backgate device laser treatment
Treating that laser treatment is complete, be placed on probe station by sample rapidly that the transfer characteristic of test Graphene backgate device and at regular intervals, test one transfer characteristic curve, the transfer characteristic curve until front and back twice does not change.
(6) the graphenic surface gas absorption time
All transfer characteristic curves before and after laser treatment are plotted in same figure and contrast, analyze the electric property situation of change of graphene device, before utilizing laser treatment cleaning graphenic surface, the dirac point (position corresponding to electric current minimum point) of graphene device is generally at Vbg> 0V region, device p-type is adulterated by this because of graphenic surface binding molecule；When, after laser treatment, during beginning, dirac point can to Vbg=0V moves position, illustrates that p-type doped source reduces；But prolongation over time, dirac point position moves right gradually, and p-type doping increases the weight of, and when dirac point no longer moves, namely the gas molecule absorption of graphenic surface reach saturated.
Although the present invention discloses as above with preferred embodiment, but is not limited to the present invention.Any those of ordinary skill in the art, without departing from, under technical solution of the present invention ambit, may utilize the method for the disclosure above and technology contents and technical solution of the present invention is made many possible variations and modification, or be revised as the Equivalent embodiments of equivalent variations.Therefore, every content without departing from technical solution of the present invention, the technical spirit of the foundation present invention, to any simple modification made for any of the above embodiments, equivalent variations and modification, all still falls within the scope of technical solution of the present invention protection.
Claims (3)
1. the monitoring method of a graphenic surface gas molecule adsorption process, it is characterised in that comprise the steps:
(1) preparing graphene device sample, this graphene device includes source and drain metal electrode and graphene-channel；
(2) graphene device sample is positioned over below the laser emitting mouth of Raman spectrum system optical microscope, adjusts graphene device sample position in field of microscope, regulate microscope focus, and focus on graphene-channel surface；
(3) with low-energy focusing laser beam be directed at graphene-channel surface, now laser intensity should at below 3mW, to ensure that laser spot is only small, registration；
(4) with high-octane laser beam irradiation or scanning Graphene sample surfaces, controlling laser intensity and time, removing the empty gas and water equimolecular of graphenic surface, thus cleaning graphenic surface；
(5) Graphene sample is put on probe station, and utilize Semiconductor Parameter Analyzer repeatedly to test the transfer characteristic curve of graphene device, till the transfer characteristic curve of front and back twice is unchanged, and according to this estimation Graphene from cleaning surface to by the time needed for the saturated adsorption process of molecule.
2. the monitoring method of graphenic surface gas molecule adsorption process as claimed in claim 1, it is characterised in that in step (4), high-octane laser beam intensity ranges for 10～40mW, and the time is within 10min to 5s scope.
3. the monitoring method of graphenic surface gas molecule adsorption process as claimed in claim 1, it is characterised in that in step (5), the device electric property of detection is I-VgThe position of curve and dirac point.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610137360.5A CN105762090B (en) | 2016-03-10 | 2016-03-10 | A kind of monitoring method of graphene surface gas molecule adsorption process |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610137360.5A CN105762090B (en) | 2016-03-10 | 2016-03-10 | A kind of monitoring method of graphene surface gas molecule adsorption process |
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| CN105762090A true CN105762090A (en) | 2016-07-13 |
| CN105762090B CN105762090B (en) | 2018-08-10 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113866095A (en) * | 2021-10-20 | 2021-12-31 | 浙江大学衢州研究院 | In-situ spectral analysis pool for gas-sensitive sensing exploration and application |
| WO2023108696A1 (en) * | 2021-12-16 | 2023-06-22 | 深圳市华星光电半导体显示技术有限公司 | Organic electroluminescent module and packaging method therefor, and display device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102590309B (en) * | 2012-02-03 | 2014-04-02 | 游学秋 | Manufacture and application method for graphene transistor and biosensor of graphene transistor |
| CN104142207B (en) * | 2014-08-05 | 2016-08-24 | 温州大学 | Vacuometer based on gas absorption and carbon nano tube field-emission principle and vacuum detecting method thereof |
| CN104181209A (en) * | 2014-08-14 | 2014-12-03 | 电子科技大学 | Nitrogen dioxide gas sensor and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113866095A (en) * | 2021-10-20 | 2021-12-31 | 浙江大学衢州研究院 | In-situ spectral analysis pool for gas-sensitive sensing exploration and application |
| WO2023065673A1 (en) * | 2021-10-20 | 2023-04-27 | 浙江大学衢州研究院 | In-situ spectral analysis cell for gas sensing exploration and application |
| WO2023108696A1 (en) * | 2021-12-16 | 2023-06-22 | 深圳市华星光电半导体显示技术有限公司 | Organic electroluminescent module and packaging method therefor, and display device |
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| CN105762090B (en) | 2018-08-10 |
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