CN105762090B - A kind of monitoring method of graphene surface gas molecule adsorption process - Google Patents
A kind of monitoring method of graphene surface gas molecule adsorption process Download PDFInfo
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- CN105762090B CN105762090B CN201610137360.5A CN201610137360A CN105762090B CN 105762090 B CN105762090 B CN 105762090B CN 201610137360 A CN201610137360 A CN 201610137360A CN 105762090 B CN105762090 B CN 105762090B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 19
- 238000012544 monitoring process Methods 0.000 title claims abstract description 17
- 238000012546 transfer Methods 0.000 claims abstract description 16
- 239000000523 sample Substances 0.000 claims description 20
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 238000012360 testing method Methods 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 4
- 239000004065 semiconductor Substances 0.000 claims description 4
- 238000001237 Raman spectrum Methods 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 238000004140 cleaning Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 21
- 238000013532 laser treatment Methods 0.000 description 9
- 238000001069 Raman spectroscopy Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- -1 Graphite Alkene Chemical class 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 230000005669 field effect Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000000463 material Substances 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
- 239000004575 stone Substances 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 239000002390 adhesive tape Substances 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
- 229910052799 carbon Inorganic materials 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
- 239000003292 glue Substances 0.000 description 1
- 238000012625 in-situ measurement Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000004519 manufacturing process 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
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Physics & Mathematics (AREA)
- Ceramic Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Carbon And Carbon Compounds (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a kind of monitoring methods of graphene device surface gas Molecular Adsorption process, this method mainly passes through the transfer characteristic of monitoring graphene device, especially dirac point position, monitor the gas absorption dynamic process of graphene surface in device in real time, the overall process that i.e. saturation is adsorbed from cleaning graphene surface to molecule, and more can accurately measure process required time.
Description
Technical field
The present invention proposes a kind of monitoring method of graphene surface gas molecule adsorption process, can be used in short-term environment
The dynamic process of lower real time monitoring graphene device surface gas Molecular Adsorption, estimation graphene device surface is completely by gas point
The time of son absorption has application prospect in fields such as chemistry, physics, materialogy, micro-nano electronics.
Background technology
Graphene is two dimensional surface crystalline material, integrates a variety of excellent specific properties, has the property such as good mechanics, electricity
Matter and wide application prospect.The sensor based on graphene causes strong concern, only graphene thickness only one recently
Carbon atom, and have the specific surface area of super large, 2630m can be reached2/ g has excellent gas molecule absorption property.
Graphene film is detected to what gas molecule adsorbed mainly by the conductance before and after detection gas Molecular Adsorption at present
Variation.Gaseous molecular adsorbate has different the Nomenclature Composition and Structure of Complexes, can be interacted in different patterns from graphene.Graphite
Alkene is usually in p-type semiconductor under atmospheric environment, and when it is exposed to various other gases, the response direction of conductance may
It is different.Such as NO2The electron concentration concentration of graphene can be changed in absorption (as a kind of doping) on the surface of graphene, to
Change the conductance of graphene, the i.e. detectable NO of detection conductance variation2。
Invention content
It, can real-time dynamic monitoring graphene device surface gas Molecular Adsorption mistake present invention aims at a kind of method is provided
Journey.
The present invention can be achieved through the following technical solutions：
A kind of monitoring method of graphene surface gas molecule adsorption process, includes the following steps：
(1) graphene device sample is prepared, which includes source and drain metal electrodes and graphene-channel；
(2) sample is positioned over below the laser emitting mouth of Raman spectrum system light microscope.Adjustment sample position arrives
In field of microscope, microscope focus is adjusted, and focus on graphene-channel surface；
(3) use the focusing laser beam alignment graphene-channel surface of low energy, at this time laser intensity should in 3mW hereinafter, with
Ensure laser spot very little, registration；
(4) laser beam irradiation or the scanning graphene-channel surface for using higher-energy, control laser intensity and time, removal
The empty gas and water equimolecular on graphene-channel surface, to obtain clean graphene-channel surface；Superlaser beam intensity is 10
~40mW, the time is within the scope of 10min to 5s；
(5) after removing graphene-channel surface molecular, the electrology characteristic of rapid in situ measurement graphene device sample is that is, sharp
With probe station or be integrated in Raman spectrometers probe station and Semiconductor Parameter Analyzer test graphene device transfer characteristic
Curve, i.e. source-drain current with back gate voltage variation.At regular intervals, a transfer characteristic curve is tested, until front and back two
Until secondary transfer characteristic curve does not change.I.e. once closing laser, the gas molecule in air starts to be adsorbed onto stone
On the surface of black alkene raceway groove, to make transfer characteristic (I-Vg) curve of graphene device change, the stone when I-Vg stablizes
Black alkene surface gas Molecular Adsorption reaches saturation immediately；By monitoring graphene device I-Vg curve monitoring graphene devices surface
Gas molecule adsorption process, and by measuring I-Vg curve stabilization process, estimation Molecular Adsorption graphene surface required time.
The technique effect of the present invention is as follows：
(1) present invention can in real time, dynamic monitoring graphene device surface gas Molecular Adsorption process.
(2) this technology can be directed to local graphite alkene surface, be suitable for monitoring graphene device entirety or local desorption mistake
Journey, and monitoring process does not influence the other regions of graphene.
(3) this technology monitors graphene surface from gas molecule by measuring graphene device transfer characteristic curve immediately
It is adsorbed to adsorption saturation overall process, more can accurately measure the time needed for the saturation absorption of graphene device molecule.
Description of the drawings
Fig. 1 graphene backgate field-effect transistors：(a) device surface AFM shape appearance figures, top are device source electrode 1, lower section
For element leakage pole 2；(b) in sample 3 corresponding position of graphene-channel Raman spectrogram, peak intensity ratio I2D/IG~1.
Fig. 2 is graphene molecules adsorption process monitoring result in embodiment：(a) graphene backgate field-effect transistor Di draws
Gram point versus time curve；(b) before laser treatment, the transfer characteristic curve of device；(c) different time after laser treatment
Interior, the transfer characteristic curve of device, the curve corresponding to time lengthening is as shown by arrows, it is seen that over time, transfer
Characteristic curve is past to move right；(d) transfer characteristic curve after graphene device laser treatment measured by the 338th minute, turns at this time
It moves characteristic curve not changing over time, Molecular Adsorption is i.e. up to saturation.
Specific implementation mode
Below by example, the present invention will be further described.It should be noted that the purpose for publicizing and implementing example is to help
It helps and further understands the present invention, but it will be appreciated by those skilled in the art that：The present invention and appended claims are not being departed from
Spirit and scope in, various substitutions and modifications are all possible.Therefore, the present invention should not be limited to interior disclosed in embodiment
Hold, the scope of protection of present invention is subject to the scope defined in the claims.
The monitoring method of graphene surface gas molecule adsorption process provided by the invention, specifically comprises the following steps：
(1) preparation of grapheme material
Graphene is prepared using mechanical stripping method, selects adhesive tape, repeatedly removes highly oriented graphite flakes, and by glue
The graphene taken is transferred to target SiO2On/Si substrates, Si is low-resistance silicon, SiO2For thermal oxide growth, thickness is usually
300nm。
(2) graphically with the preparation of source-drain electrode
By micro fabrication, in conjunction with the method for electron beam exposure (EBL) and oxygen plasma etch (ICP), to graphite
Alkene is graphical and defines source-drain electrode, recycle the method evaporation metal of electron beam evaporation and removes, and completes source and drain metal electrodes
Preparation, be the channel region of transistor between source-drain electrode.
(3) electrical performance testing before backgate device laser treatment
Sample set sample on room temperature probe station, be used in combination Semiconductor Parameter Analyzer test graphene backgate field effect transistor
The transfer characteristic curve of pipe, i.e. source-drain current with back gate voltage change curve (I-Vg).
(4) laser treatment is carried out to channel region, makes graphene surface Gas desorption
Sample is positioned over below the laser emitting mouth of Raman spectrum system, is used<The low energy of 2mW focuses laser beam, aobvious
The specific location of pending sample surfaces is found under micro mirror.With the graphite Raman spectrogram before the laser beam acquisition process of 2mW.
Then the high-energy focusing laser beam irradiating sample surface for using 30mW for a period of time, makes Gas desorption.It is adopted again with the laser beam of 2mW
Collection treated graphite Raman spectrogram, is compared with spectrum before processing, judges that processing procedure has grapheme material
Not damaged, i.e., whether there is or not the appearance of the peaks D.
(5) electrical performance testing after backgate device laser treatment
It waits for that laser treatment finishes, sample is placed on probe station rapidly, test the transfer characteristic of graphene backgate device, and
At regular intervals, a transfer characteristic curve is tested, until front and back transfer characteristic curve twice does not change.
(6) the graphene surface gas absorption time
All transfer characteristic curves before and after laser treatment are plotted in same figure and are compared, graphene device is analyzed
Electric property situation of change, using laser treatment cleaning graphene surface before, (electric current is most for the dirac point of graphene device
Position corresponding to low spot) usually in Vbg>The regions 0V, this adulterates device p-type because of graphene surface binding molecule；When through laser
After processing, dirac point can be to V when beginningbgThe positions=0V are moved, and illustrate that p-type doped source is reduced；But with the extension of time, Di
Clarke point position gradually moves right, and p-type doping aggravates, and when dirac point no longer moves, the gas molecule of graphene surface is inhaled
It is attached to reach saturation.
Although the present invention has been disclosed in the preferred embodiments as above, however, it is not intended to limit the invention.It is any to be familiar with ability
The technical staff in domain, without departing from the scope of the technical proposal of the invention, all using in the methods and techniques of the disclosure above
Appearance makes many possible changes and modifications to technical solution of the present invention, or is revised as the equivalent embodiment of equivalent variations.Therefore,
Every content without departing from technical solution of the present invention is made to the above embodiment any simple according to the technical essence of the invention
Modification, equivalent variations and modification, in the range of still falling within technical solution of the present invention protection.
Claims (2)
1. a kind of monitoring method of graphene surface gas molecule adsorption process, which is characterized in that include the following steps：
(1) graphene device sample is prepared, which includes source and drain metal electrodes and graphene-channel；
(2) graphene device sample is positioned over below the laser emitting mouth of Raman spectrum system light microscope, adjusts graphite
In alkene device example position to field of microscope, microscope focus is adjusted, and focus on graphene-channel surface；
(3) the focusing laser beam alignment graphene-channel surface of low energy is used, laser intensity should be in 3mW hereinafter, to ensure at this time
Laser spot very little, registration；
(4) laser beam irradiation or the scanning graphene sample surface for using high-energy, control laser intensity and time, remove graphene
Air, the hydrone on surface, to clean graphene surface；
(5) graphene sample is put on probe station, and tests turning for graphene device repeatedly using Semiconductor Parameter Analyzer
Move characteristic curve, until until front and back transfer characteristic curve twice is unchanged, and estimate according to this graphene from clean surface to
By the time needed for molecule saturation adsorption process.
2. the monitoring method of graphene surface gas molecule adsorption process as described in claim 1, which is characterized in that step
(4) laser beam intensity of high-energy ranging from 10~40mW in, the time is within the scope of 10min to 5s.
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| CN105762090B true CN105762090B (en) | 2018-08-10 |
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| 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 |
| CN114335378A (en) * | 2021-12-16 | 2022-04-12 | 深圳市华星光电半导体显示技术有限公司 | Organic electroluminescent module, packaging method thereof and display device |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590309A (en) * | 2012-02-03 | 2012-07-18 | 游学秋 | Manufacture and application method for graphene transistor and biosensor of graphene transistor |
| CN104142207A (en) * | 2014-08-05 | 2014-11-12 | 温州大学 | Vacuum gauge based on gas absorption and carbon nano-tube field emission principle and vacuum degree detection method of vacuum gauge |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590309A (en) * | 2012-02-03 | 2012-07-18 | 游学秋 | Manufacture and application method for graphene transistor and biosensor of graphene transistor |
| CN104142207A (en) * | 2014-08-05 | 2014-11-12 | 温州大学 | Vacuum gauge based on gas absorption and carbon nano-tube field emission principle and vacuum degree detection method of vacuum gauge |
| 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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