CN103579419B - A kind of Graphene/MoS2/ Si hetero-junction thin-film solar cell and preparation method thereof - Google Patents
A kind of Graphene/MoS2/ Si hetero-junction thin-film solar cell and preparation method thereof Download PDFInfo
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- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 97
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 97
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 56
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000010409 thin film Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
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- 235000012239 silicon dioxide Nutrition 0.000 claims description 23
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- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Inorganic materials [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 claims description 2
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/305—Sulfides, selenides, or tellurides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
- H01L31/06—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices characterised by at least one potential-jump barrier or surface barrier
- H01L31/072—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices characterised by at least one potential-jump barrier or surface barrier the potential barriers being only of the PN heterojunction type
- H01L31/074—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices characterised by at least one potential-jump barrier or surface barrier the potential barriers being only of the PN heterojunction type comprising a heterojunction with an element of Group IV of the Periodic System, e.g. ITO/Si, GaAs/Si or CdTe/Si solar cells
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The present invention relates to a kind of Graphene/MoS2/ Si hetero-junction thin-film solar cell and preparation method thereof.Gas is used to carry liquid phase MoS2The chemical gaseous phase depositing process of molecule, can preferably control flow and response speed, obtains the MoS ultra-thin, large area is uniform, surfacing roughness is the least2Thin film, effectively reduces p MoS2The interface special type of/n Si hetero-junctions, reduces leakage current, improves the photoelectric transformation efficiency of solaode.The graphene film that the large area utilizing chemical gaseous phase depositing process to obtain is uniform, transparent and electric conductivity is good is as transparency conductive electrode, MoS2/ Si hetero-junctions has the strongest collecting action to light induced electron, hole, improves photovoltaic effect and the conversion efficiency of solaode.The solaode that the present invention provides is under 100 mW white light, and its open-circuit voltage reaches 0.98V, and short circuit current reaches 4.6 mA, and light energy use efficiency reaches 4.5%.
Description
Technical field
The present invention relates to a kind of solaode, particularly to a kind of Graphene/MoS2/ Si heterojunction solar battery and
Its preparation method.
Background technology
MoS2, be also called brightness molybdenum, the black solid material of metal luster under room temperature, have excellence chemical stability,
Heat stability (fusing point 1185 DEG C) and lubricity, be generally used for machinery, the face coat of cutting element or lubricant.In structure,
Brightness molybdenum is the graphite laminate structure of hexagonal closs packing, and layer combines by the van der waals force of weak interaction with interlayer.With stone
The Graphene that ink is easily peeled off as monoatomic layer is similar, peels off brightness molybdenum by micromechanics and also easily becomes monolayer MoS2Film [S.
Bertolazzi, J. Brivio, A. Kis, Stretching and Breaking of Ultrathin MoS2, ACS
Nano, V. 5(12): 9703-9709, 2011.].Monolayer MoS2 is the regular hexagon that S-Mo-S tri-atom covalence bond is closed
Planar structure, thickness is only 0.65nm.
Block MoS2For indirect band gap (1.2eV) quasiconductor, due to quantum confined effect, monolayer MoS2It is changed into directly band
Gap (1.8eV) [K. F. Mak, C.Lee, J. Hone, J. Shan, T. F. Heinz, Atomically thin
MoS2: a new direct-gap semiconductor. Phys. Rev. Lett. V.105: 136805-08,
2010].Being direct band gap by indirect band gap transitions, photon transition gain can improve～104, make monolayer MoS2To visible ray (300-
700 nm) have catch light absorbance and light emission efficiency [G. Eda, H. Yamaguchi, D. Voiry, T. Fujita,
M. Chen, M. Chhowalla, Correction to Photoluminescence from Chemically
Exfoliated MoS2, Nano Lett.V. 12(1), 526–526, 2012.]。
Silicon solar cell (monocrystal silicon, polysilicon, non-crystalline silicon) occupies with advantages such as mature preparation process, life-span length always
The market share of more than 90%.But Si is indirect band-gap semiconductor, efficiency of light absorption is the lowest, makes commercialization silicon solar cell
Conversion efficiency is generally less than 20%.Relatively low conversion efficiency and higher cost have become the bottleneck of solar cell, seriously limit
The development of photovoltaic industry.It is known that the conversion efficiency of solaode is to be determined by the photovoltaic effect of quasiconductor.Therefore,
Searching has notable photovoltaic effect, low-cost solar battery material, it is achieved high conversion efficiency has become current solaode
The main direction of research field.
Si is indirect band-gap semiconductor, and efficiency of light absorption is the lowest, it addition, the absorption peak wavelength of silicon is 930 nm, the reddest
The radiation of outer wave band has preferably absorption, and relatively weak to the visible absorption of 300-700 nanometer.Make silicon solar cell
Conversion efficiency is relatively low.Monolayer MoS2Having the strongest absorption at 400～700nm visible light wave ranges, its absorption spectra just absorbs with Si
Spectrum defines mutual supplement with each other's advantages, covers whole visible ray and near infrared band.If by monolayer MoS2Contact with Si, form MoS2/
Si hetero-junctions can greatly strengthen the device absorption at visible light wave wave band, significantly improves device photovoltaic effect and opto-electronic conversion effect
Rate, prepares high efficiency MoS2/ Si heterojunction solar battery.
Graphene is a kind of monolayer two being only 0.35 nm by carbon atom with the thickness of the tight storehouse of hexagonal cells
Dimension (2D) cellular crystal.Graphene is to be known as material the thinnest, the hardest, that conduction velocity of electrons is the fastest in the world.It carries
Stream transport factor is up to 2 × 105cm2/ v is higher than electron mobility in silicon 100 times.Graphene also has good optical property,
Transmission of visible light is up to 98.5%, can be used for nesa coating and solaode.Therefore, at MoS2/ Si heterojunction solar
In battery, Graphene can be used as transparent conductive film.
Summary of the invention
It is an object of the invention to the deficiency overcoming prior art to exist, it is provided that one can be effectively improved photoelectric transformation efficiency
Graphene/MoS2/ Si heterojunction solar battery and preparation method thereof.
The technical scheme realizing the object of the invention is to provide a kind of Graphene/MoS2/ Si hetero-junction thin-film solar cell
Preparation method, comprise the steps:
(1) substrate cleans: withn-Si (111) sheet is substrate, removes the silicon dioxide on Si surface by dilute HF acid soak, then
Successively by acetone, ethanol, deionized water ultrasonic waves for cleaning, remove the Organic substance on silicon chip, dry up with nitrogen, put into quartz ampoule and enter
Row deposition processes；The vacuum of quartz ampoule is 10-2Pa, is heated to 300 DEG C and maintains 10 minutes, to remove the water of silicon chip surface
Vapour；
(2) MoS2Film preparation: quartz ampoule is heated to 500～600 DEG C, with argon as carrier gas, is passed through with dilute
Sulphuric acid is the MoS of solvent2Solution, at described MoS2Solution adds Al (NO3)3Solution, with Al (NO3)3As Al adulterant
To MoS2Carry out p-type doping, in mass ratio, MoS2:Al(NO3)3For 1:20～1:50；Gas carries MoS2With Al (NO3)3Enter
Quartz ampoule existsn-Si (111) sheet carries out adsorbing, nucleation and growth 5～after 10 minutes, quartz ampoule is warmed up to 950 DEG C and moves back
Fire processes, and annealing time is 20～40 minutes, obtains MoS2/ Si pn-junction；
(3) quartz ampoule temperature being maintained 950 DEG C, methane is decomposed into carbon atom and hydrogen, flows at argon 10～30 sccm
Under the vapor transportation effect of amount, carbon atom arrives established MoS2The MoS of/Si pn-junction2Surface is also adsorbed to surface, at lining
Basal surface migrate after in substrate surface nucleation, then attract other carbon atom by whose van der Waals attraction, and with the carbon of bonding
Atom forms the cancellated graphene film of hexagonal；
(4) rightnThe lower surface AM aluminum metallization electrode of-Si (111) sheet, forms the negative electrode of solaode, obtains a kind of graphite
Alkene/MoS2/ Si heterojunction solar battery.
Technical solution of the present invention also includes the Graphene/MoS prepared as stated above2/ Si hetero-junction thin-film the sun
Can battery.
The beneficial effect of technical solution of the present invention: carry liquid phase MoS owing to have employed gas2The chemical gaseous phase deposition of molecule
Method, can preferably control flow and response speed, obtains the MoS ultra-thin, large area is uniform, surfacing roughness is the least2
Thin film, such that it is able to effectively reduce p-MoS2The interface special type of/n-Si hetero-junctions, reduces leakage current, improves solaode
Photoelectric transformation efficiency.Meanwhile, large area is uniform, transparent and electric conductivity is good to utilize chemical gaseous phase depositing process to obtain
Graphene film.
Accompanying drawing explanation
Fig. 1 is Graphene/p-MoS that the embodiment of the present invention provides2The structural representation of/n-Si heterojunction solar battery
Figure；
Fig. 2 is Graphene/MoS that the embodiment of the present invention provides2The band structure signal of/Si heterojunction solar battery
Figure；
Fig. 3 is Graphene/MoS that the embodiment of the present invention provides2The operation principle of/Si heterojunction solar battery；
Fig. 4 is the MoS that the embodiment of the present invention provides2Thin film uses the structural representation of chemical gas-phase deposition system device；
Fig. 5, Fig. 6 and Fig. 7 are the MoS that the embodiment of the present invention utilizes chemical gaseous phase depositing process to prepare respectively2The table of thin film
Face pattern, x-ray diffraction pattern and Raman spectrogram；
Fig. 8 is the MoS that the embodiment of the present invention utilizes chemical gaseous phase depositing process to prepare2The optical absorption spectra figure of thin film；
Fig. 9 is the MoS that the embodiment of the present invention provides2MoS in/Si hetero-junctions2The current-voltage characteristics curve of film surface
Figure；
Figure 10, Figure 11 and Figure 12 are that the surface atom force microscope of the graphene film that the embodiment of the present invention provides shines respectively
Sheet, Raman spectrum and ultraviolet-visible light transmission spectrum；
Figure 13 is Graphene/MoS that the embodiment of the present invention provides2The dark electricity of/Si heterojunction solar battery is unglazed photograph
Stream-voltage characteristic curve figure；
Figure 14 is Graphene/MoS that the embodiment of the present invention provides under 100mW white light2The electricity of/Si solaode
Piezo-electric stream characteristic curve diagram；
Figure 15 is Graphene/MoS that the embodiment of the present invention provides under 100mW white light2The sound of/Si solaode
Answer curve chart；
In figure, 1, Graphene electrodes；2、p-MoS2Thin layer；3, n-Si conductive layer；4, Al electrode.
Detailed description of the invention
Technical solution of the present invention is further elaborated with embodiment below in conjunction with the accompanying drawings.
Embodiment 1
Seeing accompanying drawing 1, it is Graphene/MoS that the present embodiment provides2The structural representation of/Si heterojunction solar battery
Figure, it includes Graphene electrodes 1, p-MoS2Thin layer 2, n-Si layer 3 and Al electrode 4；In Fig. 1, Graphene electrodes is this sun
The anode of energy battery, p-MoS2The core cell that pn-junction is the conversion of this solar cell photoelectric constituted with n-Si layer, Al electrode
Negative electrode for this solaode.
Utilize chemical gaseous phase depositing process at n-type silicon chip (111) the ultra-thin MoS of upper growth2Thin film (several atomic layer), and
Utilizing Al atom to be doped in its growth course makes its conduction type become p-type, forms p-n with n-type silicon chip substrate contact
Knot.In p-type MoS2The graphene film of film surface recycling chemical gaseous phase depositing process 10～20 atomic layers thick of growth, should
Layer graphene thin film and MoS2/ Si pn-junction collectively forms Graphene/p-MoS2/ n-Si heterojunction solar battery.
Seeing accompanying drawing 2, it is MoS2The band structure schematic diagram of/Si pn-junction solaode；Fig. 2 (a) the right and left divides
It is not MoS2Band structure before contacting with Si.Wherein,E 0 For vacuum level,W m For MoS2Work function,F fm For MoS2Take
Rice energy level,E cm 、E vm 、EgmIt is MoS respectively2Conduction band, valence-band level and band gap, χ m For MoS2Electron affinity.W s For Si
Work function,E cs 、E vs 、E gs It is the conduction band of Si, valence-band level and band gap respectively, χ s For the electron affinity of Si,F fs For Si
Fermi level.ΔEc、ΔEvIt is MoS respectively2Conduction band and the energy level difference of valence band with Si.
MoS2Work functionW m =E 0-E fm =4.6 eV, silicon chip work functionW s =E 0-E fs =χ+[E c -E fs ], for Si, χ=
4.05 eV. E c -E fs Depend on the carrier concentration in silicon chip and doping type.The band gap of Si E g It is 1.12 eV, therefore,n-
Si, W m >W s . due to MoS2Work function more than the work function of Si, i.e.W m >W s , after the two contact, as shown in Fig. 2 (b), Si
The hole on sheet surface will be to MoS2Flowing in side, Si sheet surface leaves Immobile anion (positive center), forms space electricity
Lotus layer.Owing to the electronics of n side moves to MoS2Side, makesn-Si sheet surface forms electronics and piles up, and forms positive potential, makes conduction bandE cs , valence bandE vs End point bent upward, such as Fig. 2 (b).qV D For MoS2The barrier height of-Si hetero-junctions.MoS2Withp-type silicon face
Form p-n junction, form MoS2/ Si heterojunction solar battery.
Graphene/MoS that the present embodiment provides2The photoelectricity transformation principle of/Si heterojunction solar battery sees accompanying drawing 3.
Shown in figure, graphene layer, MoS2Thin film, p-MoS2The space-charge region of/n-Si interface composition and n-Si substrate, its photoelectricity turns
Change principle as follows:
The absorbance of Graphene is the highest, and under illumination, the light transmission Graphene of more than 85% is irradiated to MoS2Thin film, at MoS2
Surface produces electron hole pair, when the diffusion length of light induced electron is more than MoS2The thickness of thin film and be diffused into MoS2/ Si hetero-junctions
During edge, at hetero-junctions space-charge region internal electric fieldE mS Effect under light induced electron swept to rapidlyn-Si district, at n-Si table
Face forms electron accumulation；MoS2The photohole of middle generation is then swept to MoS2Surface, forms hole accumulation layer.Therefore, illumination is produced
The hole of life, electronics are respectively at MoS2Surface andn-Si forms accumulation, makes MoS2/ Si knot both sides form voltage difference, this voltage difference
It is the voltage difference that illumination produces under without extraneous bias effect, therefore there is photovoltaic effect.
Due to ultra-thin MoS2After the most several atomic layers, some light can also pass through MoS2Layer and entern-Si layer is again
Absorbed (spy is standby is the near infrared radiation near 900nm) by Si layer, produce electron hole pair, when hole is diffused into MoS2/Si
During hetero-junctions border, sweep under pn hetero-junctions built in field effectp-MoS2, light induced electron then existsn-Si face is accumulated.
MoS2/ Si hetero-junctions both sides produce voltage difference further, and produce photovoltaic effect.This photovoltaic effect is by photovoltaic effect above
It is overlapped.
During heterojunction solar battery photovoltaic effect is formed, MoS2Built in field in/SiE mS Play
Accelerate the effect of electron motion.Compared with traditional silicon pn-junction solaode, this heterojunction solar battery has double suction and produces effects
Should, MoS2The light radiation of main absorption 300～700nm, Si mainly absorbs the radiation of near infrared band, adds solaode
Absorbance and internal quantum efficiency, significantly increase photovoltaic effect, thus be greatly enhanced conversion efficiency.By measuring this device
Open-circuit voltageV oc And short-circuit current densityJ sc , it is possible to calculate the energy conversion efficiency of double-junction solar battery.
Seeing accompanying drawing 4, it is that the present embodiment uses chemical vapor deposition (CVD) method to prepare MoS2The apparatus structure of thin film shows
It is intended to.This device is made up of four parts: quartz ampoule constitute reactive deposition room, vacuum-pumping system, mass-flow gas meter and
Temperature control system.Backing material use resistivity be 3～5 Ω cm, crystal orientation (111)nType silicon (Si) sheet, a size of 12
×12 mm2×500 μm。
Preparation method comprises the steps:
Substrate cleans: first within 15 minutes, remove the silicon dioxide on Si surface by dilute HF acid soak, more successively by acetone, second
Alcohol, deionized water ultrasonic waves for cleaning, remove the Organic substance on silicon chip, finally dry up with nitrogen, be then placed in quartz ampoule.Deposit it
Before, quartz ampoule vacuum is evacuated to 10-2Pa, is heated to 300 DEG C and maintains 10 minutes, to remove the steam of silicon chip surface.
MoS2Film preparation: quartz ampoule is heated to 500 DEG C, with Ar gas as carrier gas, is passed through analytical pure MoS2Molten
Liquid (dilute sulfuric acid is solvent).And with analytical pure Al (NO3)3As Al adulterant to MoS2Carry out p-type doping.In order at MoS2Thin
It is doped, at MoS while film growth2Solution adds Al (NO with the mass ratio of 1:203)3Solution.Argon carries MoS2And Al
(NO3)3Enter quartz ampoule to existn-Si (111) sheet carries out adsorbing, nucleation and growth 10 minutes, then quartz ampoule is raised to 950 DEG C
Make annealing treatment, annealing time 30 minutes.
Electrode fabrication: Graphene is the nesa coating that a kind of electric conductivity is fabulous, has fabulous electric conductivity, can be as too
As anode in sun energy battery.The growth of Graphene: quartz ampoule temperature is still maintained at 950 DEG C, methane is at 800～950 DEG C of high temperature
Under be decomposed into carbon atom and hydrogen, under the vapor transportation effect of argon 10 sccm (10～30 sccm) flow, carbon atom arrives
Reach established MoS2The MoS of/Si pn-junction2Surface is also adsorbed to surface, last at substrate table after substrate surface migrates
Face nucleation, then attract other carbon atom by whose van der Waals attraction, and bonding forms the cancellated graphite of hexagonal therewith
Alkene thin film.Under normal circumstances, in the case of reactant abundance, the speed of the deposit thin film of CVD is the fastest.At this
In embodiment, the methane flow of employing is the least, and carbon atom the most a small amount of in the unit interval arrives silicon chip surface, anti-by controlling
At 5～10 minutes between Ying Shi, it is possible to obtain ultra-thin graphene film.After having reacted, quartz ampoule temperature is raised to 950～
1000 DEG C, sample is annealed 10 minutes.After having annealed, quartz ampoule is waited to take out sample after naturally cooling to room temperature.
Lower surface AM aluminum metallization electrode to n-silicon chip, forms the negative electrode of solaode.Complete Graphene/MoS2/ Si is different
The preparation of matter joint solar cell.
Graphene/the MoS that will prepare2/ Si heterojunction solar battery carries out surface topography and photovoltaic effect is measured,
Atomic force microscope, current/voltage test device and Hall effect is utilized to analyze surface topography and the photocurrent characteristics of this device.
Membrane structure application Raman spectrum is observed, and with ultraviolet-visible light (UV-vis) spectrophotometer (Shimadzu UV-
3600) transmitance of sample, last Graphene/MoS are analyzed2The photocurrent characteristics application of/Si heterojunction solar battery
Keithley 4200 SCS measures.
Seeing accompanying drawing 5～7, Fig. 5 is onenMultilamellar MoS of preparation on Si sheet2The typical atomic force microscope of thin film
Photo.It can be seen that many MoS2Small pieces are evenly distributed in Si sheet surface.This layer of MoS2The thickness of thin film about 5～10 nm,
Be equivalent to ten several atomic layers thick.Fig. 6 is prepared MoS2The x-ray diffraction pattern of thin film.Find 13.482 °,
32.997 °, 47.786 °, 14.460 °, 33.212 °, have 6 diffraction the strongest to meet, with MoS at 47.898 ° of 2 θ angle2Brilliant
The XRD standard card contrast of body, the most corresponding MoS of above diffraction maximum2 (002)、(104) 、(100)、 (105) (106)、
(110) diffraction peak of crystal face matches substantially, and the MoS of growth is described2Thin film is the MoS of polycrystalline2Thin film.Fig. 7 is prepared
MoS2The Raman spectrum of thin film.Figure has 2 Raman vibration peak the strongest, is positioned at 385.5 cm−1Vibration peak correspondence E1 2gFlat
In plane vibration pattern, and it is positioned at 408.1cm-1Then corresponding (A1g) the outer vibration mode of plane. E1 2gAnd A1gFor MoS2Typically
Vibration mode, further demonstrate that MoS2The existence of structure. it addition, A1gAnd E1 2gThe alternate position spike (Δ) of pattern may be used for
Rough estimate MoS2 The thickness of thin film, Δ is the biggest, MoS2 The thin film number of plies is the most.Generally monolayer MoS2 The two pattern of film
Alternate position spike Δ be 18.In our sample, the two pattern Δ is 22.6, illustrates the MoS that the present embodiment grows2 Thin film is many
Tunic.
Seeing accompanying drawing 8, it is prepared MoS2 The visible absorption spectrum of thin film.UV-3600 spectrophotometric is utilized to measure
Measure prepared MoS2Film sample absorption spectra.It can be seen that molybdenum sulfide is to the visible ray between 300 ~ 700 nm wavelength
Having the strongest absorption, this shows that molybdenum sulfide can be used as good light absorbing material.During more than 732 nm, absorption intensity subtracts rapidly
Little.Then 732nm is the absorption limit of molybdenum sulfide thin film, the relation according between semi-conducting material band gap width and wavelength: Eg=1.24/λ
(eV) band gap width that can obtain prepared molybdenum sulfide thin film is 1.69 eV.The band gap width of monolayer molybdenum bisuphide
(1.8eV), owing to the band gap width of molybdenum sulfide can reduce with the increase of the number of plies, so the band gap width drawn in Shi Yan is relatively
Little.
Seeing accompanying drawing 9, it is the surface I-V characteristic of prepared molybdenum sulfide thin film, tests by HMS-3000 Hall effect
Instrument measures the conductive characteristic on the surface of molybdenum sulfide thin film.Voltage Vab、Vbc、Vcd、VdaBe respectively molybdenum sulfide film surface a, b, c,
Voltage between tetra-symmetry electrodes of d.It can be seen that these four interelectrode voltages and the added approximately linear relation of electric current I,
Embody molybdenum sulfide thin film and there is good surface conductance characteristic.Rise and fall or interelectrode non-right because sample surfaces exists some
Title property causes straight line to produce a little fluctuation.The Hall coefficient R that Hall effect is measuredHPositive and negative values may infer that the conductive-type of sample
Type, the R of the sample that the present invention providesHIt is 1.830 × 107, illustrate that molybdenum sulfide thin film, by Al doping in situ, presents p-type special
Property.
Seeing accompanying drawing 10～12, Figure 10 is MoS2On thin film, the atomic force microscope of the graphene membrane electrode of preparation is shone
Sheet.It can be seen that many grapheme platelet are evenly distributed on substrate.The thickness of graphene film about 3～5 nm, quite
In ten several atomic layers thick.Figure 11 is the Raman spectrum of graphene membrane electrode.This spectrum has 2 significant Raman vibrations
Peak, one is G peak, is positioned at 1590 cm-1At wave number, this peak is the eigen vibration peak of graphite；Another is positioned at 2690 for 2D peak
cm-1At wave number, according to document announcement, this peak position is the eigen vibration peak of Graphene.The strength ratio at the two peak isI 2D : I G=
2.8, this ratio is the biggest, illustrates that Graphene contained in thin film is the biggest, and graphite-phase is little；Also the explanation present invention utilizes low gas
The quality of graphene film prepared by pressure, the chemical gaseous phase depositing process of low discharge is good.Figure 12 be graphene membrane electrode can
See that light transmission spectrum is composed, the light transmission spectrum of the graphene film that it provides for the present embodiment.The light transmission rate of its visible region reaches
To more than 80%.It addition, its light transmission rate is with the most certain change of wavelength change.To longer wavelength 600 800 nm wave band,
Transmitance is more than 85%, and the high permeability of this spectrum segment can be effectively improved the conversion efficiency of solaode.And utilize Hall to imitate
Answer carrier concentration and the electron mobility of apparatus measures graphenic surface.The load on the graphene film surface that we are prepared
Flowing sub-concentration is 1010 cm-2, electron mobility is 9.5 × 104 cm2 V-1 s-1, this value and the ideal value 2 × 10 of Graphene5
cm2 V-1 s-1Closely, the good conductivity of graphene film prepared by the present invention is described.
See accompanying drawing 13, Graphene/MoS that it provides for embodiment2The dark current characteristic of/Si heterojunction solar battery
(without light characteristics) curve chart；Result shows, this device has good rectification characteristic, with the rising of applied voltage, electric current in
Exponential increase.And under reverse biased, its reverse drain saturation current is the least, almost nil.
Seeing accompanying drawing 14, it is at 100 mW cm-2Graphene/MoS that under white light, the present embodiment provides2/ Si is heterogeneous
The photocurrent characteristics curve chart of joint solar cell.It can be seen that the open-circuit voltage of this solaodeV ocFor 0.89V, short
Road electric current densityJ scIt is 4.6 mA cm-2. it can be calculated that this Graphene/MoS2The energy of/Si heterojunction solar battery turns
Changing efficiency is 4.5%.
Seeing accompanying drawing 15, it is figure time response of the solaode that the present embodiment provides.It can be seen that in illumination
Under, this device has steep rising edge；When removing illumination, there is vertical trailing edge, and repeatability is very well.Current switch
RatioI on/ I offMore than 103.Showing that this response device speed of light is fast, repeatability is high, can be as high performance optical detection and photoelectricity
Sub-device.
Claims (2)
1. Graphene/MoS2The preparation method of/Si hetero-junction thin-film solar cell, it is characterised in that include walking as follows
Rapid:
(1) substrate cleans: withn-Si (111) sheet is substrate, removes the silicon dioxide on Si surface by dilute HF acid soak, more successively
By acetone, ethanol, deionized water ultrasonic waves for cleaning, remove the Organic substance on silicon chip, dry up with nitrogen, put into quartz ampoule and sink
Long-pending process；The vacuum of quartz ampoule is 10-2Pa, is heated to 300 DEG C and maintains 10 minutes, to remove the steam of silicon chip surface；
(2) MoS2Film preparation: quartz ampoule is heated to 500～600 DEG C, with argon as carrier gas, is passed through with dilute sulfuric acid
MoS for solvent2Solution, at described MoS2Solution adds Al (NO3)3Solution, with Al (NO3)3As Al adulterant pair
MoS2Carry out p-type doping, in mass ratio, MoS2:Al(NO3)3For 1:20～1:50；Gas carries MoS2With Al (NO3)3Enter stone
English pipe existsn-Si (111) sheet carries out adsorbing, nucleation and growth 5～after 10 minutes, quartz ampoule is warmed up to 950 DEG C and anneals
Processing, annealing time is 20～40 minutes, obtains MoS2/ Si pn-junction；
(3) quartz ampoule temperature being maintained 950 DEG C, methane is decomposed into carbon atom and hydrogen, at argon 10～30 sccm flow
Under vapor transportation effect, carbon atom arrives established MoS2The MoS of/Si pn-junction2Surface is also adsorbed to surface, at substrate table
Face migrate after in substrate surface nucleation, then attract other carbon atom by whose van der Waals attraction, and with the carbon atom of bonding
Form the cancellated graphene film of hexagonal；
(4) rightnThe lower surface AM aluminum metallization electrode of-Si (111) sheet, forms the negative electrode of solaode, obtain a kind of Graphene/
MoS2/ Si heterojunction solar battery.
2. Graphene/the MoS prepared by claim 12/ Si hetero-junction thin-film solar cell.
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