CN107460438A - A kind of method that the super flat NiO films of large area are prepared based on vapour deposition process - Google Patents

A kind of method that the super flat NiO films of large area are prepared based on vapour deposition process Download PDF

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Publication number
CN107460438A
CN107460438A CN201710538858.7A CN201710538858A CN107460438A CN 107460438 A CN107460438 A CN 107460438A CN 201710538858 A CN201710538858 A CN 201710538858A CN 107460438 A CN107460438 A CN 107460438A
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nio
large area
vapour deposition
nio films
super flat
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陶霞
董雪梅
郑言贞
张想凤
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5846—Reactive treatment
    • C23C14/5853—Oxidation
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
    • H10K30/15—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2
    • 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
    • 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
    • Y02E10/549—Organic PV cells
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • 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

A kind of method that the super flat NiO films of large area are prepared based on vapour deposition process, belongs to organic/inorganic composite material and optoelectronic materials technology.By vacuum evaporation system, be vapor-deposited layer of metal Ni in substrate, fine and close, smooth NiO films is prepared for via high-temperature oxydation, this film has good p-type semiconductor characteristic.The NiO films prepared compared to spin-coating method, the large area NiO surfaces of vapour deposition are more fine and close smooth, and roughness substantially reduces, and are more beneficial for extractions of the NiO to hole, promote efficient separation of charge and transmission.The work provides a kind of brand-new solution to prepare the NiO films of large area even compact.

Description

A kind of method that the super flat NiO films of large area are prepared based on vapour deposition process
Technical field
It is more particularly to a kind of based on vapour deposition the invention belongs to organic/inorganic composite material and optoelectronic materials technology Method prepares the method for the super flat NiO films of large area and its application in solar cells.
Background technology
As increasingly sharpening the problems such as energy crisis, environmental pollution, people are more next to the demand of novel renewable energy It is more notable.Novel renewable energy mainly includes solar energy, waterpower, wind-force, biomass energy, wave energy, tide energy, ocean thermal gradients Can etc..Wherein solar energy is because it there is the advantages such as unlimited, the widely distributed, cleanliness without any pollution of reserves to turn into many new renewable energies Most there is most commonly used one of prospect, research in source.Solar energy is inexhaustible clean energy resource, and it utilizes form Mainly include three kinds of forms：Photo-thermal phenomenon, photovoltaic effect and photochemical transformation.Wherein photovoltaic effect being capable of direct conversion solar Can, and application field is extensive, and this becomes, and solar energy is many to utilize most promising one kind in form.
At present, organic solar batteries and perovskite solar cell all have made great progress, before having huge application Scape.But it still has many problems, such as device poor reproducibility, hesitation is serious, and large scale application effect is bad etc..Hole Transmission material is to form the important component of solar cell, and in many inorganic hole transporters, NiO is because with big Band gap and deep valence band and be widely used.NiO preparation method is usually spin-coating method, spin-coating method have technique it is simple, can The advantages of prepared by solution, but its less effective in the uniformity of film forming and film coverage, this can be by improving film system Standby technique is resolved.
The content of the invention
It is an object of the invention to provide it is a kind of based on vapour deposition process prepare the super flat NiO films of large area method and its Application in solar cells.
The method that the super flat NiO films of large area are prepared based on vapour deposition process, it is characterised in that pass through the side of vacuum evaporation Method obtains one layer of nickel film, and then calcining obtains described NiO films.
Above-mentioned preparation method, metallic nickel is steamed by vacuum, the evaporation rate that vacuum steams metallic nickel isSteam Plate storehouse vacuum and be less than 10-6Torr；
The thickness for the nickel film that vacuum evaporation obtains is 5-200nm.
NiO films are to calcine gained through nickel film, and its calcining heat is 300-700 DEG C, calcination time 10-120min.
NiO film sizes are 0.04-100cm2。
The super flat NiO roughness of film of prepared large area is 1-5nm.
The super flat NiO films prepared using the inventive method are as hole mobile material, available for different film photoelectrics Sub- device.The film light electronic device includes organic solar batteries and perovskite solar cell.
Organic solar batteries are followed successively by from bottom to top：Substrate, transparency electrode, hole transmission layer, light absorbing layer, electronics pass Defeated layer and metal electrode, light absorbing layer are made up of the organic matter with photo-sensitive characteristic.
Perovskite solar cell is followed successively by from bottom to top：Substrate, transparency electrode, hole transmission layer, light absorbing layer, electronics Transport layer and metal electrode, light absorbing layer are made up of the photovoltaic material with perovskite structure.
Compared with prior art, the present invention has the advantage that：Utilize large area NiO films made of vapour deposition process It is more fine and close smooth, by this film with solar cells, the extraction to hole is more beneficial for, promotes efficient separation of charge With transmission.Based on the cell photoelectric transformation efficiency that vapour deposition process NiO is integrated apparently higher than based on electricity integrated spin-coating method NiO Pond.The work provides a kind of brand-new solution to prepare the NiO films of large area even compact.
Brief description of the drawings
Fig. 1, perovskite solar cell device structural representation.
Fig. 2, prepared based on spin-coating method and the vapour deposition process of embodiment 1 NiO perovskite solar cell J-V curves.
Embodiment
Below in conjunction with accompanying drawing and example, the invention will be further described, but the present invention is not limited to following examples.
Embodiment 1
Fig. 1 shows the perovskite solar cell device structure of the present invention integrated based on vapour deposition process NiO, bag Include：Transparent conductive substrate, NiO hole transmission layers, perovskite light-absorption layer, electron transfer layer, metal electrode.Preparation process is as follows：
1) cleaning of electro-conductive glass：
Continuous twice of use deionized water, acetone, isopropanol is cleaned by ultrasonic 15 minutes and UV ozone is handled 20 minutes.
2) preparation of NiO films：
The electro-conductive glass handled is placed on mask plate and moves into the evaporation of vacuum evaporation storehouse progress metallic nickel.Evaporation When by adjusting the evaporation rate of evaporation boat Power Control metallic nickel be Ensure that storehouse vacuum, which is deposited, to be less than simultaneously 10-6Torr.Evaporation arrives 30nm under this evaporation condition, obtains the nickel film of a layer depth fascia cinerea metallic luster.Plated with gold will be steamed The electro-conductive glass for belonging to nickel moves into Muffle furnace, and being warming up to 500 DEG C of calcining 60min with 2 DEG C/min speed obtains the shallow of layer of transparent Green NiO films.NiO roughness of film is 1-5nm.
3) preparation of perovskite thin film：
The preparation of perovskite solution：Glove box is then moved into by 0.5mm stirrers are added in clean 5mL sample bottles, 461mg PbI is weighed in glove box2Ready sample bottle is poured into 159mg MAI and is dissolved in 0.3mL DMF (N, N- diformazans Base formamide) and 0.7mL DMSO (dimethyl sulfoxide (DMSO)) mixed solvent.The perovskite solution prepared is placed on magnetic stirring apparatus Upper 60 DEG C of stirrings 2h.Impurity is not allowed using the preceding filtering plug filter 23 time with 0.22 μm of aperture to remove.
The preparation of perovskite thin film：We carry out the preparation of perovskite thin film using a step spin-coating method, and NiO films are carried out UVO handles 20min, then pipettes 60 μ L perovskites solution and is added dropwise thereon, and sol evenning machine condition is set as 1000r/min, 10s and 4000r/min, 45s, and 800 μ L toluene are added dropwise in 25s before spin coating terminates, and obtain light yellow perovskite thin film.By the calcium of preparation Titanium ore film is placed on warm table the 10min that annealed at 100 DEG C, and perovskite thin film gradually becomes dark-brown by light yellow, put down Whole smooth perovskite thin film.
4) preparation of PCBM electron transfer layers：
Glove box is then moved into by 0.5mm stirrers are added in clean 5mL sample bottles, weighs 20mg's in glove box PCBM and pouring into ready sample bottle is then dissolved in 1mL chlorobenzene solvents, and PCBM solution is stirred into 2h on agitator.Will The substrate for scribbling perovskite thin film is placed on sol evenning machine pallet and then is added dropwise the PCBM solution progress spin coating that 60 μ L are prepared, and sets even Glue machine rotating speed is 2000r/min, time 40s.PCBM films are prepared and completed.
5) preparation of Ag electrodes：
The device of PCBM layers in spin coating is taken out from glove box, then vertical conduction FTO scraping blades, by the conduction electricity at both ends Pole, which exposes, to be come.The substrate scraped is moved into the mask plate of customization, make conductive FTO vertical with notch, then will install substrate Mask plate be fixed in evaporation cabin and close hatch door.And then carrying out vacuum pumping to evaporation storehouse is less than chamber vacuum degree 10-6Torr.Start to be deposited after reaching requirement vacuum, pass through regulation power supply Power Control evaporation rate.Thickness and correspondingly is deposited Evaporation rate is：0-3nm,3-15nm,15-30nm,30-70nm,Work as film Thickness reaches 70nm and terminates to be deposited, and is prepared into perovskite solar cell.
From figure 2 it can be seen that the perovskite solar cell integrated based on vapour deposition process NiO, in standard sources (AM 1.5G,100mW/cm2) irradiation under, measure the i-v curve of battery, the photoelectricity for calculating perovskite solar cell turns Efficiency is changed, obtains up to 14.88% photoelectric transformation efficiency, higher than the perovskite solar-electricity integrated based on spin-coating method NiO Pond (13.07%).

Claims (10)

  1. A kind of 1. method that the super flat NiO films of large area are prepared based on vapour deposition process, it is characterised in that：Pass through vacuum evaporation Method obtains one layer of nickel film, and then calcining obtains NiO films.
  2. 2. according to a kind of method that the super flat NiO films of large area are prepared based on vapour deposition process described in claim 1, its feature It is：The evaporation rate of vacuum evaporation metallic nickel isStorehouse vacuum is deposited and is less than 10-6Torr。
  3. 3. according to a kind of method that the super flat NiO films of large area are prepared based on vapour deposition process described in claim 1, its feature It is：The thickness for the nickel film that vacuum evaporation obtains is 5-200nm.
  4. 4. according to a kind of method that the super flat NiO films of large area are prepared based on vapour deposition process described in claim 1, its feature It is：NiO films are to calcine gained through nickel film, and its calcining heat is 300-700 DEG C, calcination time 10-120min.
  5. 5. according to a kind of method that the super flat NiO films of large area are prepared based on vapour deposition process described in claim 1, its feature It is：Described NiO film sizes are 0.04-100cm2。
  6. 6. according to a kind of method that the super flat NiO films of large area are prepared based on vapour deposition process described in claim 1, its feature It is：The super flat NiO roughness of film of prepared large area is 1-5nm.
  7. 7. the super flat NiO films being prepared in accordance with the method for claim 1.
  8. 8. the application for the super flat NiO films being prepared in accordance with the method for claim 1, it is characterised in that：The gas phase is sunk NiO films prepared by area method are as hole mobile material, for different film light electronic devices, the film light electronic device bag Include organic solar batteries and perovskite solar cell.
  9. 9. according to the application of claim 8, it is characterised in that：The organic solar batteries are followed successively by from bottom to top：Substrate, thoroughly Prescribed electrode, hole transmission layer, light absorbing layer, electron transfer layer and metal electrode are formed, and light absorbing layer is by with photo-sensitive characteristic Organic matter form.
  10. 10. according to the application of claim 8, it is characterised in that：Perovskite solar cell is followed successively by from bottom to top：Substrate, thoroughly Prescribed electrode, hole transmission layer, light absorbing layer, electron transfer layer and metal electrode, light absorbing layer are by with perovskite structure Photovoltaic material is formed.
CN201710538858.7A 2017-07-04 2017-07-04 A kind of method that the super flat NiO films of large area are prepared based on vapour deposition process Pending CN107460438A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109216558A (en) * 2018-09-10 2019-01-15 陕西师范大学 Perovskite battery and preparation method thereof of the nano nickel particles containing oxychloride as hole transmission layer

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0892766A (en) * 1994-09-27 1996-04-09 Agency Of Ind Science & Technol Production of nickel oxide film by plasma oxidation
CN101174687A (en) * 2007-10-29 2008-05-07 河南科技大学 Production method for nickel oxide anode thin film used for full solid-state thin-film lithium ion battery
CN101505035A (en) * 2009-03-09 2009-08-12 武汉大学 P-zinc oxide/N- nickel oxide heterogeneous PN junction ultraviolet laser diode and method for production
CN102560361A (en) * 2012-02-28 2012-07-11 杭州电子科技大学 P-type transparent conductive lithium-doped nickel oxide film and preparation method thereof
CN103117361A (en) * 2013-02-28 2013-05-22 中国科学院合肥物质科学研究院 Organic semiconductor thin film solar cell preparation method based on nickel oxide anode interface layer
CN103921490A (en) * 2013-01-10 2014-07-16 海洋王照明科技股份有限公司 Conductive thin film, preparation method and application thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0892766A (en) * 1994-09-27 1996-04-09 Agency Of Ind Science & Technol Production of nickel oxide film by plasma oxidation
CN101174687A (en) * 2007-10-29 2008-05-07 河南科技大学 Production method for nickel oxide anode thin film used for full solid-state thin-film lithium ion battery
CN101505035A (en) * 2009-03-09 2009-08-12 武汉大学 P-zinc oxide/N- nickel oxide heterogeneous PN junction ultraviolet laser diode and method for production
CN102560361A (en) * 2012-02-28 2012-07-11 杭州电子科技大学 P-type transparent conductive lithium-doped nickel oxide film and preparation method thereof
CN103921490A (en) * 2013-01-10 2014-07-16 海洋王照明科技股份有限公司 Conductive thin film, preparation method and application thereof
CN103117361A (en) * 2013-02-28 2013-05-22 中国科学院合肥物质科学研究院 Organic semiconductor thin film solar cell preparation method based on nickel oxide anode interface layer

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109216558A (en) * 2018-09-10 2019-01-15 陕西师范大学 Perovskite battery and preparation method thereof of the nano nickel particles containing oxychloride as hole transmission layer
CN109216558B (en) * 2018-09-10 2021-11-02 陕西师范大学 Perovskite battery with chlorine-containing nickel oxide nanoparticles as hole transport layer and preparation method thereof

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