CN116081711A - Oleate modified nickel oxide nanocrystalline material and preparation method and application thereof - Google Patents
Oleate modified nickel oxide nanocrystalline material and preparation method and application thereof Download PDFInfo
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- CN116081711A CN116081711A CN202211612036.6A CN202211612036A CN116081711A CN 116081711 A CN116081711 A CN 116081711A CN 202211612036 A CN202211612036 A CN 202211612036A CN 116081711 A CN116081711 A CN 116081711A
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- nickel oxide
- oleate
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- -1 Oleate modified nickel oxide Chemical class 0.000 title claims abstract description 72
- 229940049964 oleate Drugs 0.000 title claims abstract description 45
- 239000002707 nanocrystalline material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 230000005525 hole transport Effects 0.000 claims abstract description 103
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract description 83
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract description 69
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 19
- 230000004048 modification Effects 0.000 claims abstract description 13
- 238000012986 modification Methods 0.000 claims abstract description 13
- 229940096992 potassium oleate Drugs 0.000 claims description 63
- 238000003756 stirring Methods 0.000 claims description 22
- 239000002159 nanocrystal Substances 0.000 claims description 19
- MLICVSDCCDDWMD-KVVVOXFISA-M potassium;(z)-octadec-9-enoate Chemical compound [K+].CCCCCCCC\C=C/CCCCCCCC([O-])=O MLICVSDCCDDWMD-KVVVOXFISA-M 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000000758 substrate Substances 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 6
- 238000004528 spin coating Methods 0.000 claims description 6
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 6
- 229910001887 tin oxide Inorganic materials 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 2
- FVFJGQJXAWCHIE-UHFFFAOYSA-N [4-(bromomethyl)phenyl]methanamine Chemical class NCC1=CC=C(CBr)C=C1 FVFJGQJXAWCHIE-UHFFFAOYSA-N 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims 1
- 229910052802 copper Inorganic materials 0.000 claims 1
- 239000010949 copper Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000004888 barrier function Effects 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 18
- 239000010409 thin film Substances 0.000 description 13
- 238000005424 photoluminescence Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 7
- STTGYIUESPWXOW-UHFFFAOYSA-N 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline Chemical compound C=12C=CC3=C(C=4C=CC=CC=4)C=C(C)N=C3C2=NC(C)=CC=1C1=CC=CC=C1 STTGYIUESPWXOW-UHFFFAOYSA-N 0.000 description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 5
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 125000000217 alkyl group Chemical group 0.000 description 4
- 230000002209 hydrophobic effect Effects 0.000 description 4
- 229910052738 indium Inorganic materials 0.000 description 4
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 4
- 238000002329 infrared spectrum Methods 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000001941 electron spectroscopy Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- XQPRBTXUXXVTKB-UHFFFAOYSA-M caesium iodide Chemical compound [I-].[Cs+] XQPRBTXUXXVTKB-UHFFFAOYSA-M 0.000 description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910001453 nickel ion Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 238000002207 thermal evaporation Methods 0.000 description 2
- 208000032750 Device leakage Diseases 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- QHJPGANWSLEMTI-UHFFFAOYSA-N aminomethylideneazanium;iodide Chemical compound I.NC=N QHJPGANWSLEMTI-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- ZASWJUOMEGBQCQ-UHFFFAOYSA-L dibromolead Chemical compound Br[Pb]Br ZASWJUOMEGBQCQ-UHFFFAOYSA-L 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- VRNINGUKUJWZTH-UHFFFAOYSA-L lead(2+);dithiocyanate Chemical compound [Pb+2].[S-]C#N.[S-]C#N VRNINGUKUJWZTH-UHFFFAOYSA-L 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 238000001420 photoelectron spectroscopy Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000005036 potential barrier Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
- 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
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Abstract
The invention provides an oleate modified nickel oxide nanocrystalline material and a preparation method and application thereof, and the oleate modified nickel oxide nanocrystalline material or the oleate modified nickel oxide nanocrystalline material prepared by the preparation method provided by the invention is not easy to agglomerate, has better dispersibility and stability, and is simple and environment-friendly in preparation method; the nickel oxide nanocrystalline hole transport layer based on oleate modification has better compactness and coverage; perovskite solar cell based on oleate modified nickel oxide nanocrystalline hole transport layer, the hole transport layer and the wide bandgap perovskite valence band have better energy level matching, the hole transport barrier at the perovskite interface is smaller, the open-circuit voltage is obviously improved, the perovskite solar cell has better charge transport property, the photoelectric efficiency of the perovskite cell is higher, and the distribution is more concentrated; the invention provides an effective modification strategy for the perovskite solar cell based on the nickel oxide nanocrystalline hole transport layer.
Description
Technical Field
The invention relates to the technical field of perovskite solar cells, in particular to an oleate modified nickel oxide nanocrystalline material, a preparation method of the nanocrystalline material, application of the oleate modified nickel oxide nanocrystalline material, a oleate modified nickel oxide nanocrystalline hole transport layer and a perovskite solar cell.
Background
Compared with the traditional novel thin film solar cells such as monocrystalline silicon solar cells, dye sensitized solar cells and organic solar cells, the perovskite solar cell has the advantages of low cost, simple preparation method, excellent photoelectric property and higher energy conversion efficiency, can meet rich market demands, and is highly valued in scientific research and industry.
The main stream perovskite solar cell at present is a multilayer film plane heterojunction structure composed of a charge transmission layer, a perovskite layer and an electrode. Wherein the performance of the charge transport layer is critical to the improvement of the overall performance of the perovskite solar cell. The hole transport material needs to have good hole transport and electron blocking capabilities, good energy level matching with perovskite materials, compatibility of the preparation process with the device preparation process, good chemical and photoelectric stability, and the like.
The nickel oxide nanocrystalline is used as a P-type oxide semiconductor with a wide forbidden band, has better energy pole matching with a perovskite active layer, has high hole mobility, has the advantages of simple synthesis method, low raw material cost, good thermal stability and the like, and is widely applied to a perovskite solar cell hole transport layer. However, nickel oxide nanocrystals also have problems as hole transport layers, such as the fermi level of nickel oxide being far from the valence band maximum of perovskite, which results in greater carrier energy loss in perovskite thin films; and non-radiative recombination and device leakage caused by the low conductivity of the nickel oxide itself, low carrier transport and rough interfaces, which all affect the photovoltaic performance of the perovskite solar cell, and thus the energy conversion efficiency of the perovskite solar cell.
Therefore, the novel hole transport material with more matched energy level structure and more efficient carrier extraction efficiency is developed, so that the device efficiency of the perovskite solar cell can be greatly improved.
Disclosure of Invention
Aiming at the technical problems, the invention provides an oleate modified nickel oxide nanocrystalline material, a preparation method and application thereof, wherein the oleate modified nickel oxide nanocrystalline hole transport layer has better energy level matching with a wide-bandgap perovskite valence band, the hole transport potential barrier at a perovskite interface is smaller, the open-circuit voltage is obviously improved, the oleate modified nickel oxide nanocrystalline material has better charge transport characteristics, the energy conversion efficiency of a perovskite battery device is higher, and the performance is better.
The invention is characterized in that the nickel oxide nanocrystalline is modified by oleate, the chemical property of the oleate is coordinated with the nickel oxide nanocrystalline, the material property of the nickel oxide nanocrystalline is improved, the nickel oxide nanocrystalline has better charge transmission property, the hole transmission layer of the nickel oxide nanocrystalline modified by oleate is better energy level matched with the perovskite film, and the efficiency and the device property of the perovskite solar cell device are improved.
In combination with the conception, the invention provides the following technical scheme:
in a first aspect, the present invention provides an oleate-modified nickel oxide nanocrystalline material comprising: oleate and nickel oxide nanocrystals; the mass ratio of the oleate to the nickel oxide nanocrystalline is 1:6000 to 18000.
Further, the oleate is at least one of potassium oleate, sodium oleate or ammonium oleate.
In a second aspect, the invention provides a method for preparing an oleate modified nickel oxide nanocrystalline material, which comprises the following steps:
s1, preparing oleate solution: dissolving oleate in deionized water, and fully stirring under a heating condition, wherein the mass volume ratio of the oleate to the deionized water is 0.05-0.2 mg/m1;
s2, preparing nickel oxide solution: dispersing the nickel oxide nanocrystalline in deionized water, fully stirring at room temperature, filtering, and performing ultrasonic treatment, wherein the mass volume ratio of the nickel oxide nanocrystalline to the deionized water is 15-30 mg/ml;
s3, preparing an oleate modified nickel oxide nanocrystalline material: the oleate solution prepared in S1 and the nickel oxide solution prepared in S2 are mixed according to a ratio of 1: mixing in 80-120 volume ratio, stirring at room temperature and filtering.
The room temperature is the indoor temperature, and the temperature is controlled to be 20-25 ℃.
Further, in step S1, the heating condition is 50-80 ℃, the full stirring time is 8-12 hours, and the full stirring speed is 500-1000 rpm.
Further, in the step S2, the sufficient stirring time is 8-12 hours, the sufficient stirring speed is 500-1000 rpm, the ultrasonic treatment time is 10-20 minutes, and the water temperature is controlled at 20-30 ℃ in the ultrasonic treatment process.
Further, in step S3, the sufficient stirring time is 2 to 4 hours, and the sufficient stirring speed is 500 to 1000rpm.
In a third aspect, the invention provides an oleate-modified nickel oxide nanocrystalline material according to the first aspect or an oleate-modified nickel oxide nanocrystalline material prepared by the preparation method according to the second aspect, and application of the oleate-modified nickel oxide nanocrystalline material in preparation of a hole transport layer or a perovskite solar cell.
In a fourth aspect, the present invention provides a hole transport layer comprising the oleate-modified nickel oxide nanocrystalline material of the first aspect or the oleate-modified nickel oxide nanocrystalline material prepared according to the second aspect;
in a fifth aspect, the present invention provides a method for preparing the hole transport layer according to the fourth aspect, including: and spin-coating the oleate modified nickel oxide nanocrystalline material on a conductive substrate through a spin coater.
Further, the spin coating speed is 2000 to 4000rpm for 30s.
In a sixth aspect, the present invention provides a perovskite solar cell comprising the hole transport layer of the fourth or fifth aspect.
In some embodiments, the invention provides a perovskite solar cell, which is formed by sequentially stacking a glass substrate, an indium-doped tin oxide (ITO) transparent electrode layer, a hole transport layer, a wide-bandgap perovskite layer, a C60 electron transport layer, a copper-Bath (BCP) interface modification layer and a silver (Ag) cathode electrode from bottom to top, wherein the hole transport layer is the hole transport layer in the fourth aspect or the fifth aspect.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides an oleate modified nickel oxide nanocrystalline material, a preparation method and application thereof, wherein the oleate modified nickel oxide nanocrystalline material or the oleate modified nickel oxide nanocrystalline material prepared by the preparation method provided by the invention is not easy to agglomerate, has better dispersibility and stability, and the preparation method is simple and environment-friendly; the nickel oxide nanocrystalline hole transport layer based on oleate modification has better compactness and coverage; perovskite solar cell based on oleate modified nickel oxide nanocrystalline hole transport layer, the hole transport layer and the wide bandgap perovskite valence band have better energy level matching, the hole transport barrier at the perovskite interface is smaller, the open-circuit voltage is obviously improved, the perovskite solar cell has better charge transport property, the photoelectric efficiency of the perovskite cell is higher, and the distribution is more concentrated; the invention provides an effective modification strategy for the perovskite solar cell based on the nickel oxide nanocrystalline hole transport layer.
Drawings
The invention will be described in further detail below in connection with the drawings and the preferred embodiments, but it will be appreciated by those skilled in the art that these drawings are drawn for the purpose of illustrating the preferred embodiments only and thus should not be taken as limiting the scope of the invention. Moreover, unless specifically indicated otherwise, the drawings are merely schematic representations, not necessarily to scale, of the compositions or constructions of the described objects and may include exaggerated representations.
FIG. 1 is a schematic flow chart of a method for preparing a potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) material;
FIG. 2 is a graph comparing the stability of unmodified nickel oxide nanocrystalline (NiOx) solution with potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) solution;
FIG. 3 is a scanning electron microscope contrast plot of an unmodified nickel oxide nanocrystalline hole transport layer versus a potassium oleate modified nickel oxide nanocrystalline hole transport layer;
FIG. 4 is a comparison of ultraviolet electron spectroscopy test of unmodified nickel oxide nanocrystals (NiOx) hole transport layer and potassium oleate modified nickel oxide nanocrystal hole transport layer (PO-NiOx);
FIG. 5 is a graph comparing JV curves of perovskite thin films based on unmodified nickel oxide nanocrystalline (NiOx) hole transport layers with perovskite thin films based on potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) hole transport layers;
FIG. 6 steady state Photoluminescence (PL) spectra of perovskite thin films of different types of hole transport layers;
FIG. 7 Time Resolved Photoluminescence (TRPL) spectra of perovskite thin films based on unmodified nickel oxide nanocrystalline (NiOx) hole transport layers and perovskite thin films based on potassium oleate modified nickel oxide nanocrystalline hole transport layers;
FIG. 8 is a graph of the efficiency profile of perovskite thin films for different types of hole transport layers;
FIG. 9 Fourier infrared spectra of a potassium oleate film, an unmodified nickel oxide nanocrystal (NiOx) hole transport layer, and a potassium oleate modified nickel oxide nanocrystal (PO-NiOx) hole transport layer;
FIG. 10X-ray photoelectron spectroscopy of an unmodified nickel oxide (NiOx) hole transport layer and a potassium oleate modified nickel oxide (PO-NiOx) hole transport layer.
Detailed Description
The present invention will be described in detail with reference to fig. 1 to 10.
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
EXAMPLE 1 Potassium oleate modified Nickel oxide nanocrystalline (PO-NiOx) Material
the embodiment of the invention provides a preparation method of a potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) material, which is shown in figure 1 and comprises the following steps:
s1, preparing a potassium oleate solution, namely dissolving potassium oleate into deionized water, heating and stirring for 10 hours at 60 ℃, wherein the stirring speed is 800rpm, and the mass-volume ratio of the potassium oleate to the deionized water is 0.2mg/ml;
s2, preparing nickel oxide solution: dispersing nickel oxide nanocrystals in deionized water, stirring at room temperature for 10 hours at a stirring speed of 800rpm, filtering by a Polytetrafluoroethylene (PTFE) filter head or a filter membrane with a pore diameter of 0.22 mu m, performing ultrasonic treatment for 10 minutes, and controlling the water temperature at 20-30 ℃ in the ultrasonic process, wherein the mass-volume ratio of the nickel oxide nanocrystals to the deionized water is 20mg/ml;
s3, preparing a potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) material: the potassium oleate solution prepared in S1 and the nickel oxide solution prepared in S2 are mixed according to a ratio of 1:100 by volume, for 2 hours at room temperature at 800rpm, and filtered through a PTFE filter head or membrane having a pore size of 0.22. Mu.m.
The room temperature is the indoor temperature, and the temperature is controlled to be 20-25 ℃.
FIG. 2 is a graph showing the comparison of the stability of an unmodified nickel oxide nanocrystalline (NiOx) solution and a potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) solution, as shown in FIG. 2, wherein the potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) solution still maintains a good dispersion effect after being left for 5 days; the unmodified nickel oxide nanocrystalline (NiOx) solution showed significant delamination of water from the nickel oxide solution on day 2 of the rest, and after 5 days of the rest, the nickel oxide was substantially all agglomerated at the bottom of the bottle.
Compared with the stability of figure 2, the nickel oxide nanocrystalline solution modified by potassium oleate has better stability. This is because potassium oleate is an anionic surfactant, oleate ions have hydrophilic carboxyl groups and hydrophobic alkyl chains, wherein the carboxyl groups and nickel ions of the nickel oxide species have good coordination effects, the hydrophobic alkyl chains repel each other, the dispersion of nickel oxide nanoparticles is promoted, and the stability of the nickel oxide nanocrystal solution is improved.
EXAMPLE 2 preparation of Potassium oleate modified Nickel oxide nanocrystalline hole transport layer
A preparation method of a potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) hole transport layer comprises the following steps: the oleate modified nickel oxide nanocrystalline material is spin-coated on an indium doped tin oxide (ITO) conductive substrate at a speed of 3000rpm for 30s by a spin coater to prepare the potassium oleate modified nickel oxide nanocrystalline hole transport layer.
Fig. 3 is a graph of scanning electron microscope test results of an unmodified nickel oxide nanocrystalline hole transport layer and a potassium oleate modified nickel oxide nanocrystalline hole transport layer prepared by spin coating. As shown in fig. 3, the unmodified nickel oxide nanocrystals could not completely cover the indium doped tin oxide (ITO) substrate, with large pieces of ITO substrate exposed; the hole transport layer of the nickel oxide nanocrystalline modified by potassium oleate is more compact, and completely covers the ITO substrate.
FIG. 4 is a graph of ultraviolet electron spectroscopy test results of an unmodified nickel oxide nanocrystal (NiOx) hole transport layer and a potassium oleate modified nickel oxide nanocrystal (PO-NiOx) hole transport layer, secondary electron cutoff edges were measured at a bias of-5V, the Fermi level of the different nickel oxides was determined by the formula φ= - (Ephoton-Ecutoff), where Ephoton is the photon energy of 21.22eV of He I, and the Work Function (Work Function) and valence band top position were determined by ultraviolet electron spectroscopy test to investigate the photoelectric properties of the unmodified nickel oxide nanocrystal film and the potassium oleate modified nickel oxide nanocrystal film. As shown in fig. 4, the secondary electron-cut edge binding energies of the unmodified nickel oxide nanocrystalline hole transport layer (NiOx) and the potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) hole transport layer were 16.32eV and 16.22eV, respectively, and the corresponding work functions were calculated to be-4.90 eV and-5.0 eV, respectively. According to the low energy cut-off edges of 0.40eV and 0.38eV near the valence band, the valence band top of the hole transport layer (PO-NiOx) of the potassium oleate modified nickel oxide nanocrystalline is shifted from-5.30 eV to-5.38 eV, which shows that the hole transport layer (PO-NiOx) of the potassium oleate modified nickel oxide nanocrystalline has better energy level matching with the wide-bandgap perovskite valence band, and the smaller hole transport barrier at the interface of the hole transport layer and the perovskite of the potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) is beneficial to obtaining higher open circuit voltage of the device.
The potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) solution prepared by the invention has better dispersibility, and the hole transport layer prepared by spin coating has better compactness; the potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) hole transport layer and the wide bandgap perovskite valence band have better energy level matching, and the smaller hole transport barrier at the interface of the potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) hole transport layer and the perovskite is beneficial to the device to obtain higher open circuit voltage.
Example 3 perovskite solar cell based on Potassium oleate modified Nickel oxide nanocrystalline (PO-NiOx) hole transport layer
The perovskite solar cell structure based on the potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) hole transport layer is characterized in that a glass substrate, an indium doped tin oxide (ITO) transparent electrode layer, a potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) hole transport layer, a 1.67eV wide band gap perovskite layer, a C60 electron transport layer, a BCP interface modification layer and an Ag cathode electrode are sequentially laminated from bottom to top.
The preparation method of the perovskite solar cell based on the potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) hole transport layer comprises the following steps:
s1, preparation of 1.67eV wide band gap perovskite precursor: by mixing 0.8mmol formamidine iodide (FAI), 0.2mmol cesium iodide (CsI), 0.7mmol lead iodide (PbI) 2 ) And 0.3mmol of lead bromide (PbBr) 2 ) Dissolving in 1ml of mixed solvent to prepare 1.68eV FA0.8CS0.2Pb (I0.8Br0.2) 3 perovskite precursor solution (1.087 mol/L); the mixed solvent of N-dimethylformamide (DMF, anhydrous, sigma-Aldrich) and dimethyl sulfoxide (DMSO, anhydrous, sigma-Aldrich) was used in a volume ratio of 3:1. 6.46mg (2 mol% in solution) of lead thiocyanate (Pb (SCN) 2, sigma-Aldrich, 99.5%) was then added to the solution, and the perovskite precursor solution was thoroughly mixed and aged for 12 hours before use.
S2, preparing an ITO transparent electrode layer and a glass substrate: indium doped tin oxide (ITO)/glass substrate (Advanced Election Technology co., ltd) was treated with UV ozone for 30 minutes before use.
S3, preparing a PO-NiOx hole transport layer: the potassium oleate-modified nickel oxide nanocrystalline (PO-NiOx) based material was spin coated at 2000rpm for 60 seconds and annealed in air on a hot plate at 100℃for 20 minutes, after which the substrate was transferred to a glove box.
S4, preparation of a 1.67eV wide band gap perovskite layer: the perovskite precursor prepared in S1 was spin-coated on the PO-NiOx hole transport layer at 4000rpm for 60 seconds, 700. Mu.L of diethyl ether (anhydrous, sigma-Aldrich) was dropped on the surface during the spin-coating, and the deposited film was annealed at 65℃for 2 minutes, and then at 100℃for 10 minutes. Throughout the annealing process, the film was covered with 15. Mu.L DMF glass petri dish.
S5, preparing a C60 electron transport layer and a BCP (bathocuproine) interface modification layer: the substrate was transferred to an evaporation system, followed by deposition of 20nm c60 and 8nm BCP on top by thermal evaporation.
S6, preparing an Ag cathode electrode: 100nm Ag is deposited as a cathode by thermal evaporation or magnetron sputtering, respectively.
Fig. 5 is a graph showing the JV curve results of a perovskite film based on an unmodified nickel oxide nanocrystal (NiOx) hole transport layer and a perovskite film based on a potassium oleate modified nickel oxide nanocrystal (PO-NiOx) hole transport layer, as shown in fig. 5, with a significant increase in the open circuit voltage of the perovskite film based on the PO-NiOx hole transport layer.
Fig. 6 is a steady state Photoluminescence (PL) spectrum of perovskite thin films of different types of hole transport layers, and as can be seen from fig. 6, the PL intensity of perovskite thin films based on PO-NiOx hole transport layers (perovskite/PO-NiOx structure) was significantly reduced compared to the PL intensity of perovskite thin films based on NiOx hole transport layers (perovskite/NiOx structure) and the PL intensity of perovskite thin films without hole transport layers, demonstrating an enhancement in carrier extraction capacity at heterojunction perovskite/PO-NiOx hole transport layer interfaces.
Fig. 7 is a Time Resolved Photoluminescence (TRPL) profile of a perovskite film based on an unmodified nickel oxide nanocrystalline (NiOx) hole transport layer and a perovskite film based on a potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) hole transport layer, with rapid TRPL quenching also demonstrating rapid hole transport following interface modification.
For perovskite/NiOx and perovskite/PO-NiOx structures, the fitted carrier life of carriers at the heterojunction interface is 98.5ns and 58.1ns respectively, which indicates that the surface modification of NiOx realizes ohmic contact between a Hole Transport Layer (HTL) and perovskite, inhibits charge accumulation, promotes hole extraction, and is favorable for inhibiting non-radiative recombination.
Fig. 8 is an efficiency profile of perovskite thin films of different types of hole transport layers, the efficiency profile being fitted using a gaussian formula. The efficiency of the perovskite film based on the unmodified nickel oxide (NiOx) hole transport layer is distributed at about 18%, while the efficiency of the perovskite film based on the potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) hole transport layer is distributed more intensively and is improved to about 20%, which means that the efficiency and the repeatability of the perovskite film based on the PO-NiOx hole transport layer are obviously improved.
According to the invention, through JV curve test, steady state Photoluminescence (PL) test, time-resolved photoluminescence (TRPL) test and efficiency test of a perovskite film of the perovskite solar cell based on the potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) hole transport layer, the charge transport characteristic of the perovskite film based on the potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) hole transport layer is researched, and the perovskite solar cell based on the potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) hole transport layer has the advantages of obviously improved open circuit voltage, better charge transport characteristic, higher efficiency and more concentrated distribution.
Example 4 mechanism of Potassium oleate modification of Nickel oxide nanocrystalline
The invention discusses the mechanism of the potassium oleate modified nickel oxide nanocrystalline through Fourier infrared spectrum test and X-ray photoelectron spectrum test of the unmodified nickel oxide nanocrystalline (NiOx) hole transport layer and the potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) hole transport layer.
FIG. 9 shows a potassium oleate (potassium oleate) hole transport layer, an unmodified nickel oxide nanocrystalline (NiOx) hole transport layer, and potassium oleate modified nickel oxideFourier infrared spectrum test results of nanocrystalline (PO-NiOx) hole transport layer. As shown in FIG. 9, the wave number in the infrared spectrogram of the potassium oleate hole transport layer is 1568cm -1 And 1423cm -1 The wavenumber of the infrared spectrogram of the unmodified nickel oxide nanocrystalline (NiOx) hole transport layer is 426cm -1 The telescopic vibration peak of the nickel-oxygen bond is located, the nickel-oxygen bond in the infrared spectrogram of the potassium oleate modified nickel oxide nanocrystalline (PO-NiOx) hole transport layer is blue-shifted, the telescopic vibration peak of the carboxyl group is also blue-shifted, and the absorption intensity of the telescopic vibration peak of the carboxyl group is also changed, so that the interaction between the carboxyl group in the potassium oleate and the nickel oxide is shown.
FIG. 10 is an X-ray photoelectron spectrum of an unmodified Nickel oxide (NiOx) hole transport layer and a Potassium oleate modified Nickel oxide (PO-NiOx) hole transport layer, as shown in FIG. 4, showing signals of Ni 2p3/2 orbitals, two peaks for NiOx film, 853.63eV and 855.42eV respectively, attributed to Ni 2+ And Ni 3+ Indicating NiO and Ni in the unmodified Nickel oxide (NiOx) hole transport layer 2 O 3 Both states coexist. In addition, ni of the potassium oleate modified nickel oxide (PO-NiOx) hole transport layer 2+ And Ni 3+ The peaks move 0.10eV and 0.12eV respectively towards the high binding energy direction, which shows that the combination between the potassium oleate and the nickel oxide is successful, and the chemical property of the nickel oxide is changed by the combination, so that the potassium oleate modified nickel oxide nanocrystalline material has better dispersibility, and a compact hole transport layer is generated.
The Fourier infrared spectrum test and the X-ray photoelectron spectrum test further show that the mechanism of the potassium oleate modified nickel oxide nanocrystalline is as follows: potassium oleate is an anionic surfactant, oleate ions have hydrophilic carboxyl groups and hydrophobic alkyl chains, wherein the carboxyl groups and nickel ions in nickel oxide have good coordination effect, the hydrophobic alkyl chains repel each other, the dispersion of nickel oxide nano particles is promoted, the stability of nickel oxide nano crystal solution is improved, and therefore a compact hole transport layer is generated.
The foregoing has outlined rather broadly the more detailed description of the invention in order that the detailed description of the invention that follows may be better understood, and in order that the present invention may be better understood. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
Claims (12)
1. An oleate-modified nickel oxide nanocrystalline material, characterized by comprising: oleate and nickel oxide nanocrystals; the mass ratio of the oleate to the nickel oxide nanocrystalline is 1:6000 to 18000.
2. The oleate modified nickel oxide nanocrystalline material of claim 1, wherein the oleate is at least one of potassium oleate or sodium oleate or ammonium oleate salt.
3. The preparation method of the oleate modified nickel oxide nanocrystalline material is characterized by comprising the following steps of:
s1, preparing oleate solution: dissolving oleate in deionized water, and fully stirring under a heating condition, wherein the mass volume ratio of the oleate to the deionized water is 0.05-0.2 mg/m1;
s2, preparing nickel oxide solution: dispersing the nickel oxide nanocrystalline in deionized water, fully stirring at room temperature, filtering, and performing ultrasonic treatment, wherein the mass volume ratio of the nickel oxide nanocrystalline to the deionized water is 15-30 mg/ml;
s3, preparing an oleate modified nickel oxide nanocrystalline material: the oleate solution prepared in S1 and the nickel oxide solution prepared in S2 are mixed according to a ratio of 1: mixing in 80-120 volume ratio, stirring at room temperature and filtering.
4. The method for preparing oleate-modified nickel oxide nanocrystalline material according to claim 3, wherein in step S1, the heating condition is 50 to 80 degrees celsius, the sufficient stirring time is 8 to 12 hours, and the sufficient stirring speed is 500 to 1000rpm.
5. The method for preparing oleate-modified nickel oxide nanocrystalline material according to claim 3, wherein in step S2, the sufficient stirring time is 8-12 hours, the sufficient stirring speed is 500-1000 rpm, the ultrasonic treatment time is 10-20 minutes, and the water temperature is controlled to be 20-30 ℃ during the ultrasonic treatment.
6. The method for preparing oleate-modified nickel oxide nanocrystalline material according to claim 3, wherein in step S3, the sufficient stirring time is 2 to 4 hours, and the sufficient stirring speed is 500 to 1000rpm.
7. Use of the oleate-modified nickel oxide nanocrystalline material according to any one of claims 1 to 2 or the oleate-modified nickel oxide nanocrystalline material prepared by the preparation method according to any one of claims 3 to 6 in the preparation of a hole transport layer or perovskite solar cell.
8. A hole transport layer comprising the oleate-modified nickel oxide nanocrystalline material according to any one of claims 1 to 2 or the oleate-modified nickel oxide nanocrystalline material prepared by the preparation method according to any one of claims 3 to 6.
9. A method of preparing the hole transport layer of claim 8, wherein the oleate modified nickel oxide nanocrystalline material is spin coated onto the conductive substrate by a spin coater.
10. The method for producing a hole transporting layer according to claim 9, wherein the spin coating is performed at a speed of 2000 to 4000rpm for 30s.
11. A perovskite solar cell comprising the hole transport layer according to claim 8 or 9.
12. A perovskite solar cell, from bottom to top, comprising a glass substrate, an indium-doped tin oxide transparent electrode layer, a hole transport layer, a wide-band perovskite layer, a C60 electron transport layer, a copper bath interface modification layer, and a silver cathode electrode, wherein the hole transport layer is the hole transport layer according to claim 8 or 9.
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