CN109004048A - A kind of preparation method of the inorganic perovskite quantum dot film of caesium lead bromine and photovoltaic device based on it - Google Patents
A kind of preparation method of the inorganic perovskite quantum dot film of caesium lead bromine and photovoltaic device based on it Download PDFInfo
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- CN109004048A CN109004048A CN201810823090.2A CN201810823090A CN109004048A CN 109004048 A CN109004048 A CN 109004048A CN 201810823090 A CN201810823090 A CN 201810823090A CN 109004048 A CN109004048 A CN 109004048A
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 229910052792 caesium Inorganic materials 0.000 title claims abstract description 19
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 title claims abstract description 19
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 title claims abstract description 9
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 229910052794 bromium Inorganic materials 0.000 title claims abstract description 9
- 238000004528 spin coating Methods 0.000 claims abstract description 20
- 238000000137 annealing Methods 0.000 claims abstract description 15
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims abstract description 4
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims abstract description 4
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000011521 glass Substances 0.000 claims description 19
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 229940049964 oleate Drugs 0.000 claims description 9
- 239000002243 precursor Substances 0.000 claims description 9
- 238000003786 synthesis reaction Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 7
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 6
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 6
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000005642 Oleic acid Substances 0.000 claims description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- ZASWJUOMEGBQCQ-UHFFFAOYSA-L dibromolead Chemical compound Br[Pb]Br ZASWJUOMEGBQCQ-UHFFFAOYSA-L 0.000 claims description 6
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 5
- 238000005530 etching Methods 0.000 claims description 5
- 239000012452 mother liquor Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 230000027756 respiratory electron transport chain Effects 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 claims description 3
- 229910000024 caesium carbonate Inorganic materials 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims 1
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000011161 development Methods 0.000 abstract description 2
- 238000002347 injection Methods 0.000 abstract 1
- 239000007924 injection Substances 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 43
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000002390 adhesive tape Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- XDXWNHPWWKGTKO-UHFFFAOYSA-N 207739-72-8 Chemical compound C1=CC(OC)=CC=C1N(C=1C=C2C3(C4=CC(=CC=C4C2=CC=1)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)C1=CC(=CC=C1C1=CC=C(C=C13)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)C1=CC=C(OC)C=C1 XDXWNHPWWKGTKO-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 125000000962 organic group Chemical group 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920000301 poly(3-hexylthiophene-2,5-diyl) polymer Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 238000007738 vacuum evaporation Methods 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical class CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910003074 TiCl4 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001768 cations Chemical group 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- -1 diisopropyl titanate esters Chemical class 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 125000000468 ketone group Chemical group 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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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
- H01L31/0248—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 characterised by their semiconductor bodies
- H01L31/0256—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 characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
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- H01L31/035218—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 characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions comprising a quantum structures the quantum structure being quantum dots
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Abstract
It is to warm injection method by height to synthesize CsPbBr the invention discloses a kind of preparation method of the inorganic perovskite quantum dot film of caesium lead bromine and based on its photovoltaic device3Inorganic perovskite quantum dot, and after washing centrifugal purification by methyl acetate, it is dispersed in normal octane solution, then by multiple spin coating and high annealing, quantum dot is made to form film, the light absorbing layer as photovoltaic device.The CsPbBr of the method for the present invention preparation3Film thickness accurately controls, to obtain optimal light absorpting ability, improves the photoelectric conversion efficiency of solar battery；Preparation process of the invention is simple, is not necessarily to inert atmosphere protection, without expensive equipment and material, is particularly suitable for preparation high-volume, low-cost solar battery, thus is conducive to push the development and application of inorganic perovskite solar battery.
Description
Technical field
The present invention relates to the applications that a kind of inorganic perovskite quantum dot of caesium lead bromine prepares photovoltaic device, belong to thin film solar
The preparation process field of cell photovoltaic device.
Background technique
Perovskite battery is generally represented by using perovskite thin film material as the novel solar battery of light absorbing layer
AMX3, wherein A represents cation, common to narrow (FA) and caesium (Cs) etc. for methylamine (MA), first.In recent years, hybrid inorganic-organic
Perovskite solar battery causes the extensive concern of photovoltaic circle due to its excellent photoelectric characteristic, but it is faced with a sternness
The problem of, i.e., thermal stability is bad, easily decomposes under high temperature.This causes hybrid inorganic-organic perovskite solar battery to be difficult to answer
For in actual production.
The thermostabilization difference of hybrid inorganic-organic perovskite solar battery is mainly by the heated easily decomposition of organic group, sky
The reasons such as easy moisture absorption cause in gas, therefore replace organic group to be expected to solve perovskite electricity using more stable inorganic ions Cs
The stability problem in pond.
Novel inorganic caesium lead bromine perovskite material (CsPbBr in recent years3) due to excellent photoelectric properties and good
Thermal stability, water oxygen stability and cause the extensive concern of researcher.However due to brominated elemental precursor material commonly use it is molten
Solubility in agent (such as dimethyl sulfoxide, n,N-Dimethylformamide) is lower, causes to be difficult to a traditional step solution legal system
Standby fine and close film, and since precursor concentration is low, the light absorption layer film after leading to spin coating is relatively thin, is unfavorable for filling sunlight
Divide and absorb, and there are various defects for film.The spiro-OMeTAD that is used when in addition, usually preparing perovskite solar battery or
The organic small molecule materials such as person P3HT are as hole mobile material.This material is not only expensive, but also due to its organic material
Expect that thermal stability is poor and sensitive to moisture in air.
Therefore exploitation high quality CsPbBr3Inorganic perovskite of the inexpensive technology of preparing of film for acquisition efficient stable
Solar battery is significant.The physical vapour deposition (PVD)s preparation processes such as expensive compared to equipment, processing procedure complexity vacuum evaporation, it is molten
Liquid method prepares CsPbBr3Film have it is low in cost, equipment is simple, rate of film build is fast, film thickness and pattern can be in molecule ruler
The advantages such as degree regulation.Therefore, CsPbBr is researched and developed3The good full air solution system of low cost, simple process, the stability of thin-film material
Standby technology is just particularly important.
Summary of the invention
It is an object of the invention to overcome above-mentioned deficiency of the prior art, a kind of inorganic perovskite of caesium lead bromine is provided
The preparation side of quantum dot film and photovoltaic device based on it.
The present invention is to realize goal of the invention, is adopted the following technical scheme that
The present invention discloses a kind of preparation method of inorganic perovskite quantum dot film of caesium lead bromine first, it is characterized in that,
Include the following steps:
Step 1, CsPbBr3The synthesis of inorganic perovskite quantum dot
(1) synthesis of the oleate presoma of caesium
0.5g cesium carbonate, 2mL oleic acid and 50mL 1- octadecylene are added in three-neck flask, vacuumizes logical nitrogen 3 times repeatedly
Except water oxygen, then heats at 120 DEG C and stirs 20-40 minutes, obtain the oleate precursor solution of caesium, be stored in nitrogen,
70 DEG C of heat preservation, it is spare；
(2)CsPbBr3The synthesis of quantum dot
0.7g lead bromide and 50mL1- octadecylene are added in another three-necked flask, constant temperature stirring one is small at 120 DEG C
When, 5mL oleic acid and 5mL oil ammonium is then added, continues stirring and is all dissolved to lead bromide；170 DEG C are then heated to, 8mL is injected
The oleate precursor solution of caesium synthesized by step (1), ice bath is cooled to room temperature after waiting 5 seconds, obtains CsPbBr3Quantum dot
Mother liquor；
(3)CsPbBr3The purifying of quantum dot
By methyl acetate and step (2) CsPbBr obtained32:1 is mixed the mother liquor of quantum dot by volume, 8000rpm
It is centrifuged 5min, precipitating is dispersed in 5mL normal octane, is i.e. acquisition CsPbBr3Quantum dot solution；
Step 2, CsPbBr3The preparation of inorganic perovskite quantum dot film
Spin coating and annealing: CsPbBr synthesized by 45 μ L steps (1) is taken3Quantum dot solution is spin-coated in clean substrate,
Spin speed is 2000rpm, spin-coating time 40s, is subsequently placed in 250 DEG C and heats the substrate annealing 5min, removes and be cooled to room
Temperature；
It operates that the spin coating is multiple with annealing steps, that is, obtains the CsPbBr of required thickness3Inorganic perovskite quantum dot is thin
Film." spin coating and annealing " step operation is primary, and film thickness is in 40-60nm.
In specific implementation, the dosage of above-mentioned each material can equal proportion amplification.
Preferably, the number that the spin coating and annealing steps are operated in step 2 is 3-5 times, at this time the thickness of gained film
When as photovoltaic device, best performance.
Invention additionally discloses one kind to be based on CsPbBr3The photovoltaic device of inorganic perovskite quantum dot film, as shown in Figure 1,
It is to be sequentially depositing the compacted zone TiO as electron transfer layer in FTO conductive glass surface2, as light absorbing layer
CsPbBr3Inorganic perovskite quantum dot film and C electrode as positive and negative electrode.Its preparation step is as follows:
(1) to prevent test battery film is pressed from both sides into perforating when and causes battery short circuit, by FTO conductive glass surface partial etching,
Specifically: FTO conductive glass surface being divided into crystallizing field and non-deposited area, in the upper zinc of local uniform tiling of the crystallizing field
Powder etches 5min then by the HCl drop of 2M on zinc powder；
FTO electro-conductive glass after etching (is successively used into suds, third by the cleaning of FTO electro-conductive glass, the drying after etching
Ketone, EtOH Sonicate clean 20min, then use N2Drying reuses UV-ozone cleaning machine cleaning 20min), obtain cleaning
FTO electro-conductive glass.
(2) in the crystallizing field deposition compact layer TiO of FTO conductive glass surface2As electron transfer layer；
(3) CsPbBr is formed on the electron transport layer with above-mentioned preparation method3Inorganic perovskite quantum dot film,
As light absorbing layer；
(4) in the non-deposited area of FTO conductive glass surface blade coating C electrode as negative electrode, in the light absorbing layer
Battery is placed on 150 DEG C of warm table after heating 30min to get being based on as positive electrode by upper blade coating C electrode after blade coating
CsPbBr3The photovoltaic device of inorganic perovskite quantum dot film.
Compared with the prior art, the beneficial effects of the present invention are embodied in:
1, the present invention can effectively avoid current perovskite too compared with common organic inorganic hybridization perovskite solar cell
The cumbersome glove box operation of positive energy battery preparation and expensive vacuum evaporation apparatus investment, are realized high-quality under normal atmospheric conditions
Amount, the low cost preparation for stablizing perovskite light absorbing layer film, are particularly suitable for preparation high-volume, low-cost solar battery, because
And be conducive to push the development and application of inorganic perovskite solar battery.
2, CsPbBr is prepared with a traditional step solwution method3Film is compared, and CsPbBr is utilized3The preparation of perovskite quantum dot
Film is finer and close, and can control the thickness of film by the way of multiple spin coating in the preparation, and then obtains optimal light
Absorbability improves the photoelectric conversion efficiency of solar battery, and solving solar cell device film thickness can not accurately control
The problem of processed.
3, the noble metal electrodes such as the gold or silver that are used when preparing perovskite solar battery using carbon electrode substitution tradition: the
One, carbon electrode has the ability for collecting hole, avoids using organic small molecule materials such as spiro-OMeTAD or P3HT, thus
Avoid influence of the organic cavity transmission layer unstability to battery efficiency.Second, the price of carbon electrode is than your gold such as gold, silver, platinum
Belong to cheap, and the content of carbon in nature avoids the wasting of resources, reduce costs considerably beyond these noble metals.Third,
The technique of carbon electrode is relatively easy, is conducive to industrial actual production.
Detailed description of the invention
Fig. 1 is based on CsPbBr3The structural schematic diagram of the perovskite solar battery of inorganic perovskite quantum dot film；
Fig. 2 is CsPbBr obtained in embodiment 13Transmission electron microscope (TEM) photo of quantum dot；
Fig. 3 is CsPbBr obtained in embodiment 13The surface Scanning Electron microscope photo (SEM) of film；
Fig. 4 is CsPbBr obtained in embodiment 13The section scanning electron microscope photo (SEM) of film；
Fig. 5 is that CsPbBr is based in embodiment 13The Current density-voltage (J-V) of the perovskite solar battery of film is special
Linearity curve；
Fig. 6 is CsPbBr obtained in embodiment 23The section scanning electron microscope photo (SEM) of film；
Fig. 7 is that CsPbBr is based in embodiment 23The Current density-voltage (J-V) of the perovskite solar battery of film is special
Linearity curve；
Fig. 8 is CsPbBr obtained in embodiment 33The section scanning electron microscope photo (SEM) of film；
Fig. 9 is that CsPbBr is based in embodiment 33The Current density-voltage (J-V) of the perovskite solar battery of film is special
Linearity curve.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, below with reference to embodiment to this hair
Bright specific embodiment is described in detail.The following contents is only to design example of the invention and explanation, institute
Belong to those skilled in the art to make various modifications or additions to the described embodiments or using similar
Mode substitutes, and as long as it does not deviate from the concept of invention or beyond the scope defined by this claim, should belong to the present invention
Protection scope.
Embodiment 1
The present embodiment prepares CsPbBr as follows3Inorganic perovskite quantum dot film and the solar-electricity based on it
Pond:
Step 1, CsPbBr3The synthesis of inorganic perovskite quantum dot
(11) synthesis of the oleate presoma of caesium
0.5g cesium carbonate, 2mL oleic acid and 50mL 1- octadecylene are added in three-neck flask, vacuumizes logical nitrogen 3 times repeatedly
It except water oxygen, then heats at 120 DEG C and stirs 30 minutes, obtain the oleate precursor solution of caesium, be stored in nitrogen, keep the temperature
It is 70 DEG C, spare；
(12)CsPbBr3The synthesis of quantum dot
0.7g lead bromide and 50mL1- octadecylene are added in another three-necked flask, constant temperature stirring one is small at 120 DEG C
When, 5mL oleic acid and 5mL oil ammonium is then added, continues stirring and is all dissolved to lead bromide；170 DEG C are then heated to, is rapidly injected
The oleate precursor solution of caesium synthesized by 8mL step (11), ice bath is cooled to room temperature immediately after waiting 5 seconds, is obtained
CsPbBr3The mother liquor of quantum dot；
(13)CsPbBr3The purifying of quantum dot
By methyl acetate and step (12) CsPbBr obtained32:1 is mixed the mother liquor of quantum dot by volume,
8000rpm is centrifuged 5min, and precipitating is dispersed in 5mL normal octane, i.e. acquisition CsPbBr3Quantum dot solution；Fig. 2 is the present embodiment
Obtained CsPbBr3Transmission electron microscope (TEM) photo of quantum dot, quantum dot size is in 9nm.
2、CsPbBr3The preparation of inorganic perovskite quantum dot solar cell:
(21) FTO electro-conductive glass is cut into the fritter of 20mm × 15mm, is classified as the two of 15mm width and 5mm width
Part, respectively as crystallizing field and non-deposited area.Then the 5mm width using crystallizing field far from non-deposited area is as etched area.?
The part of non-etched area touch adhesive tape, leaks out etched area.Zinc powder is evenly laid out in etched area, the HCl solution drop of 2M is being spread
On good zinc powder, 5min is etched.FTO electro-conductive glass after etching is successively cleaned into 20min with suds, acetone, EtOH Sonicate,
Then N is used2Drying reuses UV-ozone cleaning machine cleaning 20min, obtains clean FTO electro-conductive glass.
(22) in FTO conductive glass surface crystallizing field deposition compact layer TiO2As electron transfer layer: taking 1g 75% first
Bis- (levulinic ketone group) diisopropyl titanate esters aqueous isopropanols (wt%), which are added in 10.3g n-butanol, forms 0.15mol/L
TiO2Precursor liquid takes 2~3 above-mentioned solution of drop to be added drop-wise to the clean non-etched area of FTO conductive glass surface, 2000rpm spin coating
Remove substrate after 40s, 135 DEG C of dry 10min, then 500 DEG C of sintering 30min；After to be sintered, substrate is used
40mmol/L TiCl470 DEG C of processing 30min of aqueous solution, and again with 500 DEG C of sintering 30min to get arrive compacted zone TiO2。
(23) spin coating and annealing: CsPbBr synthesized by 45 μ L steps (1) is taken3Quantum dot solution is spin-coated on compacted zone TiO2
On, spin speed is 2000rpm, spin-coating time 40s, is subsequently placed in 250 DEG C and heats the substrate annealing 5min, removes and be cooled to
Room temperature；
Above-mentioned spin coating and annealing steps 5 times are operated, CsPbBr is obtained3Inorganic perovskite quantum dot film.
Fig. 3 is CsPbBr obtained by the present embodiment3The electron scanning micrograph of film surface, it can be seen that this
Film uniform compact obtained by embodiment, and crystallite dimension is larger.Fig. 4 is CsPbBr obtained by the present embodiment3The section of film
Electron scanning micrograph, it can be seen that through 5 spin coatings, film thickness obtained by the present embodiment is about 280nm.
(4) it takes and has been coated with CsPbBr3The FTO electro-conductive glass of light-absorption layer is glued the place for not needing to apply back electrode with adhesive tape
Get up, then by conductive carbon paste with scraper scratch after the region that do not tape, blade coating by battery be placed on 150 DEG C plus
After heating 30min in thermal station, adhesive tape of tearing completes the preparation of carbon electrode, obtains perovskite solar cell device.
Be tested for the property to perovskite photovoltaic device made by the present embodiment: test temperature is 25 DEG C；Relative humidity
It is 30%；The spectral irradiance of light source is 100mW/m2, and the AM1.5 solar spectrum irradiancy with standard is distributed.After tested,
Current density-voltage (J-V) characteristic curve of battery is as shown in Figure 5.
Embodiment 2
The present embodiment makes CsPbBr by the identical method of embodiment 13Film and solar battery based on it, difference is only
It is to operate spin coating and annealing steps 3 times in step (23), as shown in fig. 6, film thickness is about 170nm.After tested, this implementation
Film uniform compact made by example, the J-V characteristic curve of corresponding solar battery are as shown in Figure 7.
Embodiment 3
The present embodiment makes CsPbB by the identical method of embodiment 1r3Film and solar battery based on it, difference is only
It is to operate spin coating and annealing steps 1 time in step (23), as shown in figure 8, film thickness is about 55nm.After tested, this implementation
Film uniform compact made by example, the J-V characteristic curve of corresponding solar battery are as shown in Figure 9.
The above is only exemplary embodiment of the present invention, are not intended to limit the invention, all in spirit of the invention
With any modifications, equivalent replacements, and improvements made within principle etc., should all be included in the protection scope of the present invention.
Claims (4)
1. a kind of preparation method of the inorganic perovskite quantum dot film of caesium lead bromine, characterized by the following steps:
Step 1, CsPbBr3The synthesis of inorganic perovskite quantum dot
(1) synthesis of the oleate presoma of caesium
0.5g cesium carbonate, 2mL oleic acid and 50mL 1- octadecylene are added in three-neck flask, vacuumizes 3 water removals repeatedly of logical nitrogen
Oxygen is then heated at 120 DEG C and is stirred 20-40 minutes, obtains the oleate precursor solution of caesium, be stored in nitrogen, heat preservation
It is 70 DEG C, spare；
(2)CsPbBr3The synthesis of quantum dot
0.7g lead bromide and 50mL1- octadecylene are added in another three-necked flask, constant temperature stirring one hour at 120 DEG C, so
5mL oleic acid and 5mL oil ammonium are added afterwards, continues stirring and is all dissolved to lead bromide；170 DEG C are then heated to, 8mL step is injected
(1) the oleate precursor solution of the caesium synthesized by, ice bath is cooled to room temperature after waiting 5 seconds, obtains CsPbBr3The mother of quantum dot
Liquid；
(3)CsPbBr3The purifying of quantum dot
By methyl acetate and step (2) CsPbBr obtained32:1 is mixed the mother liquor of quantum dot by volume, 8000rpm centrifugation
Precipitating is dispersed in 5mL normal octane by 5min, i.e. acquisition CsPbBr3Quantum dot solution；
Step 2, CsPbBr3The preparation of inorganic perovskite quantum dot film
Spin coating and annealing: CsPbBr synthesized by 45 μ L steps (1) is taken3Quantum dot solution is spin-coated in clean substrate, spin coating speed
Degree is 2000rpm, spin-coating time 40s, is subsequently placed in 250 DEG C and heats the substrate annealing 5min, removes and be cooled to room temperature；
It operates that the spin coating is multiple with annealing steps, that is, obtains the CsPbBr of required thickness3Inorganic perovskite quantum dot film.
2. preparation method according to claim 1, it is characterised in that: operate the spin coating and annealing steps in step 2
Number is 3-5 times.
3. a kind of photovoltaic device based on the inorganic perovskite quantum dot film of caesium lead bromine, it is characterised in that: the photovoltaic device is
The compacted zone TiO as electron transfer layer is sequentially depositing in FTO conductive glass surface2, wanted with right as light absorbing layer
CsPbBr obtained by preparation method described in asking any one of 1~23Inorganic perovskite quantum dot film and as positive negative electricity
The C electrode of pole.
4. a kind of preparation method of photovoltaic device as claimed in claim 3, which comprises the steps of:
(1) FTO conductive glass surface is divided into crystallizing field and non-deposited area, in the upper zinc of local uniform tiling of the crystallizing field
Powder etches 5min then by the HCl drop of 2M on zinc powder；By the cleaning of FTO electro-conductive glass, the drying after etching；
(2) in the crystallizing field deposition compact layer TiO of FTO conductive glass surface2As electron transfer layer；
(3) CsPbBr is formed on the electron transport layer with preparation method of any of claims 1 or 23Inorganic perovskite quantum
Point film, as light absorbing layer；
(4) it is scraped on the light absorbing layer in the non-deposited area of FTO conductive glass surface blade coating C electrode as negative electrode
It applies C electrode and is used as positive electrode, battery is placed on on 150 DEG C of warm table heating 30min to get being based on after blade coating
CsPbBr3The photovoltaic device of inorganic perovskite quantum dot film.
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