CN108063186A - Zinc doping nickel oxide hole transmission layer inverts perovskite solar cell and preparation method - Google Patents
Zinc doping nickel oxide hole transmission layer inverts perovskite solar cell and preparation method Download PDFInfo
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- CN108063186A CN108063186A CN201711156113.0A CN201711156113A CN108063186A CN 108063186 A CN108063186 A CN 108063186A CN 201711156113 A CN201711156113 A CN 201711156113A CN 108063186 A CN108063186 A CN 108063186A
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- 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
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- 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
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- H—ELECTRICITY
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- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/30—Doping active layers, e.g. electron transporting layers
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- 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
Abstract
The invention belongs to perovskite solar cell preparing technical field, more particularly to a kind of zinc doping nickel oxide hole transmission layer inverts perovskite solar cell and preparation method thereof.Inverting perovskite solar cell is：（1）, FTO glass；（2）, prepare zinc doping nickel oxide hole transmission layer；（3）, prepare perovskite bulk heterojunction film；（4）, electron transfer layer is prepared on calcium titanium ore bed；（5）, electrode modification layer；（6）, metal electrode.The present invention uses brand-new hole transmission layer, obtains high transparency, high conductivity by adulterating zinc optimization nickel oxide film, high work content matches good hole extract layer, performance optimization, stable structure with perovskite.
Description
Technical field
The invention belongs to technical field prepared by perovskite solar cell, more particularly to a kind of zinc doping nickel oxide holes
The efficient perovskite solar cell of transport layer and preparation method.
Background technology
Perovskite solar cell is since 2009 report for the first time, and energy conversion efficiency is maked rapid progress, by initial
3.8% is promoted to 22.1%.Being announced to the world splendidly for perovskite solar cell brings new hope for the development of solar cell.Calcium
Titanium ore light-absorption layer both sides are electron transfer layer and hole transmission layer respectively, and the ability in hole-transporting layer extraction hole is directly determined
Determine the photoelectric conversion efficiency of solar cell, it is seen that the importance of hole transmission layer is self-evident.
Hole transmission layer used in the solar cell of current most of high-photoelectric transformation efficiencies transmits for organic hole
Layer（Such as PEDOT：PSS, PTAA, spiro-OMeTAD etc.）, but organic hole transport material preparation process is complicated, price is held high
It is expensive, and it is unsatisfactory for the requirement of large-scale production.Therefore, the inorganic material for finding replacement organic cavity transmission layer is most important.
Nickel oxide is a kind of p-type simconductor material, and energy gap is 3.6 eV, and perovskite level-density parameter, and
And there is high-transmittance in visible-range, it is suitable in the opto-electronic devices such as perovskite solar cell, but its is relatively low
Electrical conductivity be always the hole transmission layer inferior position where, and adulterate can change this present situation to greatest extent.
The content of the invention
It is an object of the invention to overcome above-mentioned existing technical deficiency, a kind of cheap new material of utilization is provided（Oxidation
Nickel）The efficient perovskite solar cell of zinc doping nickel oxide hole transmission layer of preparation, improves cell series resistance, by carrying
For high hole extraction efficiency so as to optimize battery performance, the perovskite solar cell to develop Cheap highly effective provides a kind of new think of
Road.
The present invention also provides the preparation methods of above-mentioned solar cell.
In order to overcome already existing technical deficiency, the technical scheme is that：
The invention discloses a kind of zinc doping nickel oxide hole transmission layers to invert efficient perovskite solar cell, it is characterised in that
It is made of following preparation method：（1）, using FTO glass as Window layer carry out partial etching；（2）, prepare zinc doping nickel oxide
Hole transmission layer；（3）, prepare perovskite bulk heterojunction film；（4）, electron transfer layer is prepared on calcium titanium ore bed；（5）, in electricity
Electrode modification layer is prepared in sub- transport layer；（6）, on electrode modification layer prepare metal electrode, so as to obtain solar cell；
The zinc doping nickel oxide hole transmission layer is made of using following methods：Zinc nitrate is mixed in proportion with nickel nitrate
Mixing precursor liquid is made in the in the mixed solvent of ethylenediamine and ethylene glycol, is subsequently placed in 12 hours of stirring on magnetic stirring apparatus,
Clarified solution is obtained after filtering, is then spin coated onto clarified solution 40s in fluorine-doped tin oxide glass（FTO glass）Substrate, finally gained
Substrate is put into 400 DEG C of annealing 3600s in quick anneal oven, obtains zinc doping nickel oxide hole transmission layer.
Above-mentioned inverts perovskite solar cell, preferably：The molar ratio of the zinc nitrate and nickel nitrate is 3-7:97-
93, the volume ratio of ethylenediamine and ethylene glycol is 1:10, zinc nitrate is 1M in the concentration of in the mixed solvent with nickel nitrate.
Above-mentioned inverts perovskite solar cell, preferably：The thickness of the FTO glass is 300nm；Zinc doping aoxidizes
The thickness of nickel hole transmission layer is 30nm；The thickness of perovskite bulk heterojunction film is 250nm；The thickness of electron transfer layer is
30nm；The thickness of electrode modification layer is 10nm；The thickness of metal electrode is 60nm.
The invention also discloses a kind of zinc doping nickel oxide hole transmission layers described in claim 1 to invert the perovskite sun
The preparation method of energy battery, it is characterised in that using following steps：
（1）FTO transparent conducting glass is cut into the strip of 1.6cm, then sticks the adhesive tape of 1cm wide, then with zinc powder and dense salt
Acid is 1 with water volume ratio:5 dilute hydrochloric acid etches 15 minutes, and remaining zinc powder is cleaned with dilute hydrochloric acid, the glass etched is cut into
1.6 × 1.7cm rectangles, with lye be cleaned by ultrasonic 30-60 min, then with alcohol be cleaned by ultrasonic 30-60 min, finally spend from
Sub- water is cleaned by ultrasonic 10-30 min, is put into drying baker drying with spare；
（2）Zinc nitrate and nickel nitrate are mixed in the in the mixed solvent of ethylenediamine and ethylene glycol in proportion, then will mix forerunner
Liquid is placed in 12 hours of stirring on magnetic stirring apparatus, and clarified solution is obtained after filtering, is then spin coated onto zinc nitrate and nickel nitrate mixing
Precursor solution 40s is in fluorine-doped tin oxide glass（FTO glass）Substrate is finally put into gained substrate in quick anneal oven
400 DEG C of annealing 3600s obtain zinc doping nickel oxide hole transmission layer；
（3）Lead acetate and iodine methylamine are dissolved in n,N-Dimethylformamide solvent, is subsequently placed on magnetic stirring apparatus and stirs 30
Min obtains perovskite precursor solution, is then spin coated onto precursor liquid and 100 DEG C of annealing obtain perovskite light-absorption layer in 10 minutes；
（4）In glove box spin coating concentration be 15-20mg/ml PCBM chlorobenzene solution, last spin coating BCP（Bathocuproine）Second
Alcoholic solution takes out the sample prepared, with vacuum thermal evaporation plated film instrument evaporation metal electrode.
The invention described above, zinc nitrate and nickel nitrate are mixed in the in the mixed solvent of ethylenediamine and ethylene glycol in proportion, 400 DEG C
Its reaction mechanism of annealing is such:Zinc nitrate is completely dissolved with nickel nitrate in the mixed solvent, the height carried out after spin-coating film
Temperature annealing is so that nickel nitrate generates a simple redox reaction.Wherein, start to decompose simultaneously shape when temperature is higher than 110 DEG C
Into basic salt, continue the mixture of the nickel sesquioxide of heating generation brownish black and the nickel protoxide of green, generation palm fibre at 400 DEG C
The nickel sesquioxide of black and nickel protoxide mixture.As for zinc oxide meeting under oxygen atmosphere of zinc nitrate pyroreaction generation
It reacts with nickel oxide, the lattice position for having entered nickel is adulterated in Zn-ef ficiency displacement, but since the two radius is not much different, makes it
Apparent distortion of lattice does not occur.
Zinc nitrate and nickel nitrate are mixed and made into zinc doping nickel oxide film as hole transmission layer by the present invention, due to oxygen
The non-stoichiometry characteristic for changing nickel causes its inside to exist from defect, and this defect is mainly to have to form the minimum nickel room of energy
Composition.The displacement doping of Zn-ef ficiency reduces further the formation can be dense so as to cause semiconductor hole so that nickel room is increased
The raising of degree, thus the electric conductivity of semiconductive hole transport layer and hole extractability significantly enhance, final result is directly determined
The raising of solar cell device performance is determined.
The zinc doping nickel oxide hole transmission layer of the present invention inverts perovskite solar cell, including hole transmission layer, light absorption
Layer, electron transfer layer, electrode modification layer, metal electrode.Zinc nitrate and nickel nitrate are mixed and made into zinc doping oxygen by the present invention for the first time
Change nickel film as hole transmission layer, and be prepared for battery.Cell series resistance is improved, and the photoelectricity for obtaining 19.5 % turns
Change efficiency.Photoactive layer is prepared by spin-coating method, and its thickness is between 200-250nm.Common inorganic electronic transmission material has
TiO2、ZnO、SnO2Deng, Organic Electron Transport Material has PCBM etc., by spin-coating method prepare PCBM electron-transport layer thickness be
30nm, the BCP electrode modifications layer thickness prepared by spin-coating method are 10nm, and the Ag thickness of electrode prepared by vacuum vapour deposition is
60nm。
The efficient perovskite solar cell of zinc doping nickel oxide hole transmission layer of the present invention using brand-new hole transmission layer, leads to
Overdoping zinc optimization nickel oxide film obtains high transparency, high conductivity, and high work content matches good hole extraction with perovskite
Layer, efficient perovskite solar cell is obtained by assembling.First by zinc nitrate and nickel nitrate precursor solution in proportion
Mixing, is then spin coated onto fluorine-doped tin oxide glass（FTO glass）On, high-performance zinc doping nickel oxide is obtained by annealing heating
Film improves film light transmittance and hole extraction efficiency, and then optimizes cell series resistance, improves cell photoelectric conversion
Efficiency.For the hole transmission layer that the present invention obtains compared with traditional hole mobile material, semiconductive thin film has high electrical conductivity,
High work content, device have many advantages, such as high efficiency, stiff stability.Its performance optimized and the structure stablized are perovskite solar energy
The commercial applications of battery provide new thinking.
Description of the drawings
Fig. 1 is the solar battery structure schematic diagram of the present invention,
Fig. 2 is not mix zinc（It is left）With mix zinc（It is right）Nickel oxide SEM figure
Fig. 3 is the I-V curve for the nickel oxide hole transmission layer/perovskite solar cell do not mixed zinc and mix zinc.
Wherein 1. FTO, 2. hole transmission layers, 3. light absorbing layers, 4. electron transfer layers, 5. electrode modification layers, 6.Ag electricity
Pole.
Specific embodiment
Embodiment 1
（1）Prepare traditional transoid planar heterojunction solar battery structure schematic diagram such as Fig. 1.FTO transparent conducting glass is cut into
The strip of 1.6cm then sticks one centimetre of wide adhesive tape, is then 1 with zinc powder and concentrated hydrochloric acid and water volume ratio:5 dilute hydrochloric acid
Etching 15 minutes cleans remaining zinc powder with dilute hydrochloric acid, the glass etched is cut into 1.6 × 1.7cm rectangles, is surpassed with lye
Sound cleans 30-60 min, then is cleaned by ultrasonic 30-60 min with alcohol, is finally cleaned by ultrasonic 10-30 min with deionized water, so
After be put into drying baker drying with spare；
（2）Nickel nitrate is dissolved in the in the mixed solvent of ethylenediamine and ethylene glycol, mixing precursor liquid is then placed in magnetic stirring apparatus
12 hours of upper stirring, clarified solution is obtained after filtering, is then spin coated onto nickel oxide precursor solution 40s in fluorine-doped tin oxide glass
Glass（FTO glass）Gained substrate is finally put into 400 DEG C of annealing 3600s in quick anneal oven and obtains nickel oxide film such as by substrate
Fig. 2（It is left）.
（3）Lead acetate and iodine methylamine are dissolved in n,N-Dimethylformamide solvent, is subsequently placed on magnetic stirring apparatus and stirs
It mixes 30 min and obtains perovskite precursor solution.It is then spin coated onto precursor liquid and 100 DEG C of annealing obtains perovskite light-absorption layer in 10 minutes.
A series of processes operate in glove box before this.
（4）In glove box spin coating concentration be 15-20mg/ml PCBM chlorobenzene solution, last spin coating BCP（Bathocuproine）
Ethanol solution, by the sample prepared take out, with vacuum thermal evaporation plated film instrument be deposited Ag electrode 60nm, evaporation rate 0.5
Å/s.Surveyed photoelectric conversion efficiency such as Fig. 3.
Embodiment 2
The present embodiment is same as Example 1, the difference is that nickel nitrate and zinc nitrate are mixed in ethylenediamine by step 2 in proportion
With the in the mixed solvent of ethylene glycol, wherein zinc nitrate molar ratio is 3%,（The molar ratio of the zinc nitrate and nickel nitrate is 3:97,
The volume ratio of ethylenediamine and ethylene glycol is 1:10, zinc nitrate is 1M in the concentration of in the mixed solvent with nickel nitrate.）It then will mixing
Precursor liquid is placed in 12 hours of stirring on magnetic stirring apparatus, obtains clarified solution after filtering, is then spin coated onto zinc nitrate and nickel nitrate
Precursor solution 40s is mixed in fluorine-doped tin oxide glass（FTO glass）Gained substrate is finally put into quick anneal oven by substrate
In 400 DEG C annealing 3600s obtain zinc doping nickel oxide film such as Fig. 2（It is right）.
Embodiment 3
The present embodiment is same as Example 2, the difference is that nickel nitrate and zinc nitrate are mixed in ethylenediamine by step 2 in proportion
With the in the mixed solvent of ethylene glycol, wherein zinc nitrate molar ratio is 5%,（The molar ratio of the zinc nitrate and nickel nitrate is 5:95,
The volume ratio of ethylenediamine and ethylene glycol is 1:10, zinc nitrate is 1M in the concentration of in the mixed solvent with nickel nitrate.）It then will mixing
Precursor liquid is placed in 12 hours of stirring on magnetic stirring apparatus, obtains clarified solution after filtering, is then spin coated onto zinc nitrate and nickel nitrate
Precursor solution 40s is mixed in fluorine-doped tin oxide glass（FTO glass）Gained substrate is finally put into quick anneal oven by substrate
In 400 DEG C annealing 3600s obtain zinc doping nickel oxide film.
Embodiment 4
The present embodiment is same as Example 3, the difference is that nickel nitrate and zinc nitrate are mixed in ethylenediamine by step 2 in proportion
With the in the mixed solvent of ethylene glycol, wherein zinc nitrate molar ratio is 7%,（The molar ratio of the zinc nitrate and nickel nitrate is 7:93,
The volume ratio of ethylenediamine and ethylene glycol is 1:10, zinc nitrate is 1M in the concentration of in the mixed solvent with nickel nitrate.）It then will mixing
Precursor liquid is placed in 12 hours of stirring on magnetic stirring apparatus, obtains clarified solution after filtering, is then spin coated onto zinc nitrate and nickel nitrate
Precursor solution 40s is mixed in fluorine-doped tin oxide glass（FTO glass）Gained substrate is finally put into quick anneal oven by substrate
In 400 DEG C annealing 3600s obtain zinc doping nickel oxide film.
Solar battery structure is made as shown in Figure 1, wherein, wherein 1. FTO, 2. hole transmission layers, 3. light absorbing layers, 4.
Electron transfer layer, 5. electrode modification layers, 6.Ag electrodes.Each layer thickness is respectively 300nm, 30nm, 250nm, 30nm, 10nm,
60nm。
The test result of above-described embodiment 1 and embodiment 2-4 are as follows.
Fig. 2 is not mix zinc（It is left）With mix zinc（It is right）Nickel oxide SEM figure
Fig. 3 is the I-V curve for the nickel oxide hole transmission layer/perovskite solar cell do not mixed zinc and mix zinc.
Abscissa is voltage, and ordinate is electric current.Top curve is to mix nickel oxide hole transmission layer/perovskite sun of zinc
The I-V curve of energy battery, lower curve are the I-V curve for the nickel oxide hole transmission layer/perovskite solar cell for not mixing zinc.
Table 1 summarizes the solar cell items photoelectric parameter that four kinds of specific embodiments obtain.What wherein embodiment 3 obtained is cell performance
Can be optimal, peak efficiency is up to 19.5%.
Finally illustrate personal view, above example is only the preferred embodiments of the present invention, is not intended to limit the invention, in every case
All any modification, equivalent and improvement done within the spirit and principles in the present invention etc. should be included in the guarantor of the present invention
Within the scope of shield.
Table 1
Claims (4)
1. a kind of zinc doping nickel oxide hole transmission layer inverts efficient perovskite solar cell, it is characterised in that uses following system
Preparation Method is made：（1）, using FTO glass as Window layer carry out partial etching；（2）, prepare zinc doping nickel oxide hole transport
Layer；（3）, prepare perovskite bulk heterojunction film；（4）, electron transfer layer is prepared on calcium titanium ore bed；（5）, in electron transfer layer
On prepare electrode modification layer；（6）, on electrode modification layer prepare metal electrode, so as to obtain solar cell；
The zinc doping nickel oxide hole transmission layer is made of using following methods：Zinc nitrate is mixed in proportion with nickel nitrate
Mixing precursor liquid is made in the in the mixed solvent of ethylenediamine and ethylene glycol, is subsequently placed in 12 hours of stirring on magnetic stirring apparatus,
Clarified solution is obtained after filtering, is then spin coated onto clarified solution 40s in fluorine-doped tin oxide glass（FTO glass）Substrate, finally gained
Substrate is put into 400 DEG C of annealing 3600s in quick anneal oven, obtains zinc doping nickel oxide hole transmission layer.
2. according to claim 1 invert perovskite solar cell, it is characterised in that：The zinc nitrate and nickel nitrate
Molar ratio is 3-7:The volume ratio of 97-93, ethylenediamine and ethylene glycol is 1:10, zinc nitrate is with nickel nitrate in the dense of in the mixed solvent
It spends for 1M.
3. according to claim 1 invert perovskite solar cell, it is characterised in that：The thickness of the FTO glass is
300nm；The thickness of zinc doping nickel oxide hole transmission layer is 30nm；The thickness of perovskite bulk heterojunction film is 250nm；Electronics
The thickness of transport layer is 30nm；The thickness of electrode modification layer is 10nm；The thickness of metal electrode is 60nm.
4. a kind of zinc doping nickel oxide hole transmission layer described in claim 1 inverts the preparation side of perovskite solar cell
Method, it is characterised in that using following steps：
（1）FTO transparent conducting glass is cut into the strip of 1.6cm, then sticks the adhesive tape of 1cm wide, then with zinc powder and dense salt
Acid is 1 with water volume ratio:5 dilute hydrochloric acid etches 15 minutes, and remaining zinc powder is cleaned with dilute hydrochloric acid, the glass etched is cut into
1.6 × 1.7cm rectangles, with lye be cleaned by ultrasonic 30-60 min, then with alcohol be cleaned by ultrasonic 30-60 min, finally spend from
Sub- water is cleaned by ultrasonic 10-30 min, is put into drying baker drying with spare；
（2）Zinc nitrate and nickel nitrate are mixed in the in the mixed solvent of ethylenediamine and ethylene glycol in proportion, then will mix forerunner
Liquid is placed in 12 hours of stirring on magnetic stirring apparatus, and clarified solution is obtained after filtering, is then spin coated onto zinc nitrate and nickel nitrate mixing
Precursor solution 40s is in fluorine-doped tin oxide glass（FTO glass）Substrate is finally put into gained substrate in quick anneal oven
400 DEG C of annealing 3600s obtain zinc doping nickel oxide hole transmission layer；
（3）Lead acetate and iodine methylamine are dissolved in n,N-Dimethylformamide solvent, is subsequently placed on magnetic stirring apparatus and stirs 30
Min obtains perovskite precursor solution, is then spin coated onto precursor liquid and 100 DEG C of annealing obtain perovskite light-absorption layer in 10 minutes；
（4）In glove box spin coating concentration be 15-20mg/ml PCBM chlorobenzene solution, last spin coating BCP（Bathocuproine）Second
Alcoholic solution takes out the sample prepared, with vacuum thermal evaporation plated film instrument evaporation metal electrode.
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Cited By (8)
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| CN108878583A (en) * | 2018-06-20 | 2018-11-23 | 东华大学 | Based on p-Si/NiO:The preparation method of the photodetection material of Zn heterojunction structure |
| CN109037456A (en) * | 2018-08-10 | 2018-12-18 | 南京邮电大学 | A kind of preparation method of zero sluggish efficiently perovskite solar battery |
| CN109346604A (en) * | 2018-09-19 | 2019-02-15 | 浙江师范大学 | A kind of perovskite solar battery |
| CN109888100A (en) * | 2019-01-22 | 2019-06-14 | 南昌大学 | A kind of preparation of rubidium Y-oxides doping film and application as hole transmission layer in perovskite solar battery |
| CN112467042A (en) * | 2020-11-25 | 2021-03-09 | 西南石油大学 | Intelligent automatic production system for perovskite solar cell module |
| CN112534596A (en) * | 2018-07-24 | 2021-03-19 | 西门子能源全球有限两合公司 | Metal-organic perovskite solar cell, tandem solar cell and manufacturing method thereof |
| CN113206198A (en) * | 2021-04-19 | 2021-08-03 | 武汉大学 | Preparation method of lanthanum nickelate nanoparticle hole transport layer, trans-perovskite solar cell and preparation method of trans-perovskite solar cell |
| WO2023060923A1 (en) * | 2021-10-15 | 2023-04-20 | 中国华能集团清洁能源技术研究院有限公司 | Multifunctional tco and battery |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108878583A (en) * | 2018-06-20 | 2018-11-23 | 东华大学 | Based on p-Si/NiO:The preparation method of the photodetection material of Zn heterojunction structure |
| CN112534596A (en) * | 2018-07-24 | 2021-03-19 | 西门子能源全球有限两合公司 | Metal-organic perovskite solar cell, tandem solar cell and manufacturing method thereof |
| CN112534596B (en) * | 2018-07-24 | 2023-09-12 | 西门子能源全球有限两合公司 | Metal organic perovskite solar cell, serial solar cell and manufacturing method thereof |
| CN109037456A (en) * | 2018-08-10 | 2018-12-18 | 南京邮电大学 | A kind of preparation method of zero sluggish efficiently perovskite solar battery |
| CN109346604A (en) * | 2018-09-19 | 2019-02-15 | 浙江师范大学 | A kind of perovskite solar battery |
| CN109888100A (en) * | 2019-01-22 | 2019-06-14 | 南昌大学 | A kind of preparation of rubidium Y-oxides doping film and application as hole transmission layer in perovskite solar battery |
| CN112467042A (en) * | 2020-11-25 | 2021-03-09 | 西南石油大学 | Intelligent automatic production system for perovskite solar cell module |
| CN113206198A (en) * | 2021-04-19 | 2021-08-03 | 武汉大学 | Preparation method of lanthanum nickelate nanoparticle hole transport layer, trans-perovskite solar cell and preparation method of trans-perovskite solar cell |
| WO2023060923A1 (en) * | 2021-10-15 | 2023-04-20 | 中国华能集团清洁能源技术研究院有限公司 | Multifunctional tco and battery |
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