CN109841740A - A kind of preparation method of the perovskite solar cell based on nickel oxide hole transmission layer - Google Patents
A kind of preparation method of the perovskite solar cell based on nickel oxide hole transmission layer Download PDFInfo
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- CN109841740A CN109841740A CN201910221097.1A CN201910221097A CN109841740A CN 109841740 A CN109841740 A CN 109841740A CN 201910221097 A CN201910221097 A CN 201910221097A CN 109841740 A CN109841740 A CN 109841740A
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Abstract
The invention discloses a kind of preparation method of perovskite solar cell based on nickel oxide hole transmission layer, preparation method of the invention, core innovative point is, in hole transmission layer preparation step, ultraviolet and ozone process of surface treatment is added.The present invention solves the problems, such as the generation hole in uneven thickness and extremely easy of the nickel oxide hole transmission layer of spin-coating method preparation, prevents perovskite thin film in device from directly contacting with transparent electrode and influencing device performance.Compared to the method for being modified processing to nickel oxide film of dopen Nano particle, the perovskite solar cell that this method is prepared is more stable, and the device inter-individual difference prepared is smaller.
Description
Technical field
The present invention relates to crystal silicon solar battery preparation field more particularly to a kind of calcium titaniums based on nickel oxide hole transmission layer
The preparation method of mine solar cell.
Background technique
Heliotechnics development substantially experienced three phases: first generation solar cell refers mainly to monocrystalline silicon and polysilicon too
Positive electricity pond, the photoelectric conversion efficiency in laboratory have respectively reached 25% and 20.4%；Second generation solar cell mainly wraps
Include amorphous silicon film battery and polycrystalline silicon thin film solar cell.The third generation solar cell refers mainly to have some new general of high conversion efficiency
Read battery.Ca-Ti ore type solar cell, be using the organic metal halide semiconductor of Ca-Ti ore type as light absorbent too
Positive electricity pond, just belongs to the third generation solar cell.
Nearly ten years, hybrid inorganic-organic perovskite solar cell is with its higher photoelectric conversion efficiency, simple preparation
Technique and lower manufacturing cost have attracted the concern of numerous researchers.The photoelectric conversion efficiency of perovskite solar cell is
Through showing huge business potential more than 23%.Wherein, the perovskite sun of planar heterojunction transconfiguration (p-i-n)
Battery is since simple with structure, preparation is easy, Current density-voltage (J-V) curve hysteretic phenomenon is weak, environmental stability is good etc.
Advantage and be concerned.However, carrier blocking layers employed in efficient perovskite solar cell are mostly organic at present
Object, such as PEDOT:PSS, spiro-OMeTAD, PTAA etc..This type organic is expensive and environmental stability is poor, no
Conducive to commercially producing.
Metal oxide often has and the matched energy level of Perovskite Phase, biggish carrier mobility, splendid environment
The advantages that stability, may replace above-mentioned organic matter as the carrier blocking layers in perovskite solar cell.Wherein nickel oxide
(NiOx) it is a good hole transport layer material, its wider band gap can efficiently reduce parasitic absorption, with calcium
The energy level that titanium ore matches can selectively extract hole, and higher carrier mobility can be effectively reduced the transmission of charge
Loss, higher stability can be improved the service life of device.However NiOxAs a kind of p-type semiconductor, the sky of its own
Cave concentration is not high, and its top of valence band and perovskite are farther out, causes biggish energy level offset, electrons and holes are in interface
There are the biggish probabilities of recombination.To NiOxThe effect of perovskite solar cell can be promoted by being modified processing and enhancing its electric property
Rate and stability.Currently, scientist is generally to NiOxProcessing is doped to promote device performance, for example, magnesium-doped, copper, silver,
The organic molecules such as the metal nanoparticles such as cobalt and F6TCNNQ21.However, these methods are more complicated and uncontrollable, device performance
To doping ratio quite sensitive, the preparation cost of perovskite solar cell is improved.In addition, generalling use solution spin-coating method at present
Prepare NiOxHole transmission layer, the film size that this method is prepared is small, and uneven film thickness is even at different zones and pole
It is easy to produce hole, perovskite thin film in device is caused directly to contact with transparent electrode and influence device performance.Therefore, using one
Simple, the controllable good NiO of new method processability of kindxHole transmission layer is necessary.
Therefore, those skilled in the art is dedicated to developing a kind of perovskite sun electricity based on nickel oxide hole transmission layer
The preparation method in pond.This method needs to solve the production in uneven thickness and extremely easy of the nickel oxide hole transmission layer of spin-coating method preparation
The problem of raw hole, prevent perovskite thin film in device from directly contacting with transparent electrode and influencing device performance.It is received compared to doping
The method that rice corpuscles is modified processing to nickel oxide film, this method processing result is more stable, between the device individual prepared
Difference is smaller.
Summary of the invention
In view of the above drawbacks of the prior art, the technical problem to be solved by the present invention is to how solve nickel oxide film
The problem of uneven thickness uniform multiple hole.The conductivity, hydrophily and work function that also solve how to improve nickel oxide film, make
The perovskite thin film crystallinity that must be prepared is more preferable, and the boundary defect of perovskite and hole transmission layer reduces, and promotes the perovskite sun
The overall performance of battery.
To achieve the above object, the present invention provides a kind of perovskite solar cells based on nickel oxide hole transmission layer
Preparation method, which is characterized in that specifically comprise the following steps:
Step 1, electro-conductive glass substrate pretreatment: etched electro-conductive glass substrate in acetone, isopropanol, ethyl alcohol and is gone
It is cleaned by ultrasonic in ionized water, with being dried with nitrogen after taking-up, and handles surface with UV ozone cleaning machine；
Step 2, hole transmission layer preparation: it is thin that nickel oxide is prepared in the electro-conductive glass substrate using electrochemical deposition method
Film, and the print being prepared is put into UV ozone cleaning machine and is exposed, it is then placed in Muffle furnace and heats；
Step 3, the preparation of perovskite precursor solution and spin coating: lead iodide and iodide ammonium are dissolved in gamma-butyrolacton
With the in the mixed solvent of dimethyl sulfoxide, it is configured to perovskite precursor solution, spin coating is carried out on the nickel oxide film, is obtained
To perovskite thin film；
Step 4, the preparation of fullerene derivate solution and spin coating: fullerene derivate is dissolved in chlorobenzene and is configured to first
Solution carries out spin coating on the perovskite thin film, obtains fullerene derivate layer；
Step 5, the preparation of bathocuproine solution and spin coating: bathocuproine is dissolved in isopropanol and is configured to the second solution, in institute
It states fullerene derivate layer and carries out spin coating, obtain bathocuproine layer；
Step 6, silver electrode preparation: under vacuum conditions, silver electrode is prepared using thermal evaporation coating process.
Further, in step 1, the electro-conductive glass use ITO or FTO electro-conductive glass, the acetone, isopropanol,
Being cleaned by ultrasonic the time in ethyl alcohol and deionized water is 15 minutes.
Further, in step 2, hole transmission layer preparation specifically includes the following steps:
Step 2.1 prepares Nickelous nitrate hexahydrate aqueous solution, is stirred at room temperature, until it is molten to form absinthe-green clarification
Liquid.Solution is filtered by aqueous filtering head later, removes impurity；
Step 2.2, by the electro-conductive glass substrate and with the nickel sheet of homalographic be inserted in parallel into prepared six water and
In nickel nitrate aqueous solution；The working electrode of the electro-conductive glass substrate connection electrochemical workstation, the nickel sheet are connected to electrode
And reference electrode；
Step 2.3, electrochemical workstation use Constant current output, and output electric current is 0.1mA/cm2, the time is 90 seconds, is obtained
To print；
Step 2.4 rinses the print with deionized water；
Step 2.5, with being dried with nitrogen print.
Further, in step 2.1, the substance withdrawl syndrome of the Nickelous nitrate hexahydrate aqueous solution is 2mMol/L, in room
The temperature lower time stirred is 1 hour；The grid spacing of the aqueous filtering head is 0.45 micron.
Further, in step 2.2, between the electro-conductive glass substrate and the nickel sheet between be divided into 5 centimetres.
Further, in step 2, it is specially 5 minutes that the print, which is put into the time exposed in UV ozone cleaning machine, institute
Heating process in Muffle furnace is stated specifically, 300 DEG C are heated 2 hours.
Further, in step 3, the molar ratio of the lead iodide and the iodide ammonium is 1:1, the γ-Ding Nei
The volume ratio of ester and the dimethyl sulfoxide is 7:3, and the obtained perovskite precursor solution concentration is 1mMol/mL, in institute
Stating and carrying out the design parameter of spin coating on nickel oxide film is 500rpm, and for 12 seconds, and then 4000rpm, continues 30 seconds.
Further, in step 4, the concentration of first solution is 20mg/mL, is revolved on the perovskite thin film
The design parameter of painting is 2000rpm, continues 30 seconds.
Further, in step 5, the concentration of second solution is 0.5mg/mL, the fullerene derivate layer into
The design parameter of row spin coating is 4000rpm, continues 30 seconds.
Further, in step 6, the vacuum condition is specially 1E-4Pa, the silver electrode with a thickness of 120nm.
Compared with the prior art, the nickel oxide film handled by UV ozone that the application proposes at least has following skill
Art advantage:
1, there is better electric conductivity under the premise of not reducing light transmittance.
2, surface hydrophilicity enhances, and prepared perovskite thin film crystallinity is high, and surface coverage is high, and crystallite dimension is big.
3, work function improves, so that the top of valence band energy level difference of hole transmission layer and perovskite thin film away from further reducing, mentions
The high extraction rate in hole, increases the open-circuit voltage of perovskite solar cell.
4, the perovskite solar cell for the nickel oxide film preparation that basic application proposes has higher photoelectric conversion efficiency
With better stability.
5, the nickel oxide film proposed to the application, the UV ozone processing by different durations, can significantly regulate and control calcium titanium
The open-circuit voltage and short-circuit current density of mine solar cell.
It is described further below with reference to technical effect of the attached drawing to design of the invention, specific structure and generation, with
It is fully understood from the purpose of the present invention, feature and effect.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the preparation-obtained perovskite solar cell of a preferred embodiment of the present invention；
Fig. 2 is, the perovskite sun that is prepared different according to ultraviolet light exposure time in 5 embodiments of the invention
The efficiency comparative of battery schemes；
Fig. 3 is the preparation-obtained perovskite solar cell of a preferred embodiment of the present invention, with prior art preparation
The environmental stability comparison diagram of obtained efficiency of solar cell.
Specific embodiment
1 preferred embodiment of the invention is introduced below with reference to Figure of description, keeps its technology contents more clear and just
In understanding.The present invention can be emerged from by many various forms of embodiments, and protection scope of the present invention not only limits
The embodiment that Yu Wenzhong is mentioned.
In fig. 1, the identical component of structure is indicated with same numbers label, everywhere the similar component of structure or function with
Like numeral label indicates.The size and thickness of each component shown in the drawings are to be arbitrarily shown, and there is no limit by the present invention
The size and thickness of each component.Apparent in order to make to illustrate, some places suitably exaggerate the thickness of component in attached drawing.
Step 1, electro-conductive glass substrate pretreatment: by etched ITO FTO electro-conductive glass substrate 1 respectively acetone,
It is cleaned by ultrasonic 15min in isopropanol, ethyl alcohol and deionized water, with being dried with nitrogen after taking-up, and is handled with UV ozone cleaning machine
Surface 20 minutes.Obtain substrate of glass 1 and ITO FTO anode layer 2 as shown in Figure 1.
Step 2: hole transmission layer preparation: preparing the Nickelous nitrate hexahydrate aqueous solution that substance withdrawl syndrome is 2mMol/L, room
Temperature lower stirring 1 hour, until forming absinthe-green clear solution.Solution was carried out by 0.45 μm of aqueous filtering head later
Filter.It is inserted in parallel into prepared solution by the electro-conductive glass substrate 1 cleaned up and with the high-purity nickel sheet of homalographic, it is ensured that
Two interplanar spacings are 5 centimetres, and electro-conductive glass and high-purity nickel sheet (purity 99.99%) are separately connected the work electricity of electrochemical workstation
Pole and to electrode carry out electrochemical deposition.Electrochemical workstation exports the constant current of 0.1mA/cm2, and duration is set as 90s, it
Print is rinsed well and is used with deionized water afterwards and is dried with nitrogen.Then with UV ozone cleaning machine handle respectively surface 1,5,
10, it 20 minutes, is put into anneal 2 hours in 300 DEG C of Muffle furnace and prepares nickel oxide film 4 as shown in Figure 1.
Step 3: the preparation of perovskite precursor solution and spin coating: by lead iodide (PbI2) and iodide ammonium (CH3NH3I it) presses
It is dissolved in the mixed solvent (volume ratio 7:3) of gamma-butyrolacton and dimethyl sulfoxide according to molar ratio for 1:1 and is configured to substance
Measure the perovskite (CH that concentration is 1mMol/mL3NH3PbI3) precursor solution.Perovskite precursor solution is spin-coated on nickel oxide
On film 4, spin coating parameters are 500 revolutions per seconds (rpm) (12 seconds) and then (30 seconds) 4000rpm, stop first 10 seconds in spin coating, will
The chlorobenzene of 100 μ L is added dropwise rapidly in sample surfaces.Then sample is placed on 70 DEG C of electric hot plate heat 10 minutes it is more to remove
Remaining organic solvent.Obtain perovskite thin film 5 as shown in Figure 1
Step 4, the preparation of fullerene derivate solution and spin coating: fullerene derivate (PCBM) is dissolved in chlorobenzene and is prepared
The solution for being 20mg/mL at concentration.With 2000rpm, fullerene derivate PCBM solution is spin-coated on perovskite by 30 seconds parameters
5 on film, fullerene derivate PCBM layer 6 is formed.
Step 5, the preparation of bathocuproine solution and spin coating: bathocuproine (BCP) is dissolved in isopropanol and is configured to concentration and is
The solution of 0.5mg/mL.Solution is filtered with the Teflon filtration head that filter opening is 0.45 micron respectively later, is removed
Insoluble impurity.With 4000rpm, bathocuproine BCP solution is spin-coated on fullerene derivate PCBM layer 6 by 30 seconds parameters, shape
At bathocuproine BCP layer 7.
Step 6, silver electrode preparation: under the high vacuum condition of 1E-4Pa, a thickness is prepared using thermal evaporation coating process
The silver electrode 3 that degree is 120 nanometers.
As shown in Fig. 2, handling surface respectively (0 minute 0,1,5,10,20 minute in UV ozone cleaning machine in step 2
It is as in the prior art not handle) after, the nickel oxide being prepared is efficiency comparative's figure of the solar cell of hole transmission layer.
It can be seen that the time of control UV ozone surface treatment, the different solar cell of available performance.Come from general effect
It sees, UV ozone is carried out to nickel oxide film 4 and is surface-treated different durations, compared with the prior art (without UV ozone
Surface treatment), the performance of perovskite solar cell can be improved to some extent.
As shown in figure 3, for the preparation method that provides through the invention obtain based on by UV ozone surface treatment
The perovskite solar cell of nickel oxide film 4 (is surface-treated) without UV ozone compared with the prior art, can be improved it
Environmental stability.
The preferred embodiment of the present invention has been described in detail above.It should be appreciated that the ordinary skill of this field is without wound
The property made labour, which according to the present invention can conceive, makes many modifications and variations.Therefore, all technician in the art
Pass through the available technology of logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea
Scheme, all should be within the scope of protection determined by the claims.
Claims (10)
1. a kind of preparation method of the perovskite solar cell based on nickel oxide hole transmission layer, which is characterized in that specifically include
Following steps:
Step 1, electro-conductive glass substrate pretreatment: by etched electro-conductive glass substrate in acetone, isopropanol, ethyl alcohol and deionization
It is cleaned by ultrasonic in water, with being dried with nitrogen after taking-up, and handles surface with UV ozone cleaning machine；
Step 2, hole transmission layer preparation: preparing nickel oxide film in the electro-conductive glass substrate using electrochemical deposition method,
And the print being prepared is put into UV ozone cleaning machine and is exposed, it is then placed in Muffle furnace and heats；
Step 3, the preparation of perovskite precursor solution and spin coating: lead iodide and iodide ammonium are dissolved in gamma-butyrolacton and two
The in the mixed solvent of methyl sulfoxide is configured to perovskite precursor solution, and spin coating is carried out on the nickel oxide film, obtains calcium
Titanium ore film；
Step 4, the preparation of fullerene derivate solution and spin coating: fullerene derivate is dissolved in chlorobenzene to be configured to first molten
Liquid carries out spin coating on the perovskite thin film, obtains fullerene derivate layer；
Step 5, the preparation of bathocuproine solution and spin coating: bathocuproine is dissolved in isopropanol and is configured to the second solution, in the richness
It strangles ene derivative layer and carries out spin coating, obtain bathocuproine layer；
Step 6, silver electrode preparation: under vacuum conditions, silver electrode is prepared using thermal evaporation coating process.
2. the preparation method of the perovskite solar cell as described in claim 1 based on nickel oxide hole transmission layer, feature
It is, in step 1, the electro-conductive glass uses ITO or FTO electro-conductive glass, in the acetone, isopropanol, ethyl alcohol and deionization
Being cleaned by ultrasonic the time in water is 15 minutes.
3. the preparation method of the perovskite solar cell as described in claim 1 based on nickel oxide hole transmission layer, feature
Be, in step 2, hole transmission layer preparation specifically includes the following steps:
Step 2.1 prepares Nickelous nitrate hexahydrate aqueous solution, is stirred at room temperature, until forming absinthe-green clear solution.It
Solution is filtered by aqueous filtering head afterwards, removes impurity；
Step 2.2 is inserted in parallel into prepared six nitric hydrate by the electro-conductive glass substrate and with the nickel sheet of homalographic
In nickel aqueous solution；The working electrode of the electro-conductive glass substrate connection electrochemical workstation, the nickel sheet are connected to electrode and ginseng
Compare electrode；
Step 2.3, electrochemical workstation use Constant current output, and output electric current is 0.1mA/cm2, the time is 90 seconds, obtains sample
Piece；
Step 2.4 rinses the print with deionized water；
Step 2.5, with being dried with nitrogen print.
4. the preparation method of the perovskite solar cell as claimed in claim 3 based on nickel oxide hole transmission layer, feature
Be, in step 2.1, the substance withdrawl syndrome of the Nickelous nitrate hexahydrate aqueous solution is 2mMol/L, be stirred at room temperature when
Between be 1 hour；The grid spacing of the aqueous filtering head is 0.45 micron.
5. the preparation method of the perovskite solar cell as claimed in claim 3 based on nickel oxide hole transmission layer, feature
Be, in step 2.2, between the electro-conductive glass substrate and the nickel sheet between be divided into 5 centimetres.
6. the preparation of the perovskite solar cell based on nickel oxide hole transmission layer as described in claim 4 or claim 5
Method, which is characterized in that in step 2, it is specially 5 minutes that the print, which is put into the time exposed in UV ozone cleaning machine, institute
Heating process in Muffle furnace is stated specifically, 300 DEG C are heated 2 hours.
7. the preparation method of the perovskite solar cell as claimed in claim 6 based on nickel oxide hole transmission layer, feature
It is, in step 3, the molar ratio of the lead iodide and the iodide ammonium is 1:1, the gamma-butyrolacton and the diformazan
The volume ratio of base sulfoxide is 7:3, and the obtained perovskite precursor solution concentration is 1mMol/mL, in the nickel oxide film
The upper design parameter for carrying out spin coating is 500rpm, and for 12 seconds, and then 4000rpm, continues 30 seconds.
8. the preparation method of the perovskite solar cell as claimed in claim 7 based on nickel oxide hole transmission layer, feature
It is, in step 4, the concentration of first solution is 20mg/mL, and the design parameter of spin coating is carried out on the perovskite thin film
For 2000rpm, continue 30 seconds.
9. the preparation method of the perovskite solar cell as claimed in claim 8 based on nickel oxide hole transmission layer, feature
It is, in step 5, the concentration of second solution is 0.5mg/mL, carries out the specific of spin coating in the fullerene derivate layer
Parameter is 4000rpm, continues 30 seconds.
10. the preparation method of the perovskite solar cell as claimed in claim 9 based on nickel oxide hole transmission layer, feature
Be, in step 6, the vacuum condition is specially 1E-4Pa, the silver electrode with a thickness of 120nm.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110289354A (en) * | 2019-06-10 | 2019-09-27 | 上海交通大学 | A kind of solar cell preparation method based on calcium titanium ore bed bilateral passivation film |
| CN111092157A (en) * | 2019-12-31 | 2020-05-01 | 桂林电子科技大学 | Preparation method of efficient and stable perovskite solar cell |
| CN111435706A (en) * | 2019-06-29 | 2020-07-21 | 杭州纤纳光电科技有限公司 | Composite hole transport layer, solar cell with composite hole transport layer and preparation method of composite hole transport layer |
| CN112467042A (en) * | 2020-11-25 | 2021-03-09 | 西南石油大学 | Intelligent automatic production system for perovskite solar cell module |
| CN112510150A (en) * | 2020-11-30 | 2021-03-16 | 无锡极电光能科技有限公司 | Hole transport layer, and preparation method and application thereof |
| CN112614940A (en) * | 2020-12-18 | 2021-04-06 | 无锡极电光能科技有限公司 | Preparation method and application of nickel oxide film for hole transport layer in perovskite battery |
| CN113421978A (en) * | 2021-05-08 | 2021-09-21 | 中国计量大学 | Preparation method of magnetic perovskite thin film under action of weak magnetic field |
| WO2023132259A1 (en) * | 2022-01-06 | 2023-07-13 | 国立研究開発法人産業技術総合研究所 | Method for treating surface of metal oxide, method for manufacturing perovskite solar cell, and metal oxide surface treatment device |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110289354A (en) * | 2019-06-10 | 2019-09-27 | 上海交通大学 | A kind of solar cell preparation method based on calcium titanium ore bed bilateral passivation film |
| CN111435706A (en) * | 2019-06-29 | 2020-07-21 | 杭州纤纳光电科技有限公司 | Composite hole transport layer, solar cell with composite hole transport layer and preparation method of composite hole transport layer |
| CN111435706B (en) * | 2019-06-29 | 2023-02-21 | 杭州纤纳光电科技有限公司 | Composite hole transport layer, solar cell with composite hole transport layer and preparation method of composite hole transport layer |
| CN111092157A (en) * | 2019-12-31 | 2020-05-01 | 桂林电子科技大学 | Preparation method of efficient and stable perovskite solar cell |
| CN112467042A (en) * | 2020-11-25 | 2021-03-09 | 西南石油大学 | Intelligent automatic production system for perovskite solar cell module |
| CN112510150A (en) * | 2020-11-30 | 2021-03-16 | 无锡极电光能科技有限公司 | Hole transport layer, and preparation method and application thereof |
| CN112614940A (en) * | 2020-12-18 | 2021-04-06 | 无锡极电光能科技有限公司 | Preparation method and application of nickel oxide film for hole transport layer in perovskite battery |
| CN113421978A (en) * | 2021-05-08 | 2021-09-21 | 中国计量大学 | Preparation method of magnetic perovskite thin film under action of weak magnetic field |
| CN113421978B (en) * | 2021-05-08 | 2023-12-01 | 中国计量大学 | Preparation method of magnetic perovskite film with weak magnetic field effect |
| WO2023132259A1 (en) * | 2022-01-06 | 2023-07-13 | 国立研究開発法人産業技術総合研究所 | Method for treating surface of metal oxide, method for manufacturing perovskite solar cell, and metal oxide surface treatment device |
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