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CN104617220A - Planar perovskite solar cell based on graphene ZnO cathode and preparation method thereof - Google Patents

Planar perovskite solar cell based on graphene ZnO cathode and preparation method thereof Download PDF

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CN104617220A
CN104617220A CN201410828282.4A CN201410828282A CN104617220A CN 104617220 A CN104617220 A CN 104617220A CN 201410828282 A CN201410828282 A CN 201410828282A CN 104617220 A CN104617220 A CN 104617220A
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graphene
solar cell
negative electrode
solution
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张春福
唐诗
张进成
陈大正
郝跃
习鹤
罗莉
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Xidian University
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    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
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    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
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    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/60—Forming conductive regions or layers, e.g. electrodes
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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Abstract

The invention discloses a planar perovskite solar cell based on graphene ZnO cathode and a preparation method thereof, which are used for solving the problems that an existing perovskite solar cell is high in transparent electrode cost, unmatched in energy level and poor in interface characteristic. The planar perovskite solar cell comprises a substrate (1), a cathode (2), an electron transfer layer (3), an optical active layer (4), a cavity transmission layer (5) and an anode (6) from bottom to top, wherein the cathode (2) is made of graphene and used for collecting electrons; the electron transfer layer is made of ZnO and used for modifying an interface, blocking a cavity and transferring electrons. The graphene is adopted as the cathode, the ZnO electron transfer layer is prepared by spinning a precursor solution, so that the work function of the graphene function is reduced, the energy level matching between the graphene and the CH3NH3PbI3 is realized, the interface characteristic is improved, and the performances of the planar perovskite solar cell are effectively improved.

Description

Based on plane perovskite solar cell and the preparation method of Graphene ZnO negative electrode
Technical field
The invention belongs to technical field of microelectronic devices, particularly solar cell, specifically a kind of perovskite solar cell and preparation method thereof, can be used for opto-electronic conversion.
Background technology
Society, economic fast development brings the such as Tough questions such as energy crisis and global warming, and the forest ecosystem of renewable and clean energy resource has been subjected to global extensive concern.Be different from the traditional energies such as coal, oil, natural gas, solar energy is a kind of green, clean, regenerative resource, inexhaustible, the potential important component part become in future source of energy supply.Solar cell is as a kind of electrooptical device, and its research and apply has been subjected to increasing attention.Compared with silica-based solar cell with high costs, perovskite solar cell adopts perovskite semi-conducting material as photoactive layer, has the features such as with low cost, the absorption coefficient of light is high, quality is light, pliability is good, manufacturing process is simple.Along with deepening continuously of recent domestic correlative study, after particularly adopting the photoactive layer structure of mesoporous battery structure and heterojunction, photoelectric conversion efficiency and the stability of perovskite solar cell constantly promote.Meso-hole structure common in perovskite solar cell, normally spin coating nano particle again on the basis of planar structure, the complexity that this process not only adds technique also improves the cost of perovskite solar cell.Thus, the perovskite solar cell of planar structure more and more comes into one's own.
In order to ensure sufficient optical absorption, solar cell must adopt transparency electrode, and this electrode needs to take into account light transmission and conductivity.At present, tin indium oxide ITO is transparency electrode most widely used in solar cell, but tin indium oxide ITO also has the problem of self, and the reserves as occurring in nature phosphide element are limited, and phosphide element itself has toxicity, and the price of tin indium oxide ITO also grows steadily in recent years.For the perovskite solar cell of low cost, produce to realize its large-scale commercial, except improving its energy conversion efficiency, lower cost and better environment friendly are also that industry is paid much attention to.In numerous potential tin indium oxide ITO substitute, Graphene has the light transmission and conductivity that surmount tin indium oxide ITO, meets the demand of transparency electrode completely, and carbon is at nature rich content, non-toxic, and Graphene is also easy to large area film forming simultaneously.Therefore Graphene is that very potential tin indium oxide ITO substitutes electrode, can be used for preparing more low cost and eco-friendly planar structure perovskite solar cell.
In order to improve the energy conversion efficiency of planar structure perovskite solar cell, usually need to add electrode modification layer to realize the level-density parameter at interface and efficient charge carrier transport in battery structure.In planar structure perovskite battery, sunlight enters to inject photoactive layer from negative electrode side, and therefore the light transmission of cathodic modification layer and the impact of conductivity on battery performance can not be ignored.In perovskite solar cell, conventional cathodic modification layer has ZnO, TiO 2, Cs 2cO 3, Ca etc., owing to having high electron mobility and high visible region transmissivity, ZnO is a kind of well decorative layer material.ZnO film can be prepared by multiple method, as rf magnetron sputtering, atomic layer deposition, pulsed laser deposition, chemical vapor deposition and sol-gal process etc., but these techniques are mostly with high costs, and need the high temperature of more than 200 DEG C, therefore be not suitable for preparing large area film, and cannot compatible flexible substrate.
Summary of the invention
The object of the invention is to the deficiency for above-mentioned prior art, a kind of plane perovskite solar cell based on Graphene ZnO negative electrode and preparation method thereof is provided, to simplify manufacture craft, reduces costs, realize the compatibility of large area film preparation and flexible substrate.
For achieving the above object, solar cell of the present invention comprises from bottom to top: substrate, negative electrode, electron transfer layer, photoactive layer, hole transmission layer, anode, is characterized in that:
Negative electrode, adopts Graphene, for collecting electronics;
Electron transfer layer, adopts ZnO, for modifying interface, and blocking hole, transmission electronic.
For achieving the above object, the method that the present invention makes planar structure perovskite solar cell comprises the steps:
(1) substrate base is cleaned: Graphene negative electrode glass substrate is placed in successively deionized water, acetone, absolute ethyl alcohol and deionized water for ultrasonic cleaning 5-15min, has cleaned rear nitrogen gun and dried up;
(2) making ZnO precursor solution:
It is in the ammoniacal liquor of 25% that ZnO powder 150mg particle size being less than 5um is dissolved in 15ml concentration, and after 5min ultrasonic vibration, put into temperature is 5 DEG C of refrigerator cold-storage 24h, obtains the ZnO precursor solution that concentration is 0.125M/L;
(3) spin coating ZnO precursor solution on the glass substrate with Graphene negative electrode, spin coating rotating speed is 2000-4000r/min, and the time is 40s, and is the baking close annealing 5-15min of 100 ~ 200 DEG C in temperature, forms ZnO electron transfer layer;
(4) spin coating PbI on ZnO electron transfer layer 2solution, and the 15min that anneals at 70 DEG C, with evaporation of organic solvent, rotating speed during spin coating is 2000-4500r/min, and the time of spin coating is 30-60s;
(5) by PbI 2layer is converted into CH 3nH 3pbI 3photoactive layer: by through step 4) substrate of gained is immersed in CH 3nH 3in I solution, at 60 DEG C of temperature, keep 5 ~ 20min, to ensure PbI 2with CH 3nH 3this bi-material of I fully reacts;
(6) anneal to before photoactive layer: in air atmosphere, will through step 5) gained substrate anneals 45min at 90 DEG C;
(7) at CH 3nH 3pbI 3spin coating Spiro-MeOTAD hole transmission layer on photoactive layer, spin coating rotating speed is 2000 ~ 4500r/min, and the time of spin coating is 30 ~ 60s;
(8) deposit Au metal anode on hole transmission layer, completes the making of planar structure perovskite solar cell.
Tool of the present invention has the following advantages:
1. improve the energy conversion efficiency of planar structure perovskite solar cell
The present invention adopts Graphene as negative electrode, adopts ZnO as electron transfer layer, because Graphene has the high transmission rate more than 90%, simultaneously not containing toxic element, thus improves environment-friendly quality.And as the ZnO of electron transfer layer, reduce the work function of Graphene negative electrode, achieve Graphene negative electrode and CH 3nH 3pbI 3level-density parameter between photoactive layer, improves Graphene negative electrode and CH 3nH 3pbI 3photoactive layer interfacial characteristics, adds the selectivity of electronics, thus improves the open circuit voltage of planar structure perovskite solar cell, short-circuit current density and fill factor, curve factor, finally achieves the energy conversion efficiency of the perovskite solar cell of planar structure.
2. reduce the cost of perovskite solar cell
The present invention by preparation ZnO precursor solution and on Graphene negative electrode the method for spin coating ZnO precursor solution carry out making ZnO electron transport layer, the method technological temperature is low, simple to operate, with low cost, can realize large area film preparation and the compatibility with flexible substrate; Meanwhile, the employing of planar structure avoids the use of mesoporous layer, simplifies technique, adds the rate of finished products of solar cell, is beneficial to the cost reducing perovskite solar cell.
Compare other preparation methods, preparation ZnO precursor solution also has better application prospect by the method that spin coating carrys out making ZnO electron transport layer.
Accompanying drawing explanation
Fig. 1 is Graphene ZnO negative electrode perovskite solar battery structure schematic diagram of the present invention;
Fig. 2 is the flow chart that the present invention makes Graphene ZnO negative electrode perovskite solar cell.
Embodiment
In order to make objects and advantages of the present invention clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
With reference to Fig. 1, the structure of Graphene ZnO negative electrode perovskite solar cell of the present invention comprises from bottom to top: substrate 1, negative electrode 2, electron transfer layer 3, photoactive layer 4, hole transmission layer 5, anode 6; Wherein, substrate 1 adopts thickness to be the glass of 1.9mm, and negative electrode 2 adopts thickness to be the Graphene of 20 ~ 40nm, and electron transfer layer 3 adopts thickness to be the ZnO of 70 ~ 100nm, and photoactive layer 4 adopts thickness to be the CH of 150 ~ 300nm 3nH 3pbI 3, hole transmission layer 5 adopts thickness to be the Spiro-MeOTAD of 10 ~ 30nm, and anode 6 adopts thickness to be the Au metal of 100nm.
With reference to Fig. 2, the present invention makes the method for Graphene ZnO negative electrode perovskite solar cell, provides following three kinds of embodiments.
Embodiment 1: making ZnO electric transmission layer thickness is the solar cell of 70nm.
Step 1, cleaning substrate base.
The Graphene glass substrate with thickness being 20nm is placed in successively deionized water, acetone, absolute ethyl alcohol and deionized water for ultrasonic cleaning 5min, has cleaned rear nitrogen gun and dried up.
Step 2, deposit ZnO electron transfer layer.
2a) configure ZnO precursor solution: it is in the ammoniacal liquor of 25% that ZnO powder 150mg particle size being less than 5um is dissolved in 15ml concentration, refrigerator cold-storage is put into after 5min ultrasonic vibration, refrigerated storage temperature is 5 DEG C, and cold preservation time is 24h, obtains the ZnO precursor solution that concentration is 0.125M/L;
2b) spin coating ZnO precursor solution on Graphene, spin coating rotating speed is 4000r/min, and spin-coating time is 40s, and is the baking close annealing 5min of 100 DEG C in temperature, and the ZnO thickness of acquisition is 70nm.
Step 3, spin coating PbI 2solution.
First by the PbI of 460mg 2be dissolved in the dimethylacetylamide DMF of 1ml, and stir 6h at 90 DEG C, obtain the clarification PbI of 460/mL 2solution; Then spin coating PbI on the substrate through step 2 2solution, spin coating rotating speed is 4000r/min, and spin-coating time is 60s, obtains the PbI that thickness is 100nm 2film, and dry more than 30 minutes in an oven, with the organic solvent of evaporation of residual.
Step 4, forms CH 3nH 3pbI 3material.
First by the CH of 80mg 3nH 3i is dissolved in the isopropyl alcohol IPA of 40ml, and ultrasonic 10min obtains settled solution, then by spun PbI 2substrate soak in the solution, 60 DEG C keep taking out after 5min, and clean with isopropyl alcohol IPA and dry up by nitrogen gun, anneal 45min at 90 DEG C, the CH obtained 3nH 3pbI 3the thickness of material is 100nm.
Step 5, spin coating Spiro-MeOTAD hole transmission layer.
Spin coating Spiro-MeOTAD chlorobenzene solution on the substrate through step 4, spin coating rotating speed is 4500r/min, and spin-coating time is 30s, and the thickness of the Spiro-MeOTAD hole transmission layer obtained is 10nm.
Step 6, deposit Au metal anode.
Substrate through step 5 being placed in vacuum degree is 4 × 10 -4pa, electric current is thermal evaporation Au in the metal evaporation room of 80A, obtains the Au anode that thickness is 100nm.
Step 7, device detection and sign.
Under AM 1.5G solar spectrum, photoelectric respone test is carried out to the device prepared.
Prepared the planar structure perovskite solar cell of the Graphene negative electrode adopting ZnO to modify by above-mentioned steps, its device effective area is 7mm 2, the energy conversion efficiency that test obtains device reaches 4.8%, and open circuit voltage is 0.72V, and short-circuit current density is-17.8mA/cm 2, fill factor, curve factor is 46%.
Embodiment 2: making ZnO electric transmission layer thickness is the solar cell of 70nm.
Step one, cleaning substrate base
Being that the Graphene glass substrate of 25nm is placed in deionized water, acetone, absolute ethyl alcohol and deionized water for ultrasonic cleaning 10min successively by being coated with thickness, having cleaned rear nitrogen gun and having dried up.
Step 2, deposit ZnO electron transfer layer.
Two. one) specific implementation of this step and the step 2a of embodiment 1) identical;
Two. two) on Graphene with the spin coating rotating speed of 3000r/min, the spin-coating time of 40s, spin coating ZnO precursor solution, and the baking close annealing 10min in temperature being 150 DEG C, the ZnO thickness of acquisition is 85nm.Step 3, spin coating PbI 2solution.
First, by the PbI of 460mg 2be dissolved in the dimethylacetylamide DMF of 1ml, and stir 6h at 90 DEG C, obtain the clarification PbI of 460/mL 2solution;
Then, with the spin coating rotating speed of 3000r/min on the substrate through step 2, the spin-coating time of 45s, spin coating PbI 2solution, obtains the PbI that thickness is 150nm 2film, and dry more than 30 minutes in an oven, with the organic solvent of evaporation of residual.
Step 4, forms CH 3nH 3pbI 3material.
First, by the CH of 80mg 3nH 3i is dissolved in the isopropyl alcohol IPA of 40ml, and ultrasonic 10min obtains settled solution;
Then, by spun PbI 2substrate soak in the solution, take out keep 10min at 60 DEG C of temperature after, clean with isopropyl alcohol IPA and dry up by nitrogen gun, then the 45min that anneals at 90 DEG C, obtaining the CH that thickness is 200nm 3nH 3pbI 3photoactive layer.
Step 5, spin coating Spiro-MeOTAD hole transmission layer.
With the spin coating rotating speed of 3000r/min on the substrate through step 4, the spin-coating time of 45s, spin coating Spiro-MeOTAD chlorobenzene solution, the thickness of the Spiro-MeOTAD hole transmission layer obtained is 20nm.Step 6, deposit Au metal anode.
Substrate through step 5 being placed in vacuum degree is 4 × 10 -4pa, electric current is thermal evaporation Au in the metal evaporation room of 80A, obtains the Au anode that thickness is 100nm.
Step 7, device detection and sign.
Under AM 1.5G solar spectrum, photoelectric respone test is carried out to the device prepared.
Prepared the planar structure perovskite solar cell of the Graphene negative electrode adopting ZnO to modify by above-mentioned steps, its device effective area is 7mm 2, the energy conversion efficiency that test obtains device reaches 5.6%, and open circuit voltage is 0.78V, and short-circuit current density is-18.3mA/cm 2, fill factor, curve factor is 49%.
Embodiment 3: making ZnO electric transmission layer thickness is the solar cell of 100nm.
Steps A, cleaning substrate base.
Being that the Graphene glass substrate of 40nm is placed in deionized water, acetone, absolute ethyl alcohol and deionized water for ultrasonic cleaning 15min successively by being coated with thickness, having cleaned rear nitrogen gun and having dried up.
Step B, deposit ZnO electron transfer layer.
B1) specific implementation of this step and the step 2a of embodiment 1) identical;
B2) on Graphene with the spin coating rotating speed of 2000r/min, the spin-coating time of 40s, spin coating ZnO precursor solution, and the baking close annealing 10min in temperature being 200 DEG C, the ZnO thickness of acquisition is 100nm.
Step C, spin coating PbI 2solution.
First by the PbI of 460mg 2be dissolved in the dimethylacetylamide DMF of 1ml, and stir 6h at 90 DEG C, obtain the clarification PbI of 460/mL 2solution; Again on the substrate through step B with the spin coating rotating speed of 2000r/min, the spin-coating time of 60s, spin coating PbI 2solution, obtains the PbI that thickness is 250nm 2film, and dry more than 30 minutes in an oven, with the organic solvent of evaporation of residual.
Step D, forms CH 3nH 3pbI 3material.
First by the CH of 80mg 3nH 3i is dissolved in the isopropyl alcohol IPA of 40ml, and ultrasonic 10min obtains settled solution; Soaked in the solution by substrate through step C, take out after keeping 20min at the temperature of 60 DEG C, clean with isopropyl alcohol IPA and dry up by nitrogen gun, anneal 45min at 90 DEG C, the CH obtained 3nH 3pbI 3the thickness of material is 300nm.
Step e, spin coating Spiro-MeOTAD hole transmission layer.
With the spin coating rotating speed of 2000r/min on the substrate through step D, the spin-coating time of 45s, spin coating Spiro-MeOTAD chlorobenzene solution, the thickness of the Spiro-MeOTAD hole transmission layer obtained is 30nm.
Step F, deposit Au metal anode.
Substrate through step e being placed in vacuum degree is 4 × 10 -4pa, electric current is thermal evaporation Au in the metal evaporation room of 80A, obtains the Au anode that thickness is 100nm.
Step G, device detection and sign.
Under AM 1.5G solar spectrum, photoelectric respone test is carried out to the device prepared.
Prepared the planar structure perovskite solar cell of the Graphene negative electrode adopting ZnO to modify by above-mentioned steps, its device effective area is 7mm 2, the energy conversion efficiency that test obtains device reaches 8.8%, and open circuit voltage is 0.87V, and short-circuit current density is-18.9mA/cm 2, fill factor, curve factor is 52%.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (10)

1. the plane perovskite solar cell based on Graphene ZnO negative electrode, comprise from bottom to top: substrate (1), negative electrode (2), electron transfer layer (3), photoactive layer (4), hole transmission layer (5), anode (6), is characterized in that:
Described negative electrode (2), adopts Graphene, for collecting electronics;
Described electron transfer layer (3), adopts ZnO, for modifying interface, and blocking hole, transmission electronic.
2. solar cell according to claim 1, is characterized in that: the thickness of negative electrode (2) is 20 ~ 40nm.
3. solar cell according to claim 1, is characterized in that: the thickness of electron transfer layer (3) is 70 ~ 100nm.
4. solar cell according to claim 1, is characterized in that: the thickness of photoactive layer (4) is 150 ~ 300nm.
5. solar cell according to claim 1, is characterized in that: the thickness of hole transmission layer (5) is 10 ~ 30nm.
6., based on the manufacture method of the plane perovskite solar cell of Graphene ZnO negative electrode, comprise the steps:
(1) substrate base is cleaned: Graphene negative electrode glass substrate is placed in successively deionized water, acetone, absolute ethyl alcohol and deionized water for ultrasonic cleaning 5-15min, has cleaned rear nitrogen gun and dried up;
(2) making ZnO precursor solution:
It is in the ammoniacal liquor of 25% that ZnO powder 150mg particle size being less than 5um is dissolved in 15ml concentration, and after 5min ultrasonic vibration, put into temperature is 5 DEG C of refrigerator cold-storage 24h, obtains the ZnO precursor solution that concentration is 0.125M/L;
(3) spin coating ZnO precursor solution on the glass substrate with Graphene negative electrode, spin coating rotating speed is 2000-4000r/min, and the time is 40s, and is the baking close annealing 5-15min of 100 ~ 200 DEG C in temperature, forms ZnO electron transfer layer;
(4) spin coating PbI on ZnO electron transfer layer 2solution, and the 15min that anneals at 70 DEG C, with evaporation of organic solvent, rotating speed during spin coating is 2000-4500r/min, and the time of spin coating is 30-60s;
(5) by PbI 2layer is converted into CH 3nH 3pbI 3photoactive layer: by through step 4) substrate of gained is immersed in CH 3nH 3in I solution, at 60 DEG C of temperature, keep 5 ~ 20min, to ensure PbI 2with CH 3nH 3this bi-material of I fully reacts;
(6) anneal to before photoactive layer: in air atmosphere, will through step 5) gained substrate anneals 45min at 90 DEG C;
(7) at CH 3nH 3pbI 3spin coating Spiro-MeOTAD hole transmission layer on photoactive layer, spin coating rotating speed is 2000 ~ 4500r/min, and the time of spin coating is 30 ~ 60s;
(8) deposit Au metal anode on hole transmission layer, completes the making of planar structure perovskite solar cell.
7., as claimed in claim 6 based on the planar structure perovskite preparation method of solar battery of Graphene ZnO negative electrode, it is characterized in that, the PbI in described step (4) 2solution is by the PbI of 460mg 2first be dissolved in the dimethyl formamide DMF of 1ml and obtain the solution that concentration is 460mg/mL; Again by the PbI of gained 2solution stirs 6h at 90 DEG C.
8., as claimed in claim 6 based on the planar structure perovskite preparation method of solar battery of Graphene ZnO negative electrode, it is characterized in that, the CH in described step (5) 3nH 3i solution is by the CH of 800mg 3nH 3the isopropyl alcohol IPA that I is dissolved in 40ml obtains the CH that concentration is 20mg/mL 3nH 3i solution.
9. as claimed in claim 6 based on the planar structure perovskite preparation method of solar battery of Graphene ZnO negative electrode, it is characterized in that, Spiro-MeOTAD solution in described step (7) obtains the solution that concentration is 90mg/mL in the chlorobenzene CB Spiro-MeOTAD of 90mg being dissolved in 1ml.
10. as claimed in claim 6 based on the planar structure perovskite preparation method of solar battery of Graphene ZnO negative electrode, it is characterized in that the deposit Au metal anode on hole transmission layer described in step (8), its process conditions are: step (7) gained substrate is put into vacuum degree and is less than 5 × 10 -4pa, electric current is in the metal evaporation room of 80A, and thermal evaporation thickness is the Au of 100nm.
CN201410828282.4A 2014-12-26 2014-12-26 Planar perovskite solar cell based on graphene ZnO cathode and preparation method thereof Pending CN104617220A (en)

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CN106957381A (en) * 2017-05-12 2017-07-18 南京工业大学 Design, synthesis and application of hole transport material of perovskite solar cell
CN109659437A (en) * 2018-11-23 2019-04-19 上海工程技术大学 Based on the perovskite solar battery of low temperature graphene aerogel and its preparation
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CN111244289B (en) * 2020-01-15 2022-09-30 重庆文理学院 Preparation method of organic photovoltaic device with ZnO film as interface layer
CN112490373A (en) * 2020-10-30 2021-03-12 西安交通大学 Method and equipment for enhancing film wettability by high-frequency micro-vibration
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CN112490370B (en) * 2020-10-30 2023-09-29 西安交通大学 High-frequency micro-vibration wetting film coating method and equipment for low-pressure chamber
CN112490373B (en) * 2020-10-30 2024-03-26 西安交通大学 Method and equipment for enhancing wettability of film by high-frequency micro-vibration
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Application publication date: 20150513