CN104617219A - Planar perovskite solar cell based on CH3NH3PbI<2+x>Cl<1-x> optical active layer and preparation method thereof - Google Patents
Planar perovskite solar cell based on CH3NH3PbI<2+x>Cl<1-x> optical active layer and preparation method thereof Download PDFInfo
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- CN104617219A CN104617219A CN201410828278.8A CN201410828278A CN104617219A CN 104617219 A CN104617219 A CN 104617219A CN 201410828278 A CN201410828278 A CN 201410828278A CN 104617219 A CN104617219 A CN 104617219A
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
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- H10K85/141—Organic polymers or oligomers comprising aliphatic or olefinic chains, e.g. poly N-vinylcarbazol, PVC or PTFE
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- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
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Abstract
The invention discloses a planar perovskite solar cell based on a CH3NH3PbI<2+x>Cl<1-x> optical active layer and a preparation method thereof, which are mainly used for solving the problem that the existing optical active layer material is poor in film-forming performance and low in flatness and visible light absorption rate. The planar perovskite solar cell comprises a substrate (1), a cathode (2), an electron transmission layer (3), an optical active layer (4), a cavity transmission layer (5) and an anode (6) from bottom to top, wherein the optical active layer (4) is made from CH3NH3PbI<2+x>Cl<1-x>; the optical active layer is formed by spinning a PbI2 and PbI<1+x Cl<1-x> solution and soaking in a 20mg/ml CH3NH3I solution. The planar perovskite solar cell can be used for reducing carrier recombination on an interface of the optical active layer and the electronic transposition layer, effectively improving the performance of the planar perovskite solar cell, and can be used for photoelectric conversion.
Description
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 organic and inorganic perovskite 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.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, this process not only adds the complexity of 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 improve the energy conversion efficiency of planar structure perovskite solar cell, usually need to control the evenness of photoactive layer and the Carrier recombination of interface.In planar structure perovskite solar cell, conventional light active material has CH
3nH
3pbI
3, CH
3nH
3pbI
3-xcl
xetc., due to CH
3nH
3pbI
3film forming difficulty in the plane, the Carrier recombination of interface is comparatively serious, thus reduces the energy conversion efficiency of planar structure perovskite solar cell.And CH
3nH
3pbI
3-xcl
xin higher chlorinity make CH
3nH
3pbI
3-xcl
xvisible-light absorptivity lower, thus effectively cannot carry out opto-electronic conversion.
Summary of the invention
The object of the invention is to the deficiency for above-mentioned prior art, provide a kind of based on CH
3nH
3pbI
2+xcl
1-xplane perovskite solar cell of photoactive layer and preparation method thereof, to improve the energy conversion efficiency of plane perovskite solar cell, simplifies the manufacture craft of perovskite solar cell, reduces the cost of perovskite solar cell.
In order to existing above-mentioned purpose, 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:
Photoactive layer, adopts CH
3nH
3pbI
2+xcl
1-xmaterial, as opto-electronic conversion active layer, for the formation of smooth photoactive layer, absorbs incident light effectively, and is electric energy by light energy conversion.
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: fluorine-doped tin oxide FTO negative electrode glass substrate is placed in successively deionized water, acetone, absolute ethyl alcohol and deionized water for ultrasonic cleaning 10 ~ 20min, has cleaned rear nitrogen gun and dried up;
(2) c-TiO is prepared
2precursor solution:
(2a) get the diacetyl acetonyl metatitanic acid diisopropyl ester TiAc solution of 75% mass fraction of 1.464mL, and in this solution, add the n-butyl alcohol dilution of 18.536mL, the ultrasonic process of the solution after this dilution 10-20min is obtained to the c-TiO of 0.15M/L
2precursor solution;
(2b) get the diacetyl acetonyl metatitanic acid diisopropyl ester TiAc solution of 75% mass fraction of 2.928mL, and in this solution, add the n-butyl alcohol dilution of 17.072mL, the ultrasonic process of the solution after this dilution 10-20min is obtained to the c-TiO of 0.3M/L
2precursor solution;
(3) spin coating c-TiO on fluorine-doped tin oxide FTO negative electrode glass substrate
2precursor solution, and the baking close annealing 5-15min in temperature being 100-500 DEG C, form c-TiO
2electron transfer layer;
(4) deposit PbI
1+xcl
1-xlayer:
(4a) PbI is prepared
2with PbI
1+xcl
1-xsolution:
Get the PbI of 460mg
2be dissolved in the dimethylacetylamide DMF of 1ml, at 90 DEG C of temperature, stir 6h obtain clarifying PbI
2solution;
Get the PbI of 391mg
2with the PbCl of 41.7mg
2be dissolved in the dimethylacetylamide DMF of 1ml, at 90 DEG C of temperature, stir 6h obtain PbI
1+xcl
1-xsettled solution;
(4b) spin coating PbI
2and PbI
1+xcl
1-xsolution:
First spin coating PbI on the substrate of step (3) gained
2solution, rotating speed during spin coating is 2000-6000r/min, and the time of spin coating is 30-60s, and the 5-15min that anneals at the temperature of 70 DEG C; Then spin coating PbI
1+xcl
1-xsolution, rotating speed during spin coating is 2000-6000r/min, and the time of spin coating is 30-60s, then the organic solvent of anneal at the temperature of 70 DEG C 5-15min, evaporation of residual;
(5) substrate of step (4) gained is immersed in CH
3nH
3in I solution, at 60 DEG C, keep 5-20min, to ensure PbI
1+xcl
1-xwith CH
3nH
3this bi-material of I fully reacts, and forms CH
3nH
3pbI
2+xcl
1-xphotoactive layer;
(6) in air atmosphere, will to anneal at 90 DEG C 45min through step (5) gained substrate;
(7) at CH
3nH
3pbI
2+xcl
1-xspin coating Spiro-MeOTAD hole transmission layer on photoactive layer, rotating speed during spin coating is 2000 ~ 4500r/min, and the time of spin coating is 45s;
(8) deposit Au metal anode on hole transmission layer.
The present invention compared with prior art tool has the following advantages:
1. improve the performance promoting perovskite solar cell
The present invention adopts CH
3nH
3pbI
2+xcl
1-xmaterial is as photoactive layer, this material has high visible-light absorptivity and evenness, effectively can reduce the Carrier recombination of photoactive layer and electron transport layer interface, thus improve the open circuit voltage of perovskite solar cell, short-circuit current density and fill factor, curve factor, finally achieve the energy conversion efficiency of the perovskite solar cell of planar structure.
2. reduce the cost of perovskite solar cell
The present invention uses spin coating PbI
2and PbI
1+xcl
1-xsolution is again at CH
3nH
3soak in I solution and form CH
3nH
3pbI
2+xcl
1-xthe method of photoactive layer, the method is simple to operate, with low cost, can realize large area film preparation; 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, the present invention is by using spin coating PbI
2and PbI
1+xcl
1-xsolution is again at CH
3nH
3soak in I solution and form CH
3nH
3pbI
2+xcl
1-xthe method of photoactive layer has better performance.
Accompanying drawing explanation
Fig. 1 is CH of the present invention
3nH
3pbI
2+xcl
1-xperovskite solar battery structure schematic diagram;
Fig. 2 is that the present invention makes CH
3nH
3pbI
2+xcl
1-xthe flow chart of 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, CH of the present invention
3nH
3pbI
2+xcl
1-xthe structure of perovskite solar cell comprises from bottom to top: substrate 1, negative electrode 2, electron transfer layer 3, photoactive layer 4, hole transmission layer 5, anode 6;
Substrate 1 adopts thickness to be the glass of 1.9mm, and negative electrode 2 adopts fluorine-doped tin oxide FTO, and thickness is 1um; Electron transfer layer 3 adopts compact titanium dioxide c-TiO
2, thickness is 70 ~ 100nm; Photoactive layer 4 adopts CH
3nH
3pbI
2+xcl
1-x, thickness is 150 ~ 300nm; Hole transmission layer 5 adopts Spiro-MeOTAD, and thickness is 10 ~ 30nm; Anode 6 adopts metal A u, and thickness is 100nm.
With reference to Fig. 2, the present invention makes CH
3nH
3pbI
2+xcl
1-xthe method of perovskite solar cell, provides following three kinds of embodiments.
Embodiment 1, makes CH
3nH
3pbI
2+xcl
1-xthickness is the solar cell of 150nm.
Step 1, cleaning substrate base.
1.9mm glass substrate containing fluorine-doped tin oxide FTO is placed in successively deionized water, acetone, absolute ethyl alcohol and deionized water for ultrasonic cleaning 10min, has cleaned rear nitrogen gun and dried up.
Step 2, deposit c-TiO
2electron transfer layer.
2a) prepare precursor solution:
First get the diacetyl acetonyl metatitanic acid diisopropyl ester TiAc solution of 75% mass fraction of 1.464mL, and in this solution, add the n-butyl alcohol dilution of 18.536mL, obtaining concentration to the ultrasonic process of the solution after this dilution 10min is the c-TiO of 0.15M/L
2precursor solution;
Get the diacetyl acetonyl metatitanic acid diisopropyl ester TiAc solution of 75% mass fraction of 2.928mL again, and in this solution, add the n-butyl alcohol dilution of 17.072mL, obtaining concentration to the ultrasonic process of the solution after this dilution 10min is the c-TiO of 0.3M/L
2precursor solution;
2b) spin coating c-TiO
2precursor solution:
First on the substrate through step 1, first time spin coating concentration is the c-TiO of 0.15M/L
2precursor solution, spin coating rotating speed is 6000r/min, and the time is 60s, and is the baking close annealing 5min of 100 DEG C in temperature;
Be the c-TiO of 0.15M/L in spun concentration again
2on the substrate of precursor solution, second time spin coating concentration is the c-TiO of 0.3M/L
2precursor solution, spin coating rotating speed is 4000r/min, and the time is 40s, and is the baking close annealing 10min of 125 DEG C in temperature;
Last is the c-TiO of 0.3M/L in spun concentration
2on the substrate of precursor solution, third time spin coating concentration is the c-TiO of 0.3M/L
2precursor solution, spin coating rotating speed is 4000r/min, and the time is 30s, is the thermal station of 500 DEG C is annealed in temperature, and the time is 15min; The c-TiO obtained
2thickness is 70nm.
Step 3, spin coating PbI
2and PbI
1+xcl
1-xsolution.
3a) prepare PbI
2and PbI
1+xcl
1-xsolution
First get the PbI of 460mg
2be dissolved in the dimethylacetylamide DMF of 1ml, at 90 DEG C of temperature, stir 6h obtain clarifying PbI
2solution;
Get the PbI of 391mg again
2with the PbCl of 41.7mg
2be dissolved in the dimethylacetylamide DMF of 1ml, at 90 DEG C of temperature, stir 6h obtain PbI
1+xcl
1-xsettled solution;
3b) spin coating PbI
2and PbI
1+xcl
1-xsolution
First, spin coating PbI on the substrate through step 2
2solution, spin coating rotating speed is 4500r/min, and spin-coating time is 60s, and dries more than 30min in an oven;
Then, at spun PbI
2spin coating PbI on the substrate of solution
xcl
1-xsolution, spin coating rotating speed is 4500r/min, and spin-coating time is 60s, and dries more than 30min, the PbI obtained in an oven
1+xcl
1-xthe thickness of film is 100nm.
Step 4, forms CH
3nH
3pbI
2+xcl
1-xmaterial.
First, by the CH of 80mg
3nH
3i is dissolved in the isopropyl alcohol IPA of 40ml, and ultrasonic process 10min obtains CH
3nH
3i solution;
Then, the substrate through step 3 is immersed in CH
3nH
3in I solution, take out after keeping 5min at 60 DEG C, and clean with isopropyl alcohol IPA, then dry up by nitrogen gun, anneal 45min at 90 DEG C, obtains the CH that thickness is 150nm
3nH
3pbI
2+xcl
1-xmaterial.
Step 5, spin coating Spiro-MeOTAD hole transmission layer.
The Spiro-MeOTAD of 90mg is dissolved in 1ml chlorobenzene CB, obtains the Spiro-MeOTAD chlorobenzene CB solution of 90mg/ml; Spin coating Spiro-MeOTAD chlorobenzene CB solution on the substrate through step 4 again, spin coating rotating speed 4500r/min, time 45s, obtain the Spiro-MeOTAD hole transport layer of thickness 10nm.
Step 6, deposit Au metal anode.
Substrate through step 5 is placed in metal evaporation room thermal evaporation Au, background vacuum 4 × 10
-4pa, electric current 80A, obtain 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.
Employing CH has been prepared by above-mentioned steps
3nH
3pbI
2+xcl
1-xthe planar structure perovskite solar cell of photoactive layer, its device effective area is 7mm
2, the energy conversion efficiency that test obtains device reaches 8.5%, and open circuit voltage is 0.82V, and short-circuit current density is-19.6mA/cm
2, fill factor, curve factor is 48%.
Embodiment 2, makes CH
3nH
3pbI
2+xcl
1-xthickness is the solar cell of 200nm.
Step one, cleaning substrate base.
1.9mm glass substrate containing fluorine-doped tin oxide FTO is placed in successively deionized water, acetone, absolute ethyl alcohol and deionized water for ultrasonic cleaning 15min, has cleaned rear nitrogen gun and dried up.
Step 2, deposit c-TiO
2electron transfer layer.
2.1) precursor solution is prepared:
The specific implementation of this step and the step 2a of embodiment 1) identical;
2.2) spin coating c-TiO
2precursor solution:
First, the c-TiO of first time spin coating 0.15M/L on the substrate through step one
2precursor solution, spin coating rotating speed is 6000r/min, and the time is 60s, and is the baking close annealing 5min of 125 DEG C in temperature;
Then, at the c-TiO of spun 0.15M/L
2the c-TiO of second time spin coating 0.3M/L on the substrate of precursor solution
2precursor solution, spin coating rotating speed is 3000r/min, and the time is 40s, and is the baking close annealing 10min of 125 DEG C in temperature;
Finally, at the c-TiO of spun 0.3M/L
2the c-TiO of third time spin coating 0.3M/L on the substrate of precursor solution
2precursor solution, spin coating rotating speed is 3000r/min, and the time is 30s, and is 15min that the thermal station of 500 DEG C is annealed in temperature, and obtaining thickness is the c-TiO of 85nm
2.
Step 3, spin coating PbI
2and PbI
xcl
1-xsolution.
3.1) PbI is prepared
2and PbI
1+xcl
1-xsolution:
The specific implementation of this step and the step 3a of embodiment 1) identical;
3.2) spin coating PbI
2and PbI
1+xcl
1-xsolution:
First, spin coating PbI on the substrate through step 2
2solution, spin coating rotating speed is 3000r/min, and spin-coating time is 60s, and dries more than 30min in an oven;
Then, at spun PbI
2spin coating PbI on the substrate of solution
1+xcl
1-xsolution, spin coating rotating speed is 3000r/min, and spin-coating time is 60s, and dries more than 30min, the PbI obtained in an oven
1+xcl
1-xthe thickness of film is 150nm;
Step 4, forms CH
3nH
3pbI
2+xcl
1-xmaterial.
4.1) by the CH of 80mg
3nH
3i is dissolved in the isopropyl alcohol IPA of 40ml, and ultrasonic process 10min obtains settled solution;
4.2) substrate through step 3 is immersed in settled solution, takes out keep 15min at 60 DEG C after, clean with isopropyl alcohol IPA and dry up by nitrogen gun, then the 45min that anneals at the temperature of 90 DEG C, obtain the CH that thickness is 200nm
3nH
3pbI
2+xcl
1-xmaterial.
Step 5, spin coating Spiro-MeOTAD hole transmission layer.
5.1) Spiro-MeOTAD of 90mg is dissolved in 1ml chlorobenzene CB, obtains the Spiro-MeOTAD chlorobenzene CB solution of 90mg/ml;
5.2) spin coating Spiro-MeOTAD chlorobenzene CB solution on the substrate through step 4, spin coating rotating speed is 3000r/min, and the time is 45s, obtains the Spiro-MeOTAD hole transport layer of thickness 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.
The employing CH prepared by above-mentioned steps
3nH
3pbI
2+xcl
1-xthe planar structure perovskite solar cell of photoactive layer, its effective area is 7mm
2, under this solar energy being placed on AM 1.5G solar spectrum, carry out photoelectric respone test, testing the energy conversion efficiency obtained is 10.7%, and open circuit voltage is 0.89V, and short-circuit current density is-19.9mA/cm
2, fill factor, curve factor is 47%.
Embodiment 3, makes CH
3nH
3pbI
2+xcl
1-xthickness is the solar cell of 300nm.
Steps A, cleaning substrate base.
1.9mm glass substrate containing fluorine-doped tin oxide FTO is placed in successively deionized water, acetone, absolute ethyl alcohol and deionized water for ultrasonic cleaning 20min, has cleaned rear nitrogen gun and dried up.
Step B, deposit c-TiO
2electron transfer layer.
B1) precursor solution is prepared:
The specific implementation of this step and the step 2a of embodiment 1) identical;
B2) spin coating c-TiO
2precursor solution:
B21) on the substrate through steps A with the spin-coating time of 6000r/min, 60s, the c-TiO of first time spin coating 0.15M/L
2precursor solution, and the baking close annealing 5min in temperature being 125 DEG C;
B22) at the c-TiO of spun 0.15M/L
2with the spin speed of 2000r/min on the substrate of precursor solution, the spin-coating time of 40s, the c-TiO of second time spin coating 0.3M/L
2precursor solution, and the baking close annealing 10min in temperature being 125 DEG C;
B23) at the c-TiO of spun 0.3M/L
2with the spin-coating time of the spin speed of 2000r/min, 30s on the substrate of precursor solution, the c-TiO of third time spin coating 0.3M/L
2precursor solution, and be 15min that the thermal station of 500 DEG C is annealed in temperature, obtain the compact titanium dioxide c-TiO that thickness is 100nm
2.
Step C, spin coating PbI
2and PbI
1+xcl
1-xsolution.
C1) specific implementation of this step and the step 3a of embodiment 1) identical;
C2) first, spin coating PbI on the substrate through step B
2solution, spin coating rotating speed is 2000r/min, and spin-coating time is 40s, and dries more than 30min in an oven;
Then at spun PbI
2spin coating PbI on the substrate of solution
1+xcl
1-xsolution, spin coating rotating speed is 2000r/min, and spin-coating time is 40s, and dries more than 30min, the PbI obtained in an oven
1+xcl
1-xthe thickness of film is 250nm;
Step D, forms CH
3nH
3pbI
2+xcl
1-xmaterial.
By the CH of 80mg
3nH
3i is dissolved in the isopropyl alcohol IPA of 40ml, and ultrasonic process 10min obtains settled solution, and the substrate through step C is immersed in CH
3nH
3in I settled solution, take out after keeping 20min at 60 DEG C, clean with isopropyl alcohol IPA and dry up by nitrogen gun, anneal 45min at 90 DEG C, obtains the CH that thickness is 300nm
3nH
3pbI
2+xcl
1-xmaterial.
Step e, spin coating Spiro-MeOTAD hole transmission layer.
First the Spiro-MeOTAD of 90mg is dissolved in the Spiro-MeOTAD chlorobenzene CB solution obtaining 90mg/ml in 1ml chlorobenzene CB; Again on the substrate through step D with the spin-coating time of 2000r/min spin speed, 45s, spin coating Spiro-MeOTAD chlorobenzene CB solution, obtains the Spiro-MeOTAD hole transport layer of thickness 30nm.
Step F, deposit Au metal anode.
Substrate through step e being placed in vacuum degree is 4 × 10
-4pa, electric current are thermal evaporation Au in the metal evaporation room of 80A, obtain 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.
Employing CH has been prepared by above-mentioned steps
3nH
3pbI
2+xcl
1-xthe planar structure perovskite solar cell of photoactive layer, device effective area is 7mm
2, the energy conversion efficiency that test obtains device reaches 14.2%, and open circuit voltage is 0.93V, and short-circuit current density is-19.9mA/cm
2, fill factor, curve factor is 54%.
The above is only several preferred implementation 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 (8)
1. one kind based on CH
3nH
3pbI
2+xcl
1-xthe plane perovskite solar cell of photoactive layer, 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:
Photoactive layer (4), adopts the CH of 150 ~ 300nm thickness
3nH
3pbI
2+xcl
1-x, for reducing the Carrier recombination between itself and electron transfer layer (3), improve the quality of forming film of photoactive layer.
2. photoactive layer (4), adopts the CH of 150 ~ 300nm thickness
3nH
3pbI
2+xcl
1-x, for reducing the Carrier recombination between itself and electron transfer layer (3), improve the quality of forming film of photoactive layer.
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 hole transmission layer (5) is 10 ~ 30nm.
5. one kind based on CH
3nH
3pbI
2+xcl
1-xthe manufacture method of the plane perovskite solar cell of photoactive layer, comprises the steps:
(1) substrate base is cleaned: fluorine-doped tin oxide FTO negative electrode glass substrate is placed in successively deionized water, acetone, absolute ethyl alcohol and deionized water for ultrasonic cleaning 10 ~ 20min, has cleaned rear nitrogen gun and dried up;
(2) c-TiO is prepared
2precursor solution:
(2a) get the diacetyl acetonyl metatitanic acid diisopropyl ester TiAc solution of 75% mass fraction of 1.464mL, and in this solution, add the n-butyl alcohol dilution of 18.536mL, the ultrasonic process of the solution after this dilution 10-20min is obtained to the c-TiO of 0.15M/L
2precursor solution;
(2b) get the diacetyl acetonyl metatitanic acid diisopropyl ester TiAc solution of 75% mass fraction of 2.928mL, and in this solution, add the n-butyl alcohol dilution of 17.072mL, the ultrasonic process of the solution after this dilution 10-20min is obtained to the c-TiO of 0.3M/L
2precursor solution;
(3) spin coating c-TiO on fluorine-doped tin oxide FTO negative electrode glass substrate
2precursor solution, and the baking close annealing 5-15min in temperature being 100-500 DEG C, form c-TiO
2electron transfer layer;
(4) deposit PbI
1+xcl
1-xlayer:
(4a) PbI is prepared
2with PbI
1+xcl
1-xsolution:
Get the PbI of 460mg
2be dissolved in the dimethylacetylamide DMF of 1ml, at 90 DEG C of temperature, stir 6h obtain clarifying PbI
2solution;
Get the PbI of 391mg
2with the PbCl of 41.7mg
2be dissolved in the dimethylacetylamide DMF of 1ml, at 90 DEG C of temperature, stir 6h obtain PbI
1+xcl
1-xsettled solution;
(4b) spin coating PbI
2and PbI
1+xcl
1-xsolution:
First spin coating PbI on the substrate of step (3) gained
2solution, rotating speed during spin coating is 2000-6000r/min, and the time of spin coating is 30-60s, and the 5-15min that anneals at the temperature of 70 DEG C; Then spin coating PbI
1+xcl
1-xsolution, rotating speed during spin coating is 2000-6000r/min, and the time of spin coating is 30-60s, then the organic solvent of anneal at the temperature of 70 DEG C 5-15min, evaporation of residual;
(5) substrate of step (4) gained is immersed in CH
3nH
3in I solution, at 60 DEG C, keep 5-20min, to ensure PbI
1+xcl
1-xwith CH
3nH
3this bi-material of I fully reacts, and forms CH
3nH
3pbI
2+xcl
1-xphotoactive layer;
(6) in air atmosphere, will to anneal at 90 DEG C 45min through step (5) gained substrate;
(7) at CH
3nH
3pbI
2+xcl
1-xspin coating Spiro-MeOTAD hole transmission layer on photoactive layer, rotating speed during spin coating is 2000-4500r/min, and the time of spin coating is 45s;
(8) deposit Au metal anode on hole transmission layer.
6. as claimed in claim 5 based on CH
3nH
3pbI
2+xcl
1-xthe plane perovskite preparation method of solar battery of photoactive layer, is characterized in that, described step 5) in CH
3nH
3i solution is by the CH of 800mg
3nH
3the isopropyl alcohol IPA that I is dissolved in 40ml obtains the solution that concentration is 20mg/mL.
7. as claimed in claim 5 based on CH
3nH
3pbI
2+xcl
1-xthe plane perovskite preparation method of solar battery of photoactive layer, is characterized in that, described step 7) in Spiro-MeOTAD solution, be obtain the solution that concentration is 90mg/mL in the chlorobenzene CB Spiro-MeOTAD of 90mg being dissolved in 1ml.
8. as claimed in claim 5 based on CH
3nH
3pbI
2+xcl
1-xthe plane perovskite preparation method of solar battery of photoactive layer, it is characterized in that step 8) described in deposit Au metal anode on hole transmission layer, its process conditions are: by step 7) gained substrate puts into metal evaporation room, is less than 5 × 10 in vacuum degree
-4pa, under the environment of electric current 80A, thermal evaporation thickness is the Au of 100nm.
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