CN105655490A - Preparation method of perovskite solar cell - Google Patents
Preparation method of perovskite solar cell Download PDFInfo
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Abstract
The invention discloses a preparation method of a perovskite solar cell. The preparation method comprises the following steps: (1) washing a transparent conductive substrate; (2) spinning and coating on the transparent conductive substrate to prepare a dense hole barrier layer; (3) spinning and coating on the dense hole barrier layer to prepare a mesoporous electron transmission layer; (4) preparing a perovskite type thin film light absorption layer on the mesoporous electron transmission layer by adopting a continuous dropping and coating method; (5) spinning and coating on the perovskite type thin film light absorption layer to prepare a hole transmission layer; and (6) evaporating a metal back electrode on the hole transmission layer to prepare the product. According to the preparation method disclosed by the invention, the perovskite absorption layer is prepared by adopting the continuous dropping and coating method, a prepared absorption layer thin film has good crystallinity and the shape of the thin film is easy to control; the fluctuation degree of obtained crystalline grains is relatively great and the crystalline grains are relatively regular; device short-circuit current, open-circuit voltage and filling factors of the prepared perovskite solar cell are higher than those of a liquid-phase two-step method in the prior art; and finally, the perovskite solar cell with high energy conversion efficiency and good device repeatability is realized.
Description
Technical field
The preparation method that present invention relates particularly to a kind of perovskite solaode.
Background technology
Perovskite solar cell is chosen as annual ten big sciences in 2013 years by " Science " magazine and breaks through, have that conversion efficiency height, cost be low and the simple potential advantages of preparation technology, the efficiency of short five year perovskite solar cells reaches just to be reached 20.1% by 3.8%, become current solar cell field of greatest concern, study the hottest, a direction with the fastest developing speed.
Perovskite solar cell currently mainly has three kinds of preparation methoies: liquid phase one-step method, liquid phase two-step method, vapour deposition process, and vapour deposition rule is only applicable to planar structure battery, and required condition is that fine vacuum Expenses Cost is high simultaneously; So adopting more perovskite deposition method at present is liquid phase one-step method or liquid phase two-step method, wherein liquid phase one-step method is very sensitive to membrance casting condition, and morphology control has bigger difficulty; Liquid phase two-step method, it is generally required to heating PbI2Thin film, with by membranes submerged to MAI/IPA solution or MAI/IPA is loaded into the PbI of heating crystalline2On thin film, this kind of method is unfavorable for realizing the conversion completely of perovskite, lead iodide residual more, film morphology is difficult to control to, be unfavorable for thin film to the absorption of photon thus device efficiency is impacted; Therefore a kind of simple to operate, film forming pattern is easily controllable, and the high efficiency perovskite solar cell preparation method of low cost is just particularly important.
Summary of the invention
It is an object of the invention to overcome prior art defect, it is provided that the preparation method of a kind of perovskite solaode.
Principles of the invention is as follows:
The concrete technical scheme of the present invention is as follows:
A kind of preparation method of perovskite solaode, this solaode is made up of electrically conducting transparent substrate, fine and close hole blocking layer, mesoporous electron transfer layer, Ca-Ti ore type thin-film light-absorbing layer, hole transmission layer and metal back electrode successively,
Its preparation method comprises the steps:
(1) electrically conducting transparent substrate is washed by rubbing with the hands with cleaning agent successively, then with deionized water rinsing, more successively with acetone, EtOH Sonicate 15��20min, dry up followed by nitrogen gun, put into cleaning 15��20min in oxygen plasma cleaning machine;
(2) in the electrically conducting transparent substrate after step (1) processes, the fine and close hole blocking layer of at least one material in titanium oxide, nickel oxide and zirconium oxide is prepared in spin coating, concrete spin coating proceeding is as follows: spin speed is 1500��2500rpm, spin coating number of times is 3 times, each spin-coating time is 20��30s, each spin coating terminates each through thermal station annealing 5��10min, annealing temperature is 100��150 DEG C, be finally transferred in Muffle furnace 400��500 DEG C annealing 30��60min;
(3) material that step (2) prepares is after titanium tetrachloride solution immersion treatment, fine and close hole blocking layer prepares mesoporous electron transfer layer with mesoporous nano material spin coating, concrete spin coating proceeding is as follows: spin speed is 4000��6000rpm, spin-coating time 20��40s, spin coating terminate after in thermal station anneal 5��10min, annealing temperature is 100��150 DEG C, be finally transferred in Muffle furnace 400��500 DEG C annealing 30��60min;
(4) preparing thickness with continuous drop-coating on mesoporous electron transfer layer prepared by step (3) is 550��650nm, crystallite dimension is the Ca-Ti ore type thin-film light-absorbing layer of 300��500nm, particularly as follows: drip the first solution on described mesoporous electron transfer layer, accelerate to 4000��6000rpm with the time of 4��8s from 0rpm and carry out spin-coating film 10��30s, spin coating 10��30s is proceeded again with the timed deceleration of 6��10s to 2000��3000rpm, when being decelerated to 2000��3000rpm, drop coating the second solution is so that the first solution and the second solution reaction film forming generate MAPbI3, then to anneal, the first solution is with PbI2Be solute, DMF with DMSO be solvent, the second solution with MAI be solute, IPA for solvent, wherein PbI2Concentration in the first solution is 0.7��1.8M, PbI2Being 1:1��3 with the mol ratio of DMSO, the concentration of the second solution is 0.189��0.503M, and the temperature of the second solution is 25��100 DEG C;
(5) on Ca-Ti ore type thin-film light-absorbing layer prepared by step (4), hole transmission layer is prepared in spin coating, and concrete spin coating proceeding is as follows: spin speed is 3000��4000rpm, and spin-coating time is 30��40s;
(6) on hole transmission layer prepared by step (5), evaporation thickness is the metal back electrode of 80��120nm.
In a preferred embodiment of the invention, the concentration of the titanium tetrachloride solution used by titanium tetrachloride solution immersion treatment of described step (3) is 35��45mM, and treatment temperature is 65��75 DEG C, and the process time is 25��35min.
In a preferred embodiment of the invention, the annealing temperature of described step (4) is 120��160 DEG C, and the time is 20��30min.
It is further preferred that described mesoporous nano material is titanium oxide and or zirconium oxide.
It is further preferred that the material of described hole transmission layer is organic material or inorganic.
It is further preferred that described organic material is at least one in Spiro-MeOTAD, P3HT, PTAA and TAPC.
It is further preferred that described inorganic is CuI, CuSCN, Cu2At least one in O, CuO, NiO and MoOx.
It is further preferred that the material of described metal back electrode is Au or Ag.
The invention has the beneficial effects as follows:
1, the preparation method of the present invention utilizes continuous drop-coating to prepare perovskite absorbed layer, the good pattern of absorbed layer crystalline property of preparation is easily controllable, obtain crystal grain during crystal grain waviness more Datong District more regular, its shorted devices electric current of perovskite solar cell obtained, open-circuit voltage, fill factor, curve factor is all high than liquid phase two-step method of the prior art, finally achieves energy conversion efficiency and the reproducible perovskite solar cell of device.
2, the preparation method of the present invention is also applied in the laminated cell prepared by planar heterojunction perovskite solar cell and inversion type perovskite solar cell or they and other solar cells, has wide range of applications.
Accompanying drawing explanation
Fig. 1 is continuous drop-coating process signal in the embodiment of the present invention 1.
The perovskite thin film CH that Fig. 2 is comparative example 1 of the present invention and embodiment 1 prepares3NH3PbI3X-ray diffraction (XRD) collection of illustrative plates (note: sample is the perovskite thin film CH on meso-porous titanium oxide3NH3PbI3).
The perovskite thin film CH that Fig. 3 is comparative example 1 (1) of the present invention and embodiment 1 (2) prepares3NH3PbI3Scanning electron microscope (SEM) exterior view.
The VA characteristic curve of the perovskite solar cell that the performance under AM1.5G illumination that Fig. 4 is comparative example 1 of the present invention and embodiment 1 prepares is best.
Fig. 5 is the statistical data figure that comparative example 1 of the present invention and 1 two kinds of methods of embodiment prepare 10 devices.
Detailed description of the invention
In conjunction with accompanying drawing technical scheme it is further detailed below by way of detailed description of the invention and describes.
FTO (the SnO used in following embodiment 1 and comparative example 12: F) transparent conducting glass from Wuhan lattice solar energy Science and Technology Ltd. buy, hole mobile material (Spiro-MeOTAD) is bought from Taiwan lumtec company, N, dinethylformamide solvent (DMF) dimethyl sulfoxide (DMSO) is purchased from Sigma-Aldrich company, lead iodide (PbI2) buy from AlfaAesar company, methylamine iodine (MAI) is buied from Xi'an Bao Laite company
Embodiment 1
(1)FTO(SnO2: F) transparent conducting glass substrate cleans and oxygen plasma surface treatment: FTO transparent conduction base sheet cleaning agent washed by rubbing with the hands 2 times, then with deionized water rinsing 2 times, inserts in rack for cleaning, successively with acetone, EtOH Sonicate 20min. Dry up by nitrogen gun, put into cleaning 15min in oxygen plasma cleaning machine.
(2) spin coating titanium oxide compacted zone: the butanol solution of the diisopropoxy bis-acetylacetonate titanium (titaniumdiisopropoxidebis (acetylacetonate)) of spin coating 0.15M on the FTO substrate that oxygen plasma processed, spin speed 2000rpm spin coating number of times is 3 each spin-coating time is 20s, and each spin coating terminates to control at 125 DEG C each through thermal station annealing 5min annealing temperature. Transfer in Muffle furnace 500 DEG C of annealing 30min afterwards and obtain being coated with the substrate A of fine and close hole blocking layer dense oxide titanium;
(3) titanium tetrachloride solution processes: by substrate A submergence and 70 DEG C, the TiCl of 40mM4In solution, process 30min. With ethanol purge and dry up by nitrogen gun and obtain substrate B;
(4) spin coating titania slurry prepares mesoporous layer: be spun on substrate B by the titania slurry configured, and spin speed is 5000rpm, spin-coating time 20s, and spin coating terminates to place the substrate in thermal station annealing 5min annealing temperature and controls at 100 DEG C. Transfer to 500 DEG C of annealing 30min in Muffle furnace afterwards and obtain substrate C;
(5) drop coating prepares the precursor solution preparation of perovskite: the lead iodide (PbI of configuration 1.3M2) with the N,N-dimethylformamide that mol ratio is 1:1.5 (DMF) solution (1.3MPbI of dimethyl sulfoxide (DMSO)2-1.5DMSO/DMF solution) and isopropanol (IPA) solution (0.377MMAI/IPA) of methylamine iodine (MAI) of 0.377M;
(6) drop coating is prepared perovskite absorbed layer and makes annealing treatment: as it is shown in figure 1, drip PbI on static substrate C2/DMF(1.3MPbI2-1.5DMSO/DMF) solution, accelerate to high speed 5000rpm spin-coating film, drop coating 0.377MMAI/IPA solution when then reduction of speed is to 3000rpm in spin coating process, the two reaction film forming generates MAPbI3, thin film is placed in thermal annealing 15min in 150 DEG C of thermal station, obtains scribbling the substrate D of perovskite thin film;
(7) preparation of hole transmission layer: Spiro-MeOTAD solution is prepared in spin coating on substrate D, spin speed is 4000rpm, and spin-coating time is 30s, obtains being coated with the substrate F of hole transmission layer;
(8) metal Au back electrode evaporation: substrate F is placed in electron beam evaporation instrument system, treats system vacuum��10-7During Torr, starting to be deposited with one layer of gold electrode, thickness of electrode is 80nm, namely obtains perovskite solar cell;
Experimental result: at AM1.5G, 100mW/cm2When the irradiation of etalon optical power, (solar simulator Newport) carries out the performance test of solar cell, and VA characteristic curve as shown in Figure 4, records battery sample open-circuit voltage 1.01V, short-circuit current density 23.62mA/cm2, fill factor, curve factor 74.39%, efficiency is 17.76%
Comparative example 1
Comparative example 1 and embodiment 1 are distinctive in that step (6) prepares perovskite absorbed layer for liquid phase two-step method: drip PbI on static substrate C2/DMF(1.3MPbI2-1.5DMSO/DMF) solution, 3000rpm spin coating 30s film forming, after spin coating instrument is static, drips 0.377MMAI/IPA solution loading loads 0s, rotating speed is that 5000rpm spin coating 30s makes the two reaction generate MAPbI3Thin film. All the other experimental procedure experimental details are all identical with embodiment 1.
Experimental result: at AM1.5G, 100mW/cm2When the irradiation of etalon optical power, (solar simulator Newport) carries out the performance test of solar cell, and VA characteristic curve as shown in Figure 4, records battery sample open-circuit voltage 0.980V, short-circuit current density 20.06mA/cm2, fill factor, curve factor 65.86%, efficiency is 12.94%
The XRD figure spectrum of the perovskite thin film of gained in embodiment 1 and comparative example 1 is carried out such as Fig. 2, wherein: perovskite characteristic main peaks 14.2 �� corresponding, 12.7 �� corresponding lead iodide characteristic main peaks, can clearly find out that perovskite XRD result perovskite characteristic peak prepared by the continuous dripping method of embodiment 1 representated by black line has less halfwidth than the perovskite characteristic peak prepared by the comparative example 1 liquid phase two-step method representated by red line from this collection of illustrative plates, the former be 0.117 �� much smaller than the latter 0.160 �� this show that the perovskite that the former obtains has better crystal property, the ratio that simultaneously the former perovskite is strong with lead iodide characteristic peak is that 23.4 more than the 18.4 of the latter, this also further illustrates the former and has higher lead iodide conversion ratio, the former also realizes converting completely of lead iodide can only having only small residual substantially simultaneously. the perovskite prepared by the continuous dripping method of the known embodiment of XRD analysis 1 has better crystallinity and lead iodide conversion ratio more fully than the perovskite prepared by comparative example 1 liquid phase two-step method, thus having the performance that better absorbs so obtain device its short circuit current device more more.
The SEM figure of the perovskite thin film in embodiment 1 and comparative example 1 is compared such as Fig. 3, known embodiment 1 adopts perovskite thin film crystallization effect prepared by continuous drop-coating better, obtain perovskite thin film finer and close, compared with in comparative example 1 adopt liquid phase two-step method prepare perovskite, crystal grain has the fluctuating become apparent from, simultaneously crystal grain presents and has more systematicness, this is beneficial to cell light and absorbs, reduce light induced electron and hole-recombination simultaneously, reduce battery drain and the situation of short circuit, thus having higher energy conversion efficiency.
10 device performances of preparation in embodiment 1 and comparative example 1 are carried out statistical analysis and compares such as Fig. 5, known embodiment obtains device performance and is substantially better than comparative example, the former obtains the average efficiency of 16.74% and the latter only has 11.48%, simultaneously short circuit current, fill factor, curve factor, open-circuit voltage average statistical value be above the latter, and the former parameters standard deviation is below the latter and shows that the former has better experimental repeatability.
Table 1 below is the data that embodiment 1 prepares 20 devices of gained, obtaining open-circuit voltage meansigma methods higher than 1V, short circuit current is 22.87, and fill factor, curve factor is 70.92%, average efficiency is 16.37%, has again showed that device prepared by the continuous drop-coating of embodiment 1 has good repeatability.
Table 1
Those of ordinary skill in the art are it can be seen that when technical scheme changes in following ranges, remain able to obtain the technique effect same or like with above-described embodiment 1:
A kind of preparation method of perovskite solaode, this solaode is made up of electrically conducting transparent substrate, fine and close hole blocking layer, mesoporous electron transfer layer, Ca-Ti ore type thin-film light-absorbing layer, hole transmission layer and metal back electrode successively,
Its preparation method comprises the steps:
(1) electrically conducting transparent substrate is washed by rubbing with the hands with cleaning agent successively, then with deionized water rinsing, more successively with acetone, EtOH Sonicate 15��20min, dry up followed by nitrogen gun, put into cleaning 15��20min in oxygen plasma cleaning machine;
(2) in the electrically conducting transparent substrate after step (1) processes, the fine and close hole blocking layer of at least one material in titanium oxide, nickel oxide and zirconium oxide is prepared in spin coating, concrete spin coating proceeding is as follows: spin speed is 1500��2500rpm, spin coating number of times is 3 times, each spin-coating time is 20��30s, each spin coating terminates each through thermal station annealing 5��10min, annealing temperature is 100��150 DEG C, be finally transferred in Muffle furnace 400��500 DEG C annealing 30��60min;
(3) after titanium tetrachloride solution immersion treatment, (concentration of titanium tetrachloride solution is 35��45mM to the material that step (2) prepares, treatment temperature is 65��75 DEG C, the process time is 25��35min), fine and close hole blocking layer prepares mesoporous electron transfer layer with mesoporous nano material spin coating, concrete spin coating proceeding is as follows: spin speed is 4000��6000rpm, spin-coating time 20��40s, spin coating terminate after in thermal station anneal 5��10min, annealing temperature is 100��150 DEG C, be finally transferred in Muffle furnace 400��500 DEG C annealing 30��60min;
(4) preparing thickness with continuous drop-coating on mesoporous electron transfer layer prepared by step (3) is 550��650nm, crystallite dimension is the Ca-Ti ore type thin-film light-absorbing layer of 300��500nm, particularly as follows: drip the first solution on described mesoporous electron transfer layer, accelerate to 4000��6000rpm with the time of 4��8s from 0rpm and carry out spin-coating film 10��30s, spin coating 10��30s is proceeded again with the timed deceleration of 6��10s to 2000��3000rpm, when being decelerated to 2000��3000rpm, drop coating the second solution is so that the first solution and the second solution reaction film forming generate MAPbI3, then annealing (annealing temperature is 120��160 DEG C, and the time is 20��30min), the first solution is with PbI2Be solute, DMF with DMSO be solvent, the second solution with MAI be solute, IPA for solvent, wherein PbI2Concentration in the first solution is 0.7��1.8M, PbI2Being 1:1��3 with the mol ratio of DMSO, the concentration of the second solution is 0.189��0.503, and the temperature of the second solution is 25��100 DEG C;
(5) on Ca-Ti ore type thin-film light-absorbing layer prepared by step (4), hole transmission layer is prepared in spin coating, and concrete spin coating proceeding is as follows: spin speed is 3000��4000rpm, and spin-coating time is 30��40s;
(6) on hole transmission layer prepared by step (5), evaporation thickness is the metal back electrode of 80��120nm.
Described mesoporous nano material is titanium oxide and or zirconium oxide. The material of described hole transmission layer is organic material or inorganic. Described organic material is at least one in Spiro-MeOTAD, P3HT, PTAA and TAPC. Described inorganic is CuI, CuSCN, Cu2At least one in O, CuO, NiO and MoOx. The material of described metal back electrode is Au or Ag.
The above, be only presently preferred embodiments of the present invention, therefore can not limit scope of the invention process according to this, and the equivalence namely made according to the scope of the claims of the present invention and description changes and modifies, and all should still belong in the scope that the present invention contains.
Claims (8)
1. the preparation method of a perovskite solaode, it is characterised in that: this solaode is made up of electrically conducting transparent substrate, fine and close hole blocking layer, mesoporous electron transfer layer, Ca-Ti ore type thin-film light-absorbing layer, hole transmission layer and metal back electrode successively,
Its preparation method comprises the steps:
(1) electrically conducting transparent substrate is washed by rubbing with the hands with cleaning agent successively, then with deionized water rinsing, more successively with acetone, EtOH Sonicate 15��20min, dry up followed by nitrogen gun, put into cleaning 15��20min in oxygen plasma cleaning machine;
(2) in the electrically conducting transparent substrate after step (1) processes, the fine and close hole blocking layer of at least one material in titanium oxide, nickel oxide and zirconium oxide is prepared in spin coating, concrete spin coating proceeding is as follows: spin speed is 1500��2500rpm, spin coating number of times is 3 times, each spin-coating time is 20��30s, each spin coating terminates each through thermal station annealing 5��10min, annealing temperature is 100��150 DEG C, be finally transferred in Muffle furnace 400��500 DEG C annealing 30��60min;
(3) material that step (2) prepares is after titanium tetrachloride solution immersion treatment, fine and close hole blocking layer prepares mesoporous electron transfer layer with mesoporous nano material spin coating, concrete spin coating proceeding is as follows: spin speed is 4000��6000rpm, spin-coating time 20��40s, spin coating terminate after in thermal station anneal 5��10min, annealing temperature is 100��150 DEG C, be finally transferred in Muffle furnace 400��500 DEG C annealing 30��60min;
(4) preparing thickness with continuous drop-coating on mesoporous electron transfer layer prepared by step (3) is 550��650nm, crystallite dimension is the Ca-Ti ore type thin-film light-absorbing layer of 300��500nm, particularly as follows: drip the first solution on described mesoporous electron transfer layer, accelerate to 4000��6000rpm with the time of 4��8s from 0rpm and carry out spin-coating film 10��30s, spin coating 10��30s is proceeded again with the timed deceleration of 6��10s to 2000��3000rpm, when being decelerated to 2000��3000rpm, drop coating the second solution is so that the first solution and the second solution reaction film forming generate MAPbI3, then to anneal, the first solution is with PbI2Be solute, DMF with DMSO be solvent, the second solution with MAI be solute, IPA for solvent, wherein PbI2Concentration in the first solution is 0.7��1.8M, PbI2Being 1:1��3 with the mol ratio of DMSO, the concentration of the second solution is 0.189��0.503, and the temperature of the second solution is 25��100 DEG C;
(5) on Ca-Ti ore type thin-film light-absorbing layer prepared by step (4), hole transmission layer is prepared in spin coating, and concrete spin coating proceeding is as follows: spin speed is 3000��4000rpm, and spin-coating time is 30��40s;
(6) on hole transmission layer prepared by step (5), evaporation thickness is the metal back electrode of 80��120nm.
2. preparation method as claimed in claim 1, it is characterised in that: the concentration of the titanium tetrachloride solution used by titanium tetrachloride solution immersion treatment of described step (3) is 35��45mM, and treatment temperature is 65��75 DEG C, and the process time is 25��35min.
3. preparation method as claimed in claim 1, it is characterised in that: the annealing temperature of described step (4) is 120��160 DEG C, and the time is 20��30min.
4. preparation method as described in any claim in claims 1 to 3, it is characterised in that: described mesoporous nano material is titanium oxide and or zirconium oxide.
5. preparation method as described in any claim in claims 1 to 3, it is characterised in that: the material of described hole transmission layer is organic material or inorganic.
6. preparation method as claimed in claim 5, it is characterised in that: described organic material is at least one in Spiro-MeOTAD, P3HT, PTAA and TAPC.
7. preparation method as claimed in claim 5, it is characterised in that: described inorganic is CuI, CuSCN, Cu2At least one in O, CuO, NiO and MoOx.
8. preparation method as described in any claim in claims 1 to 3, it is characterised in that: the material of described metal back electrode is Au or Ag.
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