CN104022226A - Perovskite-based film solar cell and preparation method - Google Patents
Perovskite-based film solar cell and preparation method Download PDFInfo
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Abstract
The invention provides a perovskite-based film solar cell and a preparation method. The perovskite-based film solar cell comprises a transparent substrate, a transparent conductive layer formed on the transparent substrate, a compact layer which is prepared by a semi-conductor material and is formed on the transparent conductive layer, a porous support layer which is prepared by an insulation material and is formed on the compact layer, and a counter electrode layer which is prepared by a conductive carbon material and is formed on the porous support layer, wherein gaps in the porous support layer are filled with an organic metal semiconductor light absorption material having a perovskite structure. The perovskite-based film solar cell employs the carbon material as the material of the counter electrode layer, on the basis of identical performances, cost of the perovskite-based film solar cell through the preparation method provided by the invention is greatly lower than cost of a precious metal counter electrode prepared through a vapor plating method. According to the perovskite-based film solar cell, after preparation, the porous support layer is directly filled with the perovskite light absorption material to form a light absorption layer, and the prepared cell has better performance parameters such as photoelectric current and photoelectric conversion efficiency compared with a perovskite-based film solar cell prepared on the basis of a carbon counter electrode in the prior art.
Description
Technical field
The present invention relates to technical field of solar cells, particularly relate to a kind of perovskite-based thin film solar cell and preparation method thereof.
Background technology
The problems such as that traditional inorganic semiconductor solar cell exists is expensive, high pollution, be therefore necessary to find be easy to synthesize, low-cost and eco-friendly new material, for third generation thin-film solar cells.Ca-Ti ore type organic metal haloid material is (such as CH
3nH
3pbX
3(X=I, Br, Cl)) in recent years with its excellent photoelectric properties, be easy to synthetic character attracted numerous scientific research personnel attention and research interest.By effort, the most effective of the thin film solar cell based on this material reached 19% in the world at present, has very large application potential.Perovskite-based thin film solar cell mainly comprises three types structure: (1) with porous wide bandgap semiconductor film (as TiO
2, ZnO, SnO
2) be the sensitization type hull cell of shelf layer; (2) with cellular insulant material film (as Al
2o
3, ZrO
2, SiO
2deng) see superstructure hetero-junction thin-film battery for Jie of shelf layer; (3) do not adopt the plane hetero-junction thin-film battery of shelf layer.
But at present, the Ca-Ti ore type thin film solar cell of these three kinds of structures all needs to use the precious metal materials such as gold, and by the methods such as vacuum evaporation paired electrode processed, material and facility cost is very expensive.Therefore in the long run set out, adopt the preparation of more cheap material to electrode, reduce the cost to electrode, for large-scale application and the market competitiveness of this kind of battery, be very important.
Chinese invention patent application CN103441217A announced a kind of based on carbon the preparation method to the Ca-Ti ore type organic metal halide thin-film solar cells of electrode, adopt material with carbon element to substitute expensive precious metal material as to electrode layer (being collecting layer, hole), greatly reduce costs.In the method, first prepare in turn mesoporous light-absorption layer, mesoporous dielectric spacer layer and mesoporous carbon to electrode layer, then the precursor liquid of perovskite is filled into downwards electrode layer surface from mesoporous carbon by dripping the method being coated with the hole of mesoporous light-absorption layer and forms battery.Owing to preparing carbon, just fill perovskite after to electrode layer, therefore, for dielectric spacer layer and carbon, to electrode layer, need extra sintering step to form mesoporous layer in the method, raised undoubtedly the production cost of battery.In addition, photoelectric current and the battery efficiency of the perovskite-based thin film solar cell obtaining in this way neither be very desirable, urgently develop new technique and prepare based on carbon the perovskite-based thin film solar cell to electrode layer.
Summary of the invention
One object of the present invention is one of above-mentioned defect for existing in prior art, and a kind of perovskite-based thin film solar cell is cheaply provided.Another further object of the present invention is the perovskite-based thin film solar cell that will provide a kind of battery efficiency higher.Another further object of the present invention is a kind of method that new perovskite-based thin film solar cell of preparation will be provided, and the method is cost-saving, is also suitable for suitability for industrialized production simultaneously.
According to one aspect of the present invention, the invention provides a kind of perovskite-based thin film solar cell, comprising:
Transparent substrates;
The transparency conducting layer forming in described transparent substrates;
That on described transparency conducting layer, form and be the compacted zone of semi-conducting material;
That on described compacted zone, form and be the porous support layer of insulating material, in the hole of described porous support layer inside, be filled with the organic metal semiconductor light absorbent of perovskite structure; And
That on described porous support layer, form and for conductive carbon material to electrode layer.
Alternatively, described electrode layer is formed on the described porous support layer of filling described organic metal semiconductor light absorbent.
Alternatively, described in electrode layer without the existence of obvious described organic metal semiconductor light absorbent.
Alternatively, described is non-porous form to electrode layer.
Alternatively, described perovskite-based thin film solar cell also comprises cap layer, is formed on described porous support layer and described between electrode layer;
Described cap layer is formed by described organic metal semiconductor light absorbent.
Alternatively, described perovskite-based thin film solar cell also comprises hole transmission layer, is formed on described cap layer and described between electrode layer; And/or
Extraction electrode, is formed on described on electrode layer.
Alternatively, the described insulating material of described porous support layer is selected from Al
2o
3, ZrO
2or SiO
2in a kind of;
Alternatively, the thickness of described porous support layer is between 100-1000nm.
Alternatively, the thickness of described cap layer is between 50-500nm.
Alternatively, to be selected from chemical general formula be ABX to described organic metal semiconductor light absorbent
3in one or more, wherein A is organic amine ion, B is bivalent metal ion, X is halide ion Cl
-, Br
-, I
-or pseudohalogen ion CN
-, NCO
-, NCS
-, NCSe
-in one or more;
Alternatively, described organic amine ion comprises CH
3nH
3 +, C
2h
5nH
3 +, NH
2cH=NH
2 +in one or more;
Alternatively, described bivalent metal ion comprises Cu
2+, Ni
2+, Co
2+, Fe
2+, Mn
2+, Cr
2+, Pd
2+, Cd
2+, Ge
2+, Sn
2+, Pb
2+, Eu
2+in one or more.
Alternatively, described conductive carbon material is selected from one or more in active carbon, carbon black, graphite, Graphene, carbon nano-tube;
Alternatively, described to the thickness of electrode layer between 5-10 μ m.
According to another aspect of the present invention, the present invention also provides a kind of method of preparing perovskite-based thin film solar cell, comprising:
Provide surface to there is the transparent substrates of transparency conducting layer;
On described transparency conducting layer, form the compacted zone of semi-conducting material;
On described compacted zone, form the porous support layer of insulating material;
The organic metal semiconductor light absorbent with perovskite structure is filled in the hole of described porous support layer inside; And
Filled on the described porous support layer of described organic metal semiconductor light absorbent, form conductive carbon material to electrode layer.
Alternatively, in the process in the hole that described organic metal semiconductor light absorbent is filled into described porous support layer inside, the surface deposition at described porous support layer forms a cap layer; Described electrode layer is formed in described cap layer.
Alternatively, described method is also included in described cap layer and forms hole transmission layer, described electrode layer is formed on described hole transmission layer; And/or
Described, form extraction electrode on to electrode layer.
Alternatively, described insulating material is selected from Al
2o
3, ZrO
2or SiO
2in a kind of, by silk screen print method, on described compacted zone, print the insulation paste that one deck is formed by described insulating material, after 60-100 ℃ of oven dry, through 300-550 ℃ of sintering, make described porous support layer.
Alternatively, described conductive carbon material and binding agent are added and in dispersant, form homodispersely to electrode slurry, by described, electrode slurry is coated on described porous support layer, drying forms described to electrode layer,
Wherein, described dispersant is non-polar organic solvent, and alternatively, described non-polar organic solvent is selected from one or more in benzene, toluene, chlorobenzene, carbon tetrachloride, ethyl acetate, benzinum, senior aliphatic hydrocarbon, higher alcohols; Described binding agent is for being dissolved in the macromolecular material of described dispersant.
Alternatively, adopt be selected from paddling process, ultrasonic method, polishing, ball-milling method one or more by described conductive carbon material and binding agent be dispersed in described dispersant, form described to electrode slurry; And/or
Employing is selected from a kind of in knife coating, spraying process, silk screen print method, squeezing and coating method and by described, electrode slurry is coated on described porous support layer.
Compare with existing perovskite-based thin film solar cell preparation method, the invention has the advantages that:
1) with low cost.Adopt material with carbon element as to electrode material, in the situation that performance is suitable, its cost well below the noble metal of preparing by the method for evaporation to electrode; In addition, carbon of the present invention does not need to carry out high-temperature calcination to electrode in the process of preparation, therefore can reduce costs further.
2) excellent performance.Perovskite light absorbent in the present invention is directly filled and is formed light-absorption layer after preparing shelf layer, do not need with precursor liquid through thick depositing to again shelf layer inside after electrode layer, can guarantee that like this light absorbent is ideally deposited in shelf layer internal voids, avoid occurring that light absorbent deposits inadequate situation.The battery of preparing so is obviously better than the perovskite-based thin film solar cell to electrode based on carbon prepared by prior art in the performance parameters such as photoelectric current, electricity conversion.
3) suitability is strong.According to the method in the present invention, by flexible adjustment binding agent and dispersant, not only can prepare the carbon of the adaptive perovskite-based thin film solar cell without hole transmission layer to electrode layer, but also the carbon that can prepare the perovskite-based thin film solar cell that adaptation contains hole transmission layer is to electrode layer.
According to the detailed description to the specific embodiment of the invention by reference to the accompanying drawings below, those skilled in the art will understand above-mentioned and other objects, advantage and feature of the present invention more.
Accompanying drawing explanation
Hereinafter in exemplary and nonrestrictive mode, describe specific embodiments more of the present invention in detail with reference to the accompanying drawings.In accompanying drawing, identical Reference numeral has indicated same or similar parts or part.It should be appreciated by those skilled in the art that these accompanying drawings may not draw in proportion.For the layer structure of perovskite-based thin film solar cell is shown significantly, the size of solar cell on is vertically than much larger times of reality.In accompanying drawing:
Fig. 1 is the structural representation of perovskite-based thin film solar cell according to an embodiment of the invention;
Fig. 2 is the structural representation of perovskite-based thin film solar cell in accordance with another embodiment of the present invention;
Fig. 3 is the structural representation of the perovskite-based thin film solar cell of another embodiment according to the present invention.
Embodiment
Before specifically describing embodiments of the present invention, paper battery efficiency method of measurement of the present invention.Constant potential/galvanostat that the photoelectric properties of battery are computerizedd control (Princeton Applied Research, Model263A).By light anode and the photocathode of the solar cell device of preparation respectively with the work electrode of constant potential/galvanostat with electrode tip is connected.Light source is used 500W xenon lamp, and incident intensity is 100mw/cm
2, illuminating area is 0.1cm
2.Except as otherwise noted, the photoelectric properties in following embodiment are measured and are all at room temperature carried out.
The term using in the present invention unless otherwise noted, is to understand in conventional sense in the art according to it.
Present inventor finds under study for action, causing in prior art is not that very desirable reason is based on carbon to the photoelectric current of the perovskite-based thin film solar cell of electrode and battery efficiency, because mesoporous carbon reaches micron dimension to the thickness of electrode layer, this is very unfavorable for electrode layer being filled in mesoporous light-absorption layer by mesoporous carbon perovskite light absorbent, cause light absorbent can not effectively contact with mesoporous light-absorption layer material, thereby affect the performance parameters such as the photoelectric current size of battery and battery efficiency.Present inventor further finds after preparing porous support layer, being about to perovskite light absorbent is filled in the hole of porous support layer, on porous support layer, prepare successively again hole transmission layer and directly prepare electrode layer to electrode layer or on porous support layer, can improve the battery efficiency of perovskite-based sun film.
Fig. 1 is the structural representation of perovskite-based thin film solar cell according to an embodiment of the invention.As shown in Figure 1, perovskite-based thin film solar cell can comprise transparent substrates 10 in general manner; Be arranged on the transparency conducting layer 11 in transparent substrates 10; The compacted zone 12 of the semi-conducting material forming on transparency conducting layer 11; The porous support layer 13 forming on compacted zone 12 is filled with the organic metal semiconductor light absorbent of perovskite structure on porous support layer 13 in inner hole; Be formed on the cap layer 14 on porous support layer 13, cap layer 14 is formed on described porous support layer 13 by described organic metal semiconductor light absorbent when being filled into porous support layer 13 internal void; In cap layer 14, form to electrode layer 16.In one embodiment, can also on to electrode layer 16, form extraction electrode 17.
In the embodiment shown in Figure 2, by further improving preparation technology, can make organic metal semiconductor light absorbent in being filled into the process of porous support layer 13, substantially flush with the upper surface of porous support layer 13, and there will not be the cap layer 14 covering on porous support layer 13.Now, electrode layer 16 is formed directly on the porous support layer 13 of filling described organic metal semiconductor light absorbent.Because to electrode layer 16 be is just formed on porous support layer 13 after porous support layer 13 is filled organic metal semiconductor light absorbent, thus in electrode layer 16 without the existence of obvious described organic metal semiconductor light absorbent.It will be appreciated by those skilled in the art that, here " without the existence of obvious described organic metal semiconductor light absorbent " refer to the present invention unlike prior art from organic metal semiconductor light absorbent is filled downwards in the surface of electrode 16, or in other words, organic metal semiconductor light absorbent is filled in the process of hole of porous support layer 13 inside without the inside to electrode layer 16, therefore, to there not being the amount of obvious organic metal semiconductor light absorbent in electrode layer 16, only may there is few amount that is not intended to mix in the process of preparation.In the present invention, because organic metal semiconductor light absorbent is filled in the process of hole of porous support layer 13 inside without the inside to electrode layer 16, therefore, the electrode layer 16 in the present invention can be non-porous form.
In the embodiment that comprises hole transmission layer 15 shown in Fig. 3, hole transmission layer 15 can be formed on cap layer 14 and between electrode layer 16.It will be appreciated by those skilled in the art that, for perovskite-based thin film solar cell of the present invention, when having filled after light absorbent in porous support layer 13, if light absorbent just in time maintains an equal level with the surface of porous support layer 13, can directly on porous support layer 13, prepare electrode layer 16, when having filled after light absorbent in porous support layer 13, if exceeding the surface of porous support layer 13, light absorbent forms cap layer 14, can in cap layer 14, prepare electrode layer 16; If also there is hole transmission layer 15 in solar cell of the present invention, on hole transmission layer 15, form electrode layer 16.
In an embodiment of the present invention, transparent substrates 10 can be clear glass, and transparency conducting layer 11 can be the FTO film on clear glass.Compacted zone 12 can be by TiO
2film forms; Its thickness can be between 20-150nm; Can be preferably 50nm.Porous support layer 13 can be by Al
2o
3, ZrO
2or SiO
2material forms; Also can be formed by other insulating material; Its thickness can be between 100-1000nm.Al
2o
3, ZrO
2or SiO
2the pattern of material can be nanocrystalline, nanometer rods, nano wire or nanotube.The thickness of cap layer can be between 50-500nm.
Being filled in organic metal semiconductor light absorbent in porous support layer 13, to be selected from chemical general formula be ABX
3in one or more materials, wherein A is organic amine ion, can include but not limited to CH
3nH
3 +, C
2h
5nH
3 +, NH
2cH=NH
2 +among one or more; B is the metal ion of divalence, can include but not limited to Cu
2+, Ni
2+, Co
2+, Fe
2+, Mn
2+, Cr
2+, Pd
2+, Cd
2+, Ge
2+, Sn
2+, Pb
2+, Eu
2+among one or more; X is halide ion Cl-, Br-, I-or pseudohalogen ion CN
-, NCO
-, NCS
-, NCSe
-among one or more.In one embodiment, described organic metal semiconductor light absorbent is chosen as CH
3nH
3pbI
3.
To electrode layer 16, can be formed by one or more materials that are selected from active carbon, carbon black, flake graphite, Graphene, graphite alkene, spherical graphite, Single Walled Carbon Nanotube, multi-walled carbon nano-tubes, carbon fiber or hard carbon material.Alternatively, can be between 5-10 μ m to the thickness of electrode layer 16.Extraction electrode 17 can be the metallic film that electric conductivity is good.For example Copper Foil, aluminium foil, or other good material of electric conductivity, as graphite paper etc.
In one embodiment, perovskite-based thin film solar cell of the present invention also can comprise positive electrode (not shown), for the ease of prepare positive electrode on transparency conducting layer 11, in the embodiment shown in Fig. 1-3, can make a part for transparency conducting layer 11 extend beyond compacted zone 12, porous support layer 13 and electrode layer 16 is come out.
Below in conjunction with the perovskite-based thin film solar cell shown in Fig. 1, preparation method of the present invention is simply described.
The transparent substrates 10 that provides surface to have transparency conducting layer 11 forms the compacted zone 12 of semi-conducting material on transparency conducting layer 11.Then on compacted zone 12, form porous support layer 13, porous support layer 13 can be formed by insulating material.The organic metal semiconductor light absorbent with perovskite structure is filled in the hole of porous support layer 13 inside; In the process of filling, partly or entirely organic metal semiconductor light absorbent permeates downwards and then is filled into the hole of porous support layer 13 inside from the upper surface of porous support layer 13.When just whole organic metal semiconductor light absorbents permeate downwards and then are filled into the hole of porous support layer 13 inside from the upper surface of porous support layer 13, and it is flushed substantially with the upper surface of porous support layer 13, now, can be on porous support layer 13 directly form conductive carbon material to electrode layer 16.When the upper surface that only has part organic metal semiconductor light absorbent from porous support layer 13 permeates downwards and then is filled into the hole of porous support layer 13 inside, and while making cap layer 14 that on porous support layer 13, residual one deck is formed by organic metal semiconductor light absorbent, in this case, can in cap layer 14, form conductive carbon material to electrode layer 16.In one embodiment, also can in cap layer 14, form one deck hole transmission layer 15, electrode layer 16 is formed on hole transmission layer 15.In one embodiment, also can on to electrode layer 16, form extraction electrode 17.In the present invention, the preparation method of compacted zone 12, porous support layer 13, hole transmission layer 15 and the method organic metal semiconductor light absorbent with perovskite structure being filled in the hole of porous support layer 13 can be that those skilled in the art are known.For example, in one embodiment, compacted zone 12 can adopt silk screen print method or spin-coating method preparation, thereby the film that these two kinds of methods obtain all obtains TiO through 450 ℃ of sintering
2compacted zone, thickness is between 20-100nm.Porous support layer 13 can adopt silk screen print method to make.In one embodiment, can on compacted zone 12, by silk screen print method, print one deck Al
2o
3, ZrO
2or SiO
2slurry, after 60-100 ℃ of oven dry, obtains porous support layer 13 through 300-550 ℃ of sintering.The thickness of porous support layer 13 can be between 100-1000nm.
Prepare after porous support layer 13, the organic metal semiconductor light absorbent with perovskite structure is filled in the hole of porous support layer 13.This process can realize by the auxiliary liquid phase method of a step liquid phase method, two step liquid phase methods, gas phase and any method in double source coevaporation method.In one embodiment, described organic metal semiconductor light absorbent can be made to the surface that spin coating liquid is applied to porous support layer 13, by a step liquid phase method, the spin coating of described spin coating liquid is filled in the hole of porous support layer 13 inside.In this process, while still having retained residue spin coating liquid on the surface of porous support layer 13 after the internal void of having filled porous support layer 13, on the surface of porous support layer 13, form one deck cap layer 14.Can utilize afterwards the methods such as spin coating, blade coating, spraying, a painting, silk screen printing, dipping lift, evaporation to prepare hole transmission layer 15 in porous support layer 13 or cap layer 14.
In preparation during to electrode layer 16, a certain proportion of conductive carbon material and binding agent can be added in dispersant, be fully mixed finely dispersed to electrode slurry.Wherein conductive carbon material can be the material with carbon element that particle diameter is suitable and electric conductivity is good, including, but not limited to material with carbon elements such as graphite, carbon black, carbon nano-tube, Graphenes.Choosing of binding agent and dispersant material should not destroy each thin layer having prepared.Dispersant can include but not limited to conventional non-polar organic solvent, as one or more among benzene, toluene, chlorobenzene, carbon tetrachloride, ethyl acetate, benzinum, senior aliphatic hydrocarbon, higher alcohols etc.Binding agent is for being dissolved in the various macromolecular materials of dispersant.Binding agent can be single binding agent, or multiple binding agent forms jointly with the additive with thickening effect.The method of mixed slurry can adopt the method for stirring, ultrasonic, grinding or ball milling, also can be as required by above-mentioned several method comprehensive utilization.By regulating the ratio of binding agent and the amount of dispersant, the slurry of finally making should have good dispersiveness, viscosity and mobility.Can, by prepare electrode slurry is coated on hole transmission layer 15, make it form the uniform conductive coating of one deck.The method that electrode slurry is applied is including but not limited to several below: blade coating, spraying, silk screen printing or squeezing and coating.Complete after coating, can adopt the means such as standing levelling, make the film of preparation more even.Also can at the temperature a little more than room temperature, will dry electrode film, or gently film be dried up with gentle breeze, obtain electrode layer 16.Because preparation is to not passing through high temperature sintering in the process of electrode layer, prepared by said method is non-porous form to electrode layer 16.By above-mentioned method preparation, to electrode layer, easily make electrode layer and hole transmission layer or cap layer or porous support layer formation ohmic contact.
Prepare after electrode layer 16, the good material of one deck electric conductivity can be compressed on electrode layer 16, be prepared into extraction electrode 17.The material of extraction electrode 17 can be the metal film that electric conductivity is good, as aluminium foil, Copper Foil, or other good material of electric conductivity, as graphite paper etc.
Below in conjunction with embodiment more specifically, describe the preparation method of solar cell of the present invention in detail.
Embodiment 1:
Perovskite-based thin-film solar cell structure in the present embodiment as shown in Figure 1.
First at FTO silk screen printing one deck on glass TiO
2thin layer, subsequently silk screen printing one deck Al
2o
3nanometer crystal layer, 450 ℃ heating 30 minutes after, obtaining thickness is the compacted zone 12 of 50nm and the porous support layer 13 that thickness is 500nm.Subsequently, adopt two step liquid phase methods to deposit CH in porous support layer 13
3nH
3pbI
3light absorbent.First by the PbI of 1.2M
2dimethyl formamide (DMF) solution under the rotating speed of 3000rpm, be spin-coated on porous support layer 13 surface, after continuing spin coating 30s, at 90 ℃, heat 2 minutes, with being about to the CH that porous support layer 13 is 10mg/mL in concentration
3nH
3in the aqueous isopropanol of I, soak 10 minutes, finally at the temperature of 90 ℃, heat 45 minutes.Like this, a part of CH
3nH
3pbI
3light absorbent is filled in the internal void of porous support layer 13, another part CH
3nH
3pbI
3light absorbent forms the cap layer 14 that a layer thickness is 100nm on porous support layer.
Preparation process to electrode slurry is as follows: 0.6 gram of graphite (1～3 micron of particle diameter) and 0.3 gram of acetylene black are added among 10 milliliters of ethyl acetate solutions containing 0.5 gram of butadiene-styrene rubber and 0.5 gram of ethyl cellulose, under the rotating speed of 200r/min, ball milling is 4 hours, can obtain electrode slurry.
Prepare after electrode slurry, it is printed on by silk screen print method on the porous support layer 13 of populated light absorbent, its standing levelling, after 5 minutes, is placed in to the dry taking-up after 10 minutes of 80 ℃ of baking ovens, make electrode layer 16.
The filtter gold of suitable dimension is pressed on electrode layer 16, makes extraction electrode 17, completed the making of whole battery.The photoelectric conversion efficiency of this battery final test is 7.2%, and current density is 18.85mA/cm
2, open circuit voltage is 850.4mV.
Embodiment 2:
Perovskite-based thin-film solar cell structure in the present embodiment as shown in Figure 3.
First at FTO silk screen printing one deck on glass TiO
2thin layer, subsequently silk screen printing one deck Al
2o
3nanometer crystal layer, 450 ℃ heating 30 minutes after, obtaining thickness is the compacted zone 12 of 50nm and the porous support layer 13 that thickness is 500nm.Subsequently, adopt two step liquid phase methods to deposit CH in porous support layer 13
3nH
3pbI
3light absorbent.First by the PbI of 1.2M
2dMF solution under the rotating speed of 3000rpm, be spin-coated on porous support layer 13 surface, after continuing spin coating 30s, at 90 ℃, heat 2 minutes, with being about to the CH that porous support layer 13 is 10mg/mL in concentration
3nH
3in the aqueous isopropanol of I, soak 10 minutes, finally at the temperature of 90 ℃, heat 45 minutes.Like this, a part of CH
3nH
3pbI
3light absorbent is filled in the internal void of porous support layer 13, another part CH
3nH
3pbI
3light absorbent forms the cap layer 14 that a layer thickness is 100nm on porous support layer.
The hole transmission layer 15 that the material that utilizes spin-coating method to be 100nm in porous support layer 13 surface formation a layer thickness is spiro-OMeTAD.
Preparation process to electrode slurry is as follows: take 0.7 gram of graphite (particle diameter 400nm), 0.2 gram of multi-walled carbon nano-tubes, they are added among 10 milliliters of ethyl acetate solutions containing 0.7 gram of butadiene-styrene rubber and 0.2 gram of ethyl cellulose, under the rotating speed of 200r/min, ball milling is 4 hours, can obtain electrode slurry.
Prepare after electrode slurry, used the method for silk screen printing to be printed on the hole transmission layer 15 having prepared, its standing levelling, after 5 minutes, is placed in to the dry taking-up after 10 minutes of 80 degrees Celsius of baking ovens, make electrode layer 16.
The aluminium foil of suitable dimension is pressed on electrode layer 16, makes extraction electrode 17, completed the making of whole battery.The photoelectric conversion efficiency of this battery final test is 10.6%, and current density is 19.01mA/cm
2, open circuit voltage is 911.6mV.
Embodiment 3:
Perovskite-based thin-film solar cell structure in the present embodiment as shown in Figure 1.
First at FTO silk screen printing one deck on glass TiO
2thin layer, subsequently silk screen printing one deck Al
2o
3nanometer crystal layer, 450 ℃ heating 30 minutes after, obtaining thickness is the compacted zone 12 of 50nm and the porous support layer 13 that thickness is 500nm.Subsequently, adopt two step liquid phase methods to deposit CH in porous support layer 13
3nH
3pbI
3light absorbent.First by the PbI of 1.2M
2dMF solution under the rotating speed of 3000rpm, be spin-coated on porous support layer 13 surface, continue spin coating 30
safterwards, at 90 ℃, heat 2 minutes, with being about to the CH that porous support layer 13 is 10mg/mL in concentration
3nH
3in the aqueous isopropanol of I, soak 10 minutes, finally at the temperature of 90 ℃, heat 45 minutes.Like this, a part of CH
3nH
3pbI
3light absorbent is filled in the internal void of porous support layer 13, another part CH
3nH
3pbI
3light absorbent forms the cap layer 14 that a layer thickness is 100nm on porous support layer.
Preparation process to electrode slurry is as follows: 0.6 gram of graphite (1～3 micron of particle diameter) and 0.3 gram of Graphene are added among 10 milliliters of ethyl acetate solutions containing 0.25 gram of butadiene-styrene rubber and 0.25 gram of ethyl cellulose, under the rotating speed of 200r/min, ball milling is 4 hours, can obtain electrode slurry.
Prepare after electrode slurry, it is printed on by silk screen print method on the porous support layer 13 of populated light absorbent, its standing levelling, after 5 minutes, is placed in to the dry taking-up after 10 minutes of 80 ℃ of baking ovens, make electrode layer 16.
The graphite paper of suitable dimension is pressed on electrode layer 16, makes extraction electrode 17, completed the making of whole battery.The photoelectric conversion efficiency of this battery final test is 9.8%, and current density is 18.32mA/cm
2, open circuit voltage is 951.2mV.
Embodiment 4:
Perovskite-based thin-film solar cell structure in the present embodiment as shown in Figure 1.
First at FTO silk screen printing one deck on glass TiO
2thin layer, subsequently silk screen printing one deck Al
2o
3nanometer crystal layer, 450 ℃ heating 30 minutes after, obtaining thickness is the compacted zone 12 of 50nm and the porous support layer 13 that thickness is 500nm.Subsequently, adopt two step liquid phase methods to deposit CH in porous support layer 13
3nH
3pbI
3light absorbent.First by the PbI of 1.8M
2dMF solution under the rotating speed of 5000rpm, be spin-coated on porous support layer 13 surface, after continuing spin coating 30s, at 90 ℃, heat 2 minutes, with being about to the CH that porous support layer 13 is 10mg/mL in concentration
3nH
3in the aqueous isopropanol of I, soak 30 minutes, finally at the temperature of 90 ℃, heat 45 minutes.Like this, a part of CH
3nH
3pbI
3light absorbent is filled in the internal void of porous support layer 13, another part CH
3nH
3pbI
3light absorbent forms the cap layer 14 that a layer thickness is 80nm on porous support layer.
Preparation process to electrode slurry is as follows: 0.75 gram of graphite (particle diameter 500 nanometers) and 0.2 gram of carbon fiber are added among 10 milliliters of ethyl acetate solutions containing 0.25 gram of butadiene-styrene rubber and 0.25 gram of ethyl cellulose, under the rotating speed of 200r/min, ball milling is 4 hours, can obtain electrode slurry.
Prepare after electrode slurry, it is printed on by silk screen print method on the porous support layer 13 of populated light absorbent, its standing levelling, after 5 minutes, is placed in to the dry taking-up after 10 minutes of 80 ℃ of baking ovens, make electrode layer 16.
The graphite paper of suitable dimension is pressed on electrode layer 16, makes extraction electrode 17, completed the making of whole battery.The photoelectric conversion efficiency of this battery final test is 10.2%, and current density is 19.02mA/cm
2, open circuit voltage is 930.7mV.
Embodiment 5:
Perovskite-based thin-film solar cell structure in the present embodiment as shown in Figure 3.
First at FTO silk screen printing one deck on glass TiO
2thin layer, subsequently silk screen printing one deck Al
2o
3nanometer crystal layer, 450 ℃ heating 30 minutes after, obtaining thickness is the compacted zone 12 of 50nm and the porous support layer 13 that thickness is 500nm.Subsequently, adopt two step liquid phase methods to deposit CH in porous support layer 13
3nH
3pbI
3light absorbent.First by the PbI of 1.8M
2dMF solution under the rotating speed of 5000rpm, be spin-coated on porous support layer 13 surface, continue spin coating 30
safterwards, at 90 ℃, heat 2 minutes, with being about to the CH that porous support layer 13 is 10mg/mL in concentration
3nH
3in the aqueous isopropanol of I, soak 10 minutes, finally at the temperature of 90 ℃, heat 45 minutes.Like this, a part of CH
3nH
3pbI
3light absorbent is filled in the internal void of porous support layer 13, another part CH
3nH
3pbI
3light absorbent forms the cap layer 14 that a layer thickness is 80nm on porous support layer.
The hole transmission layer 15 that the material that utilizes spin-coating method to be 100nm in porous support layer 13 surface formation a layer thickness is spiro-OMeTAD.
Preparation process to electrode slurry is as follows: take 0.75 gram of graphite (particle diameter 400nm), 0.2 gram of multi-walled carbon nano-tubes, they are added among 10 milliliters of ethyl acetate solutions containing 0.25 gram of butadiene-styrene rubber and 0.25 gram of ethyl cellulose, under the rotating speed of 200r/min, ball milling is 4 hours, can obtain electrode slurry.
Prepare after electrode slurry, used the method for silk screen printing to be printed on the hole transmission layer 15 having prepared, its standing levelling, after 5 minutes, is placed in to the dry taking-up after 10 minutes of 80 degrees Celsius of baking ovens, make electrode layer 16.
The aluminium foil of suitable dimension is pressed on electrode layer 16, makes extraction electrode 17, completed the making of whole battery.The photoelectric conversion efficiency of this battery final test is 12.1%, and current density is 19.01mA/cm
2, open circuit voltage is 955.3mV.
Embodiment 6:
Perovskite-based thin-film solar cell structure in the present embodiment as shown in Figure 3.
First at FTO silk screen printing layer of ZnO on glass thin layer, subsequently silk screen printing one deck Al
2o
3nanometer crystal layer, 450 ℃ heating 30 minutes after, obtaining thickness is the compacted zone 12 of 40nm and the porous support layer 13 that thickness is 500nm.Subsequently, adopt two step liquid phase methods to deposit CH in porous support layer 13
3nH
3pbI
3light absorbent.First by the PbI of 1.8M
2dMF solution under the rotating speed of 5000rpm, be spin-coated on porous support layer 13 surface, after continuing spin coating 30s, at 90 ℃, heat 2 minutes, with being about to the CH that porous support layer 13 is 10mg/mL in concentration
3nH
3in the aqueous isopropanol of I, soak 10 minutes, finally at the temperature of 90 ℃, heat 45 minutes.Like this, a part of CH
3nH
3pbI
3light absorbent is filled in the internal void of porous support layer 13, another part CH
3nH
3pbI
3light absorbent forms the cap layer 14 that a layer thickness is 80nm on porous support layer.
The hole transmission layer 15 that the material that utilizes spin-coating method to be 100nm in porous support layer 13 surface formation a layer thickness is spiro-OMeTAD.
Preparation process to electrode slurry is as follows: take 0.75 gram of graphite (particle diameter 400nm), 0.2 gram of acetylene black, they are added among 10 milliliters of ethyl acetate solutions containing 0.25 gram of butadiene-styrene rubber and 0.25 gram of ethyl cellulose, under the rotating speed of 200r/min, ball milling is 4 hours, can obtain electrode slurry.
Prepare after electrode slurry, used the method for silk screen printing to be printed on the hole transmission layer 15 having prepared, its standing levelling, after 5 minutes, is placed in to the dry taking-up after 10 minutes of 80 degrees Celsius of baking ovens, make electrode layer 16.
The aluminium foil of suitable dimension is pressed on electrode layer 16, makes extraction electrode 17, completed the making of whole battery.The photoelectric conversion efficiency of this battery final test is 12.3%, and current density is 19.12mA/cm
2, open circuit voltage is 943.2mV.
Comparative example 1:
First at FTO silk screen printing one deck on glass TiO
2thin layer, subsequently silk screen printing one deck Al
2o
3nanometer crystal layer, then silk screen printing one deck carbon is to electrode, then after 450 ℃ of heating 30 minutes, obtains porous that compacted zone that thickness is 50nm, porous support layer that thickness is 500nm and thickness is 6 μ m to electrode layer.Subsequently, adopt two step liquid phase methods to deposit CH in porous support layer
3nH
3pbI
3light absorbent.First by the PbI of 1.2M
2dMF solution under the rotating speed of 3000rpm, be spin-coated on electrode layer surface, after continuing spin coating 30s, at 90 ℃, heat 2 minutes, with being about to the CH that porous support layer is 10mg/mL in concentration
3nH
3in the aqueous isopropanol of I, soak 10 minutes, finally at the temperature of 90 ℃, heat 45 minutes.The filtter gold of suitable dimension is pressed on electrode layer, makes extraction electrode, completed the making of whole battery.The photoelectric conversion efficiency of this battery final test is 5.2%, and current density is 12.9mA/cm
2, open circuit voltage is 805.4mV.
Comparative example 2:
First at FTO silk screen printing one deck on glass TiO
2thin layer, subsequently silk screen printing one deck Al
2o
3nanometer crystal layer, one deck SiO
2film and one deck carbon is to electrode, then after 450 ℃ of heating 30 minutes, obtain compacted zone that thickness is 50nm, porous support layer that thickness is 500nm, porous dielectric layer that thickness is 500nm and thickness and be 6 μ m to electrode layer.Subsequently, adopt two step liquid phase methods to deposit CH in porous support layer
3nH
3pbI
3light absorbent.First by the PbI of 1.2M
2dMF solution under the rotating speed of 3000rpm, be spin-coated on electrode layer surface, after continuing spin coating 30s, at 90 ℃, heat 2 minutes, with being about to the CH that porous support layer is 10mg/mL in concentration
3nH
3in the aqueous isopropanol of I, soak 10 minutes, finally at the temperature of 90 ℃, heat 45 minutes.
The filtter gold of suitable dimension is pressed on electrode layer, makes extraction electrode, completed the making of whole battery.The photoelectric conversion efficiency of this battery final test is 5.6%, and current density is 12.23mA/cm
2, open circuit voltage is 820.5mV.
Comparative example 3:
First at FTO silk screen printing one deck on glass TiO
2thin layer, subsequently silk screen printing one deck Al
2o
3nanometer crystal layer, after 450 ℃ of heating 30 minutes, obtains the porous support layer that compacted zone that thickness is 50nm and thickness are 500nm.Subsequently, adopt two step liquid phase methods to deposit CH in porous support layer
3nH
3pbI
3light absorbent.First by the PbI of 1.2M
2dMF solution under the rotating speed of 3000rpm, be spin-coated on porous support layer surface, after continuing spin coating 30s, at 90 ℃, heat 2 minutes, with being about to the CH that porous support layer is 10mg/mL in concentration
3nH
3in the aqueous isopropanol of I, soak 10 minutes, finally at the temperature of 90 ℃, heat 45 minutes.Like this, a part of CH
3nH
3pbI
3light absorbent is filled in the internal void of porous support layer 13, another part CH
3nH
3pbI
3light absorbent forms the cap layer 14 that a layer thickness is 100nm on porous support layer.
The gold copper-base alloy that evaporation a layer thickness is 100nm on porous support layer to electrode layer.
The filtter gold of suitable dimension is pressed on electrode layer, makes extraction electrode, completed the making of whole battery.The photoelectric conversion efficiency of this battery final test is 8.0%, and current density is 18.12mA/cm
2, open circuit voltage is 903.7mV.
Comparative example 4:
First at FTO silk screen printing one deck on glass TiO
2thin layer, subsequently silk screen printing one deck Al
2o
3nanometer crystal layer, after 450 ℃ of heating 30 minutes, obtains the porous support layer that compacted zone that thickness is 50nm and thickness are 500nm.Subsequently, adopt two step liquid phase methods to deposit CH in porous support layer
3nH
3pbI
3light absorbent.First by the PbI of 1.2M
2dMF solution under the rotating speed of 3000rpm, be spin-coated on porous support layer surface, after continuing spin coating 30s, at 90 ℃, heat 2 minutes, with being about to the CH that porous support layer is 10mg/mL in concentration
3nH
3in the aqueous isopropanol of I, soak 10 minutes, finally at the temperature of 90 ℃, heat 45 minutes.Like this, a part of CH
3nH
3pbI
3light absorbent is filled in the internal void of porous support layer 13, another part CH
3nH
3pbI
3light absorbent forms the cap layer 14 that a layer thickness is 100nm on porous support layer.
The hole transmission layer that the material that utilizes spin-coating method to be 100nm in porous support layer surface formation a layer thickness is spiro-OMeTAD.
The gold copper-base alloy that evaporation a layer thickness is 100nm on hole transmission layer to electrode layer.
The filtter gold of suitable dimension is pressed on electrode layer, makes extraction electrode, completed the making of whole battery.The photoelectric conversion efficiency of this battery final test is 11.2%, and current density is 18.51mA/cm
2, open circuit voltage is 922.7mV.
In above-described embodiment 1-6, to electrode layer in the process of preparation all without high temperature sintering, it will be understood by those skilled in the art that final what form is not porous form to electrode layer for it.
From embodiment 1-6, can find out, of the present invention higher to the photoelectric current of the perovskite-based thin film solar cell of electrode and photoelectric conversion efficiency based on carbon.From embodiment 1-2 and comparative example 1-2, can find out, the present invention adopts material with carbon element as to electrode material, the perovskite-based thin film solar cell to electrode based on carbon that the battery of preparing so all will obviously be better than adopting the method for prior art to be prepared in each performance parameters such as photoelectric current, electricity conversion.From embodiment 1-2 and comparative example 3-4, can find out, the present invention adopts material with carbon element as to electrode material, its photoelectric conversion efficiency is more or less the same as the perovskite-based thin film solar cell performance to electrode material with adopting precious metal material, but preparation cost of the present invention well below the noble metal of preparing by the method for evaporation to electrode.
So far, those skilled in the art will recognize that, although detailed, illustrate and described a plurality of exemplary embodiment of the present invention herein, but, without departing from the spirit and scope of the present invention, still can directly determine or derive many other modification or the modification that meets the principle of the invention according to content disclosed by the invention.Therefore, scope of the present invention should be understood and regard as and cover all these other modification or modifications.
Claims (11)
1. a perovskite-based thin film solar cell, comprising:
Transparent substrates;
The transparency conducting layer forming in described transparent substrates;
That on described transparency conducting layer, form and be the compacted zone of semi-conducting material;
That on described compacted zone, form and be the porous support layer of insulating material, in the hole of described porous support layer inside, be filled with the organic metal semiconductor light absorbent of perovskite structure; And
That on described porous support layer, form and for conductive carbon material to electrode layer.
2. perovskite-based thin film solar cell according to claim 1, is characterized in that, described electrode layer is formed on the described porous support layer of filling described organic metal semiconductor light absorbent.
3. perovskite-based thin film solar cell according to claim 1 and 2, is characterized in that, described in electrode layer without the existence of obvious described organic metal semiconductor light absorbent.
4. according to the perovskite-based thin film solar cell described in any one in claim 1-3, it is characterized in that, described is non-porous form to electrode layer.
5. according to the perovskite-based thin film solar cell described in any one in claim 1-4, it is characterized in that, also comprise cap layer, be formed on described porous support layer and described between electrode layer;
Described cap layer is formed by described organic metal semiconductor light absorbent.
6. perovskite-based thin film solar cell according to claim 5, is characterized in that, also comprises hole transmission layer, is formed on described cap layer and described between electrode layer; And/or
Extraction electrode, is formed on described on electrode layer.
7. a method of preparing perovskite-based thin film solar cell, comprising:
Provide surface to there is the transparent substrates of transparency conducting layer;
On described transparency conducting layer, form the compacted zone of semi-conducting material;
On described compacted zone, form the porous support layer of insulating material;
The organic metal semiconductor light absorbent with perovskite structure is filled in the hole of described porous support layer inside; And
Filled on the described porous support layer of described organic metal semiconductor light absorbent, form conductive carbon material to electrode layer.
8. method according to claim 7, is characterized in that, the surface deposition at described porous support layer in the process in the hole that described organic metal semiconductor light absorbent is filled into described porous support layer inside forms a cap layer; Described electrode layer is formed in described cap layer.
9. method according to claim 8, is characterized in that, is also included in described cap layer and forms hole transmission layer, described electrode layer is formed on described hole transmission layer; And/or
Described, form extraction electrode on to electrode layer.
10. according to the method described in any one in claim 7-9, it is characterized in that,
Described conductive carbon material and binding agent are added and in dispersant, form homodispersely to electrode slurry, by described, electrode slurry is coated on described porous support layer, drying forms described to electrode layer,
Wherein, described dispersant is non-polar organic solvent, and alternatively, described non-polar organic solvent is selected from one or more in benzene, toluene, chlorobenzene, carbon tetrachloride, ethyl acetate, benzinum, senior aliphatic hydrocarbon, higher alcohols; Described binding agent is for being dissolved in the macromolecular material of described dispersant.
11. methods according to claim 10, is characterized in that,
Employing be selected from paddling process, ultrasonic method, polishing, ball-milling method one or more by described conductive carbon material and binding agent be dispersed in described dispersant, form described to electrode slurry; And/or
Employing is selected from a kind of in knife coating, spraying process, silk screen print method, squeezing and coating method and by described, electrode slurry is coated on described porous support layer.
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