CN107146847B - It is a kind of novel based on all solid state printable perovskite solar battery of carbon electrode - Google Patents
It is a kind of novel based on all solid state printable perovskite solar battery of carbon electrode Download PDFInfo
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- H—ELECTRICITY
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- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/30—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising bulk heterojunctions, e.g. interpenetrating networks of donor and acceptor material domains
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- H—ELECTRICITY
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
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- H—ELECTRICITY
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- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/60—Forming conductive regions or layers, e.g. electrodes
- H10K71/611—Forming conductive regions or layers, e.g. electrodes using printing deposition, e.g. ink jet printing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
It is novel based on all solid state printable perovskite solar battery of carbon electrode and preparation method thereof that the invention discloses one kind, i.e., prints TiO using screen printing technique2Working electrode, insulating layer, porous carbon are to electrode and cryogenic carbon to electrode, and wherein porous carbon is 400 DEG C of sintered porous carbon-coatings to electrode, and cryogenic carbon is the fine and close carbon-coating of 150 DEG C or less sintering to electrode.The structure generation process is simple, lower cost for material, by reducing carbon to the series resistance of the square resistance reduction solar cell device of electrode, and can greatly reduce the loading of perovskite solution.The structure is a kind of novel solar battery structure that is environmentally friendly, having grow a lot potentiality and market prospects.
Description
Technical field
The invention belongs to perovskite area of solar cell, more particularly, to a kind of novel all solid state based on carbon electrode
Printable perovskite solar battery and preparation method thereof.
Background technique
In recent years, perovskite solar battery studied the fashionable whole world, at present the highest battery efficiency through certifying authority
22% is broken through, which is more than the efficiency of conventional films solar battery.Compared with other types of solar battery, this
Class battery has many advantages, such as that material source is convenient, manufacture craft is simple, equipment requirement is not high and battery is at low cost.These advantages
Illustrate that perovskite solar battery has the development potentiality for replacing high cost polycrystalline silicon and monocrystaline silicon solar cell.
However use noble metal (gold or platinum) as the perovskite solar battery to electrode, because of the cost of precious metal material
It is higher, and the technique of the high energy consumptions such as vacuum evaporation is needed to prepare to electrode, while needing to pass using expensive hole
The disadvantages of defeated layer, so that perovskite solar battery cost is significantly increased.Therefore, seek cheap alternatively to electrode preparation work
Skill is also the hot spot of perovskite area of solar cell research.
Carbon not only has structure diversity, chemical stability and surface chemistry abundant etc. special as electrode material
Point, and carbon material rich content, cheap in the earth's crust, while carbon is similar to the fermi level of gold, is to replace noble metal
Electrode preferably selects.2013, Korea Spro's magnificence seminar, the Central China University of Science and Technology was prepared for a kind of all print for the first time and is based on carbon electrode
Without the mesoporous perovskite solar battery of hole transmission layer, 12.8% authentication efficiency is achieved and more than 1000h performance without obvious
The high stability of decaying, attracts extensive attention in the world, has huge applications prospect (Science, 2014,345,6194).
Carbon electrode is generally electrically conducting transparent substrate/electron-transport without hole transmission layer perovskite solar cell device structure
Layer/insulating layer/calcium titanium ore bed/carbon electrode, wherein back electrode of the carbon electrode as battery, is not only the important composition portion of battery
Point, also have the function of hole transport and constitutes electronic loop.Therefore, the performance of carbon electrode can greatly affect the property of battery
Energy.
It investigates carbon electrode and is mainly manifested in two without the carbon electrode performance quality of hole transmission layer perovskite solar battery
Aspect, first is that the thickness of carbon electrode layer, second is that the square resistance of carbon electrode layer.Firstly, before the thickness of carbon electrode layer is to perovskite
The filling for driving liquid has an impact, and too thick carbon electrode layer causes the filling of perovskite precursor liquid uneven, therefore, ideal carbon electrode
Thickness degree is preferably thin；But the square resistance of carbon electrode layer is also directly related with thickness, for determining carbon electrode layer material,
The square resistance of carbon electrode layer is reduced with the increase of the thickness of carbon electrode layer.As it can be seen that the thickness of carbon electrode layer and face electricity
Resistance is a pair of contradictory body, to obtain excellent carbon electrode performance, just must thickness to carbon electrode layer and surface resistance close
Reason optimization.The thickness and surface resistance that are effectively reduced carbon electrode are the prior development directions of this kind of solar battery.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the present invention provides a kind of compound carbon-coating structural carbons to electrode
Perovskite solar battery and preparation method thereof, its object is to by combining the excellent of porous carbon layer and the double carbon-coatings of low temperature carbon-coating
Point, thin porous carbon layer guarantee the loading for also greatly reducing perovskite precursor liquid while perovskite solution fills uniform, warp
It crosses after solution annealing and prints the biggish low temperature carbon-coating of a layer thickness on porous carbon layer again to reduce entire carbon to the side of electrode
Block resistance in this way on the basis of guaranteeing electrode performance, can also be greatly reduced to ring with meeting the lateral transport demand in hole
Border has the perovskite loading of potential threat, thus solves the carbon of the carbon electrode of perovskite solar battery in the prior art
Contradiction between thickness degree and surface resistance to obtain preferable electrode performance, and solves to lead when filling a large amount of perovskite precursor liquids
The technical issues of environmental pollution is serious when causing to industrialize.
To achieve the above object, according to one aspect of the present invention, a kind of carbon is provided to electrode perovskite solar-electricity
Pond, the perovskite solar battery include electrically conducting transparent substrate, light anode, insulating layer, the first carbon-coating and second from bottom to top
Carbon-coating, first carbon-coating are porous carbon layer, and second carbon-coating is low temperature carbon-coating, and the low temperature carbon-coating is that carbon pastes are being lower than
Carbon-coating made of being fired under the conditions of 150 DEG C.
Preferably, first carbon-coating with a thickness of 1-15 μm.
Preferably, first carbon-coating with a thickness of 1-4 μm.
Preferably, the thickness of second carbon-coating is not less than 10 μm.
Preferably, second carbon-coating with a thickness of 20 μm or more.
Preferably, the electrically conducting transparent substrate is FTO or ITO；The light anode includes TiO2Compacted zone and TiO2It is mesoporous
Layer；The insulating layer is ZrO2Layer.
Preferably, the perovskite solar battery further includes being distributed in the electrically conducting transparent substrate, light anode, insulating layer
With the perovskite in each layer hole of pyrocarbon layer, the perovskite after the annealed processing of perovskite precursor liquid by obtaining.
Preferably, the perovskite precursor liquid is the organic metal halide with perovskite crystal form, chemical molecular formula
It is expressed as ABX3, wherein A is organic group, and B is metal cation, and X is halide anion.
Other side according to the invention, provides a kind of carbon to the preparation method of electrode perovskite solar battery,
Include the following steps:
(1) one layer of compacted zone is prepared in electrically conducting transparent substrate；
(2) one layer of TiO is sequentially prepared by silk-screen printing on step (1) described compacted zone2Mesoporous layer and one layer of ZrO2Absolutely
Edge layer；
(3) the first carbon-coating is prepared on step (2) described insulating layer；
(4) perovskite precursor liquid is dropped into step (3) first carbon-coating surface；
(5) the second carbon-coating is prepared on first carbon-coating.
Preferably, the preparation method of step (3) first carbon-coating includes the following steps: high temperature carbon pastes passing through silk screen
Press printing is on the insulating layer, and then sintering obtains first carbon-coating at 300-400 DEG C.
Preferably, the mesh number size for printing the web plate of the high temperature carbon pastes is -500 mesh of 150 mesh.
Preferably, the high temperature carbon pastes the preparation method comprises the following steps: graphite, carbon black and organic polymer pore-creating binder are mixed
After conjunction, solvent is added, ball milling obtains the high temperature carbon pastes.
Preferably, the granular size of graphite is 200nm-30 μm in the high temperature carbon pastes.
Preferably, the preparation method of the high temperature carbon pastes includes the following steps:
S1 mixes carbon black, graphite, organic polymer pore-creating binder according to mass ratio 10-0:0-10:5-1, is mixed
Close carbon material；Then solvent is added, wherein the quality of solvent accounts for the 20%-50% of mixing carbon material quality；
Dehydrated alcohol is added in S2, until dissolving the mixing carbon material and the solvent；
S3 uses speed per hour for the ball mill ball milling 8-24h of 200-350r/h in the ball mill；
S4 obtains the high temperature carbon pastes using Rotary Evaporators revolving removal ethyl alcohol.
Preferably, step (4) specifically comprises the following steps: that the perovskite precursor liquid that will be prepared drops to institute by drop-coating
The first carbon-coating edge is stated, makes its filling into each layer porous film layer；Then annealing 5min-2h is carried out at 150 DEG C or less.
Preferably, in the perovskite precursor liquid filling work procedure, device to be filled is placed on burnishing surface, and from institute
It states the first carbon-coating edge and instills perovskite precursor liquid, stand after filling keeps the perovskite precursor liquid uniform for a period of time
It is sufficient filling with, preferably time of repose is 10min to 1h.
Preferably, the loading of step (4) the perovskite precursor liquid is 2-4.5 μ L.
Preferably, step (5) specifically comprises the following steps: low temperature carbon pastes through screen printer print described the
On one carbon-coating；Then in 150 DEG C or less sintering 10min-4h, temperature is preferably 50-150 DEG C, and sintering time is preferably 1-2h.
Preferably, the granular size of graphite is 6-30 μm in the low temperature carbon pastes.
Preferably, the preparation method of the low temperature carbon pastes includes the following steps:
S1 mixes carbon black and graphite according to mass ratio 10:0-0:10, and ball milling obtains uniformly mixed carbon black and graphite
Mixture；
By in the mixture of the obtained carbon black and graphite of appropriate solvent addition S1, ball milling obtains being coated with described S2
The mixture of the carbon black of solvent and the mixture of graphite, the carbon black and graphite and the solvent quality ratio are 1:1-10；
Binder and compound containing-COOH are 10:1-1:10 with mass ratio by S3, are added to the surface packet that S2 is obtained
Be wrapped in the carbon black of the solvent and the mixture of graphite, the low temperature carbon pastes can be obtained in ball milling, wherein binder and containing-
The gross mass and carbon black of the compound of COOH and the total mass ratio of graphite are 10:1-1:10.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, can obtain down and show
Beneficial effect.
(1) porous carbon layer (the first carbon-coating) thickness only has 2-3 μm in the perovskite solar battery structure that the present invention designs,
Far below common carbon-coating (thickness is at 10 μm or more), the loading of perovskite precursor liquid can be effectively reduced, from 5 previous μ L
It is even lower to be reduced to 3 μ L.Because may reduce loading containing harmful substances such as lead in perovskite precursor liquid and not only may be used
To reduce cost, pollution on the environment in industrialized production in future can also be reduced.
(2) low temperature carbon-coating greatly compensates for porous carbon layer (the in the perovskite solar battery structure that designs of the present invention
One carbon-coating) thickness is small, sheet resistance is big disadvantage.First carbon-coating as just hole longitudinal transmission medium, so sheet resistance is to its shadow
Very little is rung, and the low temperature carbon layers having thicknesses painted later can reach mm rank, sheet resistance is theoretically smaller than 1 Ω, is very advantageous in
The lateral transport in hole.So the carbon of this double-layer structure can ignore the sheet resistance of pyrocarbon layer, the side of overall performance to electrode
Resistance is theoretically smaller than 1 Ω.
(3) the low temperature carbon layers having thicknesses in the perovskite solar battery structure that designs of the present invention are big and fine and close, it is by first
Carbon-coating is completely covered, and the perovskite of filling can be isolated from the outside and play the role of encapsulation, effectively reduce Environmental Water
Decomposition caused by it improves the stability of this new structural carbon-based perovskite solar battery.
(4) perovskite solar battery structure simple production process of the invention, lower cost for material, by reducing carbon pair
The square resistance of electrode and then the series resistance for reducing solar cell device, and the filling of perovskite solution can be greatly reduced
Amount.The structure is a kind of novel solar battery structure that is environmentally friendly, having grow a lot potentiality and market prospects.
Detailed description of the invention
Fig. 1 is structural schematic diagram of the carbon to electrode perovskite solar battery of the embodiment of the present invention 1.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
As shown in Figure 1, a kind of carbon printable perovskite solar battery all solid state to electrode provided by the invention, passes through silk
Net printing technology is made, and to electrode and is filled in each thin including electrically conducting transparent substrate, light anode, insulating layer, carbon from bottom to top
The perovskite of film layer.Wherein electrically conducting transparent substrate is FTO or ITO；Light anode includes TiO2Compacted zone and TiO2Mesoporous layer；Absolutely
Edge layer is ZrO2Layer.Carbon includes the double-layer structure being made of the first carbon-coating and the second carbon-coating to electrode.First carbon-coating be it is a kind of very
The carbon-coating of thin porous structure is conducive to the longitudinal transmission for filling perovskite solution and hole；First carbon-coating with a thickness of 1-
15 μm, preferably 1-4 μm.Second carbon-coating is low temperature carbon-coating, and low temperature carbon layers having thicknesses are big, plays the role of hole lateral transport,
Electric conductivity is strong, low temperature carbon-coating with a thickness of 10 μm to mm rank, preferably 20 μm or more.
Printable perovskite solar battery all solid state to electrode for carbon of the invention, as long as the first carbon-coating is porous carbon
Layer, as one of the implementation modes, the first carbon-coating can be pyrocarbon layer, be that high temperature carbon pastes are burnt at 400 DEG C
Tie obtained porous carbon layer.High temperature carbon pastes are carbon material, solvent is prepared after mixing with organic polymer pore-creating binder
Carbon pastes, due to use organic polymer pore-creating binder, the carbon pastes being prepared for fire carbon electrode when, need
It is carried out at 300-400 DEG C of high temperature, therefore, is called pyrocarbon layer.Since the carbon pastes joined pore-creating in preparation process
Binder, therefore will form porous carbon layer structure in its high temperature sintering procedure.
As one of the implementation modes, the preparation method of high temperature carbon pastes of the invention can be with are as follows: by carbon black, graphite
It is mixed with organic polymer pore-creating binder (such as ethyl cellulose), solvent (such as terpinol) then is added, adds suitable
The ethyl alcohol of amount, mix after ball milling obtain high temperature carbon pastes, the high temperature carbon pastes fired at 300-400 DEG C of high temperature obtain it is porous
Carbon-coating.
Second carbon-coating namely low temperature carbon-coating, to be sintered obtained densification or porous carbon layer at 150 DEG C or less.As wherein
A kind of implementation, the preparation method of low temperature carbon-coating of the invention can be with are as follows: after mixing carbon black, graphite with solvent, adds
Enter inorganic or organic binder, the compound ball milling containing carboxyl or hydroxyl obtains low temperature carbon pastes, which can be low
Carbon electrode layer is fired at 150 DEG C.
Perovskite precursor liquid is the organic metal halide with perovskite crystal form, and molecular formula is represented by ABX3,
Middle A is organic group (such as methylamino), and B is metal cation (such as lead ion), and X is generally halide anion (such as chlorine, bromine, iodine
Ion).
Carbon of the invention includes the following steps: the preparation method of electrode perovskite solar battery
(1) one layer of compacted zone is prepared in electrically conducting transparent substrate；
(2) one layer of TiO is sequentially prepared by silk-screen printing on step (1) described compacted zone2Mesoporous layer and one layer of ZrO2Absolutely
Edge layer；
(3) porous first carbon-coating is prepared on step (2) described insulating layer；
(4) perovskite precursor liquid is dropped into step (3) first carbon-coating surface, make its filling to the compacted zone,
TiO2Mesoporous layer, ZrO2In the porous film layer of insulating layer and each layer of the first carbon-coating；
(5) the second carbon-coating is prepared on the pyrocarbon layer.
Wherein, step (3) can carry out in accordance with the following steps: by high temperature carbon pastes by screen printer print described
On insulating layer, it is then sintered 40min at 400 DEG C and obtains first carbon-coating.Print the mesh number of the web plate of the pyrocarbon layer
Size is -500 mesh of 150 mesh.The granular size of graphite is 200nm-30 μm in high temperature carbon pastes.
As one of implementation, the preparation method of high temperature carbon pastes of the invention includes the following steps:
S1 mixes carbon black, graphite, organic polymer pore-creating binder according to mass ratio 10-0:0-10:5-1, is mixed
Close carbon material；Then solvent is added, wherein the quality of solvent accounts for the 20%-50% of mixing carbon material quality；Wherein carbon black and stone
Ink can only select it is one such, can also both select simultaneously.
S2 weighs the dehydrated alcohol of suitable volumes, dissolves all of above material；
S3 uses speed per hour for the ball mill ball milling 8-24h of 200-350r/h in the ball mill；
S4 obtains the high temperature carbon pastes using Rotary Evaporators revolving removal ethyl alcohol.
Perovskite precursor liquid is dropped to step (3) first carbon-coating surface by step (4), makes its filling to the densification
Layer, TiO2Mesoporous layer, ZrO2In the porous film layer of insulating layer and each layer of the first carbon-coating, specifically comprise the following steps: by
The perovskite precursor liquid prepared drops to first carbon-coating edge by drop-coating, makes its filling to each layer porous film layer
In；Then annealing 5min-2h is carried out at 150 DEG C or less.In perovskite precursor liquid filling work procedure, by device to be filled
It is placed on burnishing surface, and instills perovskite precursor liquid from the first carbon-coating edge, stand after filling makes the calcium titanium for a period of time
Mine precursor liquid can be uniformly sufficient filling with, and preferably time of repose is 10min to 1h.Step (4) the perovskite precursor liquid is filled out
Charge is 2-4.5 μ L.
Step (5) prepares the second carbon-coating and specifically comprises the following steps: the low temperature carbon pastes of preparation passing through screen process press
It is printed on pyrocarbon layer；Then in 150 DEG C or less sintering 10min-4h, temperature is preferably 50-150 DEG C, and sintering time is preferred
For 1-2h.The granular size of graphite is 6-30 μm in low temperature carbon pastes.
As one of the implementation modes, the preparation method of low temperature carbon pastes of the invention includes the following steps:
S1 mixes carbon black and graphite according to mass ratio 10:0-0:10, and ball milling obtains uniformly mixed carbon black and graphite
Mixture；Wherein carbon black and graphite can be selected only one such, can also both select simultaneously.
By in the mixture of the obtained carbon black and graphite of appropriate solvent addition S1, ball milling obtains being coated with described S2
The mixture of the carbon black of solvent and the mixture of graphite, the carbon black and graphite and the solvent quality ratio are 1:1-10.
Binder and compound containing-COOH are 10:1-1:10 with mass ratio by S3, are added to the surface packet that S2 is obtained
Be wrapped in the carbon black of the solvent and the mixture of graphite, the low temperature carbon pastes can be obtained in ball milling, wherein binder and containing-
The gross mass and carbon black of the compound of COOH and the total mass ratio of graphite are 10:1-1:10.
Add novel additive package in above-mentioned carbon pastes preparation process, including organic or inorganic binder with containing-
The compound of COOH or-OH, under solvent such as terpinol existence condition, binder, the compound containing-COOH or-OH with
Solvent synergistic effect, the carbon pastes being prepared are low temperature carbon pastes, and 70 DEG C sinterable obtain fine and close carbon-coating.
The advantages of present invention is by combining the first carbon-coating (porous carbon layer) and the second carbon-coating (low temperature carbon-coating) double carbon-coating structures,
Thin porous carbon layer guarantees the loading for also greatly reducing perovskite precursor liquid while perovskite solution fills uniform, and process is molten
One layer of very thick low temperature carbon-coating is prepared on the first carbon-coating again after liquid annealing to reduce entire carbon to the square resistance of electrode, with
Meet the lateral transport demand in hole, in this way on the basis of guaranteeing electrode performance, can also greatly reduce that there is environment and dive
In the perovskite loading of threat.
The following are embodiments:
Embodiment 1
(1) electro-conductive glass is cut into the sheet glass of certain size, such as preferred size in the present embodiment using cutting machine
Be 100mm × 100mm but it is also possible to be other sizes, using laser on sheet glass conductive layer distance wherein one side edge
At a certain distance from one insulating tape parallel with the side of etching (preferably for example apart from edge 5mm) in the present embodiment, and be left
Region etch a plurality of parallel insulating tape sheet glass be divided into multiple regions, such as the present embodiment preferably etch 4 again
Bar parallel insulation band is to be divided into five positive pole zones and negative regions for sheet glass, prevent conductive layer is from fully on,
Sheet glass after etching successively uses detergent, distilled water, dehydrated alcohol ultrasonic cleaning.For positive pole zone or negative regions
Size is especially its width, can be specifically chosen according to actual needs, such as in the present embodiment, and positive pole zone size is excellent
It is selected as 5mm × 100mm, negative regions preferred size is 19mm × 100mm, but is not limited to this in the present invention.
(2) one layer of fine and close TiO is sprayed on the negative regions surface of sheet glass at 450 DEG C2Film.
(3) in above-mentioned TiO2The TiO of one layer of certain size is printed on compacted zone2Slurry, drying, burns under the conditions of 500 DEG C
Knot.
(4) in above-mentioned TiO2The ZrO of certain size is printed on mesoporous layer2Slurry, so that ZrO2Cover all TiO2It is mesoporous
Layer is advisable, and dries.
(5) using the web plate of 400 mesh in the ZrO2Surface of insulating layer prints the high temperature that one layer of graphite particle size is 6 μm
Carbon pastes make the slurry all be covered on ZrO2On insulating layer, then sintering forms cavernous carbon to electrode.The ruler of carbon pastes
It is very little unlimited, as long as it is made only to be placed only in the ZrO2On insulating layer.Pyrocarbon layer (the first carbon-coating) thickness is about 3 μ
m。
Wherein high temperature carbon pastes the preparation method comprises the following steps: to weigh the carbon black of mass ratio 2:2:1,6 μm of graphite, organic polymer viscous
Knot agent (ethyl cellulose) mixes, and is transferred in ball mill；Weighing carbon material, (carbon black, graphite and organic polymer are viscous
Tie the gross mass of agent): terpinol mass ratio is 1:5, is added in ball mill；The dehydrated alcohol of suitable volumes is weighed to ball mill
In, all of above material is dissolved；Speed per hour be 200r/h ball mill ball milling for 24 hours；Using Rotary Evaporators buck by nothing
Water-ethanol is evaporated, and obtains high temperature carbon pastes.
(6) the monolith device for crossing printing treatment is placed on smooth desktop, by the method for drop coating at insulating layer edge
Place instills perovskite precursor liquid, and loading is 3 μ L in the present embodiment, covers standing a period of time, keeps precursor liquid uniform
It is substantially filled to the TiO2Mesoporous layer, the ZrO2After in insulating layer, the pyrocarbon layer, drying.
(7) the low temperature carbon pastes that one layer of graphite particle size is 6 μm will be printed on the device after above-mentioned drying, make the low temperature
Carbon pastes are largely covered on the pyrocarbon layer, and another part is covered in the positive pole zone of electrically conducting transparent substrate, so
Low-temperature sintering forms low temperature carbon-coating for a period of time afterwards.The size of carbon pastes is unlimited, as long as its major part is made to be covered on the height
On warm carbon-coating, another part is covered in the positive pole zone of transparent conducting glass.In the present embodiment, preferred sintering temperature
It is 50 DEG C, sintering time 2h, low temperature carbon-coating (the second carbon-coating) thickness of formation is about 20 μm.
Wherein low temperature carbon pastes the preparation method comprises the following steps: weigh carbon black: graphite quality ratio be 1:3, be transferred in ball mill, adopt
The ball mill ball milling 30min for being 200r/h with speed per hour, so that carbon black and graphite be made to be uniformly mixed, wherein graphite is 6 μm of partial sizes
Flake graphite；Weigh carbon material (gross mass of carbon black and graphite): terpinol mass ratio is 3:5, is added in ball mill, then
With identical speed per hour ball milling 1h, so that terpinol be made uniformly to be wrapped in carbon material surface；Take tetraisopropyl titanate: acetic acid quality ratio is
8:1, gross mass and carbon material mass ratio are 1:3, are added in ball mill, then with identical speed per hour ball milling 10h, obtain low temperature
Carbon pastes.
Embodiment 2
In the present embodiment, step (1), (2), (3), (4), (6) and (7) is the same as embodiment 1.
(5) using the halftone of 500 mesh in the ZrO2Surface of insulating layer prints the high temperature that one layer of graphite particle size is 2 μm
Carbon pastes make the slurry all be covered on ZrO2On insulating layer, then sintering forms cavernous carbon to electrode.The ruler of carbon pastes
It is very little unlimited, as long as it is made only to be placed only in the ZrO2On insulating layer.In the present embodiment, pyrocarbon layer thickness is about 2 μ
m。
Wherein high temperature carbon pastes the preparation method comprises the following steps: to weigh the carbon black of mass ratio 4:4:1,2 μm of graphite, organic polymer viscous
Knot agent (ethyl cellulose) mixes, and is transferred in ball mill；Weighing carbon material, (carbon black, graphite and organic polymer are viscous
Tie the gross mass of agent): terpinol mass ratio is 1:3, is added in ball mill；The dehydrated alcohol of suitable volumes is weighed to ball mill
In, all of above material is dissolved；In the ball mill ball milling 12h that speed per hour is 300r/h；Using Rotary Evaporators buck by nothing
Water-ethanol is evaporated, and obtains high temperature carbon pastes.
Embodiment 3
In the present embodiment, step (1), (2), (3), (4), (5) and (6) is the same as embodiment 1.
(7) the low temperature carbon pastes that one layer of graphite particle size is 15 μm will be printed on the device after above-mentioned drying, keep this low
Warm carbon pastes are largely covered on the pyrocarbon layer, and another part is covered in the positive pole zone of electrically conducting transparent substrate,
Then low-temperature sintering forms low temperature carbon-coating for a period of time.The size of carbon pastes is unlimited, as long as it is described to be covered on its major part
On pyrocarbon layer, another part is covered in the positive pole zone of transparent conducting glass.In the present embodiment, sintering temperature 40
DEG C, sintering time 3h, the low temperature carbon layers having thicknesses of formation are about 30 μm.
Wherein low temperature carbon pastes the preparation method comprises the following steps: weigh carbon black: graphite quality ratio be 1:10, be transferred in ball mill,
Use speed per hour for the ball mill ball milling 30min of 200r/h, so that carbon black and graphite be made to be uniformly mixed, wherein graphite is 15 μm of partial sizes
Flake graphite；Weigh carbon material (gross mass of carbon black and graphite): terpinol mass ratio is 3:8, is added in ball mill, connects
With identical speed per hour ball milling 1h, so that terpinol be made uniformly to be wrapped in carbon material surface；Take tetraisopropyl titanate: acetic acid quality ratio
For 10:1, gross mass and carbon material mass ratio are 1:8, are added in ball mill, then with identical speed per hour ball milling 10h, obtain
Low temperature carbon pastes.
Embodiment 4
In the present embodiment, step (1), (2), (3), (4), (6) and (7) is the same as embodiment 1.
(5) using the halftone of 500 mesh in the ZrO2Surface of insulating layer prints the height that one layer of graphite particle size is 400nm
Warm carbon pastes make the slurry all be covered on ZrO2On insulating layer, then sintering forms cavernous carbon to electrode.Carbon pastes
Size is unlimited, as long as it is made only to be placed only in the ZrO2On insulating layer.Pyrocarbon layer thickness is about 1 μm.
Wherein high temperature carbon pastes the preparation method comprises the following steps: weigh mass ratio 10:2:5 carbon black, 400nm graphite, organic high score
Sub- binder (ethyl cellulose) mixes, and is transferred in ball mill；Weigh carbon material (carbon black, graphite and organic high score
The gross mass of sub- binder): terpinol mass ratio is 1:5, is added in ball mill；The dehydrated alcohol of suitable volumes is weighed to ball
In grinding machine, all of above material is dissolved；Speed per hour be 200r/h ball mill ball milling for 24 hours；Use Rotary Evaporators buck
Dehydrated alcohol is evaporated, high temperature carbon pastes are obtained.
Embodiment 5
In the present embodiment, step (1), (2), (3), (4), (6) and (7) is the same as embodiment 1.
(5) using the web plate of 500 mesh in the ZrO2Surface of insulating layer prints the height that one layer of graphite particle size is 200nm
Warm carbon pastes make the slurry all be covered on ZrO2On insulating layer, then sintering forms cavernous carbon to electrode.Carbon pastes
Size is unlimited, as long as it is made only to be placed only in the ZrO2On insulating layer.Wherein pyrocarbon layer thickness is about 1 μm.
Wherein high temperature carbon pastes the preparation method comprises the following steps: weigh mass ratio 10:1:1 carbon black, 200nm graphite, organic high score
Sub- pore-creating binder (ethyl cellulose) mixes, and is transferred in ball mill；Weigh carbon material (carbon black, graphite and organic
The gross mass of high polymer binder): terpinol mass ratio is 1:2, is added in ball mill；Weigh the dehydrated alcohol of suitable volumes
Into ball mill, all of above material is dissolved；Speed per hour be 200r/h ball mill ball milling for 24 hours；Use Rotary Evaporators liter
Dehydrated alcohol is evaporated by decompression, obtains high temperature carbon pastes.
Embodiment 6
In the present embodiment, step (1), (2), (3), (4), (6) and (7) is the same as embodiment 1.
(5) web plate for using 150 mesh, in the ZrO2Surface of insulating layer prints the height that one layer of graphite particle size is 30 μm
Warm carbon pastes make the slurry all be covered on ZrO2On insulating layer, then sintering forms cavernous carbon to electrode.Carbon pastes
Size is unlimited, as long as it is made only to be placed only in the ZrO2On insulating layer.Pyrocarbon layer thickness is about 10 μm.
Wherein high temperature carbon pastes the preparation method comprises the following steps: weigh mass ratio 10:1 30 μm of graphite and organic polymer binder
(ethyl cellulose) mixes, and is transferred in ball mill；Weigh carbon material (carbon black, graphite and organic polymer binder
Gross mass): terpinol mass ratio be 1:5, be added in ball mill；The dehydrated alcohol of suitable volumes is weighed into ball mill,
All of above material is dissolved；Speed per hour be 200r/h ball mill ball milling for 24 hours；Using Rotary Evaporators buck by anhydrous second
Alcohol is evaporated, and obtains high temperature carbon pastes.
Embodiment 7
In the present embodiment, step (1), (2), (3), (4), (5) and (7) is the same as embodiment 6.
(6) the monolith device for crossing printing treatment is placed on smooth desktop, by the method for drop coating at insulating layer edge
Place instills perovskite precursor liquid, and loading is 4.5 μ L in the present embodiment, covers standing a period of time, keeps precursor liquid equal
It is even to be substantially filled to the TiO2Mesoporous layer, the ZrO2After in insulating layer, the pyrocarbon layer, drying.
Embodiment 8
In the present embodiment, step (1), (2), (3), (4), (5) and (7) is the same as embodiment 5.
(6) the monolith device for crossing printing treatment is placed on smooth desktop, by the method for drop coating at insulating layer edge
Place instills perovskite precursor liquid, and loading is 2 μ L, covers standing a period of time, precursor liquid is enable uniformly to be substantially filled to
The TiO2Mesoporous layer, the ZrO2After in insulating layer, the pyrocarbon layer, drying.
Embodiment 9
In the present embodiment, step (1), (2), (3), (4), (5) and (6) is the same as embodiment 1.
(7) the low temperature carbon pastes that one layer of graphite particle size is 30 μm will be printed on the device after above-mentioned drying, keep this low
Warm carbon pastes are largely covered on the pyrocarbon layer, and another part is covered in the positive pole zone of electrically conducting transparent substrate,
Then low-temperature sintering forms low temperature carbon-coating for a period of time.The size of carbon pastes is unlimited, as long as it is described to be covered on its major part
On pyrocarbon layer, another part is covered in the positive pole zone of transparent conducting glass.In the present embodiment, sintering temperature 70
DEG C, the low temperature carbon layers having thicknesses of sintering time 1.5h, formation are about 1mm.
Wherein low temperature carbon pastes the preparation method comprises the following steps: weigh carbon black: graphite quality ratio be 1:3, be transferred in ball mill, adopt
The ball mill ball milling 30min for being 200r/h with speed per hour, so that carbon black and graphite be made to be uniformly mixed, wherein graphite is 30 μm of partial sizes
Flake graphite；Weigh carbon material (gross mass of carbon black and graphite): terpinol mass ratio is 3:5, is added in ball mill, then
With identical speed per hour ball milling 1h, so that terpinol be made uniformly to be wrapped in carbon material surface；Take tetraisopropyl titanate: acetic acid quality ratio is
8:1, gross mass and carbon material mass ratio are 1:3, are added in ball mill, then with identical speed per hour ball milling 10h, obtain low temperature
Carbon pastes.
Embodiment 10
In the present embodiment, step (1), (2), (3), (4), (5) and (6) is the same as embodiment 1.
(7) the low temperature carbon pastes that one layer of graphite particle size is 6 μm will be printed on the device after above-mentioned drying, make the low temperature
Carbon pastes are largely covered on the pyrocarbon layer, and another part is covered in the positive pole zone of electrically conducting transparent substrate, so
Low-temperature sintering forms low temperature carbon-coating for a period of time afterwards.The size of carbon pastes is unlimited, as long as its major part is made to be covered on the height
On warm carbon-coating, another part is covered in the positive pole zone of transparent conducting glass.In the present embodiment, sintering temperature 40
DEG C, sintering time 3h, the low temperature carbon layers having thicknesses of formation are about 10 μm.
Wherein low temperature carbon pastes the preparation method comprises the following steps: weigh carbon black: graphite quality ratio be 10:0, be transferred in ball mill,
Use speed per hour for the ball mill ball milling 30min of 200r/h, so that carbon black and graphite be made to be uniformly mixed, wherein graphite is 6 μm of partial sizes
Flake graphite；Weigh carbon material (gross mass of carbon black and graphite): terpinol mass ratio is 1:10, is added in ball mill,
Then with identical speed per hour ball milling 1h, so that terpinol be made uniformly to be wrapped in carbon material surface；Take tetraisopropyl titanate: acetic acid quality
Than being 1:10 for 10:1, gross mass and carbon material mass ratio, it is added in ball mill, then with identical speed per hour ball milling 10h, obtains
To low temperature carbon pastes.
Preparation method simple process in above-described embodiment, prepare carbon-based perovskite solar battery can be greatly reduced it is original
The thickness of high temperature carbon electrode, while reducing the loading of perovskite precursor liquid, moreover it is possible to guarantee that electron transfer layer and insulating layer are situated between
Perovskite material filling inside hole sufficiently improves charge transport properties, so that cell photoelectric efficiency greatly improves.
The carbon-based perovskite solar battery and the common perovskite sun using monolayer carbon of preparation of the embodiment of the present invention
Energy battery is compared, and advantage is that this structure does not influence battery performance, and because improves the filling of perovskite precursor liquid also
The performance of battery can be improved, incident photon-to-electron conversion efficiency is 12.3%~15%.At the same time because the first carbon layers having thicknesses are dropped from 10 μm
As low as 3 μm, the loading of perovskite precursor liquid is greatly reduced, 3 μ L is reduced to from 5 previous μ L, is very advantageous in future
Industrial production.
For the carbon of the perovskite solar battery of preparation of the embodiment of the present invention to electrode, low temperature carbon-coating is directly printed on pyrocarbon
Even thicker with a thickness of 20 μm on layer, the sintering less than 100 DEG C can not destroy the performance of perovskite light absorbent, moreover it is possible to
Guarantee carbon to the high conductivity of electrode.And original pyrocarbon can be reduced to nm or less than 10 by 10 μm to the thickness of electrode layer
μm rank guarantees that precursor liquid more infiltrates into electron transfer layer or dielectric spacer layer.
Prepared by the method New Type of Carbon based perovskite solar cell, by original stable mesoporous solar battery into
Row structure and performance optimization reduce the loading of perovskite precursor liquid, reduce cost protection by reducing the thickness of pyrocarbon layer
Environment, moreover it is possible to solve the problems, such as that carbon, because electric conductivity is not high caused by thickness reduces, finally improves its solar energy and turn to electrode
Change efficiency.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of carbon is to electrode perovskite solar battery, which is characterized in that the perovskite solar battery wraps from bottom to top
Including electrically conducting transparent substrate, light anode, insulating layer, the first carbon-coating and the second carbon-coating, first carbon-coating is porous carbon layer, described the
Two carbon-coatings are low temperature carbon-coating, and the low temperature carbon-coating is carbon-coating made of carbon pastes are fired under the conditions of being lower than 150 DEG C；
The porous carbon layer with a thickness of 1-15 μm, the low temperature carbon-coating with a thickness of 20 μm or more；
The porous carbon layer plays the role of hole and longitudinally transmits for filling perovskite solution；The low temperature carbon layers having thicknesses are big,
Play the role of hole lateral transport and reduces entire carbon to the square resistance of electrode.
2. perovskite solar battery as described in claim 1, which is characterized in that first carbon-coating with a thickness of 1-4 μm.
3. a kind of carbon is to the preparation method of electrode perovskite solar battery, which comprises the steps of:
(1) one layer of compacted zone is prepared in electrically conducting transparent substrate；
(2) one layer of TiO is sequentially prepared by silk-screen printing on step (1) described compacted zone2Mesoporous layer and one layer of ZrO2Insulation
Layer；
(3) the first carbon-coating is prepared on step (2) described insulating layer；The preparation method of first carbon-coating includes the following steps:
By high temperature carbon pastes through screen printer print on the insulating layer, then sintering obtains described the at 300-400 DEG C
One carbon-coating；First carbon-coating be porous carbon layer, the porous carbon layer with a thickness of 1-15 μm；
(4) perovskite precursor liquid is dropped into step (3) first carbon-coating surface；
(5) the second carbon-coating is prepared on first carbon-coating；Specifically comprise the following steps: low temperature carbon pastes passing through silk-screen printing
Machine is printed on first carbon-coating；Then it is obtained in 150 DEG C or less sintering；Second carbon-coating is low temperature carbon-coating, described low
Warm carbon-coating with a thickness of 20 μm or more.
4. preparation method as claimed in claim 3, which is characterized in that step (3) prints the web plate of the high temperature carbon pastes
Mesh number size is -500 mesh of 150 mesh.
5. preparation method as claimed in claim 4, which is characterized in that the high temperature carbon pastes the preparation method comprises the following steps: by graphite,
After carbon black and the mixing of organic polymer pore-creating binder, solvent is added, ball milling obtains the high temperature carbon pastes.
6. preparation method as claimed in claim 3, which is characterized in that step (4) specifically comprised the following steps: will to prepare
Perovskite precursor liquid drops to first carbon-coating edge by drop-coating, makes its filling into each layer porous film layer, described each
Layer porous film layer includes first carbon-coating, the ZrO2Insulating layer, the TiO2Mesoporous layer and the compacted zone；Then
Annealing 5min-2h is carried out at 150 DEG C or less.
7. preparation method as claimed in claim 6, which is characterized in that the loading of the perovskite precursor liquid is 2-4.5 μ L.
8. preparation method as claimed in claim 3, which is characterized in that step (5) is in 150 DEG C or less sintering 10min-4h.
9. preparation method as claimed in claim 8, which is characterized in that the granular size of graphite is 6- in the low temperature carbon pastes
30μm。
10. preparation method as claimed in claim 8, which is characterized in that the preparation method of the low temperature carbon pastes includes as follows
Step:
S1 mixes carbon black and graphite according to mass ratio 10:0-0:10, and ball milling obtains the mixing of uniformly mixed carbon black and graphite
Object；
By in the mixture of the obtained carbon black and graphite of appropriate solvent addition S1, ball milling obtains being coated with the solvent S2
Carbon black and graphite mixture, the mixture and the solvent quality ratio of the carbon black and graphite are 1:1-10；
Binder and compound containing-COOH are 10:1-1:10 with mass ratio by S3, and be added to that S2 obtains is coated with
In the carbon black of the solvent and the mixture of graphite, the low temperature carbon pastes are can be obtained in ball milling, wherein binder and contain-COOH
The gross mass of compound and the total mass ratio of carbon black and graphite be 10:1-1:10.
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| CN108539024A (en) * | 2018-04-16 | 2018-09-14 | 湖北大学 | A kind of carbon-based perovskite solar cell and preparation method thereof |
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| CN110797463B (en) * | 2019-10-30 | 2021-08-20 | 华中科技大学 | Carbon counter electrode perovskite solar cell and preparation method thereof |
| CN111628084A (en) * | 2020-05-28 | 2020-09-04 | 华中科技大学 | Perovskite laminated solar cell and preparation method thereof |
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