CN107146847A - It is a kind of new based on all solid state printable perovskite solar cell of carbon electrode - Google Patents
It is a kind of new based on all solid state printable perovskite solar cell of carbon electrode Download PDFInfo
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- H—ELECTRICITY
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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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- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
It is new based on all solid state printable perovskite solar cell of carbon electrode and preparation method thereof the invention discloses one kind, i.e., TiO is printed using screen printing technique2Working electrode, insulating barrier, 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 less than the 150 DEG C fine and close carbon-coatings sintered to electrode.The structure generation process is simple, lower cost for material, by reducing carbon to the square resistance of electrode and then reducing the series resistance of solar cell device, 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
It is new all solid state based on carbon electrode more particularly, to one kind the invention belongs to perovskite area of solar cell
Printable perovskite solar cell and preparation method thereof.
Background technology
In recent years, perovskite solar cell studied the fashionable whole world, at present the highest battery efficiency through certifying authority
22% is broken through, the efficiency exceedes the efficiency of conventional films solar cell.Compared with other types of solar cell, this
There is class battery material source to facilitate, manufacture craft is simple, equipment requirement is not high and battery low cost and other advantages.These advantages
Illustrate that perovskite solar cell has the development potentiality for replacing high cost polycrystalline silicon and monocrystaline silicon solar cell.
But with noble metal (gold or platinum) as the perovskite solar cell to electrode, because the cost of precious metal material
It is higher, and need the technique of the high energy consumptions such as vacuum evaporation to prepare to electrode, while needing to use expensive hole to pass
The shortcomings of defeated layer so that perovskite solar cell cost is significantly increased.Therefore, seek cheap alternative to electrode preparation work
Skill is also the focus of perovskite area of solar cell research.
Carbon not only has the spies such as structure diversity, chemical stability and abundant surface chemistry 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, are that instead of noble metal
Electrode is preferably selected.2013, Central China University of Science and Technology Korea Spro magnificence seminar was prepared for a kind of all print and is based on carbon electrode first
Without the mesoporous perovskite solar cell of hole transmission layer, 12.8% authentication efficiency is achieved and more than 1000h performances without obvious
The high stability of decay, causes extensive concern in the world, with huge applications prospect (Science, 2014,345,6194).
Carbon electrode is generally electrically conducting transparent substrate/electric transmission without hole transmission layer perovskite solar cell device structure
Layer/insulating barrier/calcium titanium ore bed/carbon electrode, wherein carbon electrode are not only the important composition portion of battery as the back electrode of battery
Point, the effect also with hole transport and composition electronic loop.Therefore, the performance of carbon electrode can greatly affect the property of battery
Energy.
Investigate carbon electrode performance quality of the carbon electrode without hole transmission layer perovskite solar cell and be mainly manifested in two
Aspect, one is the thickness of carbon electrode layer, and two be the square resistance of carbon electrode layer.First, 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, preferable carbon electrode
Thickness degree is preferably thin；But the square resistance of carbon electrode layer is also directly related with thickness, for the carbon electrode layer material of determination,
The square resistance of carbon electrode layer is reduced with the increase of the thickness of carbon electrode layer.It can be seen that, the thickness and face electricity of carbon electrode layer
Resistance is conflict body, wants to obtain excellent carbon electrode performance, and just the thickness and surface resistance of carbon electrode layer must be closed
Reason optimization.The thickness and surface resistance for being effectively reduced carbon electrode are the prior development directions of this kind of solar cell.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the invention provides a kind of composite carbon Rotating fields carbon to electrode
Perovskite solar cell 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 ensures also to greatly reduce the loading of perovskite precursor liquid, warp while the filling of perovskite solution is uniform
Cross after solution annealing and print the larger low temperature carbon-coating of a layer thickness to reduce side of the whole carbon to electrode on porous carbon layer again
Block resistance, to meet the lateral transport demand in hole, so on the basis of electrode performance is ensured, can also greatly reduce to ring
Border has the perovskite loading of potential threat, thus solves the carbon of the carbon electrode of perovskite solar cell of 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
Environmental pollution serious technical problem when causing to industrialize.
To achieve the above object, according to one aspect of the present invention there is provided a kind of carbon to electrode perovskite solar-electricity
Pond, the perovskite solar cell includes electrically conducting transparent substrate, light anode, insulating barrier, the first carbon-coating and second from bottom to top
Carbon-coating, first carbon-coating be porous carbon layer, second carbon-coating be low temperature carbon-coating, the low temperature carbon-coating be carbon pastes less than
The carbon-coating fired under the conditions of 150 DEG C.
Preferably, the thickness of first carbon-coating is 1-15 μm.
Preferably, the thickness of first carbon-coating is 1-4 μm.
Preferably, the thickness of second carbon-coating is not less than 10 μm.
Preferably, the thickness of second carbon-coating is more than 20 μm.
Preferably, the electrically conducting transparent substrate is FTO or ITO；The light anode includes TiO2Compacted zone and TiO2It is mesoporous
Layer；The insulating barrier is ZrO2Layer.
Preferably, the perovskite solar cell also includes being distributed in the electrically conducting transparent substrate, light anode, insulating barrier
With the perovskite in each layer hole of pyrocarbon layer, the perovskite is obtained after the annealed processing of perovskite precursor liquid.
Preferably, the perovskite precursor liquid is the organic metal halide with perovskite crystal formation, its chemical molecular formula
It is expressed as ABX3, wherein A is organic group, and B is metal cation, and X is halide anion.
According to another aspect of the present invention there is provided a kind of preparation method of carbon to electrode perovskite solar cell,
Comprise 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 barrier；
(4) perovskite precursor liquid is dropped into step (3) the 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 comprises the following steps：High temperature carbon pastes are passed through into silk screen
Press printing is on the insulating barrier, 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 the mesh of 150 mesh -500.
Preferably, the preparation method of the high temperature carbon pastes is：Graphite, carbon black and organic polymer pore-creating binding agent 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 comprises the following steps：
S1 is by carbon black, graphite, organic polymer pore-creating binding agent according to mass ratio 10-0：0-10：5-1 is mixed, and is mixed
Close carbon material；Then solvent is added, the quality of wherein solvent accounts for the 20%-50% of mixing carbon material quality；
S2 adds absolute ethyl alcohol, until making the mixing carbon material and solvent dissolving；
S3 uses speed per hour for 200-350r/h ball mill ball milling 8-24h in ball mill；
S4 removes ethanol using Rotary Evaporators revolving, obtains described high temperature carbon pastes.
Preferably, step (4) specifically includes following steps：The perovskite precursor liquid prepared is dropped into 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 below 150 DEG C.
Preferably, in the perovskite precursor liquid filling work procedure, device to be filled is placed on burnishing surface, and from institute
State the first carbon-coating edge and instill perovskite precursor liquid, stood after filling enables 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 includes following steps：By low temperature carbon pastes by screen printer print described
On one carbon-coating；Then 10min-4h is sintered below 150 DEG C, 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 comprises the following steps：
S1 is by carbon black and graphite according to mass ratio 10:0-0:10 mixing, ball milling obtains well mixed carbon black and graphite
Mixture；
S2 adds appropriate solvent in the mixture of the obtained carbon blacks of S1 and graphite, ball milling, obtains being coated with described
The carbon black of solvent and the mixture of graphite, the mixture of the carbon black and graphite are 1 with the solvent quality ratio:1-10；
Compounds of the S3 by binding agent and containing-COOH is using mass ratio as 10:1-1:10, it is added to the surface bag that S2 is obtained
In the mixture for being wrapped with the carbon black of the solvent and graphite, ball milling is that can obtain the low temperature carbon pastes, wherein binding agent and containing-
The total mass ratio of the gross mass of COOH compound and carbon black and graphite is 10:1-1:10.
In general, by the contemplated above technical scheme of the present invention compared with prior art, it 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 is designed,
Far below common carbon-coating (thickness is more than 10 μm), the loading of perovskite precursor liquid can be effectively reduced, from 5 conventional μ L
It is reduced to 3 μ L even lower.Because may be reduced loading containing harmful substances such as lead and not only may be used in perovskite precursor liquid
To reduce cost, pollution on the environment in industrialized production in future can also be reduced.
(2) low temperature carbon-coating greatly compensate 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 shortcoming.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 afterwards can reach mm ranks, sheet resistance is smaller than 1 Ω in theory, is very advantageous in
The lateral transport in hole.So the carbon of this double-decker can ignore the sheet resistance of pyrocarbon layer, the side of general performance to electrode
Resistance is smaller than 1 Ω in theory.
(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, and it is by first
Carbon-coating is completely covered, and the perovskite of filling can be isolated from the outside and play a part of encapsulation, effectively reduce Environmental Water
The decomposition caused to it, improves the stability of the carbon-based perovskite solar cell of this new structure.
(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.
Brief description of the drawings
Fig. 1 is structural representation of the carbon to electrode perovskite solar cell of the embodiment of the present invention 1.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
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 each embodiment of invention described below
Not constituting conflict each other can just be mutually combined.
As shown in figure 1, a kind of carbon printable perovskite solar cell all solid state to electrode that the present invention is provided, passes through silk
Net printing technology is made, from bottom to top including electrically conducting transparent substrate, light anode, insulating barrier, carbon is to electrode and is filled in each thin
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.The double-decker that carbon includes being made up 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 loose structure, is conducive to filling the longitudinal direction transmission in perovskite solution and hole；The thickness of first carbon-coating is 1-
15 μm, preferably 1-4 μm.Second carbon-coating is low temperature carbon-coating, and low temperature carbon layers having thicknesses are big, play a part of hole lateral transport, its
Electric conductivity is strong, and the thickness of low temperature carbon-coating is 10 μm to mm ranks, preferably more than 20 μm.
For the carbon printable perovskite solar cell all solid state to electrode of the present invention, as long as the first carbon-coating is porous carbon
Layer, as a kind of implementation therein, the first carbon-coating can be pyrocarbon layer, and it is high temperature carbon pastes in 400 DEG C of burnings
Tie obtained porous carbon layer.High temperature carbon pastes are carbon material, solvent is prepared after being mixed with organic polymer pore-creating binding agent
Carbon pastes, its due to using organic polymer pore-creating binding agent, when the carbon pastes prepared are used to fire carbon electrode, it is necessary to
Carried out at 300-400 DEG C of high temperature, therefore, be called pyrocarbon layer.Because the carbon pastes add pore-creating in preparation technology
Porous carbon layer structure can be formed during binding agent, therefore its high-temperature firing.
As a kind of implementation therein, the preparation method of high temperature carbon pastes of the invention can be：By carbon black, graphite
Mixed with organic polymer pore-creating binding agent (such as ethyl cellulose), then add solvent (such as terpinol), add suitable
The ethanol of amount, ball milling obtains high temperature carbon pastes after mixing, and the high temperature carbon pastes are fired at 300-400 DEG C of high temperature and obtain porous
Carbon-coating.
Second carbon-coating, namely low temperature carbon-coating, are that obtained densification or porous carbon layer are sintered below 150 DEG C.As wherein
A kind of implementation, the preparation method of low temperature carbon-coating of the invention can be：After carbon black, graphite are mixed with solvent, plus
Enter inorganic or organic binder bond, the compound ball milling containing carboxyl or hydroxyl and obtain low temperature carbon pastes, the carbon pastes can be low
In be fired at 150 DEG C carbon electrode layer.
Perovskite precursor liquid is the organic metal halide with perovskite crystal formation, and its molecular formula is represented by ABX3, its
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).
The carbon of the present invention comprises the following steps to the preparation method of electrode perovskite solar cell：
(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 barrier；
(4) perovskite precursor liquid is dropped into step (3) the first carbon-coating surface, make its filling to the compacted zone,
TiO2Mesoporous layer, ZrO2In the porous film layer of insulating barrier and each layer of the first carbon-coating；
(5) the second carbon-coating is prepared on the pyrocarbon layer.
Wherein, step (3) can be carried out in accordance with the following steps：By high temperature carbon pastes by screen printer print described
On insulating barrier, 40min is then sintered at 400 DEG C and obtains first carbon-coating.Print the mesh number of the web plate of the pyrocarbon layer
Size is the mesh of 150 mesh -500.The granular size of graphite is 200nm-30 μm in high temperature carbon pastes.
As one of which implementation, the preparation method of high temperature carbon pastes of the invention comprises the following steps：
S1 is by carbon black, graphite, organic polymer pore-creating binding agent according to mass ratio 10-0：0-10：5-1 is mixed, and is mixed
Close carbon material；Then solvent is added, the quality of wherein solvent accounts for the 20%-50% of mixing carbon material quality；Wherein carbon black and stone
Ink can only select one kind therein, also can the two selection simultaneously.
S2 weighs the absolute ethyl alcohol of suitable volumes, dissolves all of above material；
S3 uses speed per hour for 200-350r/h ball mill ball milling 8-24h in ball mill；
S4 removes ethanol using Rotary Evaporators revolving, obtains described high temperature carbon pastes.
Perovskite precursor liquid is dropped to step (3) the first carbon-coating surface by step (4), makes its filling to the densification
Layer, TiO2Mesoporous layer, ZrO2In the porous film layer of insulating barrier and each layer of the first carbon-coating, following steps are specifically included：Will
The perovskite precursor liquid prepared drops to the first carbon-coating edge by drop-coating, makes its filling to each layer porous film layer
In；Then annealing 5min-2h is carried out below 150 DEG C.In perovskite precursor liquid filling work procedure, by device to be filled
It is placed on burnishing surface, and perovskite precursor liquid is instilled from the first carbon-coating edge, stood after filling makes the calcium titanium for a period of time
Ore deposit 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 includes following steps：The low temperature carbon pastes of preparation are passed through into screen process press
It is printed on pyrocarbon layer；Then 10min-4h is sintered below 150 DEG C, 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 a kind of implementation therein, the preparation method of low temperature carbon pastes of the invention comprises the following steps：
S1 is by carbon black and graphite according to mass ratio 10:0-0:10 mixing, ball milling obtains well mixed carbon black and graphite
Mixture；Wherein carbon black and graphite can only select one kind therein, also can the two selection simultaneously.
S2 adds appropriate solvent in the mixture of the obtained carbon blacks of S1 and graphite, ball milling, obtains being coated with described
The carbon black of solvent and the mixture of graphite, the mixture of the carbon black and graphite are 1 with the solvent quality ratio:1-10.
Compounds of the S3 by binding agent and containing-COOH is using mass ratio as 10:1-1:10, it is added to the surface bag that S2 is obtained
In the mixture for being wrapped with the carbon black of the solvent and graphite, ball milling is that can obtain the low temperature carbon pastes, wherein binding agent and containing-
The total mass ratio of the gross mass of COOH compound and carbon black and graphite is 10:1-1:10.
Add new additive package in above-mentioned carbon pastes preparation technology, including organic or inorganic binder with containing-
COOH or-OH compound, under solvent such as terpinol existence condition, binding agent, the compound containing-COOH or-OH with
Solvent acts synergistically, and the carbon pastes prepared are low temperature carbon pastes, and 70 DEG C sinterable obtain fine and close carbon-coating.
Advantage of the invention 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 ensures also to greatly reduce the loading of perovskite precursor liquid while the filling of perovskite solution is uniform, by molten
Preparing on the first carbon-coating one layer of very thick low temperature carbon-coating after liquid annealing again reduces square resistance of the whole carbon to electrode, with
The lateral transport demand in hole is met, so on the basis of electrode performance is ensured, can also greatly reduce that there is environment and dive
In the perovskite loading of threat.
It is embodiment below：
Embodiment 1
(1) electro-conductive glass is cut into preferred size in the sheet glass of certain size, such as 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 etch an insulating tape (in the present embodiment preferably for example apart from edge 5mm) parallel with the side, and be left
The a plurality of parallel insulating tape of region etch sheet glass be divided into multiple regions, such as the present embodiment be preferably etch 4 again
Bar parallel insulation band by sheet glass so that be divided into five positive pole zones and negative regions so that conductive layer can not be fully on,
Sheet glass after etching is cleaned by ultrasonic with detergent, distilled water, absolute ethyl alcohol successively.For positive pole zone or negative regions
Size is particularly its width, can carry out according to actual needs specifically chosen, and for example in the present embodiment, positive pole zone size is excellent
Elect 5mm × 100mm as, negative regions preferred size is to be not limited to this in 19mm × 100mm, but the present invention.
(2) in one layer of fine and close TiO of negative regions surface spraying at 450 DEG C in sheet glass2Film.
(3) in above-mentioned TiO2The TiO of one layer of certain size is printed on compacted zone2Slurry, drying is burnt 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 in ZrO2On insulating barrier, then sintering forms cavernous carbon to electrode.The chi of carbon pastes
It is very little not limit, as long as so that it is only placed only in the ZrO2On insulating barrier.Pyrocarbon layer (the first carbon-coating) thickness is about 3 μ
m。
The preparation method of wherein high temperature carbon pastes is：Weigh mass ratio 2：2：1 carbon black, 6 μm of graphite, organic polymers glue
Knot agent (ethyl cellulose) is mixed, 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, added in ball mill；The absolute ethyl alcohol of suitable volumes is weighed to ball mill
In, all of above material is dissolved；In the ball mill ball milling 24h that speed per hour is 200r/h；Using Rotary Evaporators buck by nothing
Water-ethanol is evaporated, and obtains high temperature carbon pastes.
(6) the monoblock device that printing treatment is crossed is placed on smooth desktop, by the method for drop coating at insulating barrier edge
Place instills perovskite precursor liquid, and loading is 3 μ L in the present embodiment, covers standing a period of time, enables precursor liquid uniform
It is substantially filled to the TiO2Mesoporous layer, described ZrO2After in insulating barrier, described 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, makes 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 not limited, as long as so that its major part is covered in 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 preferably
For 50 DEG C, sintering time is 2h, and low temperature carbon-coating (the second carbon-coating) thickness of formation is about 20 μm.
The preparation method of wherein low temperature carbon pastes is：Weigh carbon black：Graphite quality ratio is 1：3, it is transferred in ball mill, adopts
The ball mill ball milling 30min for being 200r/h with speed per hour, so that carbon black and graphite are well mixed, wherein graphite is 6 μm of particle diameters
Flake graphite；Weigh carbon material (gross mass of carbon black and graphite):Terpinol mass ratio is 3：5, added in ball mill, then
With identical speed per hour ball milling 1h, so that terpinol is uniformly wrapped in carbon material surface；Take tetraisopropyl titanate:Acetic acid quality ratio is
8:1, its gross mass is 1 with carbon material mass ratio:3, 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) be the same as Example 1.
(5) using the half tone 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 in ZrO2On insulating barrier, then sintering forms cavernous carbon to electrode.The chi of carbon pastes
It is very little not limit, as long as so that it is only placed only in the ZrO2On insulating barrier.In the present embodiment, pyrocarbon layer thickness is about 2 μ
m。
The preparation method of wherein high temperature carbon pastes is：Weigh mass ratio 4：4：1 carbon black, 2 μm of graphite, organic polymers glue
Knot agent (ethyl cellulose) is mixed, 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, added in ball mill；The absolute ethyl 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) be the same as Example 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, makes 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 not limited, as long as so that its major part be covered in it is described
On pyrocarbon layer, another part is covered in the positive pole zone of transparent conducting glass.In the present embodiment, sintering temperature is 40
DEG C, sintering time is 3h, and the low temperature carbon layers having thicknesses of formation are about 30 μm.
The preparation method of wherein low temperature carbon pastes is：Weigh carbon black：Graphite quality ratio is 1：10, it is transferred in ball mill,
Speed per hour is used for 200r/h ball mill ball milling 30min, so that carbon black and graphite are well mixed, wherein graphite is 15 μm of particle diameters
Flake graphite；Weigh carbon material (gross mass of carbon black and graphite):Terpinol mass ratio is 3：8, added in ball mill, connect
With identical speed per hour ball milling 1h, so that terpinol is uniformly wrapped in carbon material surface；Take tetraisopropyl titanate:Acetic acid quality ratio
For 10:1, its gross mass is 1 with carbon material mass ratio:8, 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) be the same as Example 1.
(5) using the half tone 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 in ZrO2On insulating barrier, then sintering forms cavernous carbon to electrode.Carbon pastes
Size is not limited, as long as so that it is only placed only in the ZrO2On insulating barrier.Pyrocarbon layer thickness is about 1 μm.
The preparation method of wherein high temperature carbon pastes is：Weigh mass ratio 10：2：5 carbon black, 400nm graphite, organic high score
Sub- binding agent (ethyl cellulose) mixes, and is transferred in ball mill；Weigh carbon material (carbon black, graphite and organic high score
The gross mass of sub- binding agent):Terpinol mass ratio is 1：5, added in ball mill；The absolute ethyl alcohol of suitable volumes is weighed to ball
In grinding machine, all of above material is dissolved；In the ball mill ball milling 24h that speed per hour is 200r/h；Use Rotary Evaporators buck
Absolute ethyl alcohol is evaporated, high temperature carbon pastes are obtained.
Embodiment 5
In the present embodiment, step (1), (2), (3), (4), (6) and (7) be the same as Example 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 in ZrO2On insulating barrier, then sintering forms cavernous carbon to electrode.Carbon pastes
Size is not limited, as long as so that it is only placed only in the ZrO2On insulating barrier.Wherein pyrocarbon layer thickness is about 1 μm.
The preparation method of wherein high temperature carbon pastes is：Weigh mass ratio 10：1：1 carbon black, 200nm graphite, organic high score
Sub- pore-creating binding agent (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, added in ball mill；Weigh the absolute ethyl alcohol of suitable volumes
Into ball mill, all of above material is dissolved；In the ball mill ball milling 24h that speed per hour is 200r/h；Use Rotary Evaporators liter
Absolute ethyl alcohol is evaporated by decompression, obtains high temperature carbon pastes.
Embodiment 6
In the present embodiment, step (1), (2), (3), (4), (6) and (7) be the same as Example 1.
(5) using the web plate of 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 in ZrO2On insulating barrier, then sintering forms cavernous carbon to electrode.Carbon pastes
Size is not limited, as long as so that it is only placed only in the ZrO2On insulating barrier.Pyrocarbon layer thickness is about 10 μm.
The preparation method of wherein high temperature carbon pastes is：Weigh mass ratio 10：1 30 μm of graphite and organic polymer binding agent
(ethyl cellulose) is mixed, and is transferred in ball mill；Weigh carbon material (carbon black, graphite and organic polymer binding agent
Gross mass):Terpinol mass ratio is 1：5, added in ball mill；The absolute ethyl alcohol of suitable volumes is weighed into ball mill,
All of above material is dissolved；In the ball mill ball milling 24h that speed per hour is 200r/h；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) be the same as Example 6.
(6) the monoblock device that printing treatment is crossed is placed on smooth desktop, by the method for drop coating at insulating barrier edge
Place instills perovskite precursor liquid, and loading is 4.5 μ L in the present embodiment, covers standing a period of time, enables precursor liquid equal
It is even to be substantially filled to the TiO2Mesoporous layer, described ZrO2After in insulating barrier, described pyrocarbon layer, drying.
Embodiment 8
In the present embodiment, step (1), (2), (3), (4), (5) and (7) be the same as Example 5.
(6) the monoblock device that printing treatment is crossed is placed on smooth desktop, by the method for drop coating at insulating barrier edge
Place instills perovskite precursor liquid, and loading is 2 μ L, covers standing a period of time, precursor liquid is uniformly substantially filled to
The TiO2Mesoporous layer, described ZrO2After in insulating barrier, described pyrocarbon layer, drying.
Embodiment 9
In the present embodiment, step (1), (2), (3), (4), (5) and (6) be the same as Example 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, makes 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 not limited, as long as so that its major part be covered in it is described
On pyrocarbon layer, another part is covered in the positive pole zone of transparent conducting glass.In the present embodiment, sintering temperature is 70
DEG C, sintering time is 1.5h, and the low temperature carbon layers having thicknesses of formation are about 1mm.
The preparation method of wherein low temperature carbon pastes is：Weigh carbon black：Graphite quality ratio is 1：3, it is transferred in ball mill, adopts
The ball mill ball milling 30min for being 200r/h with speed per hour, so that carbon black and graphite are well mixed, wherein graphite is 30 μm of particle diameters
Flake graphite；Weigh carbon material (gross mass of carbon black and graphite):Terpinol mass ratio is 3：5, added in ball mill, then
With identical speed per hour ball milling 1h, so that terpinol is uniformly wrapped in carbon material surface；Take tetraisopropyl titanate:Acetic acid quality ratio is
8:1, its gross mass is 1 with carbon material mass ratio:3, 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) be the same as Example 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, makes 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 not limited, as long as so that its major part is covered in 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 is 40
DEG C, sintering time is 3h, and the low temperature carbon layers having thicknesses of formation are about 10 μm.
The preparation method of wherein low temperature carbon pastes is：Weigh carbon black：Graphite quality ratio is 10：0, it is transferred in ball mill,
Speed per hour is used for 200r/h ball mill ball milling 30min, so that carbon black and graphite are well mixed, wherein graphite is 6 μm of particle diameters
Flake graphite；Weigh carbon material (gross mass of carbon black and graphite):Terpinol mass ratio is 1：10, added in ball mill,
Then with identical speed per hour ball milling 1h, so that terpinol is uniformly wrapped in carbon material surface；Take tetraisopropyl titanate:Acetic acid quality
Than for 10:1, its gross mass is 1 with carbon material mass ratio:10, added in ball mill, then with identical speed per hour ball milling 10h, obtain
To low temperature carbon pastes.
Preparation method technique is simple in above-described embodiment, prepare carbon-based perovskite solar cell 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 ensure that electron transfer layer and insulating barrier are situated between
Perovskite material filling inside hole is abundant, improves charge transport properties, so that cell photoelectric efficiency is greatly improved.
The perovskite sun of carbon-based perovskite solar cell prepared by the embodiment of the present invention and common use monolayer carbon
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, electricity conversion is 12.3%~15%.At the same time because the first carbon layers having thicknesses drop from 10 μm
Low to 3 μm, the loading of perovskite precursor liquid is greatly reduced, 3 μ L is reduced to from 5 conventional μ L, is very advantageous in future
Industrial production.
The carbon of perovskite solar cell prepared by the embodiment of the present invention is to electrode, and low temperature carbon-coating is directly printed on pyrocarbon
On layer, thickness is 20 μm even thicker, and the sintering less than 100 DEG C can not destroy the performance of perovskite light absorbent, moreover it is possible to
Ensure high conductivity of the carbon to electrode.And original pyrocarbon can be reduced to nm or less than 10 to the thickness of electrode layer by 10 μm
μm rank, it is ensured that precursor liquid more infiltrates into electron transfer layer or dielectric spacer layer.
The New Type of Carbon based perovskite solar cell prepared using the present invention, the mesoporous solar cell to original stabilization is entered
Row structure and performance optimization, by reducing the thickness of pyrocarbon layer, reduce the loading of perovskite precursor liquid, reduce cost protection
Environment, moreover it is possible to solve carbon to electrode because the problem of electric conductivity is not high caused by thickness reduction, finally improve its solar energy and turn
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, it is not used to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the invention etc., it all should include
Within protection scope of the present invention.
Claims (10)
1. a kind of carbon is to electrode perovskite solar cell, it is characterised in that the perovskite solar cell is wrapped from bottom to top
Include electrically conducting transparent substrate, light anode, insulating barrier, 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 the carbon-coating that carbon pastes are fired under the conditions of less than 150 DEG C.
2. perovskite solar cell as claimed in claim 1, it is characterised in that the thickness of first carbon-coating is 1-15 μ
M, preferably 1-4 μm.
3. perovskite solar cell as claimed in claim 1, it is characterised in that the thickness of second carbon-coating is not less than 10
μm, preferably more than 20 μm.
4. a kind of carbon is to the preparation method of electrode perovskite solar cell, it is characterised in that comprise 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 ZrO2Insulation
Layer；
(3) the first carbon-coating is prepared on step (2) described insulating barrier；
(4) perovskite precursor liquid is dropped into step (3) the first carbon-coating surface；
(5) the second carbon-coating is prepared on first carbon-coating.
5. preparation method as claimed in claim 4, it is characterised in that the preparation method of step (3) first carbon-coating includes
Following steps：By high temperature carbon pastes by screen printer print on the insulating barrier, then sintered at 300-400 DEG C
To first carbon-coating；The mesh number for printing the web plate of the high temperature carbon pastes is preferably sized to the mesh of 150 mesh -500.
6. preparation method as claimed in claim 5, it is characterised in that the preparation method of the high temperature carbon pastes is：By graphite,
After carbon black and the mixing of organic polymer pore-creating binding agent, solvent is added, ball milling obtains the high temperature carbon pastes；The pyrocarbon
The granular size of graphite is preferably 200nm-30 μm in slurry.
7. preparation method as claimed in claim 4, it is characterised in that step (4) specifically includes following steps：By what is prepared
Perovskite precursor liquid drops to the 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 barrier, the TiO2Mesoporous layer and the compacted zone；Then
Annealing 5min-2h is carried out below 150 DEG C.
8. preparation method as claimed in claim 7, it is characterised in that the loading of the perovskite precursor liquid is 2-4.5 μ L.
9. preparation method as claimed in claim 4, it is characterised in that step (5) specifically includes following steps：Cryogenic carbon is starched
Material is by screen printer print on first carbon-coating；Then 10min-4h is sintered below 150 DEG C, temperature is preferably
50-150 DEG C, sintering time is preferably 1-2h；The granular size of graphite is preferably 6-30 μm in the low temperature carbon pastes.
10. preparation method as claimed in claim 9, it is characterised in that the preparation method of the low temperature carbon pastes includes as follows
Step：
S1 is by carbon black and graphite according to mass ratio 10:0-0:10 mixing, ball milling obtains the mixing of well mixed carbon black and graphite
Thing；
S2 is by the mixture of the obtained carbon blacks of appropriate solvent addition S1 and graphite, and ball milling obtains being coated with the solvent
Carbon black and graphite mixture, the mixture of the carbon black and graphite and the solvent quality ratio are 1:1-10；
Compounds of the S3 by binding agent and containing-COOH is using mass ratio as 10:1-1:10, be added to that S2 obtains is coated with
In the carbon black of the solvent and the mixture of graphite, ball milling is that can obtain the low temperature carbon pastes, wherein binding agent and contains-COOH
Gross mass and the carbon black of compound and the total mass ratio of graphite be 10:1-1:10.
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