CN206408291U - A kind of former of calcium titanium ore bed film and its application - Google Patents
A kind of former of calcium titanium ore bed film and its application Download PDFInfo
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- CN206408291U CN206408291U CN201620939493.XU CN201620939493U CN206408291U CN 206408291 U CN206408291 U CN 206408291U CN 201620939493 U CN201620939493 U CN 201620939493U CN 206408291 U CN206408291 U CN 206408291U
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Abstract
The utility model is related to former and its application of a kind of calcium titanium ore bed film, utilize a tubular housing, tubular housing is disposed with substrate approach section, deposit cavity, adapter cavity, anneal chamber and substrate take out five parts such as section, conveyer is set in tubular housing, objective table is respectively arranged with deposit cavity and anneal chamber, barometric control unit and heater, dividing plate is utilized respectively between adjacent segment and chamber and each chamber to separate, the substrate of film to be deposited is placed on frame substrate, by conveyer since substrate approach section, successively continually by deposit cavity, after adapter cavity and anneal chamber, last taken out from substrate takes out the substrate for having deposited calcium titanium ore bed film on the frame substrate of section, deposition film forming and annealing process are combined together, realize the consecutive production of calcium titanium ore bed film product.Using the calcium titanium ore bed film crystal even particle size of device fabrication of the present utility model, densification, with good photoelectric transformation efficiency.
Description
Technical field
The utility model belongs to the technical field of calcium titanium ore bed film, and more particularly to a kind of shaping of calcium titanium ore bed film is set
Standby and its application.
Background technology
Solar cell is a kind of electrooptical device, is converted solar energy into electrical energy using the photovoltaic effect of semiconductor.
It is developed so far, solar power generation has become the most important regenerative resource in addition to hydroelectric generation and wind-power electricity generation.Now it is used for
Commercialized semiconductor has monocrystalline silicon, polysilicon, non-crystalline silicon, cadmium telluride, CIGS etc., but most energy consumption is big, cost is high.
In recent years, a kind of perovskite solar cell is received significant attention, and this perovskite solar cell is with organic gold
Category halide is light absorbing layer.Perovskite is ABX3The cuboctahedron structure of type, as shown in Figure 1.Prepared by such a material thin
Film solar cell technique is easy, production cost is low, stable and high conversion rate, from 2009 so far, photoelectric transformation efficiency from
3.8% is promoted to more than 22%, higher than commercialized crystal silicon solar batteries and with larger cost advantage.
Various perovskite solar battery thin film moulding process can be divided into two major classes：Solwution method and vapor phase method.Solwution method is grasped
Make easy, film forming can be prepared at normal temperatures and pressures, but the thin homogeneity of perovskite formed is poor, in film microstructure Hole
Too much, leakage current is big, has a strong impact on the efficiency of solar cell, and poor repeatability.Therefore this method is not suitable for extensive, large scale
Production.Vapor phase method has double source coevaporation method, gas phase assisted solution method, chemical vapor deposition（CVD）Etc. method.Such as with CH3NH3I and
PbCl2As two evaporation sources, perovskite thin film can be prepared.This method is compared with solwution method, and the film prepared is more
It is homogeneous.But this method needs high vacuum and higher temperature conditionss, improve cost and can not mass produce.Thus propose gas
Phase assisted solution method solves this problem, has been made that crystallite dimension is bigger, the covering smaller calcium titanium of complete, surface roughness
Ore deposit film.
Low-pressure chemical vapor deposition（LPCVD）It is also applied to prepare perovskite thin film etc. method, has obtained better performances
Film.Existing Low Pressure Chemical Vapor Deposition（LPCVD）Need to aid in gas, the nitrogenous organic salt of evaporation in deposition process
Halide（AX）Deposit uneven in course of reaction, the putting position of substrate can largely influence property of thin film so that same
There is difference in property of thin film prepared by one batch；Simultaneously, it is impossible to annealed or solvent auxiliary annealing technique after film forming, nothing
Method realizes consecutive production.
Utility model content
Technical problem to be solved in the utility model is there is provided a kind of former of calcium titanium ore bed film and its answered
With, the reactant homogeneous film formation of calcium titanium ore bed film is made under conditions of it need not aid in gas, and by gas phase-solid phase film forming
It is combined together with annealing process, realizes the continuity automated production of calcium titanium ore bed film product.
The utility model, which is achieved in that, provides a kind of former of calcium titanium ore bed film, including tubular housing and
Conveyer, the conveyer is arranged in tubular housing, and substrate approach section is respectively arranged with before and after the tubular housing
Section is taken out with substrate, the tubular housing is respectively arranged with some deposit cavities and/or adapter cavity and/or anneal chamber, described heavy
The objective table for placing deposition reactant is provided with product chamber, the loading for placing annealing secondary solvent is provided with the anneal chamber
Platform, is also respectively provided with placement barometric control unit and heater, the heater in the deposit cavity and anneal chamber
The deposition reactant in objective table and annealing secondary solvent are heated respectively, the deposition reactant and annealing secondary solvent
After heating evaporation its gas particles deposit to positioned at film to be deposited in the chamber substrate surface on, in adjacent segment and chamber
Dividing plate is utilized respectively between room and each chamber to separate；The substrate of film to be deposited is placed on frame substrate, by conveyer from
Substrate approach section starts, successively continually by some deposit cavities and/or adapter cavity and/or anneal chamber after, finally taken from substrate
Go out on the frame substrate of section the substrate for taking out and having deposited calcium titanium ore bed film.
Further, the conveyer includes conveyer belt, and the frame substrate is set on a moving belt；The conveyer belt is set
Put in the surface of objective table, the substrate it is to be deposited down just to objective table.
Further, it is provided with the middle part of the groove for placing substrate, the groove and is provided with the middle part of the frame substrate
Recess hole, the groove is slightly larger than substrate, and the recess hole is slightly less than the surface to be deposited of substrate, on the both sides of the frame substrate
It is used for the position for fixing substrate equipped with transversely movable movable substrate fixed plate, the substrate fixed plate is fixed on substrate
The back side.
Further, the objective table top is provided with split-flow baffles, multiple points is provided with the split-flow baffles
Discharge orifice, the reactant gas of the objective table evaporation reaches substrate surface again after split-flow baffles.
Further, the heater includes the upper heating plate and lower heating plate positioned at deposit cavity, and positioned at annealing
The upper heating plate of chamber and lower heating plate, the upper heating plate of the deposit cavity and the upper heating plate of anneal chamber are respectively on frame substrate
Substrate is heated, and the lower heating plate of the deposit cavity and the lower heating plate of anneal chamber are respectively to the deposition in the objective table of place chamber
Reactant and annealing secondary solvent are heated；The temperature control of the upper heating plate of the deposit cavity and the upper heating plate of anneal chamber
At 30 DEG C ~ 150 DEG C, the objective table temperature control of the deposit cavity is in 100 DEG C ~ 200 DEG C, the temperature of the objective table of the anneal chamber
Control is at 30 DEG C ~ 200 DEG C.
The invention also discloses a kind of solar cell of calcium titanium ore bed film, above-mentioned calcium titanium ore bed film is utilized
Former manufacture the calcium titanium ore bed film layer of substrate.
The invention also discloses a kind of LED of calcium titanium ore bed film, the shaping of above-mentioned calcium titanium ore bed film is utilized
Equipment manufactures the calcium titanium ore bed film layer of substrate.
It is thin using above-mentioned calcium titanium ore bed the invention also discloses a kind of thin film field-effect pipe of calcium titanium ore bed film
The former of film manufactures the calcium titanium ore bed film layer of substrate.Compared with prior art, calcium titanium ore bed of the present utility model is thin
The former of film and its application, using a tubular housing, tubular housing is disposed with substrate approach section, deposit cavity, transition
Chamber, anneal chamber and substrate take out five parts such as section, and conveyer is set in tubular housing, in deposit cavity and anneal chamber point
Be not provided with objective table, barometric control unit and heater, be utilized respectively between adjacent segment and chamber and each chamber every
Plate is separated, and the substrate of film to be deposited is placed on frame substrate, by conveyer since substrate approach section, successively continuously
After deposit cavity, adapter cavity and anneal chamber, take out that to have deposited calcium titanium ore bed thin on the frame substrate that section is finally taken out from substrate
The substrate of film, deposition film forming and annealing process are combined together, the automatic metaplasia of continuity of calcium titanium ore bed film product is realized
Production, is greatly enhanced production efficiency.
Brief description of the drawings
Fig. 1 is calcium titanium ore bed thin-film material ABX3Crystal structure schematic diagram；
Fig. 2 is the floor map of the preferred embodiment of the utility model one；
Fig. 3 is the top view of split-flow baffles in Fig. 2；
Fig. 4 is the top view of frame substrate in Fig. 2；
Fig. 5 is the top view for the conveyer for being placed with substrate and frame substrate；
Fig. 6 is a kind of manufacture of solar cells process schematic using ITO or FTO as substrate；
Fig. 7 is to be intended to using the battery structure diagram of perovskite solar cell made from equipment of the present utility model；
Fig. 8 is the SEM figures using perovskite thin film made from equipment of the present utility model；
Fig. 9 is the XRD of Fig. 8 perovskite thin film；
Figure 10 is the Current density-voltage of the perovskite solar cell prepared using equipment of the present utility model（J-V）
Curve map.
Embodiment
In order that technical problem to be solved in the utility model, technical scheme and beneficial effect are more clearly understood, with
Lower combination drawings and Examples, the utility model is further elaborated.It should be appreciated that specific reality described herein
Example is applied only to explain the utility model, is not used to limit the utility model.
It refer to shown in Fig. 2, a kind of forming method of calcium titanium ore bed film disclosed in the utility model, be to utilize a tubulose
Cavity 2, is respectively arranged with substrate approach section M1 before and after the tubular housing 2 and substrate takes out section M5.In the utility model,
It is to be separately positioned in tubular housing 2 and be located at the rear and front end portion of tubular housing 2 that substrate approach section M1 and substrate, which take out section M5,
In the case of having, substrate approach section M1 and substrate take out section M5 and can also be separately positioned on outside tubular housing 2 near before and after it
Both ends.
Some deposit cavity M2 and/or adapter cavity M3 and/or anneal chamber M4 are respectively arranged with the tubular housing 2.
In the utility model, a deposit cavity M2, an adapter cavity M3 and an anneal chamber are disposed with respectively in tubular housing 2
M4, can require according to the number of plies of substrate deposition film, set multiple deposit cavities respectively in tubular housing 2 in some cases
M2 and/or adapter cavity M3 and/or anneal chamber M4.
The objective table 7 for placing deposition reactant is provided with the deposit cavity M2, is provided with the anneal chamber M4
The objective table 19 of annealing secondary solvent is placed, barometric control unit is also respectively provided with the deposit cavity M2 and anneal chamber M4
1 and 18 and heater 8 and 16.The heater is aided in the deposition reactant in objective table 7 and 19 and annealing respectively
Solvent is heated, after deposition reactant heating evaporation its gas particles deposit to positioned at film to be deposited in the chamber
Reaction forms ABX on substrate surface3Type perovskite.Auxiliary-solvent evaporation particle of annealing aids in perovskite crystal further growth.
Dividing plate 4,12,15 and 20 is utilized respectively between adjacent segment and chamber and each chamber to separate.
The forming method comprises the following steps：
The substrate 9 of film to be deposited is placed on frame substrate 24, by be arranged in tubular housing 2 conveyer 3,
10th, 11,14 and 22 since substrate approach section M1, successively continually by deposit cavity M2, adapter cavity M3 and anneal chamber M4 after, most
The substrate 9 for having deposited calcium titanium ore bed film is taken out on the frame substrate 24 for taking out section M5 from substrate afterwards.The deposit cavity M2 is used for
Calcium titanium ore bed film layer is deposited on the surface of substrate 9, the adapter cavity M3 is used to transmit and of short duration placement deposition has perovskite thin
The substrate 9 of film, the anneal chamber M4 is used for having perovskite thin film layer to be made annealing treatment to deposition.
Referring to shown in Fig. 2, Fig. 3, Fig. 4, Fig. 5 and Fig. 6, the invention also discloses a kind of using above-mentioned
The former that the forming method principle of calcium titanium ore bed film is made, including tubular housing 2 and the and of conveyer 3,10,11,14
22, the conveyer 3,10,11,14 and 22 is arranged in tubular housing 2.It is respectively arranged with before and after the tubular housing 2
Substrate approach section M1 and substrate take out section M5, and the tubular housing 2 is disposed with deposit cavity M2, adapter cavity M3 and annealing respectively
Chamber M4.The objective table 7 for placing deposition reactant is provided with the deposit cavity M2, placement is provided with the anneal chamber M4
The objective table 19 of annealing secondary solvent, is also respectively provided with the He of barometric control unit 1 in the deposit cavity M2 and anneal chamber M4
18 and heater 8 and 16.Heater described in M2 makes it distil deposition reactant heating in objective table 7, adds in M4
Thermal carries out heating to the annealing secondary solvent in objective table 19 evaporates it.Between adjacent segment and chamber and each chamber
4,12,15 and 20 dividing plates are utilized respectively to separate.The substrate 9 of film to be deposited is placed on frame substrate 24, by conveyer 3,10,
11st, 14 and 22 since substrate approach section M1, successively continually by deposit cavity M2, adapter cavity M3 and anneal chamber M4 after, finally
Taken out from substrate and the substrate 9 for having deposited calcium titanium ore bed film is taken out on section M5 frame substrate 24.
The former is additionally provided with dividing plate control system, the closing of the dividing plate 4,12,15 and 20 and open by every
Panel control system is controlled.
The conveyer 3,10,11,14 and 22 includes conveyer belt 23.The frame substrate 24 is set on a moving belt.Institute
State the surface that conveyer belt 23 is arranged on objective table 7 and 19, the substrate 9 it is to be deposited down just to objective table 7 and 19.
The groove 25 for placing substrate 9 is provided with the middle part of the frame substrate 24, the middle part of groove 25 is provided with recess hole 27.
Groove 25 is slightly larger than substrate 9, and recess hole 27 is slightly less than the surface to be deposited of substrate 9.The face to be deposited of substrate 9 is from recess hole 27
Reveal and be easy to deposition.It is used on the both sides of the frame substrate 24 equipped with transversely movable movable substrate fixed plate 26 solid
Determine the position of substrate 9, the substrate fixed plate 26 is fixed on the back side of substrate 9.Recess hole 27 can be according to the tune of the size of substrate 9
Section.The material of the frame substrate 24 can be the nonmetallic materials such as alloy material or glass, ceramics such as stainless steel.
The top of the objective table 7 and 19 is provided with split-flow baffles 6 and 21, on the split-flow baffles 6 and 21 respectively
It is provided with multiple tap holes 28, the reactant gas that the objective table 7 and 19 evaporates respectively through arriving again after split-flow baffles 6 and 21
Up to the surface of substrate 9.The reactant steam for causing evaporation using split-flow baffles 6 and 21 is uniformly dispersed, so as to obtain homogeneous, repetition
Property good perovskite thin film layer.Split-flow baffles 6 and 21 can be one or more layers, and tap hole 28 can be circular, square, annular etc.
Shape.
The heater includes the upper heating plate 5 and lower heating plate 8 positioned at deposit cavity M2, and positioned at anneal chamber M4's
Upper heating plate 17 and lower heating plate 16.The upper heating plate 5 of the deposit cavity M2 and anneal chamber M4 upper heating plate 17 are filled with transmission
The distance for putting the frame substrate 24 on 10 and 14 distinguishes adjustable, the upper heating plate 5 of the deposit cavity M2 and anneal chamber M4 upper heating
Plate 17 is heated to the substrate 9 on frame substrate 24 respectively, 16 points of the lower heating 6 of the deposit cavity M2 and anneal chamber M4 lower heating plate
Do not heated to the annealing secondary solvent in the deposition reactant and objective table 19 in the objective table 7 of place chamber.It is described heavy
Air pressure in product chamber and anneal chamber is controlled 10-5Pa ~105Between Pa；The temperature control of the objective table of the deposit cavity is 100
DEG C ~ 200 DEG C, preferably 120 DEG C ~ 180 DEG C；On the deposit cavity temperature control of heating plate 30 DEG C ~ 150 DEG C, preferably 30
℃~120℃；The temperature control of the objective table of the anneal chamber is at 30 DEG C ~ 120 DEG C, preferably 30 DEG C ~ 80 DEG C；The anneal chamber
Upper temperature of heating plate control, at 30 DEG C ~ 200 DEG C, is preferably 80 DEG C ~ 120 DEG C.
Deposition reactant in the deposit cavity M2 objective tables 7 is AX, wherein A be in amido, amidino groups or alkali family extremely
Few one kind, preferably methylamino (Methylammonium), ethanamidine base（Formamidinium）Or caesium X is iodine, bromine, chlorine, astatine etc.
The anion of at least one of halogen.Annealing secondary solvent in the anneal chamber M4 objective tables 19 is amide solvent, sulfone
Class/sulfoxide type solvents, esters solvent, hydro carbons, halogenated hydrocarbon solvent, alcohols solvent, ketones solvent, ether solvent, aromatic hydrocarbon are molten
Any one in agent.
The reaction time of the deposit cavity M2 is controlled in 5min ~ 2h, preferably 10min ~ 60min；The anneal chamber M4 is moved back
Fiery time control is in 5min ~ 2h, preferably 10min ~ 60min.
Gas evaporation speed and semiconductive thin film detection device are additionally provided with the deposit cavity M2 and anneal chamber M4, is used
In the evaporation capacity and the film thickness of substrate deposition of control reactant.
Air bleeding valve 13 is housed at the top of the adapter cavity M3, in row pressure or regulation deposit cavity M2 and anneal chamber M4
Air pressure.
Solvent auxiliary annealing can be carried out in the anneal chamber M4（When placing solvent on objective table 19）Or it is solvent-free auxiliary
Help annealing（When not placing solvent on objective table 19）.
The invention also discloses a kind of application of the former of foregoing calcium titanium ore bed film, it is to be applied to system
Make in solar cell or LED or thin film field-effect pipe.
Illustrate concrete application of the present utility model with reference to embodiment.
Embodiment 1
It refer to shown in Fig. 7, the former of calcium titanium ore bed film of the present utility model is making area of solar cell
In application, specifically include following steps：
（1）By 2.5 × 2.5cm ito glass plate successively through liquid detergent, deionized water, acetone, each cleaning of isopropanol ultrasound
30min, then use N2After drying 10min is handled through UV O-zone；
（2）Spin coating PEDOT:PSS, 90 DEG C ~ 150 DEG C drying 5min ~ 20min；
（3）By PbBr2It is dissolved in DMF, concentration is 1M, 70 DEG C of stirring 2h, in PEDOT:The spin coating of PSS upper stratas obtains PbBr2
Film, 70 DEG C ~ 100 DEG C annealing 5min ~ 60min；
（4）Deposition there is into precursor PbBr2One or more pieces substrates 9 be positioned over frame substrate 24, open dividing plate 4, pass through and pass
Send device 3 and 10 to be sent to deposit cavity M2 into chamber M1 through substrate, close dividing plate 4；
（5）Dividing plate 12 is opened, by barometric control unit 1 by the Stress control in deposit cavity M2 10-5Pa ~105Pa it
Between, close dividing plate 12；
（6）150 DEG C ~ 200 DEG C of 7 temperature of objective table and upper 80 DEG C ~ 120 DEG C of 5 temperature of heating plate are controlled respectively so that objective table
MABr solvents evaporation in 7, MABr gases and the PbBr on substrate 9 of evaporation2Film reacts, and generates perovskite thin film,
Reaction time is 5min ~ 30min；
（7）Dividing plate 12 is opened, using air bleeding valve 13 is closed after the row pressure of air bleeding valve 13, deposition is had into calcium by conveyer 11
The substrate 9 of titanium ore film is sent to adapter cavity M3, closes dividing plate 12；
（8）Dividing plate 15 is opened, the substrate 9 of film forming is sent to anneal chamber M4 using transmitting device 11 and 14；In objective table
Solvent is added on 19；Dividing plate 15 is closed, the air pressure in anneal chamber M4 is adjusted by barometric control unit 13, is controlled 10-5Pa ~
105Between Pa；Set the temperature control of objective table 19 at 60 DEG C ~ 100 DEG C, the temperature of upper heating plate 17 is 90 DEG C ~ 120 DEG C, is entered
The thick perovskite thin films of 200nm ~ 350nm are made in row annealing, annealing time 5min ~ 60min；
（9）Dividing plate 15 is opened, closing air bleeding valve 13 after the row pressure of air bleeding valve 13 is utilized；Dividing plate 15 is closed, dividing plate 20 is opened, will
The substrate that deposition has perovskite thin film is sent to substrate by transmitting device 22 and takes out taking-up, substrate after section, the natural cooling of substrate 9
Electron transfer layer PCBM is deposited on 9；
（10）Evaporation metal conductive layer Au electrodes, obtain solar cell.
Fig. 8 is the SEM figures using perovskite thin film made from equipment of the present utility model, can be intuitive to see from figure
By film crystal even particle size, densification made from such a method, crystallite dimension is in 500nm or so.
Fig. 9 is the XRD of Fig. 8 perovskite thin film, and MAPbBr is only observed in figure3Diffraction maximum and peak type is sharp, and
Without MABr, PbBr2Diffraction maximum, illustrate that perovskite thin film purity, crystallinity that this method is prepared are higher.
Figure 10 is the Current density-voltage of the perovskite solar cell prepared using equipment of the present utility model（J-V）
Curve map, it can be seen that the perovskite solar cell J preparedscAnd VocHigher, measurement obtains calcium titanium made from this method
The photoelectric transformation efficiency of ore deposit solar cell is up to 15.04%.
Embodiment 2
The former of calcium titanium ore bed film of the present utility model is applied in LED field is made, and is specifically included following
Step：
（1）By 2.5 × 2.5cm FTO PETs plate successively through liquid detergent, deionized water, acetone, isopropyl
Each cleaning 20min of alcohol ultrasound, then use N2After drying 15min is handled through UV O-zone；
（2）Spin coating CuSCN, 100 DEG C ~ 200 DEG C drying 5min ~ 20min；
（3）By PbCl2It is dissolved in DMF, concentration is 1M, 70 DEG C of stirring 2h, and PbCl is obtained in the spin coating of CuSCN upper stratas2It is thin
Film, 70 DEG C ~ 100 DEG C annealing 5min ~ 60min；
（4）Deposition there is into precursor PbBr2One or more pieces substrates 9 be positioned over frame substrate 24, open dividing plate 4, pass through and pass
Send device 3 and 10 to be sent to deposit cavity M2 into chamber M1 through substrate, close dividing plate 4；
（5）Dividing plate 12 is opened, by barometric control unit 1 by the Stress control in deposit cavity M2 10-5Pa~105Pa it
Between, close dividing plate 12；
（6）100 DEG C ~ 160 DEG C of 7 temperature of objective table and upper temperature 60 C ~ 120 DEG C of heating plate 5 are controlled respectively so that objective table
MACl solvents evaporation in 7, MACl gases and the PbCl on substrate 9 of evaporation2Film reacts, and generates perovskite thin film,
React 5min ~ 30min；
（7）Dividing plate 12 is opened, using air bleeding valve 13 is closed after the row pressure of air bleeding valve 13, deposition is had into calcium by conveyer 11
The substrate 9 of titanium ore film is sent to adapter cavity M3, closes dividing plate 12；
（8）Dividing plate 15 is opened, the substrate 9 of film forming is sent to anneal chamber M4 using transmitting device 14；On objective table 19
Add solvent；Dividing plate 15 is closed, the air pressure in anneal chamber M4 is adjusted by barometric control unit 13, is controlled 10-5Pa~105Pa
Between；Set the temperature control of objective table 19 at 100 DEG C ~ 160 DEG C, 80 DEG C ~ 120 DEG C of the temperature of upper heating plate 17 is annealed
The thick perovskite thin films of 180nm ~ 320nm are made in processing, annealing time 5min ~ 60min；
（9）Dividing plate 15 is opened, closing air bleeding valve 13 after the row pressure of air bleeding valve 13 is utilized；Dividing plate 15 is closed, dividing plate 20 is opened, will
The substrate that deposition has perovskite thin film is sent to substrate by transmitting device 22 and takes out taking-up, substrate after section, the natural cooling of substrate 9
Electron transfer layer PCBM is deposited on 9；
（10）Evaporation metal conductive layer aoxidizes molybdenum electrode, obtains LED.
Embodiment 3
The former of calcium titanium ore bed film of the present utility model is applied in thin film field-effect pipe field is made, specific bag
Include following steps：
（1）By 2.5 × 2.5cm ito glass plate successively through liquid detergent, deionized water, acetone, each cleaning of isopropanol ultrasound
30min, then use N2After drying 10min is handled through UV O-zone；
（2）Spin coating PEDOT:PSS, 90 DEG C ~ 150 DEG C drying 5min ~ 20min；
（3）By PbBr2It is dissolved in DMF, concentration is 1M, 70 DEG C of stirring 2h, in PEDOT:The spin coating of PSS upper stratas obtains PbBr2
Film, 70 DEG C ~ 100 DEG C annealing 5min ~ 60min；
（4）Deposition there is into precursor PbBr2One or more pieces substrates 9 be positioned over frame substrate 24, open dividing plate 4, pass through and pass
Send device 3 and 10 to be sent to deposit cavity M2 into chamber M1 through substrate, close dividing plate 4；
（5）By barometric control unit 1 by the Stress control in deposit cavity M2 10-5Pa~105Between Pa；
（6）150 DEG C ~ 200 DEG C of 7 temperature of objective table and upper 80 DEG C ~ 150 DEG C of 5 temperature of heating plate are controlled respectively so that objective table
MABr solvents evaporation in 7, MABr gases and the PbBr on substrate 9 of evaporation2Film reacts, and generates perovskite thin film,
React 5min ~ 30min；
（7）Dividing plate 12 is opened, using air bleeding valve 13 is closed after the row pressure of air bleeding valve 13, deposition is had into calcium by conveyer 11
The substrate 9 of titanium ore film is sent to adapter cavity M3, closes dividing plate 12；
（8）Dividing plate 15 is opened, the substrate 9 of film forming is sent to anneal chamber M4 using transmitting device 14；On objective table 19
Add solvent；Dividing plate 15 is closed, the air pressure in anneal chamber M4 is adjusted by barometric control unit 13, is controlled 10-5Pa~105Pa
Between；Set the temperature control of objective table 19 at 80 DEG C ~ 100 DEG C, 100 DEG C ~ 150 DEG C of the temperature of upper heating plate 17 is annealed
The thick perovskite thin films of 250nm ~ 420nm are made in processing, annealing time 5min ~ 60min；
（9）Dividing plate 15 is opened, closing air bleeding valve 13 after the row pressure of air bleeding valve 13 is utilized；Dividing plate 15 is closed, dividing plate 20 is opened, will
The substrate that deposition has perovskite thin film is sent to substrate by transmitting device 22 and takes out taking-up, substrate after section, the natural cooling of substrate 9
Electron transfer layer PCBM is deposited on 9；
（10）Evaporation metal conductive layer Au electrodes, obtain thin film field-effect pipe.
Preferred embodiment of the present utility model is the foregoing is only, it is all at this not to limit the utility model
Any modifications, equivalent substitutions and improvements made within the spirit and principle of utility model etc., should be included in the utility model
Protection domain within.
Claims (5)
1. a kind of former of calcium titanium ore bed film, it is characterised in that including tubular housing and conveyer, the transmission dress
Put and be arranged in tubular housing, substrate approach section is respectively arranged with before and after the tubular housing and substrate takes out section, the pipe
Shape cavity is respectively arranged with some deposit cavities and/or adapter cavity and/or anneal chamber, and placement deposition is provided with the deposit cavity
The objective table of reactant, is provided with the objective table for placing annealing secondary solvent in the anneal chamber, the deposit cavity and is moving back
Barometric control unit and heater are also set respectively in fiery chamber, and the heater is respectively to the deposition reactant in objective table
Heated with annealing secondary solvent, its gas particles is deposited to after the deposition reactant and annealing secondary solvent heating evaporation
Positioned at film to be deposited in the chamber substrate surface on, be utilized respectively between adjacent segment and chamber and each chamber every
Plate is separated；The substrate of film to be deposited is placed on frame substrate, is conveyed by conveyer.
2. the former of calcium titanium ore bed film as claimed in claim 1, it is characterised in that the conveyer includes transmission
Band, the frame substrate is set on a moving belt；The conveyer belt is arranged on the surface of objective table, the face to be deposited of the substrate
Down just to objective table.
3. the former of calcium titanium ore bed film as claimed in claim 2, it is characterised in that set in the middle part of the frame substrate
It is equipped with the middle part of the groove for placing substrate, the groove and is provided with recess hole, the groove is slightly larger than substrate, the recess hole is omited
Less than the surface to be deposited of substrate, it is used on the both sides of the frame substrate equipped with transversely movable movable substrate fixed plate solid
Determine the position of substrate, the substrate fixed plate is fixed on the back side of substrate.
4. the former of calcium titanium ore bed film as claimed in claim 1, it is characterised in that set on the objective table top
There are split-flow baffles, multiple tap holes are provided with the split-flow baffles, the reactant gas of the objective table evaporation is through undue
Substrate surface is reached again after stream dividing plate.
5. the former of calcium titanium ore bed film as claimed in claim 1, it is characterised in that the heater includes being located at
The upper heating plate of deposit cavity and lower heating plate, and upper heating plate and lower heating plate positioned at anneal chamber, the deposit cavity it is upper
The upper heating plate of heating plate and anneal chamber is respectively to the substrate heating on frame substrate, the lower heating plate and anneal chamber of the deposit cavity
Lower heating plate respectively to the deposition reactant in the objective table of place chamber and annealing secondary solvent heated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201620939493.XU CN206408291U (en) | 2016-08-25 | 2016-08-25 | A kind of former of calcium titanium ore bed film and its application |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201620939493.XU CN206408291U (en) | 2016-08-25 | 2016-08-25 | A kind of former of calcium titanium ore bed film and its application |
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| CN206408291U true CN206408291U (en) | 2017-08-15 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109904327A (en) * | 2017-12-07 | 2019-06-18 | 中国科学院大连化学物理研究所 | A kind of cluster formula vacuum deposition system being used to prepare perovskite solar battery |
| CN110047998A (en) * | 2018-01-17 | 2019-07-23 | 杭州纤纳光电科技有限公司 | A kind of immersion prepares the equipment and application method of perovskite solar battery |
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2016
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109904327A (en) * | 2017-12-07 | 2019-06-18 | 中国科学院大连化学物理研究所 | A kind of cluster formula vacuum deposition system being used to prepare perovskite solar battery |
| CN110047998A (en) * | 2018-01-17 | 2019-07-23 | 杭州纤纳光电科技有限公司 | A kind of immersion prepares the equipment and application method of perovskite solar battery |
| CN110047998B (en) * | 2018-01-17 | 2023-09-26 | 杭州纤纳光电科技有限公司 | Device for preparing perovskite solar cell in immersion mode and use method |
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