CN110010768A - (004) application and perovskite preparation method of solar battery of the titanium dioxide of crystal face preferentially in perovskite solar battery - Google Patents
(004) application and perovskite preparation method of solar battery of the titanium dioxide of crystal face preferentially in perovskite solar battery Download PDFInfo
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- CN110010768A CN110010768A CN201910305545.6A CN201910305545A CN110010768A CN 110010768 A CN110010768 A CN 110010768A CN 201910305545 A CN201910305545 A CN 201910305545A CN 110010768 A CN110010768 A CN 110010768A
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- titanic oxide
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- solar battery
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 239000013078 crystal Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 22
- 239000010936 titanium Substances 0.000 claims abstract description 21
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 18
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 42
- 238000000137 annealing Methods 0.000 claims description 38
- -1 ammonia lead iodine Chemical compound 0.000 claims description 33
- 239000011521 glass Substances 0.000 claims description 25
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 24
- 229910052786 argon Inorganic materials 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 16
- QEZYDNSACGFLIC-UHFFFAOYSA-N CN.[I] Chemical compound CN.[I] QEZYDNSACGFLIC-UHFFFAOYSA-N 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 14
- 239000002184 metal Substances 0.000 claims description 14
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 9
- 230000005525 hole transport Effects 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000000151 deposition Methods 0.000 claims description 8
- 230000008021 deposition Effects 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 8
- 239000010931 gold Substances 0.000 claims description 8
- 229910052737 gold Inorganic materials 0.000 claims description 8
- 238000002207 thermal evaporation Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 230000005611 electricity Effects 0.000 claims description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 2
- 229910052740 iodine Inorganic materials 0.000 claims description 2
- 239000011630 iodine Substances 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- GPESMPPJGWJWNL-UHFFFAOYSA-N azane;lead Chemical compound N.[Pb] GPESMPPJGWJWNL-UHFFFAOYSA-N 0.000 claims 1
- 238000004506 ultrasonic cleaning Methods 0.000 claims 1
- 238000004544 sputter deposition Methods 0.000 abstract description 20
- 239000000758 substrate Substances 0.000 description 26
- 238000004528 spin coating Methods 0.000 description 18
- 230000027756 respiratory electron transport chain Effects 0.000 description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 12
- 239000001301 oxygen Substances 0.000 description 12
- 229910052760 oxygen Inorganic materials 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 9
- 230000005540 biological transmission Effects 0.000 description 7
- 229910021529 ammonia Inorganic materials 0.000 description 6
- DXZHSXGZOSIEBM-UHFFFAOYSA-M iodolead Chemical compound [Pb]I DXZHSXGZOSIEBM-UHFFFAOYSA-M 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 239000012495 reaction gas Substances 0.000 description 6
- 238000004062 sedimentation Methods 0.000 description 6
- 238000005477 sputtering target Methods 0.000 description 6
- 239000013077 target material Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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Abstract
The present invention relates to the preparation methods of application and perovskite solar battery of the titanium dioxide in perovskite solar battery of a kind of (004) crystal face preferentially, belong to perovskite area of solar cell.The present invention obtains the titanic oxide electronic transport layer with different crystal structure and preferred orientation, realizes the controllable of titanic oxide electronic transport layer crystal structure and preferred orientation by the power density of titanium target surface magnetic control sputtering in control magnetron sputtering process.
Description
Technical field
The present invention relates to application and calcium titanium of the titanium dioxide in perovskite solar battery of a kind of (004) crystal face preferentially
The preparation method of mine solar battery belongs to perovskite area of solar cell.
Background technique
Kojima et al. has been prepared for the first time in 2009 and has been utilized CH3NH3PbI3And CH3NH3PbBr3Liquid as dyestuff
Electrolytic calcium ion test titanium ore solar battery, photoelectric conversion efficiency have reached 3.8%.However, the liquid electrolyte in battery can pole
Perovskite material is easily decomposed, the service life so as to cause battery is considerably reduced.Therefore, after further improving, Yang etc.
The all solid state perovskite solar battery that photoelectric conversion efficiency is 22% has successfully been prepared in 2016, has been achieved great prominent
It is broken.Such battery is mainly by FTO electro-conductive glass, compact titanium dioxide layer, porous silica titanium layer, perovskite, hole transport material
Material and metal electrode are constituted.Wherein, compact titanium dioxide layer functions as electron transfer layer.Compact titanium dioxide electricity
Sub- transport layer also plays the role of stopping hole, at this point, its high compactness is particularly important.This is because titanic oxide electronic transport layer
It is finer and close, it can the more effective physical contact stopped between light absorbing layer and electrode, so as to reduce interface charge
Charge caused by compound and energy loss, finally improve photoelectric conversion efficiency.Compact titanium dioxide layer is selected both electronics to be used as to pass
Defeated layer is used as hole blocking layer again to improve above situation, and this simple novel battery of structure is referred to as planar heterojunction calcium titanium
Mine solar battery.In planar heterojunction perovskite solar battery, titanic oxide electronic transport layer is the key that battery portion
Point, electron transfer efficiency directly affects the photoelectric conversion efficiency of battery.Since the electron transfer efficiency of crystalline titania is excellent
In the electron transfer efficiency of amorphous titanium dioxide, and in three kinds of common crystal forms of crystalline titania, the electricity of Anatase
Sub- transport efficiency is better than other two kinds, therefore how to prepare more excellent performance, electron transfer efficiency preferably fine and close rutile titania
Mine phase titanic oxide electron transfer layer is very important for preparing the perovskite solar battery of high-photoelectric transformation efficiency.
Although the preparation of current perovskite solar battery achieves significant progress, most of researchs are all using rotation
Coating prepares titanic oxide electronic transport layer, and only a few studies attempt to use other methods and prepare titanic oxide electronic biography at present
Defeated layer, and the transformation efficiency that other methods prepare the perovskite solar battery of titanic oxide electronic transport layer lags far behind in fact
The 22% of room is tested, which reflects serious problems.
Summary of the invention
The present invention obtains the anatase phase titanium dioxide electron transfer layer of (004) crystal face preferentially by post annealed, generates
It is parallel to the titanium dioxide column crystal of anatase phase titanium dioxide electron transfer layer normal direction, it is therefore, prepared by the present invention
(004) the anatase phase titanium dioxide electron transfer layer of crystal face preferentially has the characteristics that electron-transport is high-efficient, solves above-mentioned
Problem.
The present invention provides a kind of application of the titanium dioxide in perovskite solar battery of (004) crystal face preferentially.
Another object of the present invention is a kind of preparation method of perovskite solar battery is provided, the preparation method includes such as
Lower step: using magnetron sputtering method at room temperature, with high pure metal titanium target, obtained on FTO transparent conducting glass
Amorphous titanic oxide electronic transport layer, the power density of the magnetron sputtering are 0.8-3.3W/cm2;Amorphous dioxy will be deposited with
The FTO transparent conducting glass for changing titanium electron transfer layer carries out 450-550 DEG C of annealing under air conditions, is had (004) brilliant
The titanic oxide electronic transport layer of the Anatase polycrystalline structure of face preferentially;Methylamine iodine and lead iodide are dissolved in equimolar ratio
First ammonia lead iodine solution is formed in n,N-Dimethylformamide, the total mass fraction of methylamine iodine and lead iodide is in first ammonia lead iodine solution
First ammonia lead iodine solution is spin-coated on the titanium dioxide with the Anatase polycrystalline structure of (004) crystal face preferentially by 20-40wt.%
On electron transfer layer, 90-120 DEG C of annealing 15-60min is cooled to room temperature, and obtains first ammonia lead iodine layer;Hole mobile material is revolved
It is coated on first ammonia lead iodine layer, then secretly sets 12-36h under a nitrogen atmosphere, obtain hole transmission layer;Using thermal evaporation in hole
Deposition thickness is the gold electrode of 100-300nm in transport layer.
The present invention is preferably the FTO transparent conducting glass using preceding successively clear with acetone, ethyl alcohol, deionized water ultrasound
It washes.
When the present invention preferably prepares amorphous titanic oxide electronic transport layer using magnetron sputtering, working gas is high-purity argon
With high pure oxygen.
The present invention is preferably the amorphous titanic oxide electronic transport layer for utilizing magnetron sputtering to prepare with a thickness of 50-300nm.
When the present invention preferably prepares amorphous titanic oxide electronic transport layer using magnetron sputtering, annealing time is greater than
30min。
The invention has the following beneficial effects:
The present invention obtains having the not isomorphous by the power density of titanium target surface magnetic control sputtering in control magnetron sputtering process
The titanic oxide electronic transport layer of body structure and preferred orientation realizes titanic oxide electronic transport layer crystal structure and preferentially takes
To it is controllable.
The working gas that magnetron sputtering of the present invention prepares titanic oxide electronic transport layer is high-purity argon and high pure oxygen, to environment
It is pollution-free.
Preparation method of the present invention is simple, at low cost, yield is high, is convenient for large-scale industrial production.
Detailed description of the invention
2 width of attached drawing of the present invention,
Fig. 1 is the X ray diffracting spectrum in embodiment 1-4, comparative example 1-2 before the annealing of titanic oxide electronic transport layer;
Fig. 2 is the X ray diffracting spectrum in embodiment 1-4, comparative example 1-2 after the annealing of titanic oxide electronic transport layer.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Embodiment 1
A kind of preparation method of perovskite solar battery, the preparation method include the following steps:
FTO transparent conducting glass is successively cleaned by ultrasonic with acetone, ethyl alcohol, deionized water using preceding;
Using DC pulse reaction magnetocontrol sputtering method at room temperature using FTO transparent conducting glass as base material,
With high pure metal titanium target (99.99%) for sputtering target material, with high-purity argon (99.99%) for sputter gas, with high pure oxygen
(99.99%) it is reaction gas, carries out argon/oxygen cosputtering mode and prepare titanic oxide electronic transport layer, obtained titanium dioxide
Electron transport layer thickness is 300nm, and crystal structure is non crystalline structure, as shown in Figure 1;
Wherein: DC pulse shielding power supply working frequency is 200kHz, and metal titanium targets surface Sputtering power density is
0.8W/cm2, argon flow is 20sccm, and oxygen flow 4sccm, back end vacuum degree is 3.0 × 10-3Pa, sputtering vacuum degree are
0.7Pa, sedimentation time 605min;
The FTO transparent conducting glass of amorphous titanic oxide electronic transport layer will be deposited under air conditions using Muffle furnace
It anneals, annealing temperature is 500 DEG C, annealing time 60min, and the titanic oxide electronic transport layer crystal structure after annealing is
Anatase phase titanium dioxide structure, the titanic oxide electronic transport layer after annealing are in Anatase (004) Solute Content in Grain, such as
Shown in Fig. 2;
In glove box, methylamine iodine and lead iodide are dissolved in formation first ammonia in n,N-Dimethylformamide with equimolar ratio
Lead iodine solution, the total mass fraction of methylamine iodine and lead iodide is 40wt.% in first ammonia lead iodine solution, first will be above-mentioned using sol evenning machine
Substrate is rotated to 1500rpm, and first ammonia lead iodine solution is added dropwise in two with the Anatase polycrystalline structure of (004) crystal face preferentially
On titanium oxide electron transfer layer, then spin coating machine speed is adjusted to 5000rpm, spin coating 30s removes substrate, places the substrates in 100
DEG C warm table on make annealing treatment 45min, be cooled to room temperature, obtain first ammonia lead iodine layer;
In glove box, first above-mentioned substrate is rotated to 3000rpm using sol evenning machine, hole mobile material is added dropwise in first
On ammonia lead iodine layer, then spin coating 30s secretly sets for 24 hours in the glove box full of nitrogen, obtains hole transmission layer;
Use thermal evaporation on the hole transport layer deposition thickness for the gold electrode of 100nm.
Embodiment 2
A kind of preparation method of perovskite solar battery, the preparation method include the following steps:
FTO transparent conducting glass is successively cleaned by ultrasonic with acetone, ethyl alcohol, deionized water using preceding;
Using Radiofrequency muti-hook probe method at room temperature using FTO transparent conducting glass as base material, with height
Pure metal titanium target (99.99%) is sputtering target material, with high-purity argon (99.99%) for sputter gas, with high pure oxygen (99.99%)
For reaction gas, carries out argon/oxygen cosputtering mode and prepare titanic oxide electronic transport layer, obtained titanic oxide electronic transport layer
With a thickness of 200nm, crystal structure is non crystalline structure, as shown in Figure 1;
Wherein: radio-frequency power supply working frequency is 13.56MHz, and metal titanium targets surface Sputtering power density is 1.7W/cm2, argon
Flow is 20sccm, and oxygen flow 4sccm, back end vacuum degree is 3.0 × 10-3Pa, sputtering vacuum degree are 0.6Pa, sedimentation time
For 140min;
The FTO transparent conducting glass of amorphous titanic oxide electronic transport layer will be deposited under air conditions using tube furnace
It anneals, annealing temperature is 450 DEG C, annealing time 50min, and the titanic oxide electronic transport layer crystal structure after annealing is
Anatase phase titanium dioxide structure, the titanic oxide electronic transport layer after annealing are in Anatase (004) Solute Content in Grain, such as
Shown in Fig. 2;
In glove box, methylamine iodine and lead iodide are dissolved in formation first ammonia in n,N-Dimethylformamide with equimolar ratio
Lead iodine solution, the total mass fraction of methylamine iodine and lead iodide is 30wt.% in first ammonia lead iodine solution, first will be above-mentioned using sol evenning machine
Substrate is rotated to 1500rpm, and first ammonia lead iodine solution is added dropwise in two with the Anatase polycrystalline structure of (004) crystal face preferentially
On titanium oxide electron transfer layer, then spin coating machine speed is adjusted to 5000rpm, spin coating 30s removes substrate, places the substrates in 100
DEG C warm table on make annealing treatment 45min, be cooled to room temperature, obtain first ammonia lead iodine layer;
In glove box, first above-mentioned substrate is rotated to 3000rpm using sol evenning machine, hole mobile material is added dropwise in first
On ammonia lead iodine layer, then spin coating 30s secretly sets for 24 hours in the glove box full of nitrogen, obtains hole transmission layer;
Use thermal evaporation on the hole transport layer deposition thickness for the gold electrode of 100nm.
Embodiment 3
A kind of preparation method of perovskite solar battery, the preparation method include the following steps:
FTO transparent conducting glass is successively cleaned by ultrasonic with acetone, ethyl alcohol, deionized water using preceding;
Using DC pulse reaction magnetocontrol sputtering method at room temperature using FTO transparent conducting glass as base material,
With high pure metal titanium target (99.99%) for sputtering target material, with high-purity argon (99.99%) for sputter gas, with high pure oxygen
(99.99%) it is reaction gas, carries out argon/oxygen cosputtering mode and prepare titanic oxide electronic transport layer, obtained titanium dioxide
Electron transport layer thickness is 100nm, and crystal structure is non crystalline structure, as shown in Figure 1;
Wherein: DC pulse shielding power supply working frequency is 200kHz, and metal titanium targets surface Sputtering power density is
2.5W/cm2, argon flow is 20sccm, and oxygen flow 4sccm, back end vacuum degree is 3.0 × 10-3Pa, sputtering vacuum degree are
0.6Pa, sedimentation time 50min;
The FTO transparent conducting glass of amorphous titanic oxide electronic transport layer will be deposited under air conditions using tube furnace
It anneals, annealing temperature is 550 DEG C, annealing time 40min, and the titanic oxide electronic transport layer crystal structure after annealing is
Anatase phase titanium dioxide structure, the titanic oxide electronic transport layer after annealing are in Anatase (004) Solute Content in Grain, such as
Shown in Fig. 2;
In glove box, methylamine iodine and lead iodide are dissolved in formation first ammonia in n,N-Dimethylformamide with equimolar ratio
Lead iodine solution, the total mass fraction of methylamine iodine and lead iodide is 20wt.% in first ammonia lead iodine solution, first will be above-mentioned using sol evenning machine
Substrate is rotated to 1500rpm, and first ammonia lead iodine solution is added dropwise in two with the Anatase polycrystalline structure of (004) crystal face preferentially
On titanium oxide electron transfer layer, then spin coating machine speed is adjusted to 5000rpm, spin coating 30s removes substrate, places the substrates in 100
DEG C warm table on make annealing treatment 45min, be cooled to room temperature, obtain first ammonia lead iodine layer;
In glove box, first above-mentioned substrate is rotated to 3000rpm using sol evenning machine, hole mobile material is added dropwise in first
On ammonia lead iodine layer, then spin coating 30s secretly sets for 24 hours in the glove box full of nitrogen, obtains hole transmission layer;
Use thermal evaporation on the hole transport layer deposition thickness for the gold electrode of 100nm.
Embodiment 4
A kind of preparation method of perovskite solar battery, the preparation method include the following steps:
FTO transparent conducting glass is successively cleaned by ultrasonic with acetone, ethyl alcohol, deionized water using preceding;
Using high power DC pulse reaction magnetocontrol sputtering method at room temperature using FTO transparent conducting glass as substrate
Material, with high pure metal titanium target (99.99%) for sputtering target material, with high-purity argon (99.99%) for sputter gas, with high pure oxygen
(99.99%) it is reaction gas, carries out argon/oxygen cosputtering mode and prepare titanic oxide electronic transport layer, obtained titanium dioxide
Electron transport layer thickness is 50nm, and crystal structure is non crystalline structure, as shown in Figure 1;
Wherein: DC pulse shielding power supply working frequency is 100kHz, and Ti target surface sputtering power density is
0.8W/cm2, Ti target surface pulse power density is 2.5W/cm2, i.e. Ti target total surface Sputtering power density is 3.3W/cm2, argon
Flow is 20sccm, and oxygen flow 4sccm, back end vacuum degree is 3.0 × 10-3Pa, sputtering vacuum degree are 0.6Pa, sedimentation time
For 11min;
The FTO transparent conducting glass of amorphous titanic oxide electronic transport layer will be deposited under air conditions using tube furnace
It anneals, annealing temperature is 500 DEG C, annealing time 30min, and the titanic oxide electronic transport layer crystal structure after annealing is
Anatase phase titanium dioxide structure, the titanic oxide electronic transport layer after annealing are in Anatase (004) Solute Content in Grain, such as
Shown in Fig. 2;
In glove box, methylamine iodine and lead iodide are dissolved in formation first ammonia in n,N-Dimethylformamide with equimolar ratio
Lead iodine solution, the total mass fraction of methylamine iodine and lead iodide is 40wt.% in first ammonia lead iodine solution, first will be above-mentioned using sol evenning machine
Substrate is rotated to 1500rpm, and first ammonia lead iodine solution is added dropwise in two with the Anatase polycrystalline structure of (004) crystal face preferentially
On titanium oxide electron transfer layer, then spin coating machine speed is adjusted to 5000rpm, spin coating 30s removes substrate, places the substrates in 100
DEG C warm table on make annealing treatment 45min, be cooled to room temperature, obtain first ammonia lead iodine layer;
In glove box, first above-mentioned substrate is rotated to 3000rpm using sol evenning machine, hole mobile material is added dropwise in first
On ammonia lead iodine layer, then spin coating 30s secretly sets for 24 hours in the glove box full of nitrogen, obtains hole transmission layer;
Use thermal evaporation on the hole transport layer deposition thickness for the gold electrode of 100nm.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention and not to limit it, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Comparative example 1
A kind of preparation method of perovskite solar battery, the preparation method include the following steps:
FTO transparent conducting glass is successively cleaned by ultrasonic with acetone, ethyl alcohol, deionized water using preceding;
Using DC pulse reaction magnetocontrol sputtering method at room temperature using FTO transparent conducting glass as base material,
With high pure metal titanium target (99.99%) for sputtering target material, with high-purity argon (99.99%) for sputter gas, with high pure oxygen
(99.99%) it is reaction gas, carries out argon/oxygen cosputtering mode and prepare titanic oxide electronic transport layer, obtained titanium dioxide
Electron transport layer thickness is 200nm, and crystal structure is non crystalline structure, as shown in Figure 1;
Wherein: DC pulse shielding power supply working frequency is 200kHz, and metal titanium targets target surface Sputtering power density is
4.2W/cm2, argon flow is 20sccm, and oxygen flow 4sccm, back end vacuum degree is 3.0 × 10-3Pa, sputtering vacuum degree are
0.6Pa, sedimentation time 60min;
The FTO transparent conducting glass of amorphous titanic oxide electronic transport layer will be deposited under air conditions using tube furnace
It anneals, annealing temperature is 500 DEG C, annealing time 50min, and the titanic oxide electronic transport layer crystal structure after annealing is
Anatase phase titanium dioxide structure, the titanic oxide electronic transport layer after annealing are polycrystalline anatase phase titanium dioxide structure, nothing
Solute Content in Grain, as shown in Figure 2;
In glove box, methylamine iodine and lead iodide are dissolved in formation first ammonia in n,N-Dimethylformamide with equimolar ratio
Lead iodine solution, the total mass fraction of methylamine iodine and lead iodide is 40wt.% in first ammonia lead iodine solution, first will be above-mentioned using sol evenning machine
Substrate is rotated to 1500rpm, and first ammonia lead iodine solution is added dropwise in the titanic oxide electronic without Anatase polycrystalline structure preferentially
In transport layer, then spin coating machine speed is adjusted to 5000rpm, spin coating 30s removes substrate, places the substrates in 100 DEG C of warm table
Upper annealing 45min, is cooled to room temperature, and obtains first ammonia lead iodine layer;
In glove box, first above-mentioned substrate is rotated to 3000rpm using sol evenning machine, hole mobile material is added dropwise in first
On ammonia lead iodine layer, then spin coating 30s secretly sets for 24 hours in the glove box full of nitrogen, obtains hole transmission layer;
Use thermal evaporation on the hole transport layer deposition thickness for the gold electrode of 100nm.
Comparative example 2
A kind of preparation method of perovskite solar battery, the preparation method include the following steps:
FTO transparent conducting glass is successively cleaned by ultrasonic with acetone, ethyl alcohol, deionized water using preceding;
Using high power DC pulse reaction magnetocontrol sputtering method at room temperature using FTO transparent conducting glass as substrate
Material, with high pure metal titanium target (99.99%) for sputtering target material, with high-purity argon (99.99%) for sputter gas, with high pure oxygen
(99.99%) it is reaction gas, carries out argon/oxygen cosputtering mode and prepare titanic oxide electronic transport layer, obtained titanium dioxide
Electron transport layer thickness is 300nm, and crystal structure is non crystalline structure, as shown in Figure 1;
Wherein: DC pulse shielding power supply working frequency is 200kHz, and metal titanium targets surface Sputtering power density is
5.0W/cm2, argon flow is 20sccm, and oxygen flow 4sccm, back end vacuum degree is 3.0 × 10-3Pa, sputtering vacuum degree are
0.6Pa, sedimentation time 70min;
The FTO transparent conducting glass of amorphous titanic oxide electronic transport layer will be deposited under air conditions using tube furnace
It anneals, annealing temperature is 500 DEG C, annealing time 50min, and the titanic oxide electronic transport layer crystal structure after annealing is
Anatase phase titanium dioxide structure, the titanic oxide electronic transport layer after annealing are polycrystalline anatase phase titanium dioxide structure, nothing
Solute Content in Grain, as shown in Figure 2;
In glove box, methylamine iodine and lead iodide are dissolved in formation first ammonia in n,N-Dimethylformamide with equimolar ratio
Lead iodine solution, the total mass fraction of methylamine iodine and lead iodide is 40wt.% in first ammonia lead iodine solution, first will be above-mentioned using sol evenning machine
Substrate is rotated to 1500rpm, and first ammonia lead iodine solution is added dropwise in the titanic oxide electronic without Anatase polycrystalline structure preferentially
In transport layer, then spin coating machine speed is adjusted to 5000rpm, spin coating 30s removes substrate, places the substrates in 100 DEG C of warm table
Upper annealing 45min, is cooled to room temperature, and obtains first ammonia lead iodine layer;
In glove box, first above-mentioned substrate is rotated to 3000rpm using sol evenning machine, hole mobile material is added dropwise in first
On ammonia lead iodine layer, then spin coating 30s secretly sets for 24 hours in the glove box full of nitrogen, obtains hole transmission layer;
Use thermal evaporation on the hole transport layer deposition thickness for the gold electrode of 100nm.
Claims (6)
1. (004) application of the titanium dioxide of crystal face preferentially in perovskite solar battery.
2. a kind of preparation method of perovskite solar battery, it is characterised in that: the preparation method includes the following steps:
Using magnetron sputtering method at room temperature, with high pure metal titanium target, obtain amorphous on FTO transparent conducting glass
Titanic oxide electronic transport layer, the power density of the magnetron sputtering are 0.8-3.3W/cm2;
The FTO transparent conducting glass for being deposited with amorphous titanic oxide electronic transport layer is carried out 450-550 DEG C under air conditions
Annealing, is had the titanic oxide electronic transport layer of the Anatase polycrystalline structure of (004) crystal face preferentially;
Methylamine iodine and lead iodide are dissolved in formation first ammonia lead iodine solution, first ammonia lead in n,N-Dimethylformamide with equimolar ratio
The total mass fraction of methylamine iodine and lead iodide is 20-40wt.% in iodine solution, and first ammonia lead iodine solution, which is spin-coated on, has (004)
In the titanic oxide electronic transport layer of the Anatase polycrystalline structure of crystal face preferentially, 90-120 DEG C of annealing 15-60min is cooled to
Room temperature obtains first ammonia lead iodine layer;
Hole mobile material is spin-coated on first ammonia lead iodine layer, 12-36h is then secretly set under a nitrogen atmosphere, obtains hole transport
Layer;
Use thermal evaporation on the hole transport layer deposition thickness for the gold electrode of 100-300nm.
3. preparation method according to claim 2, it is characterised in that: the FTO transparent conducting glass is preceding successively in use
With acetone, ethyl alcohol, deionized water ultrasonic cleaning.
4. preparation method according to claim 3, it is characterised in that: prepare amorphous titanic oxide electronic using magnetron sputtering
When transport layer, working gas is high-purity argon and high pure oxygen.
5. the preparation method according to claim 4, it is characterised in that: utilize the non-crystal titanium dioxide electricity of magnetron sputtering preparation
Sub- transport layer with a thickness of 50-300nm.
6. preparation method according to claim 5, it is characterised in that: prepare amorphous titanic oxide electronic using magnetron sputtering
When transport layer, annealing time is greater than 30min.
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