CN103700768B - A kind of perovskite structure solaode and preparation method thereof - Google Patents

A kind of perovskite structure solaode and preparation method thereof Download PDF

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CN103700768B
CN103700768B CN201310650505.8A CN201310650505A CN103700768B CN 103700768 B CN103700768 B CN 103700768B CN 201310650505 A CN201310650505 A CN 201310650505A CN 103700768 B CN103700768 B CN 103700768B
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perovskite structure
solaode
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CN103700768A (en
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袁宁
袁宁一
董旭
丁建宁
胡宏伟
房香
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Changzhou University
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/40—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising a p-i-n structure, e.g. having a perovskite absorber between p-type and n-type charge transport layers
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/16—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering
    • H10K71/164—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering using vacuum deposition
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • 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
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K2102/00—Constructional details relating to the organic devices covered by this subclass
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    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract

The present invention relates to solaode, refer in particular to a kind of perovskite structure solaode and preparation method thereof.First it is the SnO in doped with fluorine2(FTO) electro-conductive glass first deposits one layer of titanium oxide or zinc oxide n-layer, then redeposited one layer of hydridization perovskite structure CH3NH3PbI3, then depositing p-type silicon thin film, last deposit metal electrodes layer；Wherein, zinc oxide or titanium oxide layer utilize Atomic layer deposition method to prepare, and the method can prepare the finest and close oxide, and thickness can accurately control；The CH of perovskite structure3NH3PbI3Can be prepared by solwution method or coevaporation method；P-type silicon thin film can be prepared by plasma activated chemical vapour deposition method；Metal electrode can be prepared by thermal evaporation or sputtering method, it is characterised in that utilizes p-type silicon thin film to replace spiro-OMeTAD organic p-type layer, low cost, easily realizes large area and produces, can improve the stability of battery.

Description

A kind of perovskite structure solaode and preparation method thereof
Technical field
The present invention relates to solaode, refer in particular to a kind of perovskite structure solaode and preparation method thereof.
Background technology
Now use the DSSC (DSC) of liquid electrolyte although efficiency reached 12% 【A.Yella, et al. Porphyrin-sensitized solar cells with cobalt (II/III)-based Redox electrolyte exceed 12 percent efficiency, Science, 2011,334,629 634], but The electrolyte of this kind of DSC is susceptible to leakage；To this end, solid-state sensitization solar battery has obtained studying widely, such as CsSnI3 Photoelectric transformation efficiency as solid-state DSCs of hole conductor has reached 8.5%[Chung, I.et al. All-solid- State dye-sensitized solar cells with high efficiency, Nature, 2012,485:486 489], but its efficiency is still below liquid electrolyte DSCs；Recently, a kind of novel organic inorganic hybridization perovskite structure battery obtains Breakthrough progress, efficiency exceeded liquid DSC；This novel organic inorganic hybridization perovskite battery structure is, at FTO glass Layer of titanium dioxide (TiO is grown on glass2, n type quasiconductor), deposit the CH of perovskite structure the most thereon3NH3PbI3, then Spin coating one layer 2,2', 7,7'-tetra-[N, N-bis-(4-methoxyphenyl) amino]-9, (spiro-OMeTAD, p-type has 9'-spiral shell two fluorenes Machine hole conductor), finally one layer of gold (Au) electrode of vacuum evaporation, form p-i-n structure battery, as it is shown in figure 1, such battery effect Rate has broken through 15%[Julian Burschka, Norman Pellet, et al. Sequential depositionas a route tohigh-performance perovskite-sensitized solar cells.nature,2013, 499, 316–319；Mingzhen Liu. Michael B. Johnston & Henry J. Snaith. Efficient planar heterojunction perovskite solar cells by vapour deposition. Nature,501,395– 398.], it is up to now, except silicon solar cell, the solaode that efficiency is the highest, but spiro-OMeTAD price Height, gold electrode price thereon is the highest.
Summary of the invention
For the problem existing for the p-i-n hydridization perovskite battery in background technology, the present invention proposes a kind of new knot Structure and preparation method, be first the SnO in doped with fluorine2(FTO) electro-conductive glass first deposits one layer of titanium oxide or zinc oxide n-layer, Then redeposited one layer of hydridization perovskite structure CH3NH3PbI3, then depositing p-type silicon thin film, last deposit metal electrodes layer；Its In, zinc oxide (ZnO) or titanium oxide (TiO2) layer utilizes ald (ALD) method to prepare, the method can be prepared non- The oxide of Chang Zhimi, and thickness can accurately control；The CH of perovskite structure3NH3PbI3Solwution method or common steaming can be passed through Prepared by forwarding method；P-type silicon thin film can be prepared by plasma activated chemical vapour deposition (PECVD) method；Metal electrode is permissible Being prepared by thermal evaporation or sputtering method, its feature is to utilize p-type silicon thin film to replace spiro-OMeTAD organic p-type layer, and one Being low cost, two is easily to realize large area to produce, and three is the stability improving battery.
A kind of perovskite structure solaode, described solaode sequentially consists of FTO conductive glass layer, n Type layer, the CH of hydridization perovskite structure3NH3PbI3Layer, P-type layer and metal electrode, it is characterised in that；Described P-type layer is p-type silicon Thin film.
Described n-layer is titanium oxide or zinc oxide film, and thickness is 5-15nm.
The square resistance of described FTO conductive glass layer is 10-15 Ω, and transmitance is at 78-83%.
The CH of described perovskite structure3NH3PbI3The thickness of layer is 300-500nm.
The thickness of described p-type silicon thin film is 5-15nm.
Described metal electrode is Al electrode, and thickness is 100nm.
The preparation method of a kind of perovskite structure solaode, is included in the step of FTO electro-conductive glass elder generation depositing n-type layer Suddenly, in n-layer, one layer of hydridization perovskite structure CH is prepared the most again3NH3PbI3Step, then at hydridization perovskite structure CH3NH3PbI3The step of depositing p-type layer on layer, the finally step of deposit metal electrodes layer in p-type layer；It is characterized in that: logical Cross plasma activated chemical vapour deposition method and prepare p-type layer.
CH3NH3PbI3Hybrid perovskite is combined organic component in an orderly manner by two-dimensional orientation inorganic framework On a unimolecule, organic polymer is embedded in inorganic material framework；Owing to having organic amine in calcium titanium ore bed structure, it is resistance to Hot temperature ratio is relatively low, and the stability of structure is relatively poor, therefore on depositing p-type silicon, and low temperature deposition process to be used, and etc. Gas ions power is low.
Described prepared p-type layer by plasma activated chemical vapour deposition method technological parameter be: depositing temperature 70- 90oC, radio-frequency power is 15-30W, the doping ratio 0.5-2% of boron.
Described zinc oxide or titanium oxide layer utilize Atomic layer deposition method to prepare, and the method can be prepared the finest and close Oxide, and thickness can accurately control.
The CH of described perovskite structure3NH3PbI3Layer is prepared by solwution method or coevaporation method.
Described metal electrode is prepared by thermal evaporation or sputtering method.
Realization the technical scheme is that
Selecting square resistance is 10-15 Ω, transmitance at the FTO glass of 78-83% as backing material.
1, ZnO or TiO thick for ALD method deposition 5-15nm is utilized2Layer.
2, CH thick for solution methods deposition 300-500nm is utilized3NH3PbI3Layer.
3, PECVD method is utilized to prepare the thick p-type Si layer of 5-15nm.
4, thermal evaporation method is utilized to prepare the thick aluminium lamination of 100nm.
Accompanying drawing explanation
Fig. 1 is hybrid perovskite solar battery structure figure.
Detailed description of the invention
Embodiment 1
1, select square resistance be 10 Ω, transmitance 80% FTO glass as backing material.
2, ALD technique is utilized to grow the thick ZnO layer of 10 nm
Sedimentary condition: reaction temperature 200 DEG C, is passed through Zn (CH at reaction chamber2CH3)2(DEZ) 1 s, nitrogen cleans 1.5 S, water flowing 500 ms, nitrogen cleans 1s, repeats said process 100 times.
3、CH3NH3PbI3The preparation of calcium titanium ore bed
(1) CH3NH3I aqueous isopropanol is prepared
By fill 20ml methylamine round-bottomed flask place in the frozen water of 0 DEG C, dropping limit, 22ml hydroiodic acid limit is stirred into In flask, continue after being added dropwise to complete ice-water bath stirs 2h, form water white CH3NH3I solution；Solution rotary evaporator Dry, then use ether washes clean, obtain the CH of white3NH3I crystal, by quantitative CH3NH3I crystal is dissolved in isopropanol, Solution concentration is 10mg/ml.
(2) PbI2The outfit of solution
By appropriate faint yellow PbI2Powder is added to DMF(N.N-dimethylformamide in ice-water bath) in, then heat To 70 DEG C by PbI2Powder dissolves, and obtains faint yellow PbI2Solution, solution concentration is 1mol/L.
(3) PbI2The preparation of film
In glove box, by faint yellow PbI2Solution is spun to TiO2On compacted zone, dry 10min at 70 DEG C, obtain glassy yellow PbI2Layer.
(4) CH is completed3NH3PbI3The preparation of calcium titanium ore bed
Then the substrate having been spun on is immersed in CH3NH320s in I solution, base color is rapidly from bright orange complexion changed For brownish black, it is put into after taking-up in clean isopropanol, washes away unnecessary CH3NH3I, is finally placed in 70 DEG C baking 10min, It is the CH of 400nm to thickness3NH3PbI3Calcium titanium ore bed.
4, PECVD is utilized to grow one layer of 10 p-type silicon layer thick for nm
Silane used is the silane that hydrogen dilution is crossed, wherein SiH4/SiH4+H2Ratio be 5 %, borine is that hydrogen dilution is crossed Borine, [B2H6]/ [B2H6+ H2] ratio be 0.5 %.
Growth conditions: silane flow rate 10 sccm of hydrogen dilution, borine flow 1 sccm of hydrogen dilution, hydrogen flowing quantity 50 Sccm, radio-frequency power 15 W, growth temperature 70 DEG C, growth time 15min.
5, aluminum film thick for thermal evaporation method deposition 100nm is utilized.
Base vacuum 110-4Pa, heats electrode current 40A.
Implementation result: finally carry out the performance test of battery, at AM1.5,100mW/cm2Under the irradiation of etalon optical power, too Open-circuit voltage 0.98 V, short circuit current 8.7 mA of sun battery sample, fill factor, curve factor 0.65, efficiency is 5.54 %.
Embodiment 2
1, select square resistance be 15 Ω, transmitance 83% FTO glass as backing material.
2, ALD technique is utilized to grow the thick TiO of 10 nm2Layer
Water and titanium tetraisopropylate, as source, grow the thick fine and close TiO2 layer of 10nm in substrate；Growth technique is: titanium source Heating-up temperature 70 DEG C, chamber reaction temperature 270 DEG C.Logical titanium source 1s, nitrogen purging 5s, water flowing vapour 200ms, nitrogen purging 2s, complete Become a circulation, need 160 circulations altogether.
3, coevaporation prepares CH3NH3PbI3Calcium titanium ore bed
By 10mg CH3NH3I crystal and 10 mgPbI powder are respectively put in two tungsten boats, heat to two tungsten boats simultaneously, Base vacuum 110-4Pa, heating electrode current is 25A, at TiO2The thick CH of 500nm is deposited on layer3NH3PbI3Calcium titanium ore bed； Substrate heating temperature 80oC, sedimentation time 10 min.
4, PECVD is utilized to grow one layer of 10 p-type silicon layer thick for nm
Silane used is the silane that hydrogen dilution is crossed, wherein SiH4/SiH4+H2Ratio be 5 %, borine is that hydrogen dilution is crossed Borine, [B2H6]/ [B2H6+ H2] ratio be 0.5 %.
Growth conditions: silane flow rate 10 sccm of hydrogen dilution, borine flow 1 sccm of hydrogen dilution, hydrogen flowing quantity 50 Sccm, radio-frequency power 20 W, growth temperature 80 DEG C, growth time 10min.
5, aluminum film thick for thermal evaporation method deposition 100nm is utilized.
Base vacuum 110-4Pa, heats electrode current 40A.
Implementation result: finally carry out the performance test of battery, at AM1.5,100mW/cm2Under the irradiation of etalon optical power, too Open-circuit voltage 0.95 V, short circuit current 11.5 mA of sun battery sample, fill factor, curve factor 0.69, efficiency is 7.53 %.

Claims (10)

1. a perovskite structure solaode, described solaode sequentially consists of FTO conductive glass layer, N-shaped Layer, the CH of hydridization perovskite structure3NH3PbI3Layer, P-type layer and metal electrode, it is characterised in that；Described P-type layer is that p-type silicon is thin Film.
2. a kind of perovskite structure solaode as claimed in claim 1, it is characterised in that: described n-layer is oxidation Titanium or zinc oxide film, thickness is 5-15nm.
3. a kind of perovskite structure solaode as claimed in claim 1, it is characterised in that: described FTO electro-conductive glass The square resistance of layer is 10-15 Ω, and transmitance is at 78-83%.
4. a kind of perovskite structure solaode as claimed in claim 1, it is characterised in that: described perovskite structure CH3NH3PbI3The thickness of layer is 300-500nm.
5. a kind of perovskite structure solaode as claimed in claim 1, it is characterised in that: the layer of described p-type silicon thin film Thickness is 5-15nm.
6. a kind of perovskite structure solaode as claimed in claim 1, it is characterised in that: described metal electrode is Al electricity Pole, thickness is 100nm.
The preparation method of a kind of perovskite structure solaode the most as claimed in claim 1, is included in FTO electro-conductive glass first The step of depositing n-type layer, prepares one layer of hydridization perovskite structure CH the most again in n-layer3NH3PbI3Step, then miscellaneous Change perovskite structure CH3NH3PbI3The step of depositing p-type layer on layer, the finally step of deposit metal electrodes layer in p-type layer；Its It is characterized by plasma activated chemical vapour deposition method and prepares p-type layer.
The preparation method of a kind of perovskite structure solaode the most as claimed in claim 7, it is characterised in that: described is logical Cross plasma activated chemical vapour deposition method and prepare the technological parameter of p-type layer and be: depositing temperature 70-90 DEG C, radio-frequency power is 15- 30W, the doping ratio 0.5-2% of boron.
The preparation method of a kind of perovskite structure solaode the most as claimed in claim 7, it is characterised in that: described n Type layer utilizes Atomic layer deposition method to prepare, and the method can prepare the finest and close oxide, and thickness can be accurate Control.
The preparation method of a kind of perovskite structure solaode the most as claimed in claim 7, it is characterised in that: described The CH of perovskite structure3NH3PbI3Layer is prepared by solwution method or coevaporation method；Described metal electrode by thermal evaporation or Prepared by sputtering method.
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