CN105280827A - Preparation method for perovskite type solar battery - Google Patents

Preparation method for perovskite type solar battery Download PDF

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CN105280827A
CN105280827A CN201510674050.2A CN201510674050A CN105280827A CN 105280827 A CN105280827 A CN 105280827A CN 201510674050 A CN201510674050 A CN 201510674050A CN 105280827 A CN105280827 A CN 105280827A
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CN105280827B (en
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董兵海
胡航
王世敏
陈凤翔
万丽
赵丽
李静
王二静
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Hubei University
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/0001Processes specially adapted for the manufacture or treatment of devices or of parts thereof
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/42Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof specially adapted for sensing infra-red radiation, light, electro-magnetic radiation of shorter wavelength or corpuscular radiation and adapted for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation using organic materials as the active part, or using a combination of organic materials with other material as the active part; Multistep processes for their manufacture
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L2251/00Indexing scheme relating to organic semiconductor devices covered by group H01L51/00
    • H01L2251/30Materials
    • H01L2251/301Inorganic materials
    • H01L2251/303Oxides, e.g. metal oxides
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy
    • Y02E10/549Organic PV cells

Abstract

The invention discloses a preparation method for a perovskite type solar battery, and belongs to the field of optoelectronic materials and devices. The perovskite type solar battery comprises a transparent conducting substrate, a TiO2 electron transporting layer, a perovskite light-absorbing layer, a hole transmission layer and a metal counter electrode layer that are stacked in sequence, wherein the preparation for the electronic transporting layer comprises the steps of step a, providing a transparent substrate material with a clean surface, and depositing a titanium dioxide compact thin film on the surface of the substrate material by adopting an atomic layer depositing technology; step b, depositing a titanium-contained organic-inorganic composite film on the titanium dioxide compact thin film obtained in the step a by adopting a molecular layer depositing technology; and step c, annealing the material obtained in the step b at the temperature of 400-600 DEG C for 0.5-5 hours to obtain the TiO2 electron transporting layer. The TiO2 electron transporting layer provided by the invention is higher in the degree of crystallinity, uniform in film formation and lower in impedance, so that the photo-generated current density is dramatically increased, and the photoelectric converting efficiency and the thermal stability of the devices are greatly improved.

Description

The preparation method of Ca-Ti ore type solar cell
Technical field
The invention belongs to solar cell preparation field, particularly relate to a kind of preparation method of Ca-Ti ore type solar cell.
Background technology
In recent years, in order to solve the increasingly serious energy and environmental problem, people have invested sight in the development and utilization of new forms of energy.In various new energy technology, photovoltaic generation is undoubtedly one of promising direction of most.Although traditional silica-based solar cell achieves industrialization, have comparatively ripe market, its cost performance also cannot be competed with traditional energy mutually, and pollution in manufacture process and energy consumption problem have impact on its extensive use.Therefore, the novel solar battery of research and development high efficiency, low cost is very necessary.In numerous novel solar batteries, perovskite thin film solar cell possesses high photoelectric conversion efficiency because of it, and make the advantages such as material low cost, become the study hotspot got most of the attention in novel solar battery, attracted the concern of numerous researcher, ten big sciences one of are broken through also to be chosen as 2013 by " Science ".The electricity conversion of perovskite thin film solar cell brings up to rapidly 19.3% (by the end of end of the year 2014) through certification from 3.8% within the time of 5 years, and the novel thin film such as DSSC, organic solar batteries solar cell is got rid of after one's death.The research of the aspects such as along with the record of perovskite solar battery efficiency is constantly refreshed, people start the stability more paying close attention to this battery, the preparation of the alternative and large area flexible device of useful life, heavy metal element lead.The principal element of the efficiency and life-span that affect perovskite solar cell is equilibrium carrier transmission between the layers and barrier layer, prevents exciton at the electron transfer layer of electrode interface compound quencher.In the high efficiency perovskite solar cell reported, titanium dioxide is the electron transport layer materials that utilization rate is the highest.But titanium dioxide transport layer prepared by current conventional art is under ultraviolet lighting, and the device that the oxygen molecule desorption on its surface causes is unstable, this large-scale application of perovskite solar cell that will seriously restrict.
Summary of the invention
In order to achieve the above object, the invention provides a kind of TiO 2the preparation method of the Ca-Ti ore type solar cell that electron transfer layer specific area is large, thermal stability is higher, electricity conversion greatly improves.
The invention provides a kind of preparation method of Ca-Ti ore type solar cell, it comprises the transparent conductive substrate, the TiO that stack gradually 2electron transfer layer, perovskite light-absorption layer, hole transmission layer and metal counter electrode layer, wherein, electron transfer layer preparation comprises the following steps:
Step a, provides the non-transparent substrate material of surface cleaning, adopts technique for atomic layer deposition in substrate material surface deposition of titanium oxide dense film;
Step b, the titanium dioxide dense film adopting molecular-layer deposition technology to obtain in step a deposits titaniferous Organic inorganic film;
Step c, the material obtained by step b is annealed 0.5-5h at 400-600 DEG C, obtains TiO 2electron transfer layer.
The beneficial effect of the preparation method of Ca-Ti ore type solar cell provided by the invention is:
(1) the present invention adopts double-layer nanostructured TiO prepared by technique for atomic layer deposition and molecular-layer deposition technology 2film is the dense interconnection network formed by the crystal grain that size is relatively uniform, presents surperficial relative smooth and continuous print pattern, the TiO prepared with traditional sol-gel process 2film is compared, and not only has higher degree of crystallinity, and film forming is even, and impedance is less, and photogenerated current density significantly improves, the electricity conversion of the remarkable boost device of energy and thermal stability;
(2) the double-layer nanostructured TiO for preparing of the present invention 2film has higher fill factor, curve factor and electricity conversion as the perovskite solar cell of electron transfer layer, and the good stability of device;
(3) electron transfer layer that prepared by the present invention can by the thickness regulating number of deposition cycles accurately to control compact titanium dioxide film and porous titanium dioxide thin-film;
(4) the Ca-Ti ore type solar cell prepared of the present invention, preparation technology's equipment is simple, and operating process is few, and reaction condition is gentle; production efficiency is high, cost and energy consumption lower, pollution-free to biological environment; and favorable repeatability, be suitable for scale application, have larger prospects for commercial application.
Accompanying drawing explanation
Fig. 1 is the XRD collection of illustrative plates of the titaniferous Organic inorganic film that in the embodiment of the present invention 3, step B obtains.
Fig. 2 is the volt-ampere characteristic of Ca-Ti ore type solar cell prepared by the embodiment of the present invention 3.
Embodiment
The invention provides a kind of preparation method of Ca-Ti ore type solar cell, it comprises the transparent conductive substrate, the TiO that stack gradually 2electron transfer layer, perovskite light-absorption layer, hole transmission layer and metal counter electrode layer, wherein, electron transfer layer preparation comprises the following steps:
Step a, provides the non-transparent substrate material of surface cleaning, adopts technique for atomic layer deposition in substrate material surface deposition of titanium oxide dense film;
Step b, the titanium dioxide dense film adopting molecular-layer deposition technology to obtain in step a deposits titaniferous Organic inorganic film;
Step c, the material obtained by step b is annealed 0.5-5h at 400-600 DEG C, obtains TiO 2electron transfer layer.
Preferably, described step a comprises Ultrasonic Cleaning transparent conductive substrate and dries, and UV ozone process obtains the non-transparent substrate material of surface cleaning.
Preferably, described backing material is the silicon dioxide electro-conductive glass of doped with fluorine, i.e. FTO electro-conductive glass, and indium tin oxide electro-conductive glass, i.e. ITO electro-conductive glass mix the zinc oxide electro-conductive glass of aluminium, i.e. AZO electro-conductive glass, in one.
Preferably, described perovskite light-absorption layer is for having ABX my 3-mthe material of type crystal structure is formed, and wherein, A is CH 3nH 3or C 4h 9nH 3, B is Pb or Sn, X, Y is Cl, Br or I, and m is 1,2 or 3.
Preferably, described hole transmission layer is NiO, WO 3, Spiro-OMeTAD or PTAA.
Preferably, described electric transmission layer thickness is 120-600nm, and perovskite light-absorption layer thickness is 300-2000nm, and thickness of hole transport layer is 50-400nm, and metal counter electrode layer thickness is 40-120nm.
Preferably, described step a comprises,
Step a1, puts into the backing material of surface cleaning the reaction chamber that temperature is the atomic layer deposition apparatus of 80-200 DEG C, purges 3-10min with 50-100sccm high pure nitrogen;
Step a2, is greater than the TiCl of 97% by purity 4or titanium tetraisopropylate is heated to 60-100 DEG C of formation TiCl 4or titanium tetraisopropylate steam, and with impulse form by TiCl 4or titanium tetraisopropylate steam sends into reaction cavity, the burst length is 0.05-0.2s, and open-assembly time is 8-15s, then purges with high pure nitrogen, and purge time is 15-30s;
Step a3, deionized water is sent into reaction cavity with impulse form, burst length is 0.02-0.05s, open-assembly time is 8-15s, purge with high pure nitrogen again, purge time is 15-30s, completes primary depositing circulation, namely deposited one deck compact titanium dioxide film at titanium dioxide dense film surface;
Step a4, the deposition cycle of repetition step a2-a3 1000-5000 time.
Preferably, in described step c, each deposition cycle makes the compact titanium dioxide film thickness obtained increase to 0.09-0.15nm.
Preferably, described step b comprises,
Step b1, the surface deposition obtained by step a have the backing material of titanium dioxide dense film to put into reaction chamber that temperature is the atomic layer deposition apparatus of 80-150 DEG C, purges 5-30min with 50-100sccm high pure nitrogen;
Step b2, by TiCl 4or titanium tetraisopropylate is heated to 60-100 DEG C of formation TiCl 4or titanium tetraisopropylate steam, and with impulse form by TiCl 4or titanium tetraisopropylate steam sends into reaction cavity, the burst length is 0.05-0.2s, and open-assembly time is 8-15s, then purges with high pure nitrogen, and purge time is 15-30s;
Step b3, dihydroxylic alcohols or polyalcohol are heated to 100-200 DEG C and form dihydroxylic alcohols or polyalcohol steam, reaction cavity is sent into again with impulse form, burst length is 0.1-1s, open-assembly time is 20-45s, then purges with high pure nitrogen, and purge time is 30-45s, complete primary depositing circulation, namely deposited one deck titaniferous Organic inorganic film in substrate material surface;
Step b4, the deposition cycle of repetition step b2-b3 100-20000 time.
Preferred further, in described step b3, dihydroxylic alcohols is the one in ethylene glycol, propylene glycol or butanediol; Polyalcohol is the one in glycerol, trimethylolethane, pentaerythrite, xylitol or sorbierite.
Preferred further, in described step b3, each deposition cycle makes the titaniferous Organic inorganic film thickness obtained increase to 0.06-0.12nm.
Further preferred, repeat deposition cycle 1000-10000 time of step b2-b3 in described step b4.
Preferably, TiO is obtained in described step c 2the specific area of electron transfer layer is 60-400m 2/ g, pore scale is at 8-10nm.
Below in conjunction with specific embodiment, describe the present invention further.Certainly described embodiment is only a part of embodiment of the present invention; instead of whole embodiment; based on the embodiment in the present invention, those skilled in the art, not making the every other embodiment obtained under creative work prerequisite, belong to protection scope of the present invention.
Embodiment 1
Step a, Ultrasonic Cleaning FTO electro-conductive glass is also dried, stand-by after UV ozone process, utilizes the technique for atomic layer deposition titanium dioxide dense film that deposit thickness is 120nm on clean FTO electro-conductive glass.Concrete steps comprise:
A1, puts into the FTO electro-conductive glass of surface cleaning the reaction chamber that temperature is the atomic layer deposition apparatus of 80-200 DEG C, purges 5min with 50-100sccm high pure nitrogen;
A2, is greater than the TiCl of 97% by purity 4be heated to 65 DEG C and form TiCl 4steam, and with impulse form by TiCl 4steam sends into reaction cavity, and the burst length is 0.05s, and open-assembly time is 8s, then purges with high pure nitrogen, and purge time is 15s;
A3, sends into reaction cavity by deionized water with impulse form, and the burst length is 0.02s, and open-assembly time is 8s, then purges with high pure nitrogen, and purge time is 15s, completes primary depositing circulation, namely deposited layer of titanium dioxide dense film in substrate material surface;
A4, the deposition cycle of repetition step a2-a3 1500 times.
Step b, utilizes the titaniferous Organic inorganic film that molecular-layer deposition technology deposit thickness on titanium dioxide dense film is 180nm.Concrete steps comprise:
B1, the surface deposition obtained by step a has the FTO electro-conductive glass of titanium dioxide dense film to put into the reaction chamber that temperature is the atomic layer deposition apparatus of 80 DEG C, purges 5min with 50sccm high pure nitrogen;
Purity is the TiCl of 97% by b2 4be heated to 60 DEG C and form TiCl 4steam, and with impulse form by TiCl 4steam sends into reaction cavity, and the burst length is 0.05s, and open-assembly time is 8s, then purges with high pure nitrogen, and purge time is 15s;
B3, ethylene glycol is heated to 100 DEG C and forms ethylene glycol steam, reaction cavity is sent into again with impulse form, burst length is 0.1s, open-assembly time is 20s, then purges with high pure nitrogen, and purge time is 30s, complete primary depositing circulation, namely deposited one deck titaniferous Organic inorganic film at titanium dioxide dense film surface;
B4, Using such method repeats this deposition cycle 3000 times.
Step c, the material obtained by step b is annealed 1h at 500 DEG C, obtains TiO 2electron transfer layer.
Steps d, TiO 2electron transfer layer and perovskite light-absorption layer, hole transmission layer and metal counter electrode layer stack gradually, are assembled into Ca-Ti ore type solar cell.Wherein, perovskite light-absorption layer is CH 3nH 3pbI 3, hole transmission layer is Spiro-OMeTAD, and metal counter electrode layer is Au.The photoelectric efficiency of the perovskite solar cell adopting said method to obtain can reach 10.96%.
Embodiment 2
Step a, Ultrasonic Cleaning ITO electro-conductive glass is also dried, stand-by after UV ozone process, utilizes the technique for atomic layer deposition titanium dioxide dense film that deposit thickness is 300nm on clean ITO electro-conductive glass.Concrete steps comprise:
A1, puts into the ITO electro-conductive glass of surface cleaning the reaction chamber that temperature is the atomic layer deposition apparatus of 150 DEG C, purges 5min with 50sccm high pure nitrogen;
A2, titanium tetraisopropylate purity being greater than 97% is heated to 65 DEG C of formation titanium tetraisopropylate steams, and with impulse form, titanium tetraisopropylate steam is sent into reaction cavity, burst length is 0.05s, open-assembly time is 8s, then purges with high pure nitrogen, and purge time is 15s;
A3, sends into reaction cavity by deionized water with impulse form, and the burst length is 0.02s, and open-assembly time is 8s, then purges with high pure nitrogen, and purge time is 15s, completes primary depositing circulation, namely deposited one deck compact titanium dioxide film in substrate material surface;
A4, the deposition cycle of repetition step a2-a3 3000 times.
Step b, utilizes the titaniferous Organic inorganic film that molecular-layer deposition technology deposit thickness on titanium dioxide dense film is 300nm.Concrete steps comprise:
B1, the surface deposition obtained by step a has the ITO electro-conductive glass of titanium dioxide dense film to put into the reaction chamber that temperature is the atomic layer deposition apparatus of 80 DEG C, purges 5min with 50sccm high pure nitrogen;
B2, be that the titanium tetraisopropylate of 97% is heated to 60 DEG C of formation titanium tetraisopropylate steams by purity, and with impulse form, titanium tetraisopropylate steam sent into reaction cavity, the burst length is 0.05s, and open-assembly time is 8s, then purges with high pure nitrogen, and purge time is 15s;
B3, ethylene glycol is heated to 100 DEG C and forms ethylene glycol steam, reaction cavity is sent into again with impulse form, burst length is 0.1s, open-assembly time is 20s, then purges with high pure nitrogen, and purge time is 30s, complete primary depositing circulation, namely deposited one deck titaniferous Organic inorganic film at titanium dioxide dense film surface;
B4, Using such method repeats this deposition cycle 3000 times.
Step c, the material obtained by step b is annealed 0.5h at 600 DEG C, obtains TiO 2electron transfer layer.Steps d, TiO 2electron transfer layer and perovskite light-absorption layer, hole transmission layer and metal counter electrode layer stack gradually, are assembled into Ca-Ti ore type solar cell.Wherein, perovskite light-absorption layer is CH 3nH 3pbI 3, hole transmission layer is Spiro-OMeTAD, and metal counter electrode layer is Au.The photoelectric efficiency of the perovskite solar cell adopting said method to obtain can reach 9.28%.
Embodiment 3
Step a, Ultrasonic Cleaning AZO electro-conductive glass is also dried, stand-by after UV ozone process, utilizes the technique for atomic layer deposition titanium dioxide dense film that deposit thickness is 450nm on clean AZO electro-conductive glass.Concrete steps comprise:
A1, puts into the AZO electro-conductive glass of surface cleaning the reaction chamber that temperature is the atomic layer deposition apparatus of 80-200 DEG C, purges 10min with 100sccm high pure nitrogen;
A2, is greater than the TiCl of 97% by purity 4be heated to 80 DEG C and form TiCl 4steam, and with impulse form by TiCl 4steam sends into reaction cavity, and the burst length is 0.2s, and open-assembly time is 15s, then purges with high pure nitrogen, and purge time is 30s;
A3, sends into reaction cavity by deionized water with impulse form, and the burst length is 0.05s, and open-assembly time is 15s, then purges with high pure nitrogen, and purge time is 30s, completes primary depositing circulation, namely deposited one deck compact titanium dioxide film in substrate material surface;
A4, the deposition cycle of repetition step a2-a3 5000 times.
Step b, utilizes the titaniferous Organic inorganic film that molecular-layer deposition technology deposit thickness on titanium dioxide dense film is 150nm.Concrete steps comprise:
B1, the surface deposition obtained by step a has the AZO electro-conductive glass of titanium dioxide dense film to put into the reaction chamber that temperature is the atomic layer deposition apparatus of 80 DEG C, purges 5min with 50sccm high pure nitrogen;
Purity is the TiCl of 97% by b2 4be heated to 60 DEG C and form TiCl 4steam, and with impulse form by TiCl 4steam sends into reaction cavity, and the burst length is 0.05s, and open-assembly time is 8s, then purges with high pure nitrogen, and purge time is 15s;
B3, ethylene glycol is heated to 100 DEG C and forms ethylene glycol steam, reaction cavity is sent into again with impulse form, burst length is 0.1s, open-assembly time is 20s, then purges with high pure nitrogen, and purge time is 30s, complete primary depositing circulation, namely deposited one deck titaniferous Organic inorganic film at titanium dioxide dense film surface;
B4, Using such method repeats this deposition cycle 1200 times.
Step c, the material obtained by step b is annealed 5h at 400 DEG C, obtains TiO 2electron transfer layer.
Steps d, TiO 2electron transfer layer and perovskite light-absorption layer, hole transmission layer and metal counter electrode layer stack gradually, are assembled into Ca-Ti ore type solar cell.Wherein, perovskite light-absorption layer is CH 3nH 3pbI 3, hole transmission layer is Spiro-OMeTAD, and metal counter electrode layer is Au.The photoelectric efficiency of the perovskite solar cell adopting said method to obtain can reach 7.34%.
XRD analysis is carried out to the titaniferous Organic inorganic film that step b in embodiment 3 obtains, obtain XRD collection of illustrative plates shown in Fig. 1, as shown in Figure 1: the characteristic diffraction peak of (101) (004) (200) (105) and (204) crystal face has appearred in the film after annealed, prove that this film is anatase titanium dioxide.
To the Ca-Ti ore type solar cell test volt-ampere characteristic that embodiment 3 prepares, obtain curve shown in Fig. 2, the open circuit voltage Voc of the Ca-Ti ore type solar cell obtained as shown in Figure 2 is 895mV, and short circuit current Jsc is 14.19mAcm -2.

Claims (9)

1. a preparation method for Ca-Ti ore type solar cell, it comprises the transparent conductive substrate, the TiO that stack gradually 2electron transfer layer, perovskite light-absorption layer, hole transmission layer and metal counter electrode layer, wherein, electron transfer layer preparation comprises the following steps:
Step a, provides the non-transparent substrate material of surface cleaning, adopts technique for atomic layer deposition in substrate material surface deposition of titanium oxide dense film;
Step b, the titanium dioxide dense film adopting molecular-layer deposition technology to obtain in step a deposits titaniferous Organic inorganic film;
Step c, the material obtained by step b is annealed 0.5-5h at 400-600 DEG C, obtains TiO 2electron transfer layer.
2. the preparation method of Ca-Ti ore type solar cell as claimed in claim 1, is characterized in that: described step a comprises Ultrasonic Cleaning transparent conductive substrate and dries, UV ozone process, obtains the non-transparent substrate material of surface cleaning.
3. the preparation method of Ca-Ti ore type solar cell as claimed in claim 1, is characterized in that: described backing material is the silicon dioxide electro-conductive glass of doped with fluorine, indium tin oxide electro-conductive glass or the one of mixing in the zinc oxide electro-conductive glass of aluminium.
4. the preparation method of Ca-Ti ore type solar cell as claimed in claim 1, is characterized in that: described perovskite light-absorption layer is for having ABX my 3-mthe material of type crystal structure is formed, and wherein, A is CH 3nH 3or C 4h 9nH 3, B is Pb or Sn, X, Y is Cl, Br or I, and m is 1,2 or 3.
5. the preparation method of Ca-Ti ore type solar cell as claimed in claim 1, is characterized in that: described hole transmission layer is NiO, WO 3, Spiro-OMeTAD or PTAA.
6. the preparation method of Ca-Ti ore type solar cell as claimed in claim 1, it is characterized in that: described electric transmission layer thickness is 120-600nm, perovskite light-absorption layer thickness is 300-2000nm, and thickness of hole transport layer is 50-400nm, and metal counter electrode layer thickness is 40-120nm.
7. the preparation method of Ca-Ti ore type solar cell as claimed in claim 1, is characterized in that: described step a comprises,
Step a1, puts into the backing material of surface cleaning the reaction chamber that temperature is the atomic layer deposition apparatus of 80-200 DEG C, purges 3-10min with 50-100sccm high pure nitrogen;
Step a2, is greater than the TiCl of 97% by purity 4or titanium tetraisopropylate is heated to 60-100 DEG C of formation TiCl 4or titanium tetraisopropylate steam, and with impulse form by TiCl 4or titanium tetraisopropylate steam sends into reaction cavity, the burst length is 0.05-0.2s, and open-assembly time is 8-15s, then purges with high pure nitrogen, and purge time is 15-30s;
Step a3, sends into reaction cavity by deionized water with impulse form, and the burst length is 0.02-0.05s, open-assembly time is 8-15s, then purges with high pure nitrogen, and purge time is 15-30s, complete primary depositing circulation, namely deposited one deck compact titanium dioxide film in substrate material surface;
Step a4, the deposition cycle of repetition step a2-a3 1000-5000 time.
8. the preparation method of Ca-Ti ore type solar cell as claimed in claim 1, is characterized in that: described step b comprises,
Step b1, the surface deposition obtained by step a have the backing material of titanium dioxide dense film to put into reaction chamber that temperature is the atomic layer deposition apparatus of 80-150 DEG C, purges 5-30min with 50-100sccm high pure nitrogen;
Step b2, by TiCl 4or titanium tetraisopropylate is heated to 60-100 DEG C of formation TiCl 4or titanium tetraisopropylate steam, and with impulse form by TiCl 4or titanium tetraisopropylate steam sends into reaction cavity, the burst length is 0.05-0.2s, and open-assembly time is 8-15s, then purges with high pure nitrogen, and purge time is 15-30s;
Step b3, dihydroxylic alcohols or polyalcohol are heated to 100-200 DEG C and form dihydroxylic alcohols or polyalcohol steam, reaction cavity is sent into again with impulse form, burst length is 0.1-1s, open-assembly time is 20-45s, then purges with high pure nitrogen, and purge time is 30-45s, complete primary depositing circulation, namely deposited one deck titaniferous Organic inorganic film at titanium dioxide dense film surface;
Step b4, the deposition cycle of repetition step b2-b3 100-20000 time.
9. the preparation method of Ca-Ti ore type solar cell as claimed in claim 1, is characterized in that: the specific area obtaining TiO2 electron transfer layer in described step c is 60-400m2/g, and pore scale is at 8-10nm.
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CN106058060A (en) * 2016-06-16 2016-10-26 厦门大学 Method for preparing high-quality perovskite crystal thin film
CN106898697A (en) * 2017-02-27 2017-06-27 周德明 A kind of new perovskite photodetector and preparation method thereof
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CN109518162A (en) * 2018-12-18 2019-03-26 同济大学 A kind of preparation method of bionical net mitochondrial structure thin-film material
CN110512189A (en) * 2019-06-14 2019-11-29 邱越 A kind of aperture adjustable porous metal oxide preparation method based on molecular-layer deposition

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