CN106848068A - A kind of preparation method of low temperature perovskite solar cell - Google Patents
A kind of preparation method of low temperature perovskite solar cell Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of low temperature perovskite solar cell, step is：First, CdS or CdSe nano-particles are produced, is then dispersed in a certain amount of solvent, film is prepared into electrically conducting transparent substrate by way of spin coating；Then one layer of organic inorganic hybridization perovskite light absorbing zone of spin coating on CdS or CdSe films, is then spin coated onto hole mobile material, is finally deposited with layer of metal electrode so as to perovskite solar cell is obtained.Sunshine is incident by light anode face.Preparation method of the present invention is simple, and maximum temperature used by whole technique is 180 DEG C, and the perovskite solar cell for being assembled has photoelectric transformation efficiency and good long-time stability higher.
Description
Technical field
The present invention relates to organic inorganic hybridization perovskite solar cell technical field of new energies, more particularly, to low temperature calcium
The technology of preparing of titanium ore solar cell.
Background technology
Organic inorganic hybridization perovskite material was taught in the Tsutomu Miyasaka by Japanese Tong Yin Yokohama university in 2009
First Application is awarded in photovoltaic device, the highest attention of academia is just obtained afterwards.At present, this new all solid state solar energy
Battery has shown the photoelectric transformation efficiency more than 22%.
Organic inorganic hybridization perovskite material has excellent self assembly performance, and structure and performance are manually adjustable, its
There is huge application prospect in photoelectric field.Ca-Ti ore type thin-film solar cells its theoretical conversion efficiency is reached as high as
50%, it is the twice of solar cell transformation efficiency in the market, the use cost of solar cell can be greatly reduced.And
Approximately half of sunshine can be converted into by electric power with the solar cell that new-type perovskite is manufactured as raw material, be current
2 times, therefore, only need half solar cell to provide same electric power, this will greatly reduce installation cost, so as to allow assembly
Originally significantly reduce.
Traditional organic inorganic hybridization perovskite solar cell is more with TiO2, ZnO, SnO2It is electronic transmission medium, these things
Matter is required for greatly high temperature sintering, and preparation technology is complicated, and power consumption is high.
The content of the invention
There is good long and high light photoelectric transformation efficiency it is an object of the invention to provide a kind of low temperature preparation
Organic inorganic hybridization perovskite solar cell method.
To achieve these goals, the present invention is realized according to following technical proposals：
A kind of preparation method of low temperature perovskite solar cell, specifically includes following steps：
1) CdS or CdSe nano-particles are prepared by solvent-thermal method, the granularity of the CdS or CdSe nano-particles is 4-
30nm, formation concentration is the dispersion liquid of 0.01-0.1M, stand for standby use in being scattered in organic solvent；
2) etch and clean electrically conducting transparent substrate, the dispersion liquid is spun on the electrically conducting transparent substrate surface, spin coating
Process is the speed spin coating 2-8s of 800-1500rpm, then the speed spin coating 15-25s of 5000-7000rpm, obtain CdS or
CdSe electric transmission tunics；The purpose for wherein etching is to separate the both positive and negative polarity of battery, it is to avoid short circuit；
3) lead halide and organic halogenation ammonium salt are dissolved in solvent and are configured to organic inorganic hybridization perovskite precursor solution,
It is then spin coated onto in CdS the or CdSe electric transmissions tunic surface, perovskite knot is caused in the 10-60min that annealed at 80-140 DEG C
Crystalline substance obtains organic inorganic hybridization perovskite light absorbing zone；The energy state and CdS of the organic inorganic hybridization perovskite light absorbing zone
Or CdSe matchings；
4) hole transmission layer is formed in the organic inorganic hybridization perovskite light absorbing zone surface；The hole transport layer material
Energy state matched with organic inorganic hybridization perovskite light absorption layer material；
5) metal electrode layer is formed in the hole transport layer surface.
Preferably, the preparation of the CdS nano-particles is that NaOH is dissolved in the aqueous solution of ethanol, is then added thereto to
Oleic acid, is stirring evenly and then adding into the half five water caddy aqueous solution and nine water sodium sulfide solutions, and stainless steel is poured into after stirring
In reactor, and 8-15h is reacted in 150-180 DEG C, be centrifuged out for product after terminating by reaction, and impurity is cleaned with ethanol
Obtain；The mol ratio of wherein described half five water caddies and nine water vulcanized sodium is 1:1-1:1.2.
Preferably, the preparation of the CdSe nano-particles is that NaOH is dissolved in the aqueous solution of ethanol, is then added thereto
Enter oleic acid, be stirring evenly and then adding into the half five water caddy aqueous solution and Na2SeSO3The aqueous solution, pours into stainless steel anti-after stirring
In answering kettle, and 6-10h is reacted in 60-100 DEG C, be centrifuged out for product after terminating by reaction, and impurity is cleaned with ethanol
Arrive；Wherein described half five water caddies and Na2SeSO3Mol ratio be 1:1-1:1.2.
Preferably, the volume ratio of ethanol is 60-80% in the aqueous solution of the ethanol, the half five water caddy aqueous solution
Concentration be 0.05-0.2M, the quality volume of the NaOH, the aqueous solution of ethanol, oleic acid and the half five water caddy aqueous solution
Than for：0.4-0.8g:30-50ml:3-9ml:8-12ml.
Preferably, the Na2SeSO3The aqueous solution is by Se and Na2SO3Add in distilled water, heated back at 80-120 DEG C
Stream 4-6h is obtained；Wherein Se, Na2SO3Molal volume with distilled water compares 1mol:1.5-2.5mol:8-12L, the Na2SeSO3
The concentration of the aqueous solution is 0.05-0.2M.
Preferably, step 1) in, the organic solvent is toluene, hexamethylene or chlorobenzene.
Preferably, the organic inorganic hybridization perovskite includes CH3NH3PbI3、CH3NH3PbCl3、CH3NH3PbBr3、
CH3NH3PbI2Cl、CH3NH3PbICl2、CH3NH3PbI2Br、CH3NH3PbIBr2、CH3NH3PbIClBr、(CH3NH3)0.17(CH
(NH2)2)0.83Pb(I0.83Br0.17)3、CH(NH2)2PbIxCl3-x(3≥x≥0)、Cs0.05((CH3NH3)0.17(CH(NH2)2
)0.83)0.95Pb(I0.83Br0.17)3Deng photosensitizer.
Preferably, step 3) in, the spin coating process is the low speed spin coating 2-8s of 800-1500rpm, then 3000-
The high speed spin coating 15-25s of 6000rpm, 0.5-1.5mL ether or 0.1-0.2mL chlorobenzenes are added dropwise in high speed.
Preferably, the hole transmission layer is selected from [N, the N- bis- of organic molecule hole mobile material such as 2,2', 7,7'- tetra-
(4- methoxyphenyls) amino] fluorenes of -9,9'- spiral shells two, poly- 3- hexyl thiophenes, PTAA etc. or inorganic hole transporter
Such as CuGaO2、Cu2BaSnS4, CuI, CuInS, NiO, CuSCN etc..
Preferably, the electrically conducting transparent substrate is FTO, ITO, flexible stainless steel base, ITO/PET or ITO/PEN, is had
The transparency higher, can pass through light and be absorbed by calcium titanium ore bed, and with good conductive capability.
The metal electrode is generally Au, Ag, with excellent electric conductivity, it is ensured that can be by generation after battery is assembled
Electric energy is transported to external circuit.
Electron transfer layer (i.e. CdS or CdSe film layers) prepared by the present invention has translucency higher, it is ensured that too
Sunlight can be absorbed through light anode by calcium titanium ore bed, and the photoelectricity produced by calcium titanium ore bed is streamed into external circuit.
Perovskite solar cell electron transfer layer prepared by the present invention is CdS or CdSe, will directly can be prepared
CdS (or CdSe) slurry for rotary coating in conductive substrates, it is to avoid this link of high-temperature calcination, whole flow process maximum temperature is not
More than 180 DEG C, energy resource consumption, preparation process is simple are greatly reduced.Spin coating CdS out, CdSe films have good electricity
Sub- transmittability, have good stability, service life it is more long, and possess transmitance higher so that sunshine can be through electricity
Sub- transport layer absorbs generation photoelectric current by perovskite photosensitive layer, and the perovskite solar cell for being assembled can obtain photoelectricity higher
Conversion efficiency.
The present invention will be further described for following examples, but the present invention is not limited to embodiment.
Specific embodiment
Embodiment 1
The preparation of first, CdS：0.6g NaOH are dissolved in the mixing being made up of 10ml distilled water and 30ml absolute ethyl alcohols molten
In liquid, 6ml oleic acid is then added thereto to, is stirring evenly and then adding into the half five water caddy aqueous solution and the 10ml of 10ml 0.1M
The nine water sodium sulfide solutions of 0.1M, pour into the stainless steel cauldron of 100ml after stirring, and in baking oven 180 DEG C it is anti-
Answer 12h.Be centrifuged out for product after terminating by reaction, and is cleaned impurity with ethanol, and the granularity of product CdS is 8-12nm.It
Centrifugation products therefrom is scattered in the toluene of 20ml afterwards, is stood, it is standby.
Second, using laser ablation electrically conducting transparent substrate, in case prepared perovskite solar cell short circuit.To carve
The electrically conducting transparent substrate lost is cleaned by ultrasonic with cleaning agent, distilled water, absolute ethyl alcohol successively, afterwards with UV ozone cleaning machine
Reason 30min, removes electrically conducting transparent substrate surface remnants macromoleculars.Finally molten prepared by the spin coating first step above or second step
Liquid, specific spin coating process is 1000rpm, 4s, 6000rpm, 20s.Spin coating finish after by CdS electric transmission tunics.
3rd, CH3NH3PbI3The preparation of one-step method solution：By 0.461g PbI2, 0.159g CH3NH3I is dissolved in 635 μ L
In the mixed solution of DMF and 71 μ L DMSO, it is then spin coated onto in CdS film.Specific spin coating process is 1000rpm, 4s,
4000rpm, 20s, the fast drop 1ml ether in 6s at a high speed.100 DEG C of annealing 15min, make perovskite crystalline after spin coating well,
Obtain organic inorganic hybridization perovskite light absorbing zone.
4th, the preparation of hole transmission layer solution：0.1446g SPIRO-OMETAD are dissolved in 2ml chlorobenzenes, afterwards thereto
Add 35 μ L 520mgml-1Lithium salt solution (solvent is anhydrous acetonitrile), add 57.6 μ L 4- tert .-butylpyridines.Using
The hole transmission layer solution that the spin coating process of 1000rpm, 4s, 4000rpm, 20s will be prepared is spun on CH3NH3PbI3Film
On, then aoxidize 12h under environment that is dark, drying.
5th, the Au electrodes of one layer of 100nm or so are deposited with hole transmission layer, so as to complete perovskite solar cell
Preparation.
Embodiment 2
The preparation of first, CdSe：Synthesize the Na of 0.1M first2SeSO3The aqueous solution, detailed process be by 5mmol Se,
10mmol Na2SO3Add in 50ml distilled water, 100 DEG C are heated to reflux 5h, you can obtain the Na of 0.1M2SeSO3The aqueous solution.Afterwards
By solvent-thermal process CdSe nano-particles, concretely comprise the following steps and 0.6g NaOH are dissolved in by 10ml distilled water and the anhydrous second of 30ml
In the mixed solution of alcohol composition, 6ml oleic acid is then added thereto to, is stirring evenly and then adding into the half five water chlorinations of 10ml 0.1M
The Na of the cadmium aqueous solution and 10ml 0.1M2SeSO3The aqueous solution, pours into stainless steel cauldron after stirring, and 80 in baking oven
DEG C reaction 8h.Be centrifuged out for product after terminating by reaction, and is cleaned impurity with ethanol, and the granularity of product CdSe is 4-
10nm.Centrifugation products therefrom is scattered in the toluene of 20ml afterwards, is stood, it is standby.
Second, using laser ablation electrically conducting transparent substrate, in case prepared perovskite solar cell short circuit.To carve
The electrically conducting transparent substrate lost is cleaned by ultrasonic with cleaning agent, distilled water, absolute ethyl alcohol successively, afterwards with UV ozone cleaning machine
Reason 30min, removes electrically conducting transparent substrate surface remnants macromoleculars.Finally molten prepared by the spin coating first step above or second step
Liquid, specific spin coating process is 1000rpm, 4s, 6000rpm, 20s.Spin coating finish after by CdSe electric transmission tunics.
3rd, CH3NH3PbI3The preparation of one-step method solution：By 0.461g PbI2, 0.159g CH3NH3I is dissolved in 635 μ L
In the mixed solution of DMF and 71 μ L DMSO, it is then spin coated onto on CdSe films.Specific spin coating process is 1000rpm, 4s,
4000rpm, 20s, the fast drop 1ml ether in 6s at a high speed.100 DEG C of annealing 15min, make perovskite crystalline after spin coating well,
Obtain organic inorganic hybridization perovskite light absorbing zone.
4th, the preparation of hole transmission layer solution：0.1446g SPIRO-OMETAD are dissolved in 2ml chlorobenzenes, afterwards thereto
Add 35 μ L 520mgml-1Lithium salt solution (solvent is anhydrous acetonitrile), add 57.6 μ L 4- tert .-butylpyridines.Using
The hole transmission layer solution that the spin coating process of 1000rpm, 4s, 4000rpm, 20s will be prepared is spun on CH3NH3PbI3Film
On, then aoxidize 12h under environment that is dark, drying.
5th, the Au electrodes of one layer of 100nm or so are deposited with hole transmission layer, so as to complete perovskite solar cell
Preparation.
Additionally, in above-described embodiment, toluene can also be changed to hexamethylene, chlorobenzene etc. can disperse CdS or CdSe nano-particles
Solvent.Organic inorganic hybridization perovskite also can be CH prepared by the method by being similar to3NH3PbI3、CH3NH3PbCl3、
CH3NH3PbBr3、CH3NH3PbI2Cl、CH3NH3PbICl2、CH3NH3PbI2Br、CH3NH3PbIBr2、CH3NH3PbIClBr、CH
(NH2)2PbIxCl3-x(3≥x≥0)、(CH3NH3)0.17(CH(NH2)2)0.83Pb(I0.83Br0.17)3、Cs0.05((CH3NH3)0.17
(CH(NH2)2)0.83)0.95Pb(I0.83Br0.17)3Deng photosensitizer material.Hole transport layer material can also be organic molecule
For example poly- 3- hexyl thiophenes of hole mobile material, PTAA etc. or inorganic hole transporter such as CuGaO2、Cu2BaSnS4、
CuI, CuInS, NiO, CuSCN etc..Electrically conducting transparent substrate is FTO, ITO, flexible stainless steel base, ITO/PET or ITO/PEN
Deng.
By the above method, can obtain with stability higher that (cell photoelectric conversion efficiency attenuation amplitude is less than in 1 year
10%), service life more long (3-5), the perovskite solar cell of photoelectric transformation efficiency (＞ 14%) higher, for this
The practical offer technical support of class battery.
Above-described embodiment is only used for further illustrating a kind of preparation method of low temperature perovskite solar cell of the invention,
But it is every any simply to be repaiied according to what technical spirit of the invention was made to above example the invention is not limited in embodiment
Change, equivalent variations and modification, each fall within the protection domain of technical solution of the present invention.
Claims (10)
1. a kind of preparation method of low temperature perovskite solar cell, it is characterised in that comprise the following steps：
1) CdS or CdSe nano-particles are prepared by solvent-thermal method, the granularity of the CdS or CdSe nano-particles is 4-30nm,
Formation concentration is the dispersion liquid of 0.01-0.1M, stand for standby use in being scattered in organic solvent；
2) etch and clean electrically conducting transparent substrate, the dispersion liquid is spun on the electrically conducting transparent substrate surface, spin coating process
It is the speed spin coating 2-8s of 800-1500rpm, then the speed spin coating 15-25s of 5000-7000rpm, obtains CdS or CdSe electricity
Son transmission tunic；
3) lead halide and organic halogenation ammonium salt are dissolved in solvent and are configured to organic inorganic hybridization perovskite precursor solution, then
CdS the or CdSe electric transmissions tunic surface is spun on, causes that perovskite crystalline is obtained in the 10-60min that annealed at 80-140 DEG C
To organic inorganic hybridization perovskite light absorbing zone；
4) hole transmission layer is formed in the organic inorganic hybridization perovskite light absorbing zone surface；
5) metal electrode layer is formed in the hole transport layer surface.
2. preparation method according to claim 1, it is characterised in that：The preparation of the CdS nano-particles is that NaOH is molten
In the aqueous solution of ethanol, oleic acid is then added thereto to, is stirring evenly and then adding into the half five water caddy aqueous solution and nine water sulphur
Change sodium water solution, poured into stainless steel cauldron after stirring, and 8-15h is reacted in 150-180 DEG C, reaction will after terminating
Product is centrifuged out, and with ethanol by impurity clean obtain；The mol ratio of wherein described half five water caddies and nine water vulcanized sodium
It is 1:1-1:1.2.
3. preparation method according to claim 1, it is characterised in that：The preparation of the CdSe nano-particles is that NaOH is molten
In the aqueous solution of ethanol, oleic acid is then added thereto to, is stirring evenly and then adding into the half five water caddy aqueous solution and Na2SeSO3
The aqueous solution, pours into stainless steel cauldron after stirring, and reacts 6-10h in 60-100 DEG C, reacts product after terminating
Be centrifuged out, and with ethanol by impurity clean obtain；Wherein described half five water caddies and Na2SeSO3Mol ratio be 1:1-1:
1.2。
4. the preparation method according to Claims 2 or 3, it is characterised in that：The volume of ethanol in the aqueous solution of the ethanol
Than being 60-80%, the concentration of the half five water caddy aqueous solution is 0.05-0.2M, the NaOH, the aqueous solution of ethanol, oil
The mass volume ratios of acid and the half five water caddy aqueous solution are：0.4-0.8g:30-50ml:3-9ml:8-12ml.
5. preparation method according to claim 3, it is characterised in that：The Na2SeSO3The aqueous solution is by Se and Na2SO3Plus
In entering distilled water, at 80-120 DEG C being heated to reflux 4-6h obtains；Wherein Se, Na2SO3Molal volume with distilled water compares 1mol:
1.5-2.5mol:8-12L, the Na2SeSO3The concentration of the aqueous solution is 0.05-0.2M.
6. preparation method according to claim 1, it is characterised in that：Step 1) in, the organic solvent is toluene, hexamethylene
Alkane or chlorobenzene.
7. preparation method according to claim 1, it is characterised in that：The organic inorganic hybridization perovskite includes
CH3NH3PbI3、CH3NH3PbCl3、CH3NH3PbBr3、CH3NH3PbI2Cl、CH3NH3PbICl2、CH3NH3PbI2Br、
CH3NH3PbIBr2、CH3NH3PbIClBr、CH(NH2)2PbIxCl3-x(3≥x≥0)、(CH3NH3)0.17(CH(NH2)2)0.83Pb
(I0.83Br0.17)3、Cs0.05((CH3NH3)0.17(CH(NH2)2)0.83)0.95Pb(I0.83Br0.17)3。
8. preparation method according to claim 1, it is characterised in that：Step 3) in, the spin coating process is 800-
The low speed spin coating 2-8s of 1500rpm, then the high speed spin coating 15-25s of 3000-6000rpm, 0.5-1.5mL is added dropwise in high speed
Ether or 0.1-0.2mL chlorobenzenes.
9. preparation method according to claim 1, it is characterised in that：The hole transmission layer is selected from organic molecule hole
Transmission material 2,2', 7,7'- tetra- [N, N- bis- (4- methoxyphenyls) amino] fluorenes of -9,9'- spiral shells two, poly- 3- hexyl thiophenes, poly- thiophene
Fen acetic acid or inorganic hole transporter CuGaO2、Cu2BaSnS4、CuI、CuInS、NiO、CuSCN。
10. preparation method according to claim 1, it is characterised in that：The electrically conducting transparent substrate includes FTO, ITO, soft
The stainless steel base of property, ITO/PET, ITO/PEN.
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| CN109473550A (en) * | 2018-10-15 | 2019-03-15 | 深圳华中科技大学研究院 | A kind of large area perovskite solar battery and preparation method thereof |
| CN111725406A (en) * | 2020-06-29 | 2020-09-29 | 暨南大学 | Ultraviolet photoelectric detector of lead-free perovskite single crystal and preparation method thereof |
| CN112993167A (en) * | 2021-02-07 | 2021-06-18 | 重庆大学 | Application of organic ammonium salt modified metal oxide nanoparticles in positive perovskite solar cell and preparation method of device |
| CN115572946A (en) * | 2022-09-16 | 2023-01-06 | 华为数字能源技术有限公司 | Perovskite preparation method and preparation equipment and photoelectric converter |
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| CN115572946A (en) * | 2022-09-16 | 2023-01-06 | 华为数字能源技术有限公司 | Perovskite preparation method and preparation equipment and photoelectric converter |
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