CN103943368A - Novel germanium-containing perovskite material and solar cell comprising same - Google Patents

Novel germanium-containing perovskite material and solar cell comprising same Download PDF

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CN103943368A
CN103943368A CN201410173750.9A CN201410173750A CN103943368A CN 103943368 A CN103943368 A CN 103943368A CN 201410173750 A CN201410173750 A CN 201410173750A CN 103943368 A CN103943368 A CN 103943368A
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solar cell
perovskite material
layer
germanic
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黄长水
闫星辰
崔光磊
刘志宏
逄淑平
徐红霞
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Qingdao Institute of Bioenergy and Bioprocess Technology of CAS
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Qingdao Institute of Bioenergy and Bioprocess Technology of CAS
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Abstract

The invention provides a germanium-containing material with a perovskite structure, and the germanium-containing material is prepared through liquid phase reaction. The chemical general formula of the germanium-containing perovskite material is AGeX3, AGe (XnY1-n)3 and AGe (XmYnZ1-m-n)3, A is Cs+ or NH4+ or CH3NH3+, Ge is bivalence, X, Y and Z are halogens. The method for obtaining the germanium-containing material comprises the steps that GeO2 is added in hydrogen halide solution, hypophosphorous acid is added in the mixture to recover the GeO2 to be divalent, and then haloids cesium salt or ammonium salt is added in the mixture to directly obtain sediment containing the germanium-containing perovskite material. An FTO/ electronic transport layer/ meso pore layer is provided with the dissolved material in a spin coating mode, and through the spin-coating hole transport layer and evaporation electrodes, a solar cell device based on the AGeX3, AGe (XnY1-n)3 and AGe (XmYnZ1-m-n)3 can be constructed. The material is simple in preparation and synthesis, low in cost, and good in light absorption property, photovoltaic conversion performance and electron hole transmission capacity, and the solar cell device has high stability and long service life.

Description

A kind of novel germanic perovskite material and solar cell thereof
Technical field
The invention belongs to photoelectric material technical field, be specifically related to a kind of germanic perovskite material.
The invention still further relates to above-mentioned germanic perovskite material in the application of preparing in solar cell.
Background technology
Along with advancing of society, the mankind are increasing to the demand of the energy.The energy is divided into two kinds of non-regeneration energy and regenerative resources, and our the used energy mostly belongs to non-regeneration energy at present.Calculate according to the fossil fuel reserves of verifying for 2002, oil, natural gas and coal can maintain respectively about 40,60 and 200 years.Solar energy has the incomparable advantage of other energy as a kind of regenerative resource.Therefore, rationally making good use of solar energy will be the developing long-term strategy that the mankind solve energy problem, and the research and development of solar cell have become a focus in the whole world.
According to the difference of material therefor, solar cell can be divided into: silicon solar cell, multi-element compounds thin-film solar cells, organic solar batteries, dye sensitized nano crystal salar battery.These several batteries have his own strong points, but also all to exist cost high simultaneously, and efficiency is low, toxic, material rareness, various potential danger such as processing technology complexity.In order to make more suitably solar cell, we need to be from meeting large-scale production, and material is easy to get, and on cost is lower, makes an effort.
1991, O ' Regan etc. assembles first photoelectric conversion efficiency and reaches 7.1% ~ 7.9% dye sensitized nano crystal salar battery (Nano-crystalline Dyesensitized Solar Cells, DSSCs), started the uncharted field of solar cell research and development.Subsequently, Gratzel etc. has developed photovoltaic energy conversion efficiency and has reached 10% ~ 11% DSSCs.1998, the people such as Gratzel further develop all-solid-state dye-sensitized solar cell, use SOLID ORGANIC hole mobile material to replace liquid electrolyte, monochromatic light ray photoelectric transformation efficiency reaches 33%, thereby has caused the concern of whole world scientist to DSSC.The photoelectric conversion efficiency of DSSC is stabilized in more than 10% at present, and cost is only 1/5 to 1/10 of silicon solar cell, and can reach more than 15 years useful life.Due to the relatively cheap price of DSSC, simple manufacture craft and potential high-photoelectric transformation efficiency, making it likely replace traditional silicon is solar cell, becomes the leading of following solar cell.
As the one of DSSC, the solar cell using perovskite as sensitizer has obtained increasing concern, and most study is oxide perovskite material.There is ABO 3the oxide perovskite material of structure has much character, and contains element nearly all in the periodic table of elements.Research about oxide perovskite material has (201110102113.9,201110142339.1), but they research be up conversion property.The application of the novel perovskite material of iodide on solar cell is a brand-new field, is also current very popular research direction.Such material of having reported comprises (CH 3nH 3) PbI 3(can referring to: Jeong-Hyeok Im, Chang-Ryul Lee, Jin-Wook Lee, Sang-Won Park, Nam-Gyu Park. Nanoscale, 2011,3,4088), (CH 3cH 2nH 3) PbI 3(can referring to: Jeong-Hyeok Im, Jaehoon Chung, Seung-Joo Kim, Nam-Gyu Park. Nanoscale Res. Lett., 2012,7,353), CsSnI 3(can referring to: In Chung, Byunghong Lee, Jiaqing He, Robert P. H. Chang, Mercouri G. Kanatzidis1. Nature, 2012,485,487), (CH 3nH 3) SnI 3(can referring to: Constantinos C. Stoumpos, Christos D. Malliakas, Mercouri G. Kanatzidis. Inorg. Chem., 2013,52,9019) etc.This class material has certain toxicity, easily to environment.Germanic perovskite is the brand-new photoelectric conversion material of a class, has extraordinary application prospect in DSSC, and not yet someone reports at present.
Summary of the invention
The object of the present invention is to provide a kind of novel germanic perovskite as photoelectric conversion material.
Another object of the present invention is to apply above-mentioned germanic perovskite material and prepares solar cell.
For achieving the above object, the germanic perovskite material for solar cell provided by the invention, chemical general formula is AGeX 3, AGe (X ny 1-n) 3and AGe (X my nz 1-m-n) 3, wherein A is Cs +or NH 4 +or CH 3nH 3 +, Ge is divalence, X, and Y, Z is halogen, is obtained by following preparation process:
1) by GeO 2join in 10 mL halogen acids;
2) in step 1 solution, add hypophosphorous acid by GeO 2be reduced into germanous;
3) in the solution obtaining to step 2, add cesium salt or ammonium salt or the methylamine salt of halogen, directly obtain the precipitation of perovskite material;
4) precipitation step 3 being obtained is centrifugal, dry, in glove box, preserves.
In this synthetic method, add before hypophosphorous acid temperature is increased to 90 ~ 95 DEG C, react 10 min after adding hypophosphorous acid, react 10 min after adding the cesium salt of halogen or ammonium salt or methylamine salt.
The germanic perovskite material AGeX of synthesized 3, AGe (X ny 1-n) 3and AGe (X my nz 1-m-n) 3comprise CsGeCl 3, CsGeBr 3, CsGeI 3, CsGe (Cl nbr 1-n) 3, CsGe (Cl ni 1-n) 3, CsGe (Br ni 1-n) 3, CsGe (Cl mbr ni 1-m-n) 3, NH 4geCl 3, NH 4geBr 3, NH 4geI 3, NH 4ge (Cl nbr 1-n) 3, NH 4ge (Cl ni 1-n) 3, NH 4ge (Br ni 1-n) 3, NH 4ge (Cl mbr ni 1-m-n) 3, CH 3nH 3geCl 3, CH 3nH 3geBr 3, CH 3nH 3geI 3, CH 3nH 3ge (Cl nbr 1-n) 3, CH 3nH 3ge (Cl ni 1-n) 3, CH 3nH 3ge (Br ni 1-n) 3and CH 3nH 3ge (Cl mbr ni 1-m-n) 3.
The germanic perovskite material AGeX of synthesized 3, AGe (X ny 1-n) 3and AGe (X my nz 1-m-n) 3the value of middle m and n is not fixed, and can regulate the content of halogen by the ratio that regulates raw material, and then regulate their position of energy band and spectral absorption scope.
The material that adopts this synthetic method to obtain, purity is higher, and preparation process is simple, lower to equipment requirement.
This germanic perovskite material can be prepared in air, but due to less stable in solvent, while dissolving assembly device, will in nitrogen environment, carry out.
What this patent provided utilizes above-mentioned germanic perovskite material to prepare the method for solar cell, and key step is:
1) germanic perovskite material is dissolved in DMF, is spin-coated on FTO/ electron transfer layer/mesoporous going up layer by layer, leave standstill one day, vapor away solvent;
2) spin coating hole transmission layer on the calcium titanium ore bed obtaining to step 1;
3) on the hole transmission layer obtaining to step 2, gold evaporation electrode, is assembled into solar cell device.
The structure of solar cell device prepared by employing the method is FTO/ electron transfer layer/mesoporous layer/active material/hole transmission layer/electrode.
Wherein, electron transfer layer material therefor comprises TiO 2, ZnO and Nb 2o 5.
Wherein, mesoporous layer material therefor comprises TiO 2, ZnO and Nb 2o 5or insulator Al 2o 3, SiO 2.
Wherein, AGeX 3, AGe (X ny 1-n) 3and AGe (X my nz 1-m-n) 3the thin film-forming method of type perovskite material comprises spin coating, lifts, sprays, and after film forming, obtains being scattered in the AGeX in mesoporous layer by suitable heat treated 3, AGe (X ny 1-n) 3and AGe (X my nz 1-m-n) 3solid-phase construction.
Wherein, in hole transmission layer, P type semiconductor is organic p-type semi-conducting material Spiro-OMeTAD and P3HT or p-type inorganic compound V 2o 5and MoO 3.
This germanic perovskite material can be prepared in air, but due to less stable in solvent, while dissolving assembly device, will in nitrogen environment, carry out.
Above preparation process is synthetic simple compared with silica-based solar cell device, and cost is low, and the life-span is long, and efficiency approaches polycrystalline silicon device, is conducive to spread.
Brief description of the drawings
The theory structure schematic diagram of Fig. 1 perovskite solar cell.
Fig. 2 CsGeCl 3xRD.
Fig. 3 CsGeCl 3ultraviolet-visible absorption spectroscopy.
Fig. 4 CsGeBr 3xRD.
Fig. 5 CsGeBr 3ultraviolet-visible absorption spectroscopy.
Fig. 6 CsGeI 3xRD.
Fig. 7 CsGeI 3ultraviolet-visible absorption spectroscopy.
Fig. 8 is based on CsGeI 3the IV curve of solar cell device.
Fig. 9 TiO 2the SEM photo of mesopore film.
Figure 10 SiO 2the SEM photo of mesopore film.
Embodiment
Below by embodiment, the present invention is further illustrated, but the present invention is not limited to following examples.
Embodiment 1
First synthetic perovskite material.By 1 g GeO 2join in 10 mL hydroiodic acids, be heated to 90 ~ 95 DEG C, then add 1 mL hypophosphorous acid by GeO 2be reduced into divalence, after 10 min, add 2.48 g CsI, have black precipitate to produce.To precipitate centrifugally, put into vacuum desiccator dry, finally obtain CsGeI 3perovskite material.Secondly prepare TiO with sol-gal process 2colloid, is spun on the FTO cleaning on glass, and then 550 DEG C of heat treated 30 min, obtain fine and close TiO 2film.Spin coating TiO in dense film 2slurry, TiO 2granular size be about 20 nm, and then further 550 DEG C of heat treated 30 min, obtain TiO 2mesopore film.By synthetic CsGeI 3perovskite is dissolved in DMF, is then spun to TiO 2on mesopore film, leave standstill one day, vapor away solvent.Finally spin coating hole transmission layer P3HT on calcium titanium ore bed, gold evaporation electrode, is assembled into solar cell device, obtains 3% photoelectric conversion efficiency.
Embodiment 2
First synthetic perovskite material.By 1 g GeO 2join in 10 mL hydroiodic acid solution, be heated to 90 ~ 95 DEG C, add hypophosphorous acid by GeO 2be reduced into divalence, after 10 min, add 1.38 g NH according to mol ratio 1:1 4i, has precipitation to produce.By sedimentation and filtration, put into vacuum desiccator dry, finally obtain NH 4geI 3perovskite material.Secondly prepare TiO with sol-gal process 2colloid, is spun on the FTO cleaning on glass, and then 550 DEG C of heat treated 30 min, obtain fine and close TiO 2film.Spin coating TiO in dense film 2slurry, TiO 2granular size be about 20 nm, and then further 550 DEG C of heat treated 30 min, obtain TiO 2mesopore film.By synthetic CsGeI 3perovskite is dissolved in DMF, is then spun to TiO 2on mesopore film, leave standstill one day, vapor away solvent.Finally spin coating hole transmission layer P3HT on calcium titanium ore bed, gold evaporation electrode, is assembled into solar cell device, obtains 3% photoelectric conversion efficiency.

Claims (9)

1. for a germanic perovskite material for solar cell, chemical general formula is AGeX 3, AGe (X ny 1-n) 3and AGe (X my nz 1-m-n) 3, wherein A is Cs +or NH 4 +or CH 3nH 3 +, Ge is divalence, X, and Y, Z is halogen; Obtained by following preparation process:
1) by GeO 2join in 10 mL halogen acids;
2) in step 1 solution, add hypophosphorous acid by GeO 2be reduced into germanous;
3) in the solution obtaining to step 2, add cesium salt or ammonium salt or the methylamine salt of halogen, directly obtain the precipitation of perovskite material;
4) precipitation step 3 being obtained is centrifugal, dry, in glove box, preserves.
2. as claimed in claim 1 for the germanic perovskite material of solar cell, wherein, perovskite material AGeX 3, AGe (X ny 1-n) 3and AGe (X my nz 1-m-n) 3comprise CsGeCl 3, CsGeBr 3, CsGeI 3, CsGe (Cl nbr 1-n) 3, CsGe (Cl ni 1-n) 3, CsGe (Br ni 1-n) 3, CsGe (Cl mbr ni 1-m-n) 3, NH 4geCl 3, NH 4geBr 3, NH 4geI 3, NH 4ge (Cl nbr 1-n) 3, NH 4ge (Cl ni 1-n) 3, NH 4ge (Br ni 1-n) 3, NH 4ge (Cl mbr ni 1-m-n) 3, CH 3nH 3geCl 3, CH 3nH 3geBr 3, CH 3nH 3geI 3, CH 3nH 3ge (Cl nbr 1-n) 3, CH 3nH 3ge (Cl ni 1-n) 3, CH 3nH 3ge (Br ni 1-n) 3and CH 3nH 3ge (Cl mbr ni 1-m-n) 3.
3. as claimed in claim 1 for the germanic perovskite material of solar cell, wherein, Perovskite Phase AGeX 3, AGe (X ny 1-n) 3and AGe (X my nz 1-m-n) 3the value of middle m and n is not fixed, and can regulate the content of halogen by the ratio that regulates raw material, and then regulate their position of energy band and spectral absorption scope.
4. as claimed in claim 1 for the germanic perovskite material of solar cell, wherein, temperature is increased to 90 ~ 95 DEG C before adding hypophosphorous acid, react 10 min after adding hypophosphorous acid, react 10 min after adding the cesium salt of halogen or ammonium salt or methylamine salt.
5. utilize germanic perovskite material described in claim 1 to prepare a method for solar cell, the structure of device is FTO/ electron transfer layer/mesoporous layer/active material/hole transmission layer/electrode; Key step is:
1) germanic perovskite material is dissolved in DMF, is spin-coated on FTO/ electron transfer layer/mesoporous going up layer by layer, leave standstill one day, vapor away solvent;
2) spin coating hole transmission layer on the calcium titanium ore bed obtaining to step 1;
3) on the hole transmission layer obtaining to step 2, gold evaporation electrode, is assembled into solar cell device.
6. method according to claim 5, wherein, electron transfer layer material therefor comprises TiO 2, ZnO and Nb 2o 5.
7. method according to claim 5, wherein, mesoporous layer material therefor comprises TiO 2, ZnO and Nb 2o 5or insulator Al 2o 3, SiO 2.
8. method according to claim 5, wherein, AGeX 3, AGe (X ny 1-n) 3and AGe (X my nz 1-m-n) 3the thin film-forming method of type perovskite material comprises spin coating, lifts, sprays, and after film forming, obtains being scattered in the AGeX in mesoporous layer by suitable heat treated 3, AGe (X ny 1-n) 3and AGe (X my nz 1-m-n) 3solid-phase construction.
9. method according to claim 5, wherein, in hole transmission layer, P type semiconductor is organic p-type semi-conducting material Spiro-OMeTAD and P3HT or p-type inorganic compound V 2o 5and MoO 3.
CN201410173750.9A 2014-04-28 2014-04-28 Novel germanium-containing perovskite material and solar cell comprising same Pending CN103943368A (en)

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Cited By (9)

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CN104124291A (en) * 2014-07-24 2014-10-29 华中科技大学 Perovskite solar battery and preparation method thereof
CN107195785A (en) * 2017-05-23 2017-09-22 郑州大学 A kind of few Pb perovskite materials and preparation method thereof and perovskite solar cell
CN107325812A (en) * 2017-07-03 2017-11-07 苏州虹霞晶体科技有限公司 A kind of perovskite structure luminescent material and its production method based on anti-solvent
JP2018129506A (en) * 2017-02-10 2018-08-16 パナソニックＩｐマネジメント株式会社 Light-absorbing material and manufacturing method thereof, and solar battery arranged by use of light-absorbing material
CN108831999A (en) * 2018-06-14 2018-11-16 南京邮电大学 A kind of preparation method of accuracy controlling perovskite thin film crystallite dimension
CN108832003A (en) * 2018-06-14 2018-11-16 南京邮电大学 A method of improving perovskite solar cell photoelectric transfer efficiency
CN109786561A (en) * 2019-01-22 2019-05-21 南京华群光电技术有限公司 A kind of technique with perovskite active layer in amine liquefaction perovskite method recycling and reusing perovskite device
CN110311040A (en) * 2019-06-11 2019-10-08 东南大学 A kind of Ca-Ti ore type molecule ferroelectricity photovoltaic material and its band structure regulation method and method for manufacturing thin film
CN112993198A (en) * 2021-01-26 2021-06-18 浙江大学 Germanium-based perovskite photoelectric material, application, preparation method, device and device preparation method

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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104124291A (en) * 2014-07-24 2014-10-29 华中科技大学 Perovskite solar battery and preparation method thereof
CN104124291B (en) * 2014-07-24 2016-08-31 华中科技大学 A kind of perovskite solar cell and preparation method thereof
JP2018129506A (en) * 2017-02-10 2018-08-16 パナソニックＩｐマネジメント株式会社 Light-absorbing material and manufacturing method thereof, and solar battery arranged by use of light-absorbing material
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CN107195785A (en) * 2017-05-23 2017-09-22 郑州大学 A kind of few Pb perovskite materials and preparation method thereof and perovskite solar cell
CN107325812A (en) * 2017-07-03 2017-11-07 苏州虹霞晶体科技有限公司 A kind of perovskite structure luminescent material and its production method based on anti-solvent
CN108831999B (en) * 2018-06-14 2022-03-22 南京邮电大学 Preparation method for accurately regulating and controlling crystal grain size of perovskite thin film
CN108832003A (en) * 2018-06-14 2018-11-16 南京邮电大学 A method of improving perovskite solar cell photoelectric transfer efficiency
CN108831999A (en) * 2018-06-14 2018-11-16 南京邮电大学 A kind of preparation method of accuracy controlling perovskite thin film crystallite dimension
CN108832003B (en) * 2018-06-14 2022-06-03 南京邮电大学 Method for improving photoelectric conversion efficiency of perovskite solar cell
CN109786561A (en) * 2019-01-22 2019-05-21 南京华群光电技术有限公司 A kind of technique with perovskite active layer in amine liquefaction perovskite method recycling and reusing perovskite device
CN109786561B (en) * 2019-01-22 2023-07-11 华清创智光电科技(清远)有限公司 Process for recycling perovskite active layer in perovskite device by amine liquefied perovskite method
CN110311040A (en) * 2019-06-11 2019-10-08 东南大学 A kind of Ca-Ti ore type molecule ferroelectricity photovoltaic material and its band structure regulation method and method for manufacturing thin film
CN112993198A (en) * 2021-01-26 2021-06-18 浙江大学 Germanium-based perovskite photoelectric material, application, preparation method, device and device preparation method
CN112993198B (en) * 2021-01-26 2022-02-08 浙江大学 Germanium-based perovskite photoelectric material, application, preparation method, device and preparation method

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