CN106299127A - A kind of preparation method of novel lead-free P-N junction methylamine bustamentite perovskite battery - Google Patents
A kind of preparation method of novel lead-free P-N junction methylamine bustamentite perovskite battery Download PDFInfo
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- CN106299127A CN106299127A CN201510358528.0A CN201510358528A CN106299127A CN 106299127 A CN106299127 A CN 106299127A CN 201510358528 A CN201510358528 A CN 201510358528A CN 106299127 A CN106299127 A CN 106299127A
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Abstract
The invention belongs to perovskite photovoltaic cell field, disclose a kind of unleaded P-N junction methylamine bustamentite and derivant perovskite battery thereof, including substrate, transparency electrode, N-type methylamine bustamentite and derivant perovskite semiconductive thin film thereof, p-type methylamine bustamentite and derivant perovskite semiconductive thin film, rear electrode.The present invention passes through P-N homojunction or the hetero-junctions of the intermembranous formation of perovskite semiconductor film, light is conducive to excite the efficiently separating and transmitting of electron-hole pair of generation, rely on unleaded methylamine bustamentite and the long-life carrier of derivant perovskite quasiconductor self thereof simultaneously, the high-photoelectric transformation efficiency of battery can be realized.Additionally, the present invention is without preparing hole transmission layer, thus simplify the preparation technology of existing perovskite battery, reduce preparation cost；Use metal Pb without a large amount of, be conducive to green, the industrialization process of environmental protection.
Description
Technical field
This new technique/technological invention belongs to methylamine bustamentite perovskite solar-energy photo-voltaic cell device technology industry, and correlation technique manufacturing process.
Background technology
No matter the early stage mankind exploit the fuel energy of carbonization stone in a large number, or the oil shale energy (shale oil) of recent development, these broadly fall into non-renewable energy resources, bring the disaster of serious carbon dioxide pollution, greenhouse effect and unusual weather conditions to the earth.Over the crystal silicon solar technology of sixty-year-old, not only production cost is too high, and there is the contamination hazard of Silicon chloride..Plus nearly 2 years silicon production capacity surpluses, the vicious cycle of distress sale between industry, and the drawback such as external double counter sanctions, advanced technology country has shifted focus development thin film solar technology, as used the CIGS thin-film and Cadimium telluride thin film heterojunction solar technology that vacuum coating manufactures.The exploitation of these thin film techniques and commercially produce just at high speed development, compared with silica-based solar, they the most singly have obvious production cost advantage, and its conversion ratio is the most close to even more than silica-based solar.
Since two thousand nine start a kind of employing methylamine bustamentite (CH3NH3PbI3 occurring and developing rapidly, it being abbreviated as MALI) perovskite material and derivant thereof be as the brand-new thin film technique of light absorbing zone, it uses low cost production thereof plated film, and carrier can maintain longer electron-hole separation state in film layer, carrier can be prevented effectively from and recombinated before operation to forward and backward electrode.This kind of methylamine bustamentite perovskite battery is to use without the intrinsic semiconductor mixed as photovoltaic absorption layer, rather than p-type or N-type mix quasiconductor.
Usual this kind of methylamine bustamentite perovskite battery needs to add the titanium dioxide layer of porosity and looseness, ensures that the large area of methylamine bustamentite perovskite material is adhered to fully absorb sunlight.Additionally, the organic cavity transmission layer (HTL) that methylamine bustamentite perovskite battery also needs to one layer of less stable carrys out effective transporting holes, to recombinate with hole before hindering electronics electrode after arrival.Price is sufficiently expensive owing to purity requirement is high for this organic cavity transmission layer, and the hole transmission layer simultaneously using existing general solwution method to prepare contains pin hole, is easily caused the infiltration of dampness and reduces methylamine bustamentite perovskite battery performance.Above-mentioned two-layer interpolation material and technique thereof cause increase and the complexity of technique of methylamine bustamentite perovskite battery cost, for solar energy farm, require that battery maintains the life-span of more than 30 years in the desert Environment of the big dust storm of high temperature, be the most arduous a challenge.
A kind of methylamine bustamentite perovskite battery of research and development can remove the hole transmission layer of costliness, instability and complex process from the recent period4, the substitute is in titanium oxide film layer, attach zirconium oxide (zirconium oxide).Zirconium oxide can play the effect that hole transmission layer is the same in the battery, i.e. hinders the restructuring before electronics and hole electrode after arrival.Though the photoelectric efficiency of current this kind of methylamine bustamentite perovskite battery the most successfully accomplishes 11.6%, but less than the methylamine bustamentite perovskite battery efficiency with hole transmission layer.The most this methylamine bustamentite perovskite material also needs the cation adding 5-aminovaleric acid to reinforce its contacting with loose titanium oxide film layer, also needs to one layer of fine and close titanium oxide film layer simultaneously.
Methylamine bustamentite perovskite battery is in addition to above-mentioned meso-hole structure, and also a class is planar structure.Methylamine bustamentite perovskite absorbed layer in plane perovskite battery is neither P-type semiconductor is not N-type semiconductor, but neutrality.Therefore the structure of plane perovskite battery is p-i-n type, it needs to use hole transmission layer as P-type semiconductor, it is also required to titanium oxide film layer as N-type semiconductor, so its preparation or be unable to do without and use expensive, the unstable and hole transmission layer of complicated technology.
In sum, the no matter preparation of the methylamine bustamentite perovskite battery of which kind of structure, nearly all it be unable to do without and use hole transmission layer or add other film layer to hinder the electronics restructuring with hole (although compared to other photovoltaic cell, carrier lifetime in methylamine bustamentite perovskite battery is long, electronics and cavity energy maintain long released state, can be prevented effectively from restructuring).In addition to the complexity of hole transmission layer, the methylamine bustamentite as perovskite battery obsorbing layer also can be dissolved in water, is therefore easily subject to deliquescence, and containing heavy metal element lead, is unfavorable for realizing green, the industry process of environmental protection.
Summary of the invention
The present invention provides the methylamine bustamentite perovskite battery of a kind of simplification, and this battery was both avoided that/reduces the use of heavy metal element lead, moreover it is possible to avoid using complicated process of preparation, unstable properties and expensive hole transmission layer.It is proposed that use P-N homojunction or the plane methylamine bustamentite perovskite battery structure of hetero-junctions, be conducive to light to excite the efficiently separating and transmitting of electron-hole pair of generation, the long-life carrier of methylamine bustamentite perovskite absorbed layer self can be relied on to realize high photoelectric transformation efficiency simultaneously.
Have theoretical research at present to show, can get p-type methylamine bustamentite perovskite quasiconductor by manufacturing lead vacancy defect, can get N-type methylamine bustamentite perovskite quasiconductor by manufacturing methylamine functional group space6.The energy level of these defects (lead vacancy or methylamine functional group space) very close to conduction band or the edge of valence band rather than is positioned at band gap deep layer, so being not result in the restructuring of electron-hole pair.Specifically, the energy level of space methylamine functional group is positioned at below conduction band at 0.05eV, and the energy level of lead vacancy is positioned at above valence band at 0.2eV.
The present invention uses the P-N junction methylamine bustamentite perovskite thin film of low cost, between the sandwich transparent front electrode on upper strata and the rear electrode of lower floor, glass, flexible polymer or metal basal board can be used as substrate.Different from traditional methylamine bustamentite perovskite battery, it without the titanium dioxide of porosity and looseness as electron transfer layer, it is not required that complex process, unstable properties and expensive hole transmission layer.
Meanwhile, it is proposed that the lead element using tin element to replace makees cation to reduce environmental pollution, it is possible to use wolfram element replaces, coating process suggestion includes solution spin coating or sputtering.
Accompanying drawing illustrates:
Fig. 1 is the cross-sectional of tradition methylamine bustamentite perovskite battery；
Fig. 2 is the cross-sectional of methylamine bustamentite perovskite battery of the present invention；
Fig. 3 is the energy band schematic diagram of P-N junction methylamine bustamentite perovskite battery of the present invention.
Detailed description of the invention:
Fig. 1 is the most general methylamine bustamentite perovskite battery technology, using glass or polymer is substrate (1), the stannum oxide (FTO) plating indium tin oxide (ITO) or doped with fluorine makees transparency electrode (2), or other similar high light permeable rate, high conductivity material；The lower floor of transparency electrode is titanium dioxide, aluminium oxide or other similar mesoporous material (3)；Then the lower floor of mesoporous material is methylamine bustamentite perovskite absorbed layer (4)；Lower floor is hole transmission layer (5) again, such as spiro-OMeTAD；It is finally rear electrode (6), as golden or silver-colored.
It is 0.2 μm that each thicknesses of layers is respectively as follows: FTO or ITO, loose mesoporous titanium dioxide layer is 0.5 ~ 2.0 μm (some methylamine bustamentite perovskite battery can add the compact titanium dioxide film of one layer of 0.06 μm to regulate energy level between mesoporous layer and transparency conductive electrode), methylamine bustamentite perovskite absorbed layer is 0.3 μm, hole transmission layer is 0.3 μm, and last metal electrode is 0.1 μm.Substrate can use glass, polymer or metallic plate, the most cheap substrate to be soda-lime glass.
Described below is the perovskite with MALI as representative and derivant solar cell thereof, including some organic material such as R.NH3.PbI3 or HC (NH2) 2 PbI3, or completely or partially replace lead with stannum or tungsten, or other halogen (such as chlorine, bromine or fluorine) is used completely or partially to replace iodine.The most above-mentioned methylamine bustamentite perovskite film layer also can carry out mixing of a small amount of trivalent metallic element (such as boron, aluminum, gallium, indium).
Claims (8)
1.First claim of the present invention is:As in figure 2 it is shown, the title of its device is consistent with Fig. 1；The most newly added film layer is N-type methylamine bustamentite perovskite film layer (7) and p-type methylamine bustamentite perovskite film layer (8) respectively；The thickness of N-type thin film is 0.1 ~ 1.0 μm, and preferred thickness is 0.2 μm (this thickness is the most favourable to electric transmission)；The thickness of p-type thin film is 0.5 ~ 200 μm, and preferred thickness is 1 ~ 2 μm, and its resistivity is 50 ~ 200 Ohm.cm, preferably 1.0 ~ 10 Ohm.cm；The preparation technology of P-N junction methylamine bustamentite calcium titanium battery is varied, such as inorganic film and metal level in battery can use the method for sputtering to prepare, and light absorbing zone can use spin-coating method to prepare；Light absorbing zone is preparation technology concretely comprise the following steps: use 60 ~ 65 DEG C, 100 μ L concentration be N, the N-dimethylformamide solution of lead iodide of 1M, through 3000 r/min, 15 seconds spin feedings, substrate plates bustamentite；Then the substrate of good for spin coating bustamentite is immersed in the iodine methylamine solution of 60 ~ 80 DEG C 1 ~ 5
Min, cleans through isopropanol, and nitrogen dries up, and wherein iodine methylamine solution is to use the 100mg/ml isopropanol of 60 DEG C to make solvent, can add the lead chloride of 20% weight ratio to increase chloride ion simultaneously；There is different crystal phase structures, so the crystal phase structure of thin film can change along with temperature and the change of exposure degree in general methylamine bustamentite perovskite and derivant thereof；Further, light absorbing zone thin film prepared by solwution method will not produce luminescence generated by light phenomenon, can be shown that do not have atom defect center in the band gap of thin film；Carrier concentration can be less than 109/ cc, if atom defect center is embedded in band gap deep layer, they can become the compound trap of electron-hole pair；It is very suitable for preparing perovskite absorbed layer based on solution spin-coating method seen from this；Simultaneously, stannum is used to replace the luminescence generated by light derivant of lead also can prepare by non-solwution method, produce N-type methylamine bustamentite perovskite quasiconductor including the heating in sealing pipe by lead iodide and methylamine iodine, maybe viscous mill material is produced p-type methylamine bustamentite perovskite quasiconductor in the heating of non-tight pipe；Above-mentioned way all can replace lead with tungsten；P-type methylamine bustamentite perovskite quasiconductor can be prepared with a small amount of lead iodide, i.e. uses lead chloride and methylamine iodine solution to prepare methylamine bustamentite perovskite absorbed layer；Also can be with different halogen material (i.e. with the chloride of heterogeneity, bromide, fluoride or iodide)；With sample preparation method can use heating in vacuum to the lead element that volatilizees, or other volatile compound (such as the selenium in CIGS, or the zinc in zinc sulfide)；Equally, N-type methylamine bustamentite perovskite quasiconductor can use a large amount of methylpyridinium iodide amine forcibly to allow methyl amine functional group playback in clearance position；Or use methylamine gas or solution, hydrogen can be used when using methylamine gas simultaneously, prepare under the air of 1.1Pa, forcibly allow methyl amine functional group playback in clearance position；Another kind of way, the mixing of N-type methylamine bustamentite perovskite quasiconductor can be varied the atomicity of cation and complete, as used three-group metal element (such as aluminum, gallium, indium or boron) to replace lead；Because the outermost electron track of substitution atoms is with 3 positive charges rather than 2 of original lead；This replaces the copper of unit price with interpolation bivalence cadmium in CIGS thin-film solar cell, and it is the same for preparing N-type CIGS to optimize the way at PN junction interface；The electric conductivity of semiconductive thin film to be optimized, only need to mix the impurity of indivisible (ppm level)；It is similar in CIGS thin-film solar cell, mix monovalence sodium, and sodium occupies the brilliant position of trivalent indium, only need the sodium of 0.05 ~ 0.1 atomic percent just can improve the electric conductivity of P-type semiconductor film layer；In like manner, joining pentavalent phosphorus and promote the electric conductivity of N-type semiconductor thin film, also have only to the phosphorus of 0.1 ~ 100 ppm in crystal silicon thin film solar cell, the elementary cell constant of the methylamine bustamentite perovskite quasiconductor that trace mixes simultaneously is unaffected；Fig. 3 is the energy band schematic diagram of P-N junction methylamine bustamentite perovskite battery；Wherein the 9th the suitable metal anode being to collect hole；10th the suitable N-type semiconductor being to collect, transmit electronics, such as the zinc oxide being plated on FTO or ITO or titanium oxide film layer；11st is p-type methylamine bustamentite perovskite quasiconductor or derivatives thereof；12nd is N-type methylamine bustamentite perovskite quasiconductor and derivant thereof；13rd is P-N junction region；14th is valence band edge；15th is conduction band edge；16th is fermi level, and for methylamine bustamentite perovskite battery, the band gap between conduction band and valence band is 1.52
eV；For preventing electronics and hole-recombination, the conduction band positions of methylamine bustamentite perovskite quasiconductor and derivant thereof is compared with the conduction band positions of its adjacent materials, it should low 0.0 ~ 0.3 eV；Its valence band location is compared with the valence band location of the thin-film material that it is neighbouring, it should high 0.0 ~ 0.2 eV7；Meanwhile, the P-N junction of methylamine bustamentite perovskite quasiconductor is preferably homogeneous P-N junction；The hetru P-N junction being different between CIGS thin-film and cadmium sulphide membrane should be noted that can band coupling；The methylamine bustamentite perovskite of p-type or N-type all can use as the p-type of other composition hetero-junctions or n type material；Meanwhile, methylamine bustamentite perovskite quasiconductor is direct band gap material, is conducive to the raising of efficiency as copper-indium-gallium-selenium semiconductor.
2.Second claim of the present invention is:Such as the methylamine bustamentite perovskite battery of Fig. 2, the lead element of the 8th p-type methylamine bustamentite perovskite semiconductor film completely or partially can replace with wolfram element；Owing to tungsten exists divalent oxidation state as lead, and there is similar atomic wts (tungsten is 183.83 and lead is 207.19), but want height compared to stannum (118.69), therefore be likely to cause the Quantum geometrical phase effect of class leady；For avoiding this effect, present claims suggestion uses tungsten dichloride, and it is a kind of liquefiable nonvolatile pale yellow solid at 500 DEG C, water soluble, at wet environment not facile hydrolysis, and being different from the halogen tungsten compound of high oxidation valence state, it is difficult to chemically react；But owing to can decompose when tungsten dichloride dissolves, coating process is preferably spin-coating method or vacuum sputtering, and should not use evaporation；Plated film need to carry out avoiding the oxidation of tungsten under noble gas (such as nitrogen) environment simultaneously；Equally, pure iodine device can prepare tungsten iodide thin film with spin-coating method or vacuum sputtering；The preparation of perovskite light absorbing zone thin film can use radio frequency cosputtering methylamine bustamentite perovskite and tungsten dichloride/tungsten iodide, it is possible to the single target material using radio-frequency sputtering to contain methylamine bustamentite perovskite and tungsten dichloride/tungsten iodide is prepared；Can be heated or not heated in the middle of sputtering simultaneously；Plated film can use the annealing process of 200 DEG C to promote crystal growth after completing；Methylamine bustamentite perovskite quasiconductor after optimization, list can use iodine to be used as different halogen material to regulate its energy gap；In addition bivalence tungsten has less ionic radius, and mixing of it can reduce lattice paprmeter, changes the energy gap of methylamine bustamentite perovskite quasiconductor；Such as CIGS thin-film solar cell, manufacturer intentionally adds the indium that gallium replaces nearly 30%, expands energy gap and absorbs broader solar spectrum with help, it be also possible to use sulfur to replace selenium for absorbing more photon；But, the energy gap of stannum attribute perovskite battery is little compared to lead attribute perovskite battery, uses band gap engineering to design and more preferably replaces atom；P-type methylamine bustamentite perovskite quasiconductor to be prepared, tungsten and the lead of different atomic ratio can be used, owing to perovskite semiconductor film comprising only the lead element of ppm magnitude, slightly heat the lead that just can drive these trace away, be therefore readily devised out the perovskite thin film of lead vacancy defect；The present invention has only to the lead element of trace and mixes and realize atom defect design, far below the lead content of tradition methylamine bustamentite perovskite used in battery；Use vacuum pipe method to prepare methylamine bustamentite perovskite quasiconductor, a small amount of lead can be used to be set in the annealing cold end of pipeline to realize mixing of micro lead；The use of these micro lead elements can keep the nonhazardous that industry is applied.
3.3rd claim of the present invention is:Use sputtering technology to prepare to mix or pure methylamine bustamentite perovskite absorbed layer；The present invention includes tungstenic or lead, or traditional leaded halogen-containing methylamine bustamentite perovskite battery, also includes that tradition contains hole transmission layer, or containing titanium dioxide or zirconium dioxide etc. without the methylamine bustamentite perovskite battery mixed；Equally, N-type methylamine bustamentite perovskite quasiconductor can use sputter coating；The preparation of target can first be clayed into power with the perovskite solution of ginseng aluminum is viscous together with the halogen compounds of aluminum chloride or three-group metal element (including indium, gallium and boron), this mixture of powders vacuum cold compaction or hot pressing is formed；It is used as traditional radio-frequency sputtering, or uses the fixing or magnetron RF sputtering system mode of movement；It is used as DC pulse sputtering to prepare electric conductivity and suitably mix perovskite quasiconductor.
4.4th claim of the present inventionMain purpose be to prevent the chain rupture of P-N junction；In the case of preferable lattice is intact, carrier can preferably pass through P-N junction region, thing manufacture N-type silicon chip is mixed as added in the P-type silicon sheet of crystal silicon solar energy battery, thus form P-N junction region, in p-type CIGS thin-film, and for example add cadmium ion, manufacture N-type copper-indium-gallium-selenium semiconductor film layer；Or use extension coating method, and use heterojunction material to constitute P-N junction, the differences between lattice constant of its semiconductor film is less than 10%；For manufacturing P-N junction methylamine bustamentite perovskite battery, three-group metal element (such as aluminum, gallium, indium and boron etc.) can be mixed at the upper epidermis of p-type methylamine bustamentite perovskite semiconductor film and convert thereof into n type material, add these metallic elements a small amount of, complete to mix through pervaporation or the technique such as sputtering and annealing；Similarly, the halogen compounds of three-group metal element (such as aluminum, gallium, indium and boron etc.) can carry out mixing and heat treatment in an identical manner；It practice, lesser amount of lead iodide can be used to prepare p-type methylamine bustamentite perovskite quasiconductor, the iodide being also accomplished by more three-group metal element carry out the content of iodine in compensation film preparation；And three-group metal element is more prone to mix at lead vacancy；This mix with Cd lean copper p-type CIGS thin-film copper empty place formed N-type semiconductor thin film principle identical；General technology is, uses and mixes metal (50 ~ 90 DEG C) at low temperatures heating 10 ~ 30 min having low concentration (0.0015M), preferably heats 20 min at 60 DEG C.
5. 5th claim of the present invention is:Methylamine bustamentite perovskite quasiconductor is mixed in the method preparation using ion implanting；Ion implanting is usually used in the inorganic semiconductor of silicon one class, but the most also uses it to make organic material；The method that can use ion implanting is at room temperature prepared and is mixed hybrid inorganic-organic methylamine bustamentite perovskite semiconductor film, can make up lattice damage through subsequent anneal.
6.6th claim of the present invention is:Encapsulation technology about methylamine bustamentite perovskite battery; to prevent in battery each thin film by the chemical attack of air; conventional solar energy and the encapsulation technology of flat panel display can serve as reference; for protecting the organic-inorganic material film layer of the present invention; prevent dampness and oxygen invasion and attack, need to separately add cover glass.
7. the claim more than is directed to P-N junction methylamine bustamentite perovskite and the solar cell of derivant thereof, is not limited to single celled solar battery structure, the same it can also be used to the batch production of the only block of large area with CIGS thin-film solar cell, uses transparency electrode.
8. last, front and back electrode is the same with other thin film technique, it is possible to use nanoparticle conductive material, carbonaceous conductive material, consume the materials such as micro-tube material, Graphene, and substrate can use glass, flexible polymer or Metal Substrate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108400331A (en) * | 2018-02-05 | 2018-08-14 | 超威电源有限公司 | Secondary cell |
| CN109713131A (en) * | 2018-12-30 | 2019-05-03 | 华北电力大学 | A kind of organic inorganic hybridization perovskite homojunction solar cell based on n-i-p structure |
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2015
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108400331A (en) * | 2018-02-05 | 2018-08-14 | 超威电源有限公司 | Secondary cell |
| CN108400331B (en) * | 2018-02-05 | 2021-07-16 | 超威电源集团有限公司 | Secondary battery |
| CN109713131A (en) * | 2018-12-30 | 2019-05-03 | 华北电力大学 | A kind of organic inorganic hybridization perovskite homojunction solar cell based on n-i-p structure |
| CN109713131B (en) * | 2018-12-30 | 2020-10-09 | 华北电力大学 | Organic-inorganic hybrid perovskite homojunction solar cell based on n-i-p structure |
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