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GB2528831A - Perovskite pigments for solar cells - Google Patents

Perovskite pigments for solar cells Download PDF

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Publication number
GB2528831A
GB2528831A GB1410011.9A GB201410011A GB2528831A GB 2528831 A GB2528831 A GB 2528831A GB 201410011 A GB201410011 A GB 201410011A GB 2528831 A GB2528831 A GB 2528831A
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metal
layer
oxide
perovskite
powder
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GB201410011D0 (en
Inventor
Eurig Jones
Peter James Holliman
Matthew Lloyd Davies
Arthur Connell
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Swansea University
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Swansea University
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F71/00—Manufacture or treatment of devices covered by this subclass
    • H10F71/138—Manufacture of transparent electrodes, e.g. transparent conductive oxides [TCO] or indium tin oxide [ITO] electrodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/20—Light-sensitive devices
    • H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
    • H01G9/2031—Light-sensitive devices comprising an oxide semiconductor electrode comprising titanium oxide, e.g. TiO2
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00—Constructional details of devices covered by this subclass
    • H10F77/10—Semiconductor bodies
    • H10F77/12—Active materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00—Constructional details of devices covered by this subclass
    • H10F77/20—Electrodes
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/50—Organic perovskites; Hybrid organic-inorganic perovskites [HOIP], e.g. CH3NH3PbI3
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
    • H10K30/15—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2
    • H10K30/151—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2 the wide bandgap semiconductor comprising titanium oxide, e.g. TiO2
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/542—Dye sensitized solar cells
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/549—Organic PV cells
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Power Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

A method of making an electrode to be used in solar cells, where a metal oxide and a perovskite pigment is mixed without using hazardous solvents and the powder mix is heated to anneal said powder onto the electrode or metal oxide layer. This process can be used to produce solar cells in a more environmentally friendly and efficient way because damage caused by using hazardous solvents is mitigated by the Solid State process. When fabricating a solar cell perovskite precursors can be dispensed upon a mesoporous TiO2 scaffolding layer 3, 4 by spin-coating before being annealed or heated at 100 degrees for 45 minutes. A hole transporter layer, e.g. spiro-OMeTAD, can be deposited upon the perovskite metal oxide layer to enable a second electrode to be later formed.

Description

Peravsidte Pigments for Solar Cells Fieki of the bnation The present invention relates to a methcd of making pcrovskitc pign3nis and in; pardeular hut njE ecI usiveiy to the use of solid state reactions to process those pigr icz.ts TtK ivven.unn fUrther ielaLs die Jse of ef asenh' po.edures sis that these td.fliCJtS ma" be safely mc crpoi atod ii oI ii u ts without the nec u to USc hazardous ojvert..
Badigrour$ ofIthe First generation (crysLdlmt s1iIon and second ge ictation (arnphoro.is s'con, thin THin (die or copoer mchurn gadium (di)sclenic e omrnon1y known a' ClGS' co1a cells (cr phctdvoltaic cells 4W cells) generate electricity from s.unlight.through. the photovoi:taic effect. The phct<n'oltaic effect is observed, when incident sunlight promotes electrons' jn a scimc:mduet; ng material from the v&erice band, to te conduc don. band. This effect. allo.ckc'trons to diow through a circuft attached t& c&L.Snlth.: eilis *haed on sihcon semiconductors have been knowh. tot fnaay yeth's and exteniye. reae±ch has Ted to the d clot meet of re1ative.l.efftcient ersions (2O % coinersior of scident s&dar energy into electnutv) Houver the high cost of the niateridla and ec,xppiçated prgdtictioit,nwtjtods have blnered large scale prodqction. çf silfeonbased ?V modules bath the'rcsuh that: such silicombaaed o1ar cclls. and the ekctrioiy.enerated from.f eu,Ih as run.aned. .rekttivelty expetsive.
Second geaerton (Lni1m) mu thrd generation (d'sen-itmci or nrgnic photovctai -OPVi scar cells have been dctck'pcd as an ahernauve to whcon basest ceU Dye-scnsmsed sothr cells (PSSCI, weLt devclocd as Lady as 1991 b:r (YRgan and (iriitzei and can he ptod.uced Using. tow cost materials aM relatively simple mn.anmacturtng techniq s which cr be scaled up using roll-to' oil processinu.
A tp'eal DSSC includes an anode Compr sng a ui ed 1102 layer on an intl urn-tm oxide (ITO) coated conducting subtrafe; a. metaltI.c catlude on a secn4 conducin.g sLhstratc, a-elecuolyte seflrating the cathede and anode, M a circuit cornevtng the anode and cathode. The two condutng suktrates font. two sides oi a seated utht.
tnclosing the electroMe and the electrodes. At least one of the ccnducting substrates is opticaLly transparent. to ali.ow solar energy to enter the cell, Perovsk.ite sokw ce s:use a perovskite-bsed pigment. to absorb hia, The pigment can.
he attadhed either to a me porous metI oxide film otto a planar metal oxide surilce.
The metal oidclo eat be taken froths hugo range but typically tItanium ifioxide or alumjun*n u'o& is used Duun operalion icc'dcnt light smkes t'c pgtncat and promotes electrons with sufficient energy across the hand gap Charge is then extracted from the pigment in.the. form of negatively charged e ctrons which tnwe3 to one electrode which is usually a compaet titanta layer end posttuvciy enargod holce whidh. itavlel to the opposite ëletrode -cia a hole tdinsport medium sucth as spiro-' OMcTA1T}, Povsce solar.ceUs v generate lrgc voltages and currents. 1.0 V agd 15 mA cm resulting indevice eftkiencies of 1>1 3% however; a disadvantage of petovsllcite*-hased solar cefls is that the pet.ovskite pigments roust. be synthesized using Thxic. solvents suok as dItnethyl fdrinamide or gamtna.butvroiaetone. This: problent is ihtensif.ed hecause the toxic organic sotvents are evaporated during device processing.
hurthernore, peiovsk&te pgrnents are synthest7ed fion component oiga no amine halide salts and a metal halile. However these. difièrent components have different ohibi.hties. depending on the organic atnines, halides or metal ions used. in addifion heating of thç initial, precipitate fogie4 after these. components hzwe been mixed.
meaps that voIat1e components are often lost, front the pigment.. T[bir, nutkes i difficult to control the preOisO stoichionetry of tue final pigment and cart also make it.
YCIY di ificult. to produce ortie.particWat p.erovakne pigments.
j5 an 1ni of the ptesen invention to oveniome te disadvantages of the prior art by ptosiding a process that eliminates the need to use tØxic sven and nthidh j<ç.
cnah es m k h more praise contr of the stotchiometry of the pero\ skitc pgniuU lm mjxing. the constituent.igment precursor. .matenals fri the corrtc.t stoi.chiotiietxy to create the desired. pigments using solid state reactions.. The present. invention also describes prccdurcs to slf-assetble the pie-made perovskite pigments into solar ccli devices either b\ using affect mixing ii; another so1 em-free, ohd stak reactIon or by using linker molecules and non-toxic solvents or by using a coi.nbm.atn.m. Of bOth, 01' these procedures.
Siimmt ot tht lii vmitnn cecdtnp to a u asp&cl of the pien inve'itinn there > mcvnted a method ol making an electrode to be used. fl: solar. cells, the rn thod compriing coating a) a.
surface of an electroce o-I') L melal crode I iyer cflvermp,aid eleLtrodo with a powder mbc ineftiding at least pnç metal palde and a pcrcryskitç ThFowing which the.
powder mix ia heated anut.ai said powder mix not the electrode or inea. ode:.
layer; It. is:envisagcd that the:.elcaodc is.forme cf..a conducting substra.t that. is optically trausnarent.
1.'yjicaII the conduetllng substmte is metal, tiass or a pciymer coated with n opft ally trnnspareht condudiiig iayt.r.
It j envisage.d that C conu.ctjpg.salstrate i coated. with a metal grid and/or indium hi oxide and/or fluorine-doped tin oxid,o ht4 mnstprefer.ahy it is coated iitft fluorine doped tn o*ide. coated. gaas Prelk ahi wiicrc tho dC uode a t. overed h) a metal O\dt L the I yrr sl-oulJ have. a thickness of at least turn more preferahi.y at least 3m, and even more prJLrably at least lQnm I he compact layer is coated substantially across the whoLe surth.ee of one: bce of the coii.ductiI:og substrate so tnning a coherent film on the substrath sürthcé.
ft is envisaged tbatthe metal oxide. compact layer is coated With a.mesoorou metal oxtde iaer The provson o" a metal oxwle assists more of tin pigmert ii be ng deposited metal hxide surfaee It is envisaged that the mesopomus layer of metal oxide may h* ave. a thickness of up to Sthtm. uitdNy UP.: to lOm, for example upto 5nn.
:Prefratd metal oddes:j the. powder mix are transiEion mctu oxides or rare earth metal oxides, including n1xed metal oxides: Or PhitturQs theteof M:osr preferred are transitioc metal oxides, P.refeiahly e n&etai oxide Is jec.ted ffc)m cme or more. csf aluminium oxide, j oxide, tiohium oxide. zinc, oxide and titanium *dioxide Utamum dioxide or ainminiom oxide are especially preferred.
?rekrably the pc.rovkftc 1. a oganpetihahd.e.pcrovskitc.
Preftu&iy the p.erovskitc is selected &rn one or mere of lead ha.idc-aik4 amine.
q.Jt, irckdn' CH,N}i3PhBr. C h Cl lNH3PhBr CHNUPhl2 and ki ønsageci that. the pereyskie is mie4 with etI or, more pigments.
It is envisaged that the one: or more i.gmcnts iiith.des quantum dot ao4 fucther perovskte pigments.
Pmfc.rred quept.um. clots hche one ions of cations of gallium qr cadmium or. .1e vrth an uu.s m2uwvg arcaidc tlpudc, bdc)teo r te unde It is.envisayed that a dye: is inc.iude.d..in tbe.powder The dye issekcted to have eompiuncntary light absorption to The. .nne. or more nigments on the metal oxid.e sur&e and can e used to improyc the abso.rbanee oil] V/visible light of a solar cell and in particular a.layer of pemvskite-eoated.eop0rous flQ..
Ic is also envisaged that the. amount of dye can he adjasted. to c.hiigethe c.opur of a sor ccii comprising a layer of perovskIteeoathd incsoporou TiC)2..
tooM1r". to i tj:":'s' of the Lnwentton Sc 3 p"t g, firs 4* (ónnedI!ry a method t:j.'s:: &"dSd os t s:'" " cot,sØçpfl4çQfl4qçflg,",fl,,, and ns'b:wntj$efl'a',tM'tbót"& tbe dice,', stt&ti', , d'dig s Se of st'S leS gflç: of the. ctrqdj optAeay eansYØ, : aS:wlwetn tb,' ls d màAt. oxide.coM, øne pigs't Prejkably then s a charge athr such as a tiole ttaspwt matedai eleatrolyk ! tt"Ssagd S tfis:eSitS' ,:"Ssg.&c',',,diagstu, ,.
tflc'c9p4uci,'. S*,,t:oPfr'fl,,flS ft S ttw' that the Thit:' S nønd, *Snathi& s4b**,, are $14 tUrt s seOk' efldS". :eda' S' H âfl,. M $: $fl"tht itrole; Mnt ccli U suit ably comprkes an eleetneat circuit cotntedng the anode an the mdiodt th ttrJ apd ççç41çflp4ct " ttl a''é 4j atXWsay e. n4,:d,.,..
or csn"ajc;Wi ithoØ 01 tE. te: a't *& tb*d" bioth 0* ,j &a.
Th* ,#,S,a,y bnie,, . 1*w!!t1 tupOUnt% u'4a''4 and S,:fltphW#t øionb*a4 The:cSd,,, j$:.1 be fin" t"a: cos'b' n: tg:S S*ate iot- 6pwexarnft* ,,,,,,, ,,dctlpgp4,, ,:.. includëPEDOT a,, "$thOMotAt..
6. &:". tsi pet*W tàft'd SWt&1ø,sp lid W',,:Jñ,,..
hdk"pShu'' Sut't Solid tt4:S$t$ su'i' asftuJ: 4'or c*wSs: :P*F, k as $ spirobnluorcae spro-OVe AD) or pois meric Fole transpon 7Ialenals such &s paRC 4etnienedioxvthrnphent polyisyrenesaP'oiat& (P1 DOT PSS, schAch may be doped to Improve conduetivity or instance with lithium salts oran antioxidant.
Pardeularadvantages of tile present inenthm are that it avoids the need to se toxic solvents lit th prcpatution of the pigment materials or the sohir ccli device. In as tie solar (oil typna ly itciuds reiovski gmens nut I' tv to us.
solvents elintinates sny limitations.qausçd. y varying so.luh.ihty. :ikitther there is. the advantage that a oiar cell prpvide$ by the present hwenti.on. pbcrbs more light at a *specittc wavelength titan a.comparbie oiar cell because of the:a.hn ty to eqntroj the amctnt of pign ort in. the ccii.
lkkf Descriptkn Qf the Drawings ALP wnbQdlTneJ)t 01 mnycittion ivit b described by. çjf example and as :iiusflati htthc accompanying figurnin whIch; 1 igme -. shows a represcntauon at a solar oct11 with a a scaffold YJ uU we and h) a planar junctiOn according to an embodiment of the thve.h:tion.
DetaiM. Dstripthni fth.e Invention As shown ut Fagun I an decirode is tbrrred of a suh9trate ateh pinlly i 8 layer of netal or glass I the glass,uhstraw may he lrcatcd to unarove ts U tahilit) for cse in the producuon of an d"ctradc for a solar ccii The icument may mo' etching the.glas stihstrae. for example with a powder and a solution, of Rd. Also Lie gla's,uh5tzate may be Ue.avC tb in aqueous sulactant soljton acetone isopr.opanol or a. combutation thereof, fiyt example a sequential additIon of these liquids. I')oth of these proeesae.s rite used to iutprove.the. connection hetw&xn dilThrcnt la,yçis eJa soar ccli.
A laycrof transparent conducting oxide lv then deposited layer 2 These conductmg layers can includd transparent.con4dcthig oxides such' as bui not llmite4 to fluc*inc' doped ttn a'ude, mdum-uoped t n node a alum mmn$opect zinc oxide 0mev ctndpcting. iyçrs can.inc]fttde metal grids coated.. onto the substrate suiface: either alone or n. combination with a. t:ransparetit conducting oxide layer. For plastic substrates these are preferably made from polyethylene terephthalatc (PET) or pohethylene nanhthaiate (PENj 1uch is either cored with t 110131 griC a JJer tin oxide Most p eferably toe..nnJuct1ng suhstrdte is a glass suhtrate vhi1 has a low iron content to reduce opical losses. This can be coaled with a metal grid an&or indiam tin oxide and/or fiuorinsdoped tin oxide hut most prefbrahIy it is ooated. with.iluothne doped. tin. oxideco etch ginsi.
A metal oxid,e layer 3 i. then 4eposited for example a layer of titanium dioxide.
Depsinng a hlokng layer ofn'ctt oxide may ic cainect ou by any suitable means for earnç e by screen prntmg or gravure prlnt% in the ca'e & hOd it nay he drpnsitcd by spin eoatr the glass cubstrate with a anhnion nlanmrn isopropoxide or by spray coating a solttion f titamnv oxide precursor such as titanium Oil sontepexiuc bis(accty1aetonatc) An option ii sKp I rVUiVe Thin ti 4 1Th5OR1 (Mb tUtU 7 on tie u lantern dnnide blocking layer 3 The mesopbrons flint tompries inetLd oxide in a colloidal compoc't on comprising metal oxtde partiees, preferably netat oxide nariopamdes in a swtahk solvent Swtabh the metal oxide nanopartacles have an average particle size of I to 5.OOnm to create a mesoporous fljm, .typiàiiy with a pore dkuncter of from 2 to.
SOnni Most prrfeiahh the layer o' meta1 oxice is a layer of mec)poto is itamum dioxide 01 ahirninum o,dc. 11w thickness ci tee in opc.ro.us meul oxide ti m may aitably he fron 100 urn o Okm dcrndint on vi1'tcther th electroNic is solid or liquid and the r la ye nalance et\yeep ptgtmit aDsorbers lo.r Iiqm4. cjeçtrdyie athed. to. .dye uhorhers the metal odk1; thiekuess is preferably from. to.20 pui.Ad.
tnoa pref'erabh' 7 to 10 ptw For s0k1 e.lwtrolytes gibed to pigment a1norbeti the metal oxIde thbkness k.prefdrably.from. 100 nit to.5 p.m atkd moit.preferibiy 3:00 urn. to 2
The rnesoporou gi oxide thye ie coated onto the eendactin substrate In parti:culate iemi and then sintere4 toforni amesoporous substrate oflih surface area Suitable. slintcrihg is eatria.ti out at. a.teñIpetathre of between 400°C and. 600°( Sintering temperatures. oan..aiso be lowered, to 300 or.even I 50°C
S
The metal: oxile (compact layer or mesoporous layer) is then coated:ith a perovskite pigment which comprises a lead haLite salt and a mc.thylamine halide saiL Suitably the methylamim halides itlt scleetcd from CI I3NLhC 1, CFfaNl3iRr C.H3NH3T. and ntnuuros thereof. Suitably The lead halide salt i. selected from Pb13i1. Phi2 and mixtures thereof The perbissute pian ent can thc a hi. acdniotath onttieied With additon ii alP) I anun salt Lad hal J saLti edhei with or c uhout,&ven i*thg. present wicl can ehatigc. the ratio of ts..ccuisiituen.t.pan.s. and also its pigment.
tharactristis such:: as co.kur and Ught.ahsorrtion ip the dhecpce of solvent, a solid state reactier can eccur 1w hrmgw the pigmert a& salt together in repeated dose cnntact for instance, by. hding the rmrte.tiaI.s toet:her. Typitally the perov?dcite pinicnts arc selected from RNflaPbX where R. .a.lkyi. and' X haide incthdirtg mxtates of aiq 1 or h&ides It H pessrile to use J iluXture ol pignunr or p gmcrt pacuror so ulio i and metal oodes: p j]'[: the characteristics of the solar cell. .A dye atay he added 1w irnmerting tic layer of metal oxide in the solution onpmng the dc to fern ekualerU bond beteen the metal oxide rid the ctye piedi y hs ineohec a chexnsorptwa process whieh results m the fom'ttion of a covalent ester bond etvect a carboxylate4dcc tnker roar of the dyc cnd surface hyci:5nyi grc. ups on the weta' oxide surface Any cunable method of contocung the solution cc npnsirg the dye \U h the QT of metal oxidemaybe used Prekral$y the perovskitc pigmcnt is provided, j c.rvstidlin'c ibmi which c.u lHe cubic or i.etrago.nah Suitably the.erystuls ait ptts;at in tetragon& frrn tend. to have IQW band gtis am! anorb t i1ther across inc sohir pectnmi thau perosisaW crystals ii the cubw tt"nj ftch tend to have brgtn band g çs and so urili< absorb higher enei&J radiation Ideally the vystds are n1na-'ved and form a thin, colThnaoLs film on the aurfa4e of a nw:o-po ou. suppot which is typically a niet& oxide such as titania or zi.hc ox.{,de.
The peuivskre pigniento rnas be seiec ed to haw at least pamaly complnnentaiy Ilelt ahsorpton. For exaniple, me. pignieiii.. may he selected which strongly ahsorh light in:a region of the TJVA'isible spethim whe the other e]ete.d pigment wcakly absorbs Iiaht.and. vice. versa.
A surface modIfying agent may optionally also be added te the. surtace of the. metal axde i-i an cidet wnh tIc pign en; Tms sutfice mod1ying agent thould be abie to tink to the. metal orthie.uurTh.ce preferably through a covalent: bond audi as a silan.e or linkage I ie surface nio±fymg aicn 1hould she po3sN4 UI dll1⁄4yl J<un which ma or ma not Inc Iluennated The urn of this surface modV\ ng am! n to reas the hI dropl obcity of the absorber layer on the metal oxa'e SUi4hle sutface itjodil5tins:igvnts aickud ch1oro-dirnethyi-alkyi silanes. or fatty aei4s or aiky1uarhoylie acids rr al kyl. phosphates or &.kyl sulfoziatea To n-eke the solsi cell a scaffold may he included as Inown n) or the tevze ias a planar jtuictton with no scaffold is made as shcwn. at h) Typ.icafly the solar cell will have two ejccPDUes whi Ibrm a sancwi.eh around a 5014i incitation nhsorbrip "actwc' layc. 5 One &uctrodc shoule he s ort;aFy transparent as posshle to alloi co1ar adiatmi to Lirpinge apon the adne" light absoib ug material Smtahc non-ransparer conducting sabstiates taclude meta 5 alloys such as but not flmitcd to steel,. alurirdurti or tirth.tm:. polymers such as. hut no nmted to, pot)umde PC ot poly ethet icetone (P IX) ssFtich bae bcea coated with a conducting iy.Cr. or poiyamline, andior graphite [ayers.
rho present. invention may lirther provIde a solar panel comprising a pIwailty of solar cells <f the eco4 aspect..
4 specific process Itbr.raak&ng. solar cells of the inventIon compnsmg a layer df mesupcrous TiO and a perossictic ptgn'ent vere prepared according to Vie following piccech?e A vihstrate consictmg of fkonnedopec tin oxide coated g as NSG Pilkr*en I PC 71 i nfl a sheet reststanec oil (Fri as patteined hy etchIng witn Zi povdar and t \4 HCl11 The etched qphstrate ias then eeancd scqucnnahy wfl an urfa taut oh4tIcn, acetone aid sopwpanol before dr'1⁄4nig with ?(2 oetore treating with anD2 plasma. fr 20 mm. A. dompaCt tktaiiurn doxide hkclki:ng layer Was then dcptsited onto this cleaned ubtr$e by spñ coatiiig I m:i f a: itariiurn iopropoxide oLuUon diluted in thanoI w: by spray pyth:Iysi cf a ttaniwt precursor SDiUtlAifl; SUCh as titwijum. sopopoxidc. or tiEaniuh. ttrachioride onto a. suhstate. held at appoxirnateiY greater than 3002C. e msoponius layer eonsistm.g of Tb2 nan-oparticies (approximately 500 urn thick) was then optionally deposited. by apin oatuig (2000 RM) a hO2 onubung eullute DycsolAO wtuch hal been diluted (l:3) in anhydrous ethanoL. The Utani laycrs vre-then sintered itt air 4 500 °C tbr mm ik Organolesd pign'ents scxe then cyntheswed u\ing solvent-free sohd state teCctionS by rnxing the pgtvei'r raw matenals in the des red ano and gnndmg or heating or grinding and heating these matetials together. The perovskite raw materials hiciude. a lead halide salt (fq cpmpie. PhBri *e FbI2) an4 a nethyIaniiae halide salt (11w cxatnnk Cl-[,NFI3X where x C Br or I) The pignetu crstaic s'vere than dposited. obto a titania surface. This WasP etber a. m.vsoporous titania hIm to fbrm: a tnesporeus devineor a ctm.paet layer of titani.a to.torm a planar j.u.netIoti device.
Deposition of the.pre.I]3ade pigent$. was tarn outusfr! a nwnher of techniques inchdlmg ntwuteh u ixmg h&e nigrneut u4h mct4 oxidc pirtleics ad sucncung the tesUtant pouder in a benwu sohuit such as an alcohol in whieh the pigment does nOt dissolve and sproading thih Onto fit titania chVted utftate: oi itid by heating.
Aiternanveb the pie-made pigment was spread onto the nwn'a,urtace a a powder ni afler suspension in a. benign solvent such as an alcohol in which the pigment does not ctsohe lolIe\\-ed by heating Ahern4tnely the premade pigment na suspended rn a benign. solvent 1. \thk.h it does not di:ssoit and a cbamic.al briking agent was added either to. the pigment suspension or to the. t.itania: surthe or to both. to ensure. tbe pignen handed L') the titanic co\cred susbnmc In theac eawnles otner metal o'jde, could.lso be used as wiI as titan.ia..suc-b as aluminium oxide, zinc oxide etc. Suitable.
chemical.iinkiug agents require one linkec group to attach to tfte. metal o?dde. and another to attach to tne pcrovskitc pigrcnt Typtal e\ampes includt Jktl diearboxylates s-ac Ii as oxalate,ebaeic acid, terephthahe aeW or lohracry he acad.
alkyl ch-su-ines ane oteame molecules contammg tvo {uncuonci roups such as a phos1'hate, carboxylate or cijare o link to thi metal oxtde and a hal±de, amine group, a nine bahk or acid halide to huk to the peros-slute The po ktec ited metal oxkk tilinawere tben. optionally heated at itO c( for 45 minutes i n.air.. 1*11
A hole'c.onducting material was then deposited onto th.e pemvskite-coate.d s metal nxdc, fo.x np{c by spin coatni; a 100 u chloiobenzeut solution C.OItIUUPg 68 mM Spiro-OMel AD, 5 mM:etar) -huLyl pyrdmc and 9 mM I timm bia(frithiomrnethytyfo.nyl)inii tie salt onto the iertwsidtocçiatcd suhstrate at 00O RPM ibr 60 seond Sok-cells kero left m tin, dark n dir nernight puor to thenml evanoratin 3f a c'd back ccintb ct upproxonatch 60 it ii thu. k 1w lure. jo em voflae charactensttcs were measured and the device efficiency calculated, using standard procedures ko to those.skiiled in the art Compaativc EaxupLp -Mall.faethre of Me.soporois.Sohir Celli A suh,ra cqnis;ing. of t1perincdpp.ed tin oxide coated. glass (NSCH!.Hkhrgton fEC 7) with a sheet resistance of 7 Wr was. pattend. by etching wi:h /n poder and 4 lvi i4Cl.).. *fit* etched;suhllt1at. Wa then cleaned. sequenriat1y with an aqueous sudIteLdat oIuti:n ucione and isopropano hi'fuc d int tth N24 tetore trCatu1t ss U an 2 plasma for 10 mm k compact ttanuin dtocidc hoc1ong layet v'as then deposited entp this cleaned substrate by pin cptipg I ml of a titanium isopropoxide solution tiliuted In ethanol. ,4 tnespporous layer crosisUng of Ti02 nanoparticlcs ppoxwiae y 0Q urn thick; wac then deposited by spm-eoaUng (2000 RPM) 4 contain n eoPcud (Dy sol-AD) hu.h iad ht,en dthned (, 3 g anln&ous cthano1 tin ayrs \1re then smtercd a air at 00 c\ fur 30 mtnutes On a this had eoocd to mon tempeictuic a peroskae grecursur olution 4O'i wt) stas 1ispercd,TttC1 th uu.soporous cIet.trock film h'1 spm coating 4t 2000 RPM r hO seconds I he peravskixe ntecursor solutibu comairied a lead halide afl. (fr cxampk PhBr2 or.Pb12.) ad a muhvlammc tal de sat (fur a'ott wit t"H\l 13X where X -(1, Hi or I) the pcro' kitecoatec metal oxide films ere they heated at I CO C iir 45 rnmute n atr A hoiecnn&eting taateriai was, then deposited onto the perovakite-coated mesoporous metal oxide, t0y example by spot coatri a 100 J chiorobenzc'ne solnuon containing 68 mM Spwo OMeTAD, 55 tiM terCary-butyl pyrJ.aie ad 9 mM littiuan his(tnfluoronieihylso vl)mide sal unto the pexovck'tc-coated st bstrate at 2000 RPM for.60 seconds. Solar cells, were left lit the dark in nit oern'ight prior to thermal evaporation of a gt1d back ccntact approximately 60 rtm thick befre eewvoltage* citaracteristies were measured arid the deyie. ef6eiency calculated using standard procedures known to those skilled in the art. Exanmies. of typicai data. are shown:. Hi Tabkl.
Table 1 shoy sOlar cell data: for two dIfforent perovskito pigtnent precuraom. Sola' cell A. shews &ta fo the eThm brunide l'aed pero'Jstte CFLNf1,P9r showing short circuit current of 5.1 6 rn.A.em and cfIic.ienc of 2.0%. Solar ecU 13 shows the Qata Ibr the hrowntblack, nuxec hJide4nsed perov'kite CftNII3PbJ0..CL hownu jrçrçsc thort circi t current of] 3.30 mA cni2 and efficiency o15.2.
Table I /
Comparative Puonkte Cokus mA v I em Tyi;bBV1)W tT?io O45 20 Compaatvc Fxai pIes Solution S nth esh of Penn skites As further compara:tive examples from. the prior art Ia show pigtmrnt colour, a perovlçitçptengsor qJutmr wa. prepwcd by addipg. it lead halide: salt. (for eamçile Pbfb or PbI.) iand a neihyiamFnc hl ie s41t (Thy vampic Cth.t'9l:X wh.erc N CL Br or I i dm't w lint namWo)MF 11 s peanskd4 pitwsur solution V 0°/c w) was. dkpcitsed. onto the mesoporous electiode film by spin--coating ar 2000 1PM.{br seconds, This procedure Srved two-purposes -namely t& bring flt pemvskite precursor c&miponttts mth close contact whit the substrate and also. m.remcive excess DM1 sohen; 1 he perovclote ptecuNoE -coated roeta oxide filmq seie thea heated at IOU C o' up o 45 mmutes 1) mrg this icatctg step. tb. deposued urns changed c a-dopenclmg Or the hcthde', pi C stnl 5cC kM dI% tO 1 abk 2 iahk2 Couipantive Enniple C 1) Perovskate Cl-13\l l3EbBr3 Cll,Nli.hI, Cl (olour of proetirser sohffion Colotles Ye1io Colour of depoted film CoIoui1cs Ytilow Crthsatu,a ume (mri) c 4$ Ainuiil tutu (uui) 4S90 nn 4590 Colour of film airneakd at 105 C Ydilow Browzilb!ack Comparathe Example -Manufacture of Planar Junction Perovsbte Solar Cells Solar cells comins ig a thin compact layer of TiC)' and a pero\ skite pimcnt WCTC prepared aecomThig to the following pi cedure. A..snbstrate c.onswtmg of fluorine-doped tin. o>ide coated...giass (NSO.-Pilkington.TEC 7) with..a sheet resistance of 7 Lh was patterned by' etching th Zn powder and.4 M.UC.tq The etched. suhtrate w then cleaned seque.nda.ilv with an aqaeovs sqifactant sQ.lutk)n. cetoe* ap4 isopropanol before dr rig With N belore trathg tuth an 02 phrra for 20 mn oth.ptct titanium 4io»=ddt blockIng Met was then ieposited onto this, cleaned sukEtate by' spin coating im! of a titanium Spropoxide sdlutimi dilUted in ethanol.
The layer'was then. intered. in air at 500 °C1 for 30 minutes. Once thIs' had cooled to rno1n temperatute, a peio skte çrecunor solution (40% wt) was d3pensed onto the mcsopoi ius elecirode film b spn-eoatmg at 2000 RPM for 60 seconds, 1 1-c perovakite precursor oiutitm contained.a kad halide salt:(for example, PFl3r2 or Phi2) and a.methyiamine* halide ialt (for example, CHNli3X wh&e X (1. Pr or I). The perovskitecoated metal oxide films'were then heated at 100 °C for 45 minutes in air.
A hweconductmg nate-jal as then deiccited onto the perovskitecoated mesopoc metal o'i,'$e f example by spin coating a. 1.00 pA chior6henzene solution containmg 8 m4 4p ro-OMel AD, 5c mM temary-butyl p',r'dine ana 9 riM lithium bis(trl flu'oror thyIfonyl)irnidC salt nato the petovskite-c&ted stthsuate t 2000 RPM liyr 60 seconds. Solar cells were left in the dark in air overni' t prior' to thermal evapuafloc of a gold hak contact approximately 50 em thtk hefoic the turent voltage thataoteristics were measured and. the device effici.eney calculated using 1.4 standard procedures known to those skilled, in the art. Dlata for a planar:unction device are shown in TaMe 3.
Tahk 3, Comparative Ve/ 1c / (okiur FF i%
Example V nAtm
L (JllhP1,CL Brown Lttt 0 *1 130 -05 55 --.--Perovskite Svrnbesis trout Component Piasder nsan.g Solid Shift. Reactions Example 1 Perovskifr' .SyntbSs froP Contpo.nent Powdert u.ing So1vent-Ies Solid State RvactIonnnd Mbdñg Aikyl amntoniuni brom:de such as methyl or etini nium bromide is svntlesised -3y 1utng an ethanol c cluboii of Inc conespondirg elks! amnc anti hydrogen bromide wider ritregcr at room crnperatu e to 2 hourq the product s Iccovered bc evaporat ion of the.: solvent followfrtg by th.ying. in a vacuum. oven. .thr 2 hours.. \Vhite methyl ammon.iu.m hromid.e powder (020 g) was gently mixed with White lead bromide powder (09i 8:g) io prod uce a.white. n:owder, When the.pawder is ground in: a pestle and mortar, material becomes'. inereashglv coloured until it finally he conies brigitte nac as methyl ainmonium lead bromice forms.
Exiunple 2 Perovskttt SyntheS from Component:. POwders using Sohat-dess Solid State.Rea ona and Ikating.
axnmoidum brunjide ucb. as methyl or ethyl ararnoniarn hmrni.d is synthesised Dy storing <in othanolic,oluUot o he coresponding alkyl amine a IL II'U ogen bromide under nitrogen at room te.mØcraturc for 2 hours. The prothic:t IS: Eccoveted by' eva)oraiion. of the solveilt.{bllo'wing by drying in a vacuwn. oven fhr 2 hthira, White methyl amrnoniuni. bromide. powder (0.280 g) was gently mi xecl with. white: cad hton.jde powder ij) 91g to ruoduce a whlte powdLr Wuen the powder r bcattd S temperatures between ambient temperature and 1 00CC, the material becomes: increasingly Coloured until it finally becomes bright' orange as'methyl amnnu.oniumiea.d bromide thrms.X-my powder diffraction data confirm the change from. raw materiaLs into the corresponding organolead perovskite tructure..
Example 3 Peoiskite S thes from Different Pci onkate Pewdem using Solid :Sthte Reactins When re-rnade orante metii/F amnionium lead bmffiide powder and hiak methyl aththomiuth lead.iodide.pswdet arC tdixed togat.her, they undergo. a saii:d state reactieii.
1ff produce a brown: powder which f5 a mixed halide: organolead perovskite. Visual inspection confirms that. the methyl ammonium lead trotnide. :r.ac4mt js an orange powdt*r ind he methyl ammoniun3 lead Iodide Is a bthck.powde. The, product.. of this reaction. ië. a brov..h powder which isa mixed h.rothideio4ide.orgauo.Eead.PerovLcit.
Xray diffraction data of the brown. powder confirm this...
Ejapk. 4 Additions *t Pre-nad.. PerpvsJft.e Powden; bthtg solid Statt ReaeUou When ptt made alkyl amnumhnn lead laud nowder and a metal. halide. afl rti.ixed togthhe ethr ny grmding ancwr heating, thy t nderg a so id sLøe reaction Lu produce v iecs organometa haLde perovskte which mcorporres he new components into the cryai LSttice. For example., when preade oinge methyl ammonium lead htornide poder and ied iodide powcie are mixed 1ogelhe, they undrgo a state reaction to produce; brown powda.r which is. a mxd hivmide/iodi.de organolead p.rovakite.
Example 5. AdditIons to P'çmdç çroysJtç rowder nsin SøUd State.
Seattions.
When pro-mzde al.kyl. mnIonium lead ludide powder and an alkyl amtnQnium halide are' rtixed together. either by grinding and/or heating, they undergo a solid state reachon to prance a new organometal iahdc perovsRnc \hKh incerpoiatcs the tiew components mto the. crystal la'tice, lor exaiple, when preni.ade biacic methyl arm.onittrn. 104 kdid 1owder 4nd.methy *mpnhtr' bromide powder are in'ixpd tocthct, they a ider.go a solid state eacuon to imC ice a hi own powdci wheh s a mixed. h.rorhide/idd'iciC otgaaioieud re:rovsicite.
Exampie 6 Additions to Pre.nade Perovskhe. Powders using Solid State Reaetion When pre-made álkyi ammoniuni lead halide, powder and a mxLtre of a metal halide ?flJ an aWy trrinonujrn me. b.ide ate rnixe together, uther h gfnding ciOCt/Ol heating they undergo a solid state reataion tn produce a new' nrgarmmetal halide cemvsldte whIch incorporates the flew cOMpOflettts' into the crystal lattice, For ecainpk, ;hen pm-mace orange niethy n incnucn ki hiomid. pcrdei, methyl unnornxr ehlonde and lead iodide powdci are mixed togethei the' uadexgo a so.jd scate redtion to prodnee: .a ciysta.hiae powder which is a mixed ch'ionde/bronude/todzd.e organolead perovskite.
ftc present invention aUov for the' p idi.ction of solar cells that ha% c art mpr ncd abcorhance of L\Jsisiblc light at specfc winJentth cocupated to known DSSC The solar ceIl 50kW eelS of the piçcit jivntou may ha' art miproved overall absorhance of IJV/vihibio IiSht c*cnntyared to known DSSC*s. Furthermore the solar celib of the oIestn Invention m1y nave.&n,nned efficitnicy ot coilvetslcm CL incident sunliglitto electrical energy compared to known' D'SSCs.
The colar cells of Ike present mvonuon are partie.ilarly edvantaJeous heuuse ties can bepreparee in a range of colours, it should he understood. that various dhai es and modic.ato s to the pressi'th* prcftrred ernbodunenis deerahed intern tj0 he apoarent to those scilled in the trt Such'e hange.s and modifications can he made without departing from, th. spirit id scope of thoriresen invention and. withc ut diminishing:, its attondani advantages. it i therefore a tended that such changes and itodifLatlans are co'.rcC by lhc appended claiws, The *conrnt ci' all rcftaences tefen'ed to herein. are I;rporae herein. by reference in their entirety.
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JP2015535390A (en) * 2012-09-18 2015-12-10 イシス イノベイション リミテッド Optoelectronic device
GB2536862A (en) * 2014-12-19 2016-10-05 Bangor Univ Solar cells
CN109927435A (en) * 2017-12-15 2019-06-25 Tcl集团股份有限公司 A kind of transfer method of quantum dot film

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WO2013171520A1 (en) * 2012-05-18 2013-11-21 Isis Innovation Limited Optoelectronic device comprising perovskites
EP2693503A1 (en) * 2012-08-03 2014-02-05 Ecole Polytechnique Fédérale de Lausanne (EPFL) Organo metal halide perovskite heterojunction solar cell and fabrication thereof
WO2014045021A1 (en) * 2012-09-18 2014-03-27 Isis Innovation Limited Optoelectronic device

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WO2013171520A1 (en) * 2012-05-18 2013-11-21 Isis Innovation Limited Optoelectronic device comprising perovskites
EP2693503A1 (en) * 2012-08-03 2014-02-05 Ecole Polytechnique Fédérale de Lausanne (EPFL) Organo metal halide perovskite heterojunction solar cell and fabrication thereof
WO2014045021A1 (en) * 2012-09-18 2014-03-27 Isis Innovation Limited Optoelectronic device

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* Cited by examiner, † Cited by third party
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JP2015535390A (en) * 2012-09-18 2015-12-10 イシス イノベイション リミテッド Optoelectronic device
GB2536862A (en) * 2014-12-19 2016-10-05 Bangor Univ Solar cells
CN109927435A (en) * 2017-12-15 2019-06-25 Tcl集团股份有限公司 A kind of transfer method of quantum dot film
CN109927435B (en) * 2017-12-15 2021-01-12 Tcl科技集团股份有限公司 Transfer printing method of quantum dot film

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