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Spiro ometad

Manufactured by Merck Group
Sourced in Germany

Spiro-OMeTAD is a small organic molecule that is commonly used as a hole-transporting material in perovskite solar cells and other optoelectronic devices. It has a spiro-bifluorene core structure with methoxy substituents. Spiro-OMeTAD is a critical component in the fabrication of high-performance perovskite solar cells, enabling efficient charge extraction and transport.

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20 protocols using spiro ometad

1

Planar PSC Fabrication with Perovskite

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The planar PSC device structure was fabricated using an ITO glass substrate as a bottom electrode, a c-TiO2 layer as an ETL by spray pyrolysis as described previously, a light-absorbing perovskite layer (MAPbI3), 2,2′,7,7′-tetrakis{N,N-di(4-methoxyphenyl)amino}-9,9′-spirobifluorene (Spiro-OMeTAD, Merck) as an HTL, and a top Au electrode deposited by thermal evaporation. After the c-TiO2 layer on the ITO substrate was cooled to room temperature, a one-step method developed by Ahn N. et al.,17 (link) was used with 422 mg of PbI2, 159 mg of MAI, and 78 mg of DMSO (molar ratio 1 : 1 : 1) as perovskite precursor. Then, raw materials were mixed in 600 mg of DMF solution and stirred for one hour at room temperature. The perovskite was spin-coated onto the compact TiO2 layer at 5000 rpm for 30 s with 300 μl of diethyl ether as an antisolvent solution. Then the samples were annealed at 100 °C for 30 min. Next, the Spiro-OMeTAD solution was prepared by using 80 mg Spiro-OMeTAD, 22.5 ml 4-tertbutylpyridine (Sigma-Aldrich) and 17.5 ml lithium bis(trifluoromethane sulfonyl)imide (Li-TFSI, Sigma-Aldrich) solution (520 mg Li-TFSI in 1 ml acetonitrile) in 1 ml chlorobenzene, and then spin-coating the resulting solution onto the perovskite layer at 3000 rpm for 30 s. Finally, Au was deposited on this HTL by thermal vacuum evaporation as a top electrode.
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2

Perovskite Solar Cell Fabrication

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After the perovskite annealing, the substrates were cooled down for a few minutes, and a spiro-OMeTAD (Merck) solution (70 mM in chlorobenzene) was spin-coated at 4,000 rpm for 20 s. spiro-OMeTAD was doped with bis(trifluoromethylsulfonyl)imide lithium salt (Li-TFSI) (Sigma-Aldrich), tris(2-(1H-pyrazol-1-yl)-4-tert-butylpyridine)-cobalt(III) tris(bis(trifluoromethylsulfonyl)imide) (FK209) (Dynamo), and 4-tert-butylpyridine (tBP) (Sigma-Aldrich). The molar ratios of additives for spiro-OMeTAD were 0.5, 0.03, and 3.3 for Li-TFSI, FK209, and tBP, respectively. Finally, 80 nm of gold top electrode were thermally evaporated under high vacuum.
Perovskite solar cells were then stabilized with a photopolymerized coating accordingly to previously reported procedure (26 (link)).
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3

Perovskite Solar Cell Fabrication

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CsI (99.9%), acetonitrile (99.5%) and chlorobenzene (99.8%, anhydrous) were obtained from Acros, while bismuth (III) iodide (99%), dimethyl sulphoxide (DMSO, anhydrous, ≥99.9%), acetylacetone (99.6%), Bis (trifluoromethane) sulphonamide lithium salt (99.95%, Li-TFSI, trace metals basis), Spiro-OMeTAD (99% HPLC) and methanol (99.9%) were purchased from Sigma Aldrich. N-N dimethylformamide (DMF, anhydrous, 99.8%) was obtained from Alfa Aser,4-tert-butyl pyridine was purchased from Aladdin, FK 209-cobalt(III)-TFSI was purchased from MaterWinChemicals and tris(2-(1H-pyrazol-1-yl)-4-tert-butylpyridine)cobalt(III)tris(trifluoromethylsulfonyl)imide) was obtained from Aladdin while isopropanol was from J&K Scientific and Dyesol 30 NR-D (Queanbeyan, Australia). All chemicals were utilised directly without further purification.
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4

Perovskite Solar Cell Fabrication

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The perovskite precursor solutions were spin-coated on the nanopatterned mp-TiO2 layer by using the hot-casting technique at 90 °C and then annealed at 130 °C for 1 h. The hole transport materials were prepared by stirring 73.5 mg of spiro-OMeTAD (99.62%, Feiming Chemical Limited, Shenzhen, China), 17 µL of Bis (trifluoromethane)sulfonamide lithium salt (Li-TFSI, 99.95%, Sigma-Aldrich, St. Louis, MO, USA) solution (574.2 mg of Li-TFSI in 1 mL of acetonitrile), and 36.2 µL of 4-tert-butylpyridine (98%, Sigma-Aldrich, St. Louis, MO, USA) in 1 mL of chlorobenzene (99.8%, Sigma-Aldrich, St. Louis, MO, USA) at room temperature for 2 h. The spiro-OMeTAD was spin-coated at 4000 rpm for 60 s, followed by drying in a glovebox overnight. The above procedures were implemented inside a dried air-filled glovebox at a dew point of approximately −40 °C. Finally, the Au electrode was deposited by the thermal evaporator.
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5

Fabrication of Perovskite Solar Cells

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To prepare the devices, F-doped tin oxide (FTO) substrates were cleaned with deionized water mixed with surfactant and then with acetone and isopropyl alcohol on an ultrasonic bath for 20 minutes each time. SnO2 ETL was spin-coated and annealed at 200 °C for 40 minutes. The (Cs0.05(MA0.17FA0.83)0.95Pb(I0.83Br0.17)3) perovskite solution is then prepared in 4 : 1 ratio of DMF : DMSO. The perovskite layer is spin coated over SnO2 and annealed at 100 °C temperature for 30 minutes. Then spiro-OMeTAD doped with Li-TFSI and TBP (Sigma Aldrich), was spin-coated over the perovskite layer. The molar ratios for Li-TFSI and TBP were 0.5 and 3.3. In case of PBDTP-DTDPP polymer, undoped sample of 20% w/w is spin coated whereas for doped samples, TBP and Li-TFSI were used. Finally Au electrodes were thermally deposited by vacuum evaporation (<10−6 torr). For ultrafast measurements, all the layers have been deposited in similar manner on quartz substrate except the electrodes. Current density–voltage measurement was conducted with a mask in a glovebox under AM1.5 G illumination with an intensity of 100 mW cm−2 (Oriel 1 kW solar simulator) using Keithley 4200. SEM image of film was obtained using Hitachi S-4800.
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6

Fabrication of Perovskite Solar Cell Devices

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PbI2 (99.99%) was purchased from TCI America. MAI (>99%), BAI (> 99%), and TiO2 paste (30 NR-D) were purchased from Greatcell Solar. DMF (>99.8%), ACN (>99.8%), THF (>99.8%), and IPA (>99.8%) were purchased from Acros Organics. AcetylAcetone (>99%), titanium diisopropoxide (75 wt. % in isopropanol), Spiro-OMeTAD (>99%), Li-TFSI (99.95%), t-BP (98%) were purchased from Sigma Aldrich. Acetone, ethanol and other solvents were purchased from Fisher Scientific. All chemicals were used as received without further purification. Solar cell substrates are pre-patterned fluorine-doped tin-oxide-coated (FTO) glass (<15 Ω/square) obtained from Yingkou Advanced Election Technology Co., Ltd. The CIFs we employed for this study were downloaded from CCDC. Their reference numbers are:
(CH3-PA)2PbI4: CCDC 665689 [10.5517/ccqbpvk]
(COOH–PA)2PbI4: CCDC 267398 [10.5517/cc8z7r6],
(OH–PA)2PbI4: CCDC 746125 [10.5517/cct1dks],
(CN–EA)2PbI4: CCDC 705087 [10.5517/ccrnprt]
(PEA)2PbI4: CCDC 1841681 [10.5517/ccdc.csd.cc1ztf29],
(BDA)PbI4: CCDC 1053651 [10.5517/cc14cdrn]
(NAPH)2PbI4: CCDC 1840803 [10.5517/ccdc.csd.cc1zshr0].
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7

Perovskite Solar Cell Fabrication

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2-Thiopheneethylamine
(TEA,
98%), lead(II) iodide (PbI2, 99.999%, metals basis), isopropyl
alcohol, formamidinium iodide (FAI), methyl ammonium iodide (MAI,
99.9%), dimethylformamide (DMF), dimethyl sulfoxide (DMSO), hydroiodic
acid (HI), tin(IV) oxide (SnO2), titanium diisopropoxide
bis(acetylacetonate), toluene, anhydrous ethanol, chlorobenzene, acetonitrile,
bis(trifluoromethane)sulfonamide lithium salt (Li-TFSI), ethanol,
4-tert-butylpyridine (TBP), tris(2-(1H-pyrazol-1-yl)-4-tert-butylpyridine)cobalt(III)
tris(bis(trifluoromethyl sulfonyl)imide) (FK209), 1-butanol, and 2,2′,7,7′-tetrakis-(N,N-di-p-methoxyphenylamine)-9,9′-spirobifluorene
(Spiro-OMeTAD) were purchased from Sigma-Aldrich. All the materials
were utilized without further purification.
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8

Fabrication of Perovskite Solar Cells

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All reagents and chemicals were purchased from commercial
suppliers
without further purification. Tin dioxide(IV) and 15% hydrocolloid
dispersion (SnO2) were purchased from Alfa Aesar. Nickel(II)
acetate tetrahydrate (Ni(OCOCH3)2·4H2O, 99.995% trace metals basis), PbI2, spiro-OMeTAD
(purity ≥99.8%), sodium dodecylbenzene sulfonate (SDBS), isopropanol
(IPA), N,N-dimethylformamide (DMF),
dimethyl sulfoxide (DMSO), chlorobenzene (CB), acetonitrile (ACN),
4-tert-butylpyridine (tBP), lithium bis(trifluoromethane
sulfonyl)imide (Li-TFSI), and FK 209 Co(III) TFSI salts were from
Sigma-Aldrich. Formamidinium iodide (FAI), methylammonium chloride
(MACl), and methylammonium bromide (MABr) were obtained from GreatCell
Solar.
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9

Synthetic Procedures for Organic Compounds

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3-aminopyrazole, 3-amino-5-phenylpyrazole, 9H-carbazole, ethyl phenylpropiolate, 4,4-dimethoxydiphenylamine, 1,3-diphenyl-1,3-propanedione, ethyl benzoylacetate, tri-tert-butylphosphine (P(t-Bu)3), palladium acetate (Pd(OAc)2), bis(pinacoloto)diboron, 1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (Pd(dppf)Cl2), sodium hydride (NaH), N-bromosuccinimide (NBS), phosphorus(V) oxychloride (POCl3), benzyl bromide, potassium iodate (KIO3), sodium carbonate (Na2CO3), potassium iodide (KI), potassium tert-butoxide (t-BuOK), 1,4-dibromobenzene, N,N-dimethylaniline, potassium phosphate tribasic (K3PO4), copper(I) iodide (CuI), trans-1,2-diaminecyclohexane, potassium acetate (KoAC), Spiro-OMeTAD, formamidinium iodide (FAI), cesium iodide (CsI), lead iodide (PbI2), lead bromide (PbBr2), N,N-dimethylformamide (DMF), tin(IV) oxide (SnO2), magnesium sulfate (MgSO4), tetraethylammonium tetrafluoroborate (Et4NBF4), ferrocene, silica gel (SiO2), dichloromethane (DCM), chloroform (CHCl3), acetic acid (AcOH), dimethyl sulfoxide (DMSO), 1,4-dioxane, tetrahydrofuran (THF), toluene and ethanol (EtOH) were purchased from Sigma-Aldrich, Alfa Aesar or Fluorochem and used as received without any further purification.
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10

Perovskite Solar Cell Fabrication

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Acetonitrile [CAS 75-05-8; high-performance liquid chromatography (HPLC) grade, ≥99.9%], toluene [CAS 108-88-3; American Chemical Society (ACS) grade], acetone (CAS 67-64-1; ACS grade), spiro-OMeTAD (CAS 207739-72-8; HPLC grade, 99%), FK 102 Co(III) bis(trifluoromethane)sulfonimide (TFSI) salt (Sigma-Aldrich, product number 805203; 98%), and 4-tert-butylpyridine (CAS 3978-81-2; 96%) were purchased from Sigma-Aldrich and were used without further purification. Extran 300 detergent (EX0996-1) and 2-propanol (ACS grade, ≥99.5%) were purchased from EMD Millipore Corporation and were used without further purification. Microscope slide substrates (75 mm by 25 mm by 1 mm; VWR, catalog no. 16004-430) were purchased from VWR International.
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