MAI and PbI2 were added into a mixture of GBL and DMSO (7 : 3 v/v) at 60°C for 12 h. The precursor solution was coated onto the TiO2 layer with and without APMS modification at 5000 r.p.m. for 55 s. During the spin-coating process, the substrate was treated by chlorobenzene drop-casting [15 (link)]. The substrate was then dried on a hot plate at 100°C for 10 min. A spiro-MeOTAD solution was prepared by dissolving 72.3 mg of spiro-MeOTAD in 1.0 ml of chlorobenzene, into which 28.8 µl of tBP and 17.5 µl of a Li-TFSI solution (520 mg Li-TFSI in 1 ml acetonitrile, Sigma-Aldrich, 99.8%) were added. The spiro-MeOTAD solution was spin-coated onto the perovskite films at 5000 r.p.m. for 30 s. Finally, an Au electrode with a thickness of 80 nm was thermally evaporated onto the spiro-MeOTAD-coated substrates.
Litfsi
Manufactured by Merck Group
Sourced in United States, Germany, China, Spain
LiTFSI is a lithium-based salt with the chemical formula Li[N(SO2CF3)2]. It is a key component in various electrochemical applications, including lithium-ion batteries, supercapacitors, and fuel cells. LiTFSI is known for its high ionic conductivity and thermal stability, making it a widely used electrolyte material in these applications.
Automatically generated - may contain errors
Lab products found in correlation
Lino3, by Merck Group (14 mentions)
Spiro ometad, by Merck Group (10 mentions)
Dimethyl sulfoxide (dmso), by Merck Group (9 mentions)
4 tert butylpyridine, by Merck Group (8 mentions)
Acetonitrile, by Merck Group (7 mentions)
N n dimethylformamide (dmf), by Merck Group (7 mentions)
Chlorobenzene, by Merck Group (6 mentions)
Spiro ometad, by Xi'an Yuri Solar Co. (6 mentions)
4 tert butylpyridine tbp, by Merck Group (5 mentions)
Tegdme, by Merck Group (5 mentions)
Chlorobenzene, by Thermo Fisher Scientific (4 mentions)
D α tocopherol polyethylene glycol 1000 succinate tpgs, by Merck Group (4 mentions)
Emim tfsi, by Merck Group (3 mentions)
Lino3, by Thermo Fisher Scientific (3 mentions)
Lipf6, by Merck Group (3 mentions)
Pedot pss, by Xi'an Yuri Solar Co. (3 mentions)
Spiro meotad, by Xi'an Yuri Solar Co. (3 mentions)
Natfsi, by Merck Group (2 mentions)
Acetylacetone, by Merck Group (2 mentions)
Acetone, by Thermo Fisher Scientific (2 mentions)
109 protocols using litfsi
1
Perovskite Solar Cell Fabrication
2
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.
3
Solid Polymer Electrolyte Membrane Fabrication
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All experiments were performed in glove boxes under argon atmosphere to minimize the influence of water and oxygen on the raw materials. The PEO-LiTFSI-10 wt% Pyr1,3TFSI-10 wt% LLZO (PLL) electrolyte solution was fabricated via a conventional solution casting technique. First, PEO (MW = 4 × 105 g, Sigma) and LiTFSI (99%, Sigma) were dissolved in acetonitrile (ACN, 99%, Sigma) to obtain a homogeneous solution, where the molar ratio of PEO and LiTFSI was 18:1. Next, 10 wt% of ionic liquid Pyr1,3TFSI (TCI, 99%) was slowly added into the slurry, and 10% of LLZO powder was also added. The mixture was sonicated for 1 h using an ultrasonic machine at high power to improve the dispersion of LLZO. The homogeneous slurry was continuously stirred overnight inside the glove box. Subsequently, the electrolyte membrane was gained by wet coating the final slurry on a Teflon plate and drying at 45°C in a vacuum oven for 24 h to evaporate the acetonitrile. They were then stored in a glove box for 12 h before being used to assemble the cell for electrochemical analysis. PL (without LLZO) was also obtained using the same method. The thickness of the electrolyte membrane was controlled and measured using thickness gauges. The average thickness of the electrolyte membrane was ~100 μm.
4
Perovskite Solar Cell Fabrication
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After the perovskite annealing, the substrates were cooled down and a Spiro-OMeTAD (Lumtec) solution (70 mM in chlorobenzene) was spin coated at 4000 rpm for 20 s. Spiro-OMeTAD was doped with bis(trifluoromethylsulfonyl)imide lithium salt (Li-TFSI, SigmaAldrich) and 4-tert-Butylpyridine (TBP, SigmaAldrich) in the molar ratio of 0.5 and 3.3 for Li-TFSI and TBP, respectively.
Finally, gold with 80 nm thickness was thermally evaporated under high vacuum as top electrode33 (link).
Finally, gold with 80 nm thickness was thermally evaporated under high vacuum as top electrode33 (link).
5
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.
6
Preparation of Solid Polymer Electrolytes
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PEO Mw = 5 × 106 g·mol−1 from Sigma-Aldrich (Sigma-Aldrich, St. Louis, MO, USA) was used to prepare the composites. LiTFSI, from Aldrich and neat sepiolite, kindly supplied by TOLSA S.A. (TOLSA, Madrid, Spain), were dried under a vacuum for 24 h. d -α-tocopherol polyethylene glycol 1000 succinate (TPGS), used to prepare the modified sepiolite TPGS–S, was purchased from Aldrich and used as received. Details on the preparation of TPGS-S have appeared elsewhere [14 (link)]. The RTILs employed to prepare the electrolytes listed in Table 1 were purchased from Solvionic (Solvionic, Toulouse, France), all of them with 99.5% purity. They are the following: 1-ethyl-3-methylimidazolium bis(fluorosulfonyl)imide (EMIFSI), N-propyl-N-methylpyrrolidinium bis(fluorosulfonyl)imide (PMPFSI); N-propyl-N-methylpyrrolidinium bis(trifluoromethanesulfonyl)imide (PMPTFSI), 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl) imide (EMITFSI).
Solutions of LiTFSI with RTILs and poly(ethylene glycol) methyl ether (PEG), Mn = 550 g·mol−1 from Sigma-Aldrich (Sigma-Aldrich, St. Louis, MO, USA) were prepared by magnetic stirring for 30–120 min, as model liquid phases for the solid polymer electrolytes.
Solutions of LiTFSI with RTILs and poly(ethylene glycol) methyl ether (PEG), Mn = 550 g·mol−1 from Sigma-Aldrich (Sigma-Aldrich, St. Louis, MO, USA) were prepared by magnetic stirring for 30–120 min, as model liquid phases for the solid polymer electrolytes.
7
Quasi-Solid-State Polymer Electrolyte Synthesis
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Commercial BDE (50 mg, liquid chromatography purity ≥95 %, Sigma–Aldrich), PEO (30 mg, Mw≈5×106, Sigma–Aldrich), LLZ (25 mg, NEI Corporation), and LiTFSI, (EO/Li+=8 in molar, ion chromatography purity ≥98.0 %, Alfa‐Aesar) were added stepwise to ED600 (Jeffamine®, 245 mg, Mr≈600, Aldrich) during stirring at 1200 rpm. After degassing the polymer, sol was solidified into a quasi‐solid‐state gel through polymerization of terminal active groups at 90 °C for 12 h, as depicted in Figure 1 a. The monomer molar ratio of ED600 and BDE was set to 1:1.5 to obtain a proper film‐processing ability. The casted composite electrolyte film was abbreviated as BEPEO‐LLZ. To achieve sufficient mechanical strength for film processing, small quantities of LLZ filler and macromolecular PEO were added into the BEPEO‐LLZ. The incorporated LLZ was a garnet‐type solid electrolyte, which was used here to improve mechanical strength and ionic conductivity.60 As references, films consisting of PEO+LiTFSI and PEO+LiTFSI+LLZ dissolved in dimethyl carbonate (DMC, gel chromatography purity ≥99.0 %, Merck KGaA) were prepared through gel‐casting, abbreviated as PEO‐Li and PEO‐LLZ, respectively (for details of the composition see Table 2 ). BEPEO without LLZ fillers was too sticky to be used as a free‐standing film. Thus, it is not discussed here.
8
Optimized Li-Sulfur Cell Assembly
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Coin cells were assembled with a cathode described above, a Li-foil anode (14 mm in diameter), a glass microfiber separator (Whatman), and 20 μl of electrolyte solution. The electrolyte/sulfur ratio was 6–12 μl mg−1, which is slightly lower as compared to ref. 32 . This separator exhibited an improved performance and higher cycling stability in coin cells as compared to the commonly used polypropylene Celgard separator. The electrolyte used for Li–sulfur cells consisted of 1.0 M lithium bis-(trifluoromethanesulfonyl) imide (LiTFSI, Aldrich) dissolved in a mixture of 1,3-dioxolane and 1,2-dimethoxyethane (1 : 1 by volume) with 1.0 wt% LiNO3 (Aldrich) as an electrolyte additive. LiTFSI was dried in a vacuum at 130 °C overnight, LiNO3 at 50 °C in a vacuum overnight, and the mixture of organic solvents was dried over a molecular sieve 4 Å (Aldrich). The electrolyte used for cyclic voltammetry of pristine LiHEOFeCl consisted of 1 M LiPF6 in ethylene carbonate/dimethyl carbonate (1 : 1 by volume). Both electrolyte solutions contained 8–12 ppm H2O as determined by Karl Fischer coulometric titration (Mettler Toledo). Electrolytes and solvents were of standard quality (p. a. or electrochemical grade) purchased from Aldrich or Merck.
9
Lithium-Ion Battery Electrolytes Preparation
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Two different electrolyte
solutions were
used, each consisting of a DME (Sigma-Aldrich, >99.5%) solvent
that
was further dried for several days over freshly activated molecular
sieves (type 4 Å) (Sigma-Aldrich) and lithium bis(trifluoromethanesulfonyl)imide
salt (LiTFSI, 99.95%, Aldrich), dried in a vacuum oven at 80 °C
for 24 h. One electrolyte consisted of a solution of 0.5 M LiTFSI
dissolved in DME, while the other consisted of a solution of 0.05
M LiI and 0.5 M LiTFSI dissolved in DME. These electrolytes will be
termed the DME and DME/LiI electrolytes, respectively. All the electrolyte
preparations were performed in an argon-filled glovebox (H2O and O2 content of <1 ppm). On the basis of the liquid
chromatogram test, there is still a large amount of water (∼4000
ppm) in the electrolyte during the battery test.
solutions were
used, each consisting of a DME (Sigma-Aldrich, >99.5%) solvent
that
was further dried for several days over freshly activated molecular
sieves (type 4 Å) (Sigma-Aldrich) and lithium bis(trifluoromethanesulfonyl)imide
salt (LiTFSI, 99.95%, Aldrich), dried in a vacuum oven at 80 °C
for 24 h. One electrolyte consisted of a solution of 0.5 M LiTFSI
dissolved in DME, while the other consisted of a solution of 0.05
M LiI and 0.5 M LiTFSI dissolved in DME. These electrolytes will be
termed the DME and DME/LiI electrolytes, respectively. All the electrolyte
preparations were performed in an argon-filled glovebox (H2O and O2 content of <1 ppm). On the basis of the liquid
chromatogram test, there is still a large amount of water (∼4000
ppm) in the electrolyte during the battery test.
10
Perovskite Solar Cell Fabrication
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Chemically etched FTO glass substrates were cleaned with a detergent solution, deionized water, acetone, and anhydrous ethanol for 15 min, respectively. Next, the substrates were further cleaned with plasma treatment for 15 min. The SnO2 solution (Alfa) was spin-coated on the FTO substrates at 3000 rpm for 30 s, followed by annealing at 150 °C for 30 min. The SnO2-cPCN solution also underwent the same procedures. The substrate was then cool down to room temperature on a spin coater. The (FAPbI3)0.9(MAPbBr3)0.1 perovskite solution (PbI2, FAI, PbBr2, MACl, MABr, in DMF: DMSO = 9:1 volume ratio) was spin-coated at 1000 rpm for 10 s and 5000 rpm for 30 s onto the FTO/SnO2 substrate. 200 μL of chlorobenzene was dropped on the spinning substrate at 8 s before the program finish, and the FTO/SnO2/perovskite sample was heat-treated at 150 °C for 15 min. Then, the hole transporting layer was deposited on top of the perovskite layer at a spin rate of 4000 rpm for 20 s using a spiro-OMeTAD solution. For the spiro-OMeTAD solution, 72.3 mg of spiro-OMeTAD was dissolved in 1 mL of chlorobenzene with additives of 17.5 μL of bis(trifluoromethylsulfonyl)imide lithium salt (Li-TFSI, Sigma-Aldrich) solution (520 mg mL−1 in acetonitrile), 28.8 μL of 4-tert-butylpyridine (TBP, Sigma-Aldrich). Finally, 120 nm of the silver counter electrode was thermally evaporated under a high vacuum.
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