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10 protocols using 2 methoxyethanol

1

Methylamine-Based Perovskite Synthesis

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Methylamine solution (33 wt% in absolute ethanol), PbI2 (99%), and hydroiodic acid (HI) (57 wt% in water, γ‐butyrolactone (GBL, 99%) were purchased from Sigma‐Aldrich and used as received without further purification. EDTA, Zn(CH3COO)2·2H2O, 2‐methoxyethanol and ethanolamine were purchased from Alfa Aesar and without any purification.
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2

Zirconium Propoxide Precursor Preparation

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The ZrO2 precursor, including zirconium n‐propoxide (TCI, 70% in 1‐proponol) is dissolved into 2‐methoxyethanol (Alfa Aesar, 99%) and dilute to 0.3 m by 2‐methoxyethanol. The solution maintains stability in a sealed vessel for 1–2 days at room temperature.
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3

Synthesis of Y2/3Cu3Ti4O12 Ceramic

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Y(NO3)3·6H2O (99.80%, Aldrich), Cu(NO3)2·3H2O (99.0%, Junsei), TiO2 (99.9%, Sigma Aldrich), and 2-methoxyethanol (99.0%, Alfa Aesar) were used to prepare the Y2/3Cu3Ti4O12 (YCTO). A stoichiometric amount of Y(NO3)3·6H2O and Cu(NO3)2·3H2O was dissolved in a minimum amount of 2-methoxyethanol. A stoichiometric amount of solid TiO2 was added to the homogeneous metal nitrate solution of Y3+ and Cu2+, and sonicated for 10–15 min. The heterogeneous mixture of metal ions was formed and heated to 90–120 °C for 30–35 min on a hot plate using a magnetic stirrer to evaporate the organic solvent until self-ignition took place, which exhausted a large amount of gases with a greenish flame, and produced a fluffy mass of YCTO precursor powder within 15–20 s. Upon cooling, the resulting product was ground using pestle and mortar and sintered without a pre-calcination step at 950 and 1050 °C for 15 hrs in an electrical furnace.
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4

Synthesis of Nickel-Acrylic Acid Precursor

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Acrylic acid (anhydrous, 99%), propylene glycol monomethyl ether acetate (PGMEA) (>99.5%), dichloromethane (anhydrous, ≥99.8%), 2-methoxyethanol (anhydrous, 99.8%), and isopropyl alcohol (IPA) (99.7%) were purchased from Sigma Aldrich. Nickel 2-methoxyethoxide, 5% w/v in 2-methoxyethanol was purchased from Alfa Aesar, and 7-diethylamino-3-thenoylcoumarin was purchased from Exciton. Acrylic acid (100 mg) was slowly added to nickel 2-methoxyethoxide solution (1290 mg) in a glove box and manually agitated. We observed the nearly immediate change of the solution color from brown to green, which is indicative of a ligand exchange reaction48 (link). The mixture was held at low pressure in the antechamber of the glove box for 45 min to remove ~60% of 2-methoxyethanol. The resulting precursor was then taken out of the glove box, mixed with 300 mg of pentaerythritol triacrylate, and agitated using a vortex mixer for 1 min. 7-diethylamino-3-thenoylcoumarin (23 mg) was dissolved in 100 mg of dichloromethane, added to the mixture, which was then agitated using a vortex mixer for 1 min.
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5

Synthesis of Perovskite Thin Films via Solution Processing

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Indium nitrate hydrate (In(NO3)3·xH2O, 99.999%) powder, N,N-dimethylacetamide (DMAC, 99.5%) were purchased from Sigma-Aldrich. 2-methoxyethanol (2-ME, 99.3%), acetylacetone (AcAc, 99%) and ammonium hydroxide (NH3·H2O, 28%) were obtained from Alfa Aesar. Formamidinium iodide (FAI, >98.0%), Methylammonium iodide (MAI, >99.0%), Cesium iodide (CsI, >99.0%), Lead (II) iodide (PbI2, 99.99%), Methylammonium bromide (MABr, >99.0%) and Lead(II) bromide (PbBr2, 99.99%) were purchased from Tokyo Chemical Industry Co. Ltd (TCI). Temozolomide (DMSO, 99%), N,N-Dimethylformamide (DMF, 98%) and chlorobenzene (CB, 99.8%) were purchased from J&K Scientific. Dichloromethane (DCM) was obtained from Innochem Science & Technology Co., Ltd. Colorless polyimide (CPI) powder was from Zhejiang OCAs New Materials Co. Ltd. Silicon wafer with 100 nm thick SiO2 layer was obtained from Silicon Valley Microelectronics, Inc. Isopropyl alcohol (AR, 99.7%), acetone (AR, 99.5%) and hydrochloric acid (HCl; AR, 36–38%) were provided by China National Medicines Co. Ltd. (Shanghai, China). Poly(perfluoroalkyl vinyl ether) (CYTOP) was purchased from Asahi glass company (Japan) and consisted of CTL-809M (solute) and CT-Solv.180 (solvent). Polymethyl methacrylate (PMMA, 495 K A2) was purchased from Kayaku Advanced Materials.
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6

Synthesis of Bis(2-methoxyethyl) Carbonate

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Bis(2-methoxyethyl) carbonate (BMC, C7H14O5) (Supplementary Figs. 51 and 52) was synthesized according to the method previously described39 (link). More specifically, to a mixture of 114 g (1.5 mol) 2-methoxyethanol (99%, Alfa Aesar) and 67.5 g (0.75 mol) dimethyl carbonate (DMC, 99.9%, DodoChem), 0.7 g (13 mmol) sodium methoxide (NaOMe, 97%, Aladdin) was added under N2 atmosphere. Subsequently, the mixture was stirred at 95 °C overnight. Following this, generated methanol was removed via rotary evaporation and the reaction was terminated by introducing water. The resulting solution was then transferred to a separatory funnel and extracted with dichloromethane (3 × 50 mL). The obtained organic phase was dried using anhydrous MgSO4 and then vacuum evaporated on rotavapor to remove volatiles. The crude product was vacuum distilled (4 mm Hg, 103 °C) three times to yield ∼40 g colorless liquid as the product. Yield: 30%. 1H NMR (400 MHz, DMSO-d6) δ 4.19 (dd, J = 5.4, 3.7 Hz, 4H), 3.52 (dd, J = 5.4, 3.7 Hz, 4H), 3.26 (s, 6H). 13C NMR (100 MHz, CDCl3) δ 154.99 (s), 69.99 (s), 66.71 (s), 58.70 (s).
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7

Synthesis of Semiconductor Nanocrystals

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Cadmium oxide (CdO, 99.99%), selenium (Se, −200 mesh, 99.999%), zinc acetate (Zn(ac)2, 99.99%), sulfur (S, 99%), oleic acid (OA, 90%), 1-octadecene (ODE, 90%), tri-n-octylphosphine (TOP, 97%), magnesium acetate tetrahydrate ((CH3COO)2Mg·4 H2O, 99.997%) and 2-methoxyethanol (CH3OCH3CH3OH, 99.3%) were purchased from Alfa Aesar. Ethanolamine (99.5%), Poly(amidoamine)dendrimers (PAD), methanol (99.8%) and toluene (99.8%) were purchased from Sigma Aldrich. Tris(4-carbazoyl-9-ylphenyl)amine (TCTA, 99.5%) was purchased from Lumtec. All chemicals were used as is without additional purification.
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8

Organic Photovoltaic Material Synthesis

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PTB7-Th, PC71BM, and ITIC were purchased from Luminescence Technology Corp. O-dichlorobenzene (ODCB) and chlorobenzene (CB) were purchased from Aladdin Corp. Zinc acetate dihydrate [Zn(CH3COO)2•2H2O, 98%], ethanolamine (NH2CH2CH2OH, 99.5%), and 2-methoxyethanol (CH3OCH2CH2OH, 99.8%) were purchased from Acros. 2,3,5,6-Tetrafluoro-7,7,8,8-tetracyanoquinodimethane (F4TCNQ) was provided by Sigma-Aldrich. Molybdenum oxide (MoO3) was provided by Shanghai Han Feng Chemical Corp. All chemicals were used as obtained.
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9

Organic Photovoltaic Device Fabrication

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Patterned tin-doped indium
oxide (ITO) covered glass substrates were obtained from Naranjo substrates.
Poly(3,4-ethylenedioxythiophene):polystyrene sulfonate (PEDOT:PPS)
(Clevios P, VP Al 4083) was purchased from Heraeus. Active layers
consist of poly[[2,5-bis(2-hexyldecyl)-2,3,5,6-tetrahydro-3,6-dioxopyrrolo[3,4-c]pyrrole-1,4-diyl](3‴,4′-dihexyl-[2,2′:5′,2″:5″,2‴:5‴,2′′′′-quinquethiophene]-5,5′′′′-diyl)]
(PDPP5T)37 and 2,2′-[[4,4,9,9-tetrakis(4-hexylphenyl)-4,9-dihydro-s-indaceno[1,2-b:5,6-b′]dithiophene-2,7-diyl]bis[[4-[(2-ethylhexyl)oxy]-5,2-thiophenediyl]methylidyne(5,6-difluoro-3-oxo-1H-indene-2,1(3H)-diylidene)]]bis[propanedinitrile]
(IEICO-4F) (Solarmer Materials). Zinc acetate dihydrate (98+%) (Acros
Organics), 2-methoxyethanol (99+%) (Acros Organics), ethanolamine
(>99.5%) (Aldrich), MoO3 (99.99%) (Aldrich), DIO (97+%
copper stabilized) (Alfa Aesar), and calcium (99.5%) (Alfa Aesar)
were used as received.
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10

Organic Photovoltaic Materials Preparation

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The polymer PTB7-Th and PM6, as well as the nonfullerene acceptors (FOIC, IEICO-4F, Y6, SiOTIC-4F and COTIC-4F) were purchased from 1-material. All photoactive materials were used as received without further purification. The solutions of organic electron-transporting materials: PDIN (1-Material), PEIE (Aldrich, CAS No.: 26658-46-8) and PFN-Br (Ossila) were prepared in methanol (0.5 vol% acetic acid, 4 mg/mL), ultrapure water (6 mg/mL) and methanol (1 mg/mL) at room temperature, respectively. The sol-gel ZnO precursor (0.45 M) was prepared by dissolving zinc acetate dehydrate (Aldrich, 99.9%, 0.5 g) and ethanolamine (Aldrich, 99.5%, 0.14 g) in 2‐methoxyethanol (Acros Organics, 99.8%, 5 mL) under vigorously stirring at 60 °C for 2 h in air for hydrolysis reaction58 (link). PCE10: COTIC-4F blend solution: PCE10 and COTIC-4F (with a weight ratio of 1:1.5) were dissolved in chlorobenzene (with 2 vol% 1-chloronaphthalene) at 60 °C overnight at a total concentration of 40 mg/mL. PCE10: FOIC (SiOTIC-4F) blend solutions: PCE10 and FOIC (SiOTIC-4F) (with a weight ratio of 1:1.5) were dissolved in chloroform (with 2 vol% 1-chloronaphthalene for SiOTIC-4F blend) at 50 °C for 2 h at a total concentration of 30 mg/mL. All the bulk heterojunction blend solutions were prepared in a N2-filled glovebox with O2 and H2O level ˂ 1 ppm.
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