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8 protocols using ti och ch3 2 4

1

Synthesis of Titanium-based Nanocomposites

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We purchased urea (CH4N2O), La(NO3)3, dicyandiamideand (99%), and TiCl4 from Sinopharm Chemical Reagent Co. (Shanghai, China) Ti(OCH(CH3)2)4 and P123 (PEO-PPO-PEO) were purchased by Sigma-Aldrich. The water used throughout all of the experiments was purified using a Millipore system.
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2

Hydrothermal Synthesis of BaTiO3 Nanostructures

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The BaTiO3 samples were synthesized via a hydrothermal method,12 as illustrated in Scheme 1. As a Ti precursor, the Ti(OCH(CH3)2)4 (≥97% purity, Sigma Aldrich) was added dropwise to 15 mL of ice cold distilled water while being constantly stirred. Upon addition of the Ti(OCH(CH3)2)4, the distilled water became turbid then a white precipitate formed. The reaction mixture was stirred in ice bath for 1 h then at room temperature for a further 2 h to allow the reaction to reach completion. To make up the Ba precursor, an appropriate amount of Ba(OH)2·8H2O (≥98% purity, Emsure) was dissolved in 55 mL of distilled water. The exact concentration of each precursor used is specific to the reaction parameter being investigated and is specified in the results and discussion section. The Ba precursor solution was added to the Ti precursor suspension to make up the reaction mixture. The reaction mixture was then transferred to an autoclave where it was sealed and heated. Each reaction mixture was heated at a specific temperature in an oven for 16 h. The white solid that formed in the reaction was collected and washed in a centrifuge at 4500 rpm for 8 min. The solid was washed with diluted HCl once, then with distilled water 3 times. After that, the solid was dried at 80 °C for 12 h in a vacuum oven to obtain BaTiO3 samples.
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3

Synthesis of Pure TiO2 and Ag/TiO2

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All the chemicals used were of reagent-grade and they were used without any further purification. Materials used for synthesis of pure TiO2 and Ag/TiO2 were titanium isopropoxide (Ti[OCH(CH3)2]4, 97% Sigma-Aldrich) and Silver nitrate (AgNO3, 99.9% Sigma-Aldrich) and ethanol (99.5% J.T Baker). All solutions were prepared using deionized water.
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4

Synthesis and Analysis of S-Met and TiO2 NPs

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Sulfuric acid (H2SO4 Sigma Aldrich), sodium bicarbonate (NaHCO3, Sigma Aldrich), hydrochloric acid (HCl Sigma Aldrich), magnesium (Mg, Golden Bell), titanium isopropoxide (Ti[OCH(CH3)2]4, Sigma Aldrich) and comm TiO2 (TiO2, Fermont) were used as reagents for the analysis of S-Met and TiO2 NPs synthesis. The furfural (C4H3OCHO, Sigma Aldrich) was used as the standard for the calibration curve. The RM, MO and BS plants were collected nearest Chapala Lake, in Jalisco, México. For the photohydrolysis reaction, the nejayote sample was obtained from a local industry in Sahuayo, Michoacán, México. Nejayote is considered fresh and useful up to 3 days before its collection.
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5

Synthesis of Metal Oxide Nanoparticles

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Citric acid (99.5%), calcium nitrate tetrahydrate (97%, Ca(NO3)2·4H2O), ethyl alcohol (anhydrous, 99%), isopropyl alcohol (anhydrous, 99.5%, IPA, Seosan, Korea), and titanium isopropoxide (97%, Ti[OCH(CH3)2]4) were purchased from Sigma-Aldrich (St. Louis, MO, USA). Acetic acid (99.5%, CH3CO2H) and nitric acid (60%, HNO3) were supplied from Duksan (Ansan-si, Korea) and Samchun (Pyeongtaek-si, Korea). In the synthesis process, calcium nitrate tetrahydrate, titanium isopropoxide, and citric acid were used as the metal element sources and fuel material, respectively. Nitric acid and acetic acid were used to adjust the pH of the precursor solution.
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6

Perovskite Solar Cell Fabrication

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We used patterned indium-doped tin oxide (ITO) coated glass substrates (15 Ω cm−2), lead iodide (PbI2, Sigma Aldrich, 99.9%), lead bromide (PbBr2, Sigma Aldrich, 99.99%), [6,6]-phenyl-C61-butyric acid methyl ester (PCBM, Solenne BV), PEDOT:PSS (Clevios F HC Solar, SCA 418-12), nickel chloride hexahydrate (NiCl2·6H2O, Sigma Aldrich, 99.9%), cesium iodide (CsI, Sigma Aldrich, 99.99%), and sodium hydroxide (NaOH, Sigma Aldrich, ≥98%). Methyl ammonium bromide (MABr), methyl ammonium iodide (MAI) and formamidinium iodide (FAI) were synthesized in our lab, as mentioned in the synthesis of organic halides. Titanium(iv) isopropoxide (Ti[OCH(CH3)2]4, Sigma Aldrich, 99.9+%), isopropanol, hydroiodic acid (HI, 57 wt% in H2O), hydrobromic acid (HI, 57 wt% in H2O), methylamine (CH3NH2, Aldrich, 33 wt% in absolute ethanol), aluminum, N,N-dimethylformamide (DMF, anhydrous, Sigma Aldrich), dimethylsulfoxide (DMSO, Anal. R. VWR chemicals, 99.5%), acetone, ethanol, Helmanex® detergent, chlorobenzene, 2-methoxyethanol (CH3OCH2CH2OH, Sigma Aldrich, 99.9%) and ethanolamine (H2NCH2CH2OH, Sigma Aldrich, 99%) were also used.
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7

Synthesis of Amino-Functionalized MIL-125(Ti)

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Example 1

Synthesis of NH2-MIL-125(Ti)

On the basis of the following literature: S.-N. Kim et al., Catalysis Today 2013, 204, 85-93

A solution of 3 mmol of titanium isopropoxide (Ti[OCH(CH3)2]4, Aldrich, 97%) and 6 mmol of 2-aminoterephthalic acid (H2BDC—NH2, Aldrich, 99%) in 50 mL of N,N-dimethyl formamide/methanol (1:1, v/v) was produced. Said solution was transferred to a 250-mL steel autoclave (DAB-3 from Berghof) having a PTFE insert. The autoclave was held at 150° C. for 16 h by means of a convection oven. After cool-down to room temperature, the yellow powder was filtered, washed twice with DMF, and then washed with ethanol.

The yield was 760 mg.

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8

Synthesis of TiOx via Sol-Gel Method

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TiOx was synthesized using the sol–gel method, which is based on the hydrolysis of alkoxides in alcoholic solutions in the presence of an acid catalyst. Titanium isopropoxide (TTIP, Ti[OCH(CH3)2]4, Aldrich Chemical Co., 97%), ethanol (C2H5OH, Daejung 99.9%), and nitric acid (HNO3, Merck, 70%) were used as the starting materials, and distilled (DI) water was used for hydrolysis. The molar ratio of the starting solution was 1 of TTIP, 1 of DI water, 25 of ethanol, and 0.2 of nitric acid47 (link). The solution of nitric acid, DI water, and half ethanol was added dropwise to the solution of TTIP and ethanol at 0 °C under continuous vigorous stirring. The transparent solution finally resulted, and it was diluted using ethanol with a ratio of 1:1.
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