FTO (F:SnO2) (TEC-7, 8 ohm square) was cleaned by ultrasonic agitation in detergent, deionized water and a mixture solution of ethanol, acetone and deionized water with a volume ration of 1 : 1 : 1 for 15 min, respectively. The FTO substrates were immersed in an aqueous of 0.5 M TiCl4 (99%, Merck) at 80°C for 30 min and followed by heat treatment at 500°C for 30 min to generate a compact TiO2 layer. The TiCl4-treated substrates were then suspended in a reagent solution that contained 6 ml 2-butanone (more than 99%, Merck), 6 ml HCl (12 M, Merck) and 0.6 ml tetrabutyl titanate (more than 97%, Alderich) in a Telflon vessel. The telflon vessel was sealed in an autoclave and heated at 200°C for 1.5 h. After further annealing at 500°C for 30 min, the crystallinity of TiO2 NWs was grown on FTO substrates. The electrodeposition of CQDs onto TiO2 NWs was performed with a standard three-electrode system (electronic supplementary material, figure S1), consisting of a TiO2 NW electrode as the working electrode, Ag/AgCl as the reference electrode and platinum sheet as the counter electrode, at –3.0 V for 1 h.
Ticl4
Manufactured by Merck Group
Sourced in United States, Germany
TiCl4, also known as titanium tetrachloride, is a colorless to pale yellow liquid that is widely used in various industrial applications. It is a chemical compound composed of one titanium atom and four chlorine atoms. TiCl4 is known for its high reactivity and is commonly employed as a precursor in the production of titanium-based materials and coatings.
Automatically generated - may contain errors
Lab products found in correlation
Absolute ethanol, by Merck Group (3 mentions)
Hydrochloric acid (hcl), by Merck Group (2 mentions)
Alginate, by Merck Group (2 mentions)
Water purification system 18 mω, by Merck Group (2 mentions)
Fecl3 6h2o, by Merck Group (2 mentions)
Fecl2 4h2o, by Merck Group (2 mentions)
Nh3 h2o, by Merck Group (2 mentions)
C44h56o4, by Merck Group (2 mentions)
Isopropanol, by Merck Group (2 mentions)
Titanium tetrachloride, by Merck Group (2 mentions)
2 butanone, by Merck Group (1 mentions)
M 2000fi, by J.A. Woollam Co. (1 mentions)
Di h2o, by Merck Group (1 mentions)
Hydrochloric acid (hcl), by Avantor (1 mentions)
Ethanol, by Avantor (1 mentions)
Ethanol, by Merck Group (1 mentions)
Lead iodide, by Merck Group (1 mentions)
Lithium bis trifluoromethylsulfonyl imide, by Merck Group (1 mentions)
Spiro ometad, by Lumtec (1 mentions)
Spiro ometad, by Merck Group (1 mentions)
39 protocols using ticl4
1
Fabrication of TiO2 Nanowire-CQD Heterostructures
2
Atomic Layer Deposition of TiO2 on Mg-Patterned Substrates
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The 7.5 μm thick
Mg patterns were e-beam evaporated onto compression-molded PLDLA 96/4
substrates (0.4 mm × 30 mm × 40 mm). Thereafter, ALD TiO2 coatings were deposited onto the metallized substrates at
60 °C by using a Beneq TFS 200 ALD reactor. ALD TiO2 films were grown from titanium tetrachloride (TiCl4)
(Sigma-Aldrich) and water, both vaporized from the source at 20 °C.
One deposition cycle for TiO2 consisted of a 0.5 s TiCl4 pulse, a 20 s N2 purge, a 0.5 s water pulse, and
a 20 s N2 purge. The ALD TiO2 film thickness
was varied by alternating the number of ALD cycles. The amount of
cycles was 150, 250, and 500. Each ALD cycle corresponded to about
1 Å. The film thicknesses were measured from silicon (100) witness
pieces by using spectroscopic ellipsometry (J.A. Woollam Co., Inc.,
model M-2000FI).
Mg patterns were e-beam evaporated onto compression-molded PLDLA 96/4
substrates (0.4 mm × 30 mm × 40 mm). Thereafter, ALD TiO2 coatings were deposited onto the metallized substrates at
60 °C by using a Beneq TFS 200 ALD reactor. ALD TiO2 films were grown from titanium tetrachloride (TiCl4)
(Sigma-Aldrich) and water, both vaporized from the source at 20 °C.
One deposition cycle for TiO2 consisted of a 0.5 s TiCl4 pulse, a 20 s N2 purge, a 0.5 s water pulse, and
a 20 s N2 purge. The ALD TiO2 film thickness
was varied by alternating the number of ALD cycles. The amount of
cycles was 150, 250, and 500. Each ALD cycle corresponded to about
1 Å. The film thicknesses were measured from silicon (100) witness
pieces by using spectroscopic ellipsometry (J.A. Woollam Co., Inc.,
model M-2000FI).
3
Atomic Layer Deposition of Titanium Dioxide and Alumina
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ITO/glass substrates (15 ×
15 mm) were cleaned with detergent, rinsed with demineralized water,
acetone, and isopropanol, and dried with a N2 stream. A
thin TiO2 layer was then deposited on the substrates with
atomic layer deposition in a home-built system. The first few millimeters
of the sample surface were covered with a Kapton tape, in order to
leave a part of the surface conductive to do the electrical connections
during the photoelectrochemical characterization of the samples. The
samples were positioned in the chamber on a copper plate, heated up
to 100 °C, and TiCl4 (≥99.995%, Sigma-Aldrich)
and H2O (MilliQ) vapor pulses were injected with 18 s delay
in between each pulse (20 ms duration for both TiCl4 and
H2O). The base pressure of the system was 0.04–0.07
mbar, while during the deposition, the pressure was kept at 1.1 mbar
with an influx of N2. After the deposition of around 22
nm of TiO2, which corresponded to 300 cycles (∼0.07
nm/cycle), the samples were annealed in a tube furnace in air for
3 h at 350 °C with a heating rate of 11 °C/min. A similar
procedure was followed for the deposition of the alumina (Al2O3) thin layers on Au nanoislands. In the Al2O3 ALD process, the chamber was heated up to 250 °C
and trimethylaluminum (TMA) and H2O (MilliQ) vapor pulses
were injected with 18 s delay in between each pulse (10 ms duration
for both TMA and H2O).
15 mm) were cleaned with detergent, rinsed with demineralized water,
acetone, and isopropanol, and dried with a N2 stream. A
thin TiO2 layer was then deposited on the substrates with
atomic layer deposition in a home-built system. The first few millimeters
of the sample surface were covered with a Kapton tape, in order to
leave a part of the surface conductive to do the electrical connections
during the photoelectrochemical characterization of the samples. The
samples were positioned in the chamber on a copper plate, heated up
to 100 °C, and TiCl4 (≥99.995%, Sigma-Aldrich)
and H2O (MilliQ) vapor pulses were injected with 18 s delay
in between each pulse (20 ms duration for both TiCl4 and
H2O). The base pressure of the system was 0.04–0.07
mbar, while during the deposition, the pressure was kept at 1.1 mbar
with an influx of N2. After the deposition of around 22
nm of TiO2, which corresponded to 300 cycles (∼0.07
nm/cycle), the samples were annealed in a tube furnace in air for
3 h at 350 °C with a heating rate of 11 °C/min. A similar
procedure was followed for the deposition of the alumina (Al2O3) thin layers on Au nanoislands. In the Al2O3 ALD process, the chamber was heated up to 250 °C
and trimethylaluminum (TMA) and H2O (MilliQ) vapor pulses
were injected with 18 s delay in between each pulse (10 ms duration
for both TMA and H2O).
4
TiO2 Thin Film Deposition by ALD
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The n-type Si wafers in our experiments were 380-µm-thick, 3-inch-diameter, single-side polished, <100> oriented, and with a resistivity of 1–10 Ω⋅cm. Prior to ALD, Si wafers were washed with acetone, isopropanol, and deionized (DI) water in an ultrasonic bath for 20 min sequentially, followed by immersing in 5 wt% HF solution to remove the native oxide. TiO2 was deposited in a homemade ALD system following reported procedures2 (link),9 (link). In specific, N2 gas with a flow rate of 40 sccm was introduced into the chamber to serve as the carrier gas. The system base pressure was kept at 780 mTorr. The chamber temperature was maintained at 100 °C for depositions. Precursors used for TiO2 deposition were TiCl4 (Sigma-Aldrich, 99.9%) and DI H2O. TiCl4 (Sigma-Aldrich, 99.9%). Both precursor vapors were pulsed into the deposition chamber separately with a pulsing time of 0.5 s each and separated by 60 s N2 purging. Therefore, one deposition cycle involves 0.5 s of H2O pulse + 60 s of N2 purging + 0.5 s of TiCl4 pulse + 60 s of N2 purging. Through this procedure, ~15 nm TiO2 film was obtained after 200 cycles. For TDMAT-TiO2 film, the film was deposited under a recommended temperature of 250 °C in Fiji G2 ALD with TDMAT precursor (Sigma-Aldrich, 99.99%) with 300 cycles for comparison.
5
Fabrication of Dye-Sensitized TiO2 Electrodes
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A 40 mM titanium tetrachloride (TiCl4, Aldrich) solution was prepared, and cleaned FTO substrates were immersed in this solution for 30 min (70 °C). Using the screen-print technique, nanocrystalline transparent TiO2 electrodes (TiO2 paste-Dyesol 18NR-T) were deposited onto the FTO glass substrates and then annealed at 500 °C for 30 min. The thickness of this layer was confirmed using an Alpha-step 250 surface profilometer (Tencor Instruments). The as-prepared TiO2 electrodes were annealed at 500 °C for 30 min and then immersed in a THF/ethanol (v/v, 2:1) solution containing 0.3 mM JK-306 dye and 0.3 mM 4-[bis(9,9-dimethyl-9H-fluoren-2-yl)amino]benzoic acid coadsorbent for 12 h at room temperature.
6
Synthesis of Metal Oxide Nanoparticles
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Aqueous solutions of metal oxide nanoparticles were prepared following the literature methods59 (link). For the TNP sol, 11.0 ml of TiCl4 (Aldrich, 99.8%) was added drop by drop into the 189 ml of 6 M HCl (Samchun Chemical, 34–36%) aqueous solution under vigorous stirring at 1 °C for 10 min. After aging at room temperature for 3 h and then 16 h at 80 °C, a transparent sol, containing titania nanoparticles with about 4 nm average particle size, was obtained. The tin oxide and mixed oxide nanoparticles are also obtained by a similar method with the preparation of TNP. For the SNP sol solution, 35.0 g of TEOS (Aldrich, 98%) and 35.0 g of ethanol (JT Baker, 98%) were added into 16.0 mL of 10−3 M HCl aqueous solution, and further stirred for 12 h at 40 °C. The SNP sol thus obtained was poured into 100 mL of the TNP sol in a designated Si/Ti ratio at 30 °C under vigorous stirring. The mixture solution was titrated by dropwising a 1 M NaOH solution. After the titration (to reach pH 1.5) and stirring for 1 d at 30 °C, the reaction batch was transferred to a 100 °C oven and kept there for 1 d. White powders were obtained by filtration and drying at 80 °C, which, upon treating in 100 ml of 1 M NaOH aqueous solution at 70 °C for 1 h followed by filtration, produced the MT-x samples.
7
Synthesis of Anatase Titania Nanoparticles
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8
Perovskite Solar Cell Fabrication
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FTO glass, Ti(iPrO)2(acac)2 and spiro-OMeTAD were ordered from LumTec. Lithium bis-(trifluoromethylsulfonyl)imide (>99.95%), CH3NH3I (MAI), lead iodide, TiCl4, and benzoic acid (BA, 99%, Mw = 122.12 g mol−1) were provided from Aldrich.
9
Fabrication of Dye-Sensitized TiO2 Electrodes
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TiO2 and N-doped TiO2 porous electrodes were deposited on pre-cleaned FTO glass substrates initially covered with a TiO2 blocking layer deposited by chemical spray pyrolysis, using spin-coating from formulations based on ethanol, α-terpineol and ethyl-cellulose (EC), as previously described [38 (link)]. These films were progressively sintered up to 430 °C during 40 min in air. A TiCl4 treatment (Aldrich, 0.04 M in deionized water) was performed on these films before a final sintering step at 430 °C in air during 45 min. The 1.8 µm thick electrodes were then immersed in D102 dye (Mitsubishi Paper Mills, Tsukuba, Japan) dissolved in an acetonitrile:tert-butanol mixture (1:1 in volume) at 80 °C overnight. The sensitized electrodes were rinsed and infiltrated by the hole transporting material (HTM) spiro-OMeTAD (Merck KGaA, Darmstadt, Germany) by spin-coating in ambient conditions, following recipes previously reported [37 (link),38 (link)]. Gold counter electrodes were evaporated through a shadow mask at 10−6 mbar, leading to two independent active areas of 0.18 cm² per cell.
10
Synthesis of Carbon-Doped Black TiO2 Nanomaterial
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Carbon doped black TiO2 nanomaterial was synthesized via a modified chemical precipitation method, as reported in previous work [25 (link)]. Figure 1 shows a schematic illustration of the synthesis carbon doped black TiO2 nanomaterial. TiCl4 (Merck, 99.9%) was used as a precursor and 0.10 mole of it were added dropwise into a mixture of water and glycerol (9:1, v/v) (100 mL) under vigorous stirring. The TiO2 precipitates were obtained by adding NH4OH (2.5 M) into the Ti(OH)4 sol.
The precipitates were recovered by centrifugation at 6000 rpm for 10 min, and washed thoroughly with deionized water to remove residual chloride ions, followed by drying at 80 °C for 24 h in an oven (Memmert, Schwabach, Germany). The dried powder was grinded and calcined at 300 °C for an hour in a muffle furnace (Nabertherm) to get carbon doped black TiO2 nanomaterial. For ease of referencing, the carbon doped black TiO2 nanomaterial was labeled as CB-TiO2.
The precipitates were recovered by centrifugation at 6000 rpm for 10 min, and washed thoroughly with deionized water to remove residual chloride ions, followed by drying at 80 °C for 24 h in an oven (Memmert, Schwabach, Germany). The dried powder was grinded and calcined at 300 °C for an hour in a muffle furnace (Nabertherm) to get carbon doped black TiO2 nanomaterial. For ease of referencing, the carbon doped black TiO2 nanomaterial was labeled as CB-TiO2.
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