研究目的
The first objective was to synthesize 1D TiO2 photocatalysts using an alkaline hydrothermal method. The second objective was to evaluate the effects of hydrothermal process conditions on photocatalytic H2 production rate using a Box Behnken design. The third objective was to optimize hydrothermal conditions for maximum H2 production. The final objective was to decorate the optimized catalyst with noble metals and investigate H2 production using various electron donors.
研究成果
The hydrothermal synthesis of 1D TiO2 with optimized conditions (126°C, 15 M NaOH, 49 g/L TiO2) produced anatase phase with a mean crystal size of 20.1 nm, achieving a maximum H2 production rate of 475 μmol/h. Decoration with Pt and Au further enhanced H2 production. The phase structure and crystal size are critical factors, with anatase showing superior performance over biphasic structures. This method offers an efficient and low-cost approach for H2 production from various electron donors.
研究不足
The study is limited to specific hydrothermal conditions and electron donors; it may not generalize to other synthesis methods or substrates. The use of UV light restricts applicability to solar-based systems without modification. The model's accuracy is constrained by the experimental design and assumptions in statistical analysis.
1：Experimental Design and Method Selection:
A 3-factor 3-level Box Behnken design (BBD) was used to optimize hydrothermal synthesis conditions (temperature, NaOH concentration, TiO2 concentration) for H2 production. The alkaline hydrothermal method was employed for synthesizing 1D TiO2. Photocatalytic H2 production experiments were conducted under UV light irradiation with ethanol as the primary electron donor.
2：Photocatalytic H2 production experiments were conducted under UV light irradiation with ethanol as the primary electron donor.
Sample Selection and Data Sources:
2. Sample Selection and Data Sources: Commercial TiO2 nanoparticles (P25) were used as a precursor. Samples were synthesized under 15 different conditions as per the BBD matrix. Data on H2 production rates, crystal size, and BET SSA were collected from experiments.
3：List of Experimental Equipment and Materials:
Equipment included hydrothermal reactors (Teflon containers in stainless-steel bombs), FESEM (JEOL), HRTEM (JEOL 3010), XRD (Rigaku with Cu Kα radiation), Raman spectrometer (WITec Alpha300 RA), UV-Vis spectrometer (Cary 300, Agilent), BET analyzer (Micromeritics ASAP 2020), photocatalytic reactors (quartz tubes), UV light source (LZC-UVB-016 lamp, Luzchem), gas chromatograph (Varian CP-3800). Materials included TiO2 P25 (Degussa/Evonik), NaOH, ethanol, methanol, formic acid, 1,2,3 propanetriol, HAuCl4, H2PtCl6, FTO glass, PEG, HCl.
4：0). Materials included TiO2 P25 (Degussa/Evonik), NaOH, ethanol, methanol, formic acid, 1,2,3 propanetriol, HAuCl4, H2PtCl6, FTO glass, PEG, HCl.
Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: For synthesis, TiO2 P25 was mixed with NaOH solution, heated in a Teflon container at specified temperatures for 48 h, washed with HCl and water, and calcined at 400°C. For photocatalytic experiments, reaction mixtures with photocatalyst and electron donor were purged with N2, stirred in dark for 1 h, irradiated with UV light at 37°C, and H2 concentration was measured by GC at intervals. Noble metal decoration involved dispersing TiO2 in water-ethanol, adding metal precursors, and reducing with ethanol or UV light.
5：Data Analysis Methods:
H2 production rates were modeled using a quadratic equation via multiple regression analysis in Minitab. ANOVA was used to assess model significance. Quantum efficiency was calculated based on photon numbers. Crystal size was determined using the Scherrer equation from XRD data. BET SSA was measured from nitrogen adsorption isotherms.
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