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Abstract
The configuration and geometry of chemical reactors underpins the accuracy of performance evaluation for photocatalytic materials and, accordingly, the development and validation of thermodynamic and kinetic model reactions. The lack of accurate photonic, mass, and heat transport profiles for photochemical reactors hinder standardization, scale-up, and ultimately comparison between different experiments. This work proposes two contributions at the interface between engineering of chemical process and materials science: (A) an automated compact stainless-steel photoreactor with 40 cm3 and 65 cm2 of volume and area, respectively, for hydrogen photoproduction as a model reaction and (B) the synthesis, characterization, and performance of TiO2 Schottky junctions, using Pd, Pt, or Au nanoparticles (ca. 0.5, 1, 2wt.% loadings each) to validate the operation of the reactor. A photonic profile methodology is implemented to the studied reactor to obtain the local light absorption profile, opening up for evaluation of the local quantum yield calculation for the selected materials. A combination of transmission electron microscopy, (X-ray/ultraviolet) photoelectron/electron, energy loss/infrared spectroscopies, X-ray scattering, inductively coupled plasma atomic emission spectroscopy, and ultraviolet-visible spectrophotometry is employed to determine the distinctive surface and bulk properties to build structure-function correlations. The (Pd, Pt, Au)/TiO2 Schottky junction exhibits H2 production rates slightly higher than previous studies, with quantum yields almost 2-fold higher than reported values. These results, demonstrate that the proposed novel geometry of the photoreactor improves the photonic, heat, and mass profiles. An in-depth analysis of the Au plasmon was investigated coupling electron energy loss spectroscopy, UV-vis, and transmission electron microscope, resulting in insightful information about the Au NP mode at the TiO2 interface.
Supplementary materials
Title
A compact photoreactor for automated H2 photoproduction: revisiting the (Pd, Pt, Au)/TiO2 (P25) Schottky junctions
Description
List of content:
S1 Photonic model methodology: Liquid phase reactor
Figure S1 Schematic representation of the experimental photoreactor setup
Table S1 Physicochemical and electronical properties of the materials
Figure S2 Metal NP size distribution and average size obtained by TEM of the materials
Figure S3 FT-IR spectra of the materials
Figure S4 XRS diffractograms of the materials
Figure S5 UV-vis spectra of the materials
Figure S6 XPS survey, Ti 2p, C1s, and O1s spectra of the materials
Figure S7 UPS spectra of the materials
Figure S8. Nominal metal loading of the materials
Figure S9 EELS of the 2%Au/TiO2(P25) composite
Figure S10 Light emission spectra of the Hg arc lamp
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