86feb9a3ef6c9d17028fe61748d5d727 jouofsynrad_a2024_v31.pdf 616ad3a4d5761e8670716acbad0df8012273ca09 jouofsynrad_a2024_v31.pdf b0abee8224924377c4a764da8113e8fcfe6f6c67d824e69f0b424a548d6a1ad6 jouofsynrad_a2024_v31.pdf Title: In situ photodeposition of ultra-small palladium particles on TiO2 Subject: In situ and operando investigation of photocatalysts plays a fundamental role in understanding the processes of active phase formation and the mechanisms of catalytic reactions, which is crucial for the rational design of more efficient materials. Using a custom-made operando photocatalytic cell, an in situ procedure to follow the formation steps of Pd/TiO2 photocatalyst by synchrotron-based X-ray absorption spectroscopy (XAS) is proposed. The procedure resulted in the formation of ∼1 nm Pd particles with a much narrower size distribution and homogeneous spreading over TiO2 support compared with the samples generated in a conventional batch reactor. The combination of in situ XAS spectroscopy with high-angle annular dark-field scanning transmission electron microscopy demonstrated the formation of single-atom Pd(0) sites on TiO2 as the initial step of the photodeposition process. Palladium hydride particles were observed for all investigated samples upon exposure to formic acid solutions. Author: Kozyr, E. Creator: pdftk-java 3.2.2 Producer: International Union of Crystallography CreationDate: Mon Jul 15 14:00:00 2024 CEST ModDate: Tue Oct 22 16:40:05 2024 CEST Custom Metadata: yes Metadata Stream: yes Tagged: no UserProperties: no Suspects: no Form: none JavaScript: no Pages: 7 Encrypted: no Page size: 609.676 x 793.701 pts Page rot: 0 File size: 1119439 bytes Optimized: yes PDF version: 1.6 name type encoding emb sub uni object ID ------------------------------------ ----------------- ---------------- --- --- --- --------- YEESPR+Optima_Bold Type 1 Builtin yes yes yes 362 0 YEESPR+Optima_Italic Type 1 Builtin yes yes yes 367 0 YEESPR+Optima_Roman Type 1 Builtin yes yes yes 372 0 YEESPR+Optima_Bold_Italic Type 1 Builtin yes yes yes 377 0 YEESPR+Times-93Italic Type 1 Builtin yes yes yes 382 0 YEESPR+Times-93Roman Type 1 Builtin yes yes yes 387 0 JFRBIV+TeX_Times_Math_Symbol Type 1 Builtin yes yes yes 392 0 JFRBIV+TeX_Times_Math_Italic Type 1 Builtin yes yes yes 282 0 JFRBIV+PI_chars_1 Type 1 Builtin yes yes yes 281 0 JFRBIV+Times-93Bold Type 1 Builtin yes yes yes 284 0 Jhove (Rel. 1.28.0, 2023-05-18) Date: 2024-11-22 02:47:02 CET RepresentationInformation: jouofsynrad_a2024_v31.pdf ReportingModule: PDF-hul, Rel. 1.12.4 (2023-03-16) LastModified: 2024-10-23 03:44:40 CEST Size: 1119439 Format: PDF Version: 1.6 Status: Well-Formed and valid SignatureMatches: PDF-hul MIMEtype: application/pdf Profile: Linearized PDF PDFMetadata: Objects: 0 FreeObjects: 1 IncrementalUpdates: 0 DocumentCatalog: ViewerPreferences: HideToolbar: false HideMenubar: false HideWindowUI: false FitWindow: false CenterWindow: false DisplayDocTitle: true NonFullScreenPageMode: UseNone Direction: L2R ViewArea: CropBox ViewClip: CropBox PrintArea: CropBox PageClip: CropBox PageLayout: SinglePage PageMode: UseNone Outlines: Item: Title: Abstract Destination: 1 Item: Title: 1. Introduction Destination: 1 Item: Title: 2. Materials and methods Destination: 1 Children: Item: Title: 2.1. Chemicals Destination: 1 Item: Title: 2.2. In situ XAS measurements Destination: 1 Item: Title: 2.3. HAADF-STEM measurements Destination: 1 Item: Title: 3. Results and discussion Destination: 1 Children: Item: Title: 3.1. In situ photodeposition of Pd on TiO2 Destination: 1 Item: Title: 3.2. Morphology of Pd/TiO2 samples Destination: 1 Item: Title: 4. Conclusions Destination: 1 Item: Title: Acknowledgements Destination: 1 Item: Title: Funding information Destination: 1 Item: Title: References Destination: 1 Filters: FilterPipeline: FlateDecode FilterPipeline: JPXDecode Images: Image: NisoImageMetadata: FormatName: image/jpx ImageWidth: 286 ImageHeight: 193 ColorSpace: RGB BitsPerSample: 8 BitsPerSampleUnit: integer Filter: JPXDecode Image: NisoImageMetadata: FormatName: image/jpx ImageWidth: 215 ImageHeight: 83 ColorSpace: CMYK BitsPerSample: 8 BitsPerSampleUnit: integer Filter: JPXDecode Image: NisoImageMetadata: FormatName: image/jpx ImageWidth: 52 ImageHeight: 52 ColorSpace: RGB BitsPerSample: 8 BitsPerSampleUnit: integer Filter: JPXDecode Image: NisoImageMetadata: FormatName: image/jpx ImageWidth: 256 ImageHeight: 35 BitsPerSample: 8 BitsPerSampleUnit: integer Filter: JPXDecode Image: NisoImageMetadata: FormatName: image/jpx ImageWidth: 795 ImageHeight: 250 BitsPerSample: 8 BitsPerSampleUnit: integer Filter: JPXDecode Image: NisoImageMetadata: FormatName: image/jpx ImageWidth: 797 ImageHeight: 316 ColorSpace: RGB BitsPerSample: 8 BitsPerSampleUnit: integer Filter: JPXDecode Image: NisoImageMetadata: FormatName: image/jpx ImageWidth: 817 ImageHeight: 324 ColorSpace: RGB BitsPerSample: 8 BitsPerSampleUnit: integer Filter: JPXDecode Image: NisoImageMetadata: FormatName: image/jpx ImageWidth: 612 ImageHeight: 413 ColorSpace: RGB BitsPerSample: 8 BitsPerSampleUnit: integer Filter: JPXDecode Image: NisoImageMetadata: FormatName: image/jpx ImageWidth: 653 ImageHeight: 405 ColorSpace: RGB BitsPerSample: 8 BitsPerSampleUnit: integer Filter: JPXDecode Fonts: Type1: Font: BaseFont: YEESPR+Times-93Roman FontSubset: true FirstChar: 32 LastChar: 251 FontDescriptor: FontName: YEESPR+Times-93Roman Flags: Symbolic FontBBox: -50, -180, 1000, 720 FontFile: true FontFile3: true ToUnicode: true Font: BaseFont: YEESPR+Optima_Roman FontSubset: true FirstChar: 33 LastChar: 251 FontDescriptor: FontName: YEESPR+Optima_Roman Flags: Symbolic FontBBox: -50, -180, 1000, 720 FontFile: true FontFile3: true ToUnicode: true Font: BaseFont: JFRBIV+TeX_Times_Math_Symbol FontSubset: true FirstChar: 1 LastChar: 138 FontDescriptor: FontName: JFRBIV+TeX_Times_Math_Symbol Flags: Symbolic FontBBox: -50, -180, 1000, 720 FontFile: true FontFile3: true ToUnicode: true Font: BaseFont: YEESPR+Optima_Bold_Italic FontSubset: true FirstChar: 33 LastChar: 251 FontDescriptor: FontName: YEESPR+Optima_Bold_Italic Flags: Symbolic, ForceBold FontBBox: -50, -180, 1000, 720 FontFile: true FontFile3: true ToUnicode: true Font: BaseFont: JFRBIV+PI_chars_1 FontSubset: true FirstChar: 33 LastChar: 126 FontDescriptor: FontName: JFRBIV+PI_chars_1 Flags: Symbolic FontBBox: -50, -180, 1000, 720 FontFile: true FontFile3: true ToUnicode: true Font: BaseFont: YEESPR+Optima_Bold FontSubset: true FirstChar: 33 LastChar: 251 FontDescriptor: FontName: YEESPR+Optima_Bold Flags: Symbolic, ForceBold FontBBox: -50, -180, 1000, 720 FontFile: true FontFile3: true ToUnicode: true Font: BaseFont: JFRBIV+TeX_Times_Math_Italic FontSubset: true FirstChar: 1 LastChar: 127 FontDescriptor: FontName: JFRBIV+TeX_Times_Math_Italic Flags: Symbolic FontBBox: -50, -180, 1000, 720 FontFile: true FontFile3: true ToUnicode: true Font: BaseFont: JFRBIV+Times-93Bold FontSubset: true FirstChar: 32 LastChar: 251 FontDescriptor: FontName: JFRBIV+Times-93Bold Flags: Symbolic, ForceBold FontBBox: -50, -180, 1000, 720 FontFile: true FontFile3: true ToUnicode: true Font: BaseFont: YEESPR+Times-93Italic FontSubset: true FirstChar: 32 LastChar: 251 FontDescriptor: FontName: YEESPR+Times-93Italic Flags: Symbolic FontBBox: -50, -180, 1000, 720 FontFile: true FontFile3: true ToUnicode: true Font: BaseFont: YEESPR+Optima_Italic FontSubset: true FirstChar: 33 LastChar: 251 FontDescriptor: FontName: YEESPR+Optima_Italic Flags: Symbolic FontBBox: -50, -180, 1000, 720 FontFile: true FontFile3: true ToUnicode: true XMP: True This work is licensed under a <a rel="license" href="http://creativecommons.org/licenses/by/4.0/">Creative Commons Attribution 4.0 UK: England & Wales License</a>. This work is licensed under a <a rel="license" href="http://creativecommons.org/licenses/by/4.0/">Creative Commons Attribution 4.0 UK: England & Wales License</a>. 2024-07-15 true 10.1107/S1600577524004788 iucr.org 10.1107/S1600577524004788 noindex 2024-07-15 true iucr.org 10.1107/S1600577524004788 VoR doi:10.1107/S1600577524004788 J. Synchrotron Rad (2024). 31, 1071-1077 [doi:10.1107/S1600577524004788] application/pdf research papers In situ photodeposition of ultra-small palladium particles on TiO2 en In situ and operando investigation of photocatalysts plays a fundamental role in understanding the processes of active phase formation and the mechanisms of catalytic reactions, which is crucial for the rational design of more efficient materials. Using a custom-made operando photocatalytic cell, an in situ procedure to follow the formation steps of Pd/TiO2 photocatalyst by synchrotron-based X-ray absorption spectroscopy (XAS) is proposed. The procedure resulted in the formation of ∼1 nm Pd particles with a much narrower size distribution and homogeneous spreading over TiO2 support compared with the samples generated in a conventional batch reactor. The combination of in situ XAS spectroscopy with high-angle annular dark-field scanning transmission electron microscopy demonstrated the formation of single-atom Pd(0) sites on TiO2 as the initial step of the photodeposition process. Palladium hydride particles were observed for all investigated samples upon exposure to formic acid solutions. 2024-07-15 International Union of Crystallography PHOTOCATALYSIS PD/TIO2 OPERANDO SPECTROSCOPY XANES Kozyr, E. Marti-Sanchez, S. Skorynina, A. Arbiol, J. Escudero, C. Mino, L. Bugaev, A. 2024-07-15T12:00Z pdftk-java 3.2.2 2024-10-22T14:40:05Z 2024-10-22T14:40:05Z International Union of Crystallography uuid:e256dd7a-f5f6-4376-8fb0-b2cd49703602 uuid:28f3ca86-1496-4ac1-87d9-fc1f70ec5d8f Pages: Page: Sequence: 1 Annotations: Annotation: Subtype: Link Rect: 371, 20, 526, 28 Flags: Print Annotation: Subtype: Link Rect: 44, 696, 152, 706 Flags: Print Annotation: Subtype: Link Rect: 79, 538, 125, 545 Flags: Print Annotation: Subtype: Link Rect: 125, 538, 154, 545 Flags: Print Annotation: Subtype: Link Rect: 154, 538, 183, 545 Flags: Print Annotation: Subtype: Link Rect: 44, 528, 88, 535 Flags: Print Annotation: Subtype: Link Rect: 88, 528, 111, 535 Flags: Print Annotation: Subtype: Link Rect: 44, 54, 173, 61 Flags: Print Annotation: Subtype: Link Rect: 44, 44, 156, 51 Flags: Print Annotation: Subtype: Link Rect: 283, 581, 345, 588 Flags: Print Annotation: Subtype: Link Rect: 44, 768, 70, 742 Page: Sequence: 2 Page: Sequence: 3 Page: Sequence: 4 Annotations: 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