70fbe844145135236cf7b2bb0ae1916b pmc_34947718.pdf 7252ac6f809db4bc41f2521069b1c11fe81fce93 pmc_34947718.pdf 418728817758f318af35a0f3919d1115c80a65f525a4a9dae7ffb8d6ee31ed54 pmc_34947718.pdf Title: Heat-Up Colloidal Synthesis of Shape-Controlled Cu-Se-S Nanostructures—Role of Precursor and Surfactant Reactivity and Performance in N2 Electroreduction Subject: Copper selenide-sulfide nanostructures were synthesized using metal-organic chemical routes in the presence of Cu- and Se-precursors as well as S-containing compounds. Our goal was first to examine if the initial Cu/Se 1:1 molar proportion in the starting reagents would always lead to equiatomic composition in the final product, depending on other synthesis parameters which affect the reagents reactivity. Such reaction conditions were the types of precursors, surfactants and other reagents, as well as the synthesis temperature. The use of ‘hot-injection’ processes was avoided, focusing on ‘non-injection’ ones; that is, only heat-up protocols were employed, which have the advantage of simple operation and scalability. All reagents were mixed at room temperature followed by further heating to a selected high temperature. It was found that for samples with particles of bigger size and anisotropic shape the CuSe composition was favored, whereas particles with smaller size and spherical shape possessed a Cu2-xSe phase, especially when no sulfur was present. Apart from elemental Se, Al2Se3 was used as an efficient selenium source for the first time for the acquisition of copper selenide nanostructures. The use of dodecanethiol in the presence of trioctylphosphine and elemental Se promoted the incorporation of sulfur in the materials crystal lattice, leading to Cu-Se-S compositions. A variety of techniques were used to characterize the formed nanomaterials such as XRD, TEM, HRTEM, STEM-EDX, AFM and UV-Vis-NIR. Promising results, especially for thin anisotropic nanoplates for use as electrocatalysts in nitrogen reduction reaction (NRR), were obtained. Keywords: bottom-up synthesis; electrochemistry; wet chemistry; morphology; copper chalcogenides; nitrogen reduction reaction; metal-organic chemistry Author: Stefanos Mourdikoudis, George Antonaropoulos, Nikolas Antonatos, Marcos Rosado, Liudmyla Storozhuk, Mari Takahashi, Shinya Maenosono, Jan Luxa, Zdeněk Sofer, Belén Ballesteros, Nguyen Thi Kim Thanh and Alexandros Lappas Creator: LaTeX with hyperref Producer: pdfTeX-1.40.21 CreationDate: Sun Dec 12 11:54:14 2021 CET ModDate: Sun Dec 12 12:07:36 2021 CET Tagged: no UserProperties: no Suspects: no Form: none JavaScript: no Pages: 21 Encrypted: no Page size: 595.276 x 841.89 pts (A4) Page rot: 0 File size: 5184109 bytes Optimized: no PDF version: 1.7 name type encoding emb sub uni object ID ------------------------------------ ----------------- ---------------- --- --- --- --------- BTFGED+VnURWPalladioL-Bold Type 1 Custom yes yes no 10 0 QRZTQD+URWPalladioL-Ital Type 1 Custom yes yes no 15 0 NDYGIC+URWPalladioL-Bold Type 1 Custom 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no 254 0 DDLLHK+PalatinoLinotype,Italic TrueType WinAnsi yes yes no 257 0 DDLLGH+PalatinoLinotype,Bold TrueType WinAnsi yes yes no 271 0 DDLLGJ+PalatinoLinotype TrueType WinAnsi yes yes no 274 0 DDLLHK+PalatinoLinotype,Italic TrueType WinAnsi yes yes no 277 0 DDLLGH+PalatinoLinotype,Bold TrueType WinAnsi yes yes no 292 0 DDLLGJ+PalatinoLinotype TrueType WinAnsi yes yes no 295 0 DDLLHK+PalatinoLinotype,Italic TrueType WinAnsi yes yes no 298 0 UNSLQC+EURM10 Type 1 Builtin yes yes no 308 0 DDLLGH+PalatinoLinotype,Bold TrueType WinAnsi yes yes no 322 0 DDLLGI+PalatinoLinotype CID TrueType Identity-H yes yes yes 325 0 DDLLGJ+PalatinoLinotype TrueType WinAnsi yes yes no 331 0 DDLLHK+PalatinoLinotype,Italic TrueType WinAnsi yes yes no 334 0 DDMDGM+Arial CID TrueType Identity-H yes yes yes 337 0 DDMDHM+Arial,Bold CID TrueType Identity-H yes yes yes 343 0 Jhove (Rel. 1.22.1, 2019-04-17) Date: 2023-05-27 02:52:40 CEST RepresentationInformation: pmc_34947718.pdf ReportingModule: PDF-hul, Rel. 1.12.1 (2019-04-17) LastModified: 2023-03-31 12:06:38 CEST Size: 5184109 Format: PDF Version: 1.7 Status: Well-Formed and valid SignatureMatches: PDF-hul MIMEtype: application/pdf PDFMetadata: Objects: 571 FreeObjects: 1 IncrementalUpdates: 0 DocumentCatalog: PageLayout: SinglePage PageMode: UseNone Outlines: Item: Title: Introduction Destination: edu.harvard.hul.ois.jhove.module.pdf.PdfSimpleObject@44c8afef Item: Title: Results and Discussion Destination: edu.harvard.hul.ois.jhove.module.pdf.PdfSimpleObject@7b69c6ba Children: Item: Title: Synthesis, Composition and Morphology Destination: edu.harvard.hul.ois.jhove.module.pdf.PdfSimpleObject@46daef40 Item: Title: Tauc Plots Band Gaps Destination: edu.harvard.hul.ois.jhove.module.pdf.PdfSimpleObject@12f41634 Item: Title: Nitrogen Reduction Reaction Destination: edu.harvard.hul.ois.jhove.module.pdf.PdfSimpleObject@13c27452 Item: Title: Conclusions Destination: edu.harvard.hul.ois.jhove.module.pdf.PdfSimpleObject@262b2c86 Item: Title: Materials and Methods Destination: edu.harvard.hul.ois.jhove.module.pdf.PdfSimpleObject@371a67ec Children: Item: Title: Synthesis of CuSe Nanostructures Destination: edu.harvard.hul.ois.jhove.module.pdf.PdfSimpleObject@5ed828d Item: Title: Characterisation Instruments Destination: edu.harvard.hul.ois.jhove.module.pdf.PdfSimpleObject@50d0686 Item: Title: References Destination: edu.harvard.hul.ois.jhove.module.pdf.PdfSimpleObject@7a3d45bd Info: Title: Heat-Up Colloidal Synthesis of Shape-Controlled Cu-Se-S Nanostructures Role of Precursor and Surfactant Reactivity and Performance in N2 Electroreduction Author: こぴづてちのはび〠きはふひつどにはふつどび〬〠ぇづはひでづ〠ぁのぴはのちひはばはふぬはび〬〠ぎどにはぬちび〠ぁのぴはのちぴはび〬〠きちひっはび〠げはびちつは〬〠がどふつねべぬち〠こぴはひはぺとふに〬〠きちひど〠ごちにちとちびとど〬〠ことどのべち〠きちづのはびはのは〬〠おちの〠がふへち〬〠ずつづのㅜ〳㍜〰に〠こはてづひ〬〠あづぬラの〠あちぬぬづびぴづひはび〬〠ぎでふべづの〠ごとど〠かどね〠ごとちのと〠ちのつ〠ぁぬづへちのつひはび〠がちばばちび Subject: Copper selenide-sulfide nanostructures were synthesized using metal-organic chemical routes in the presence of Cu- and Se-precursors as well as S-containing compounds. Our goal was first to examine if the initial Cu/Se 1:1 molar proportion in the starting reagents would always lead to equiatomic composition in the final product, depending on other synthesis parameters which affect the reagents reactivity. Such reaction conditions were the types of precursors, surfactants and other reagents, as well as the synthesis temperature. The use of ‘hot-injection’ processes was avoided, focusing on ‘non-injection’ ones; that is, only heat-up protocols were employed, which have the advantage of simple operation and scalability. All reagents were mixed at room temperature followed by further heating to a selected high temperature. It was found that for samples with particles of bigger size and anisotropic shape the CuSe composition was favored, whereas particles with smaller size and spherical shape possessed a Cu2-xSe phase, especially when no sulfur was present. Apart from elemental Se, Al2Se3 was used as an efficient selenium source for the first time for the acquisition of copper selenide nanostructures. The use of dodecanethiol in the presence of trioctylphosphine and elemental Se promoted the incorporation of sulfur in the materials crystal lattice, leading to Cu-Se-S compositions. A variety of techniques were used to characterize the formed nanomaterials such as XRD, TEM, HRTEM, STEM-EDX, AFM and UV-Vis-NIR. Promising results, especially for thin anisotropic nanoplates for use as electrocatalysts in nitrogen reduction reaction (NRR), were obtained. Keywords: bottom-up synthesis; electrochemistry; wet chemistry; morphology; copper chalcogenides; nitrogen reduction reaction; metal-organic chemistry Creator: LaTeX with hyperref Producer: pdfTeX-1.40.21 CreationDate: Sun Dec 12 11:54:14 CET 2021 ModDate: Sun Dec 12 12:07:36 CET 2021 ID: 0xc11c22ec1edf7584858790cbb219ecc9, 0xc11c22ec1edf7584858790cbb219ecc9 Filters: FilterPipeline: FlateDecode Fonts: Type1: Font: BaseFont: NDYGIC+URWPalladioL-Bold FontSubset: true FirstChar: 3 LastChar: 151 FontDescriptor: FontName: NDYGIC+URWPalladioL-Bold Flags: Symbolic FontBBox: -152, -301, 1000, 935 FontFile: true EncodingDictionary: Differences: true Font: BaseFont: UNSLQC+EURM10 FontSubset: true FirstChar: 21 LastChar: 22 FontDescriptor: FontName: UNSLQC+EURM10 Flags: Symbolic FontBBox: -32, -243, 1060, 720 FontFile: true Font: BaseFont: NKKHRM+URWPalladioL-Roma FontSubset: true FirstChar: 2 LastChar: 223 FontDescriptor: FontName: NKKHRM+URWPalladioL-Roma Flags: Symbolic FontBBox: -166, -283, 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