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Recently, Cs<jats:sub>2<\/jats:sub>AgBiBr<jats:sub>6<\/jats:sub> has emerged as a promising material, with suboptimal photon\u2010to\u2010charge carrier conversion efficiency, yet well suited for high\u2010energy photon\u2010detection applications. Here, the optoelectronic and structural properties of pure Cs<jats:sub>2<\/jats:sub>AgBiBr<jats:sub>6<\/jats:sub> and alkali\u2010metal\u2010substituted (Cs<jats:sub>1\u2212<\/jats:sub><jats:italic><jats:sub>x<\/jats:sub><\/jats:italic>Y<jats:italic><jats:sub>x<\/jats:sub><\/jats:italic>)<jats:sub>2<\/jats:sub>AgBiBr<jats:sub>6<\/jats:sub> (Y: Rb<jats:sup>+<\/jats:sup>, K<jats:sup>+<\/jats:sup>, Na<jats:sup>+<\/jats:sup>; <jats:italic>x<\/jats:italic>\u00a0= 0.02) single crystals are investigated. Strikingly, alkali\u2010substitution entails a tunability to the material system in its response to X\u2010rays and structural properties that is most strongly revealed in Rb\u2010substituted compounds whose X\u2010ray sensitivity outperforms other double\u2010perovskite\u2010based devices reported. While the fundamental nature and magnitude of the bandgap remains unchanged, the alkali\u2010substituted materials exhibit a threefold boost in their fundamental carrier recombination lifetime at room temperature. Moreover, an enhanced electron\u2013acoustic phonon scattering is found compared to Cs<jats:sub>2<\/jats:sub>AgBiBr<jats:sub>6<\/jats:sub>. The study thus paves the way for employing cation substitution to tune the properties of double perovskites toward a new material platform for optoelectronics.<\/jats:p>","DOI":"10.1002\/adma.202001878","type":"journal-article","created":{"date-parts":[[2020,8,31]],"date-time":"2020-08-31T03:49:00Z","timestamp":1598845740000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":117,"title":["Tuning the Structural and Optoelectronic Properties of Cs<sub>2<\/sub>AgBiBr<sub>6<\/sub> Double\u2010Perovskite Single Crystals through Alkali\u2010Metal Substitution"],"prefix":"10.1002","volume":"32","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-3685-6778","authenticated-orcid":false,"given":"Masoumeh","family":"Keshavarz","sequence":"first","affiliation":[{"name":"Molecular Imaging and Photonics Department of Chemistry KU Leuven  Celestijnenlaan 200F Leuven 3001 Belgium"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1087-4759","authenticated-orcid":false,"given":"Elke","family":"Debroye","sequence":"additional","affiliation":[{"name":"Molecular Imaging and Photonics Department of Chemistry KU Leuven  Celestijnenlaan 200F Leuven 3001 Belgium"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Martin","family":"Ottesen","sequence":"additional","affiliation":[{"name":"Department of Chemistry and iNANO Aarhus University  Langelandsgade 140 Aarhus C 8000 Denmark"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Cristina","family":"Martin","sequence":"additional","affiliation":[{"name":"Molecular Imaging and Photonics Department of Chemistry KU Leuven  Celestijnenlaan 200F Leuven 3001 Belgium"},{"name":"Departamento de Qu\u00edmica F\u00edsica, Facultad de Farmacia de Albacete UCLM  Albacete 02071 Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Heng","family":"Zhang","sequence":"additional","affiliation":[{"name":"Max Planck Institute for Polymer Research  Ackermannweg 10 Mainz 55128 Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Eduard","family":"Fron","sequence":"additional","affiliation":[{"name":"Molecular Imaging and Photonics Department of Chemistry KU Leuven  Celestijnenlaan 200F Leuven 3001 Belgium"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Robert","family":"K\u00fcchler","sequence":"additional","affiliation":[{"name":"Max Planck Institute for Chemical Physics of Solids  N\u00f6thnitzer Str. 40 Dresden 01187 Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Julian A.","family":"Steele","sequence":"additional","affiliation":[{"name":"cMACS Department of Microbial and Molecular Systems KU Leuven  Celestijnenlaan 200F Leuven 3001 Belgium"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Martin","family":"Bremholm","sequence":"additional","affiliation":[{"name":"Department of Chemistry and iNANO Aarhus University  Langelandsgade 140 Aarhus C 8000 Denmark"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Joris","family":"Van de Vondel","sequence":"additional","affiliation":[{"name":"Quantum Solid\u2010State Physics (QSP) Department of Physics and Astronomy KU Leuven  Celestijnenlaan 200D Leuven 3001 Belgium"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hai I.","family":"Wang","sequence":"additional","affiliation":[{"name":"Max Planck Institute for Polymer Research  Ackermannweg 10 Mainz 55128 Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Mischa","family":"Bonn","sequence":"additional","affiliation":[{"name":"Max Planck Institute for Polymer Research  Ackermannweg 10 Mainz 55128 Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-6582-6514","authenticated-orcid":false,"given":"Maarten B. 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