Document Detail

The Importance of Nanocrystal Precursor Conversion Kinetics: Mechanism of the Reaction Between Cadmium Carboxylate and Cadmium Bis-diphenyldithiophosphinate.
MedLine Citation:
PMID:  23043371     Owner:  NLM     Status:  Publisher    
We describe the synthesis of cadmium bis-(diphenyldithiophosphinate) (Cd(S(2)PPh(2))(2)) from secondary phosphine sulfides and its conversion to cadmium sulfide nanocrystals. Heating Cd(S(2)PPh(2))(2) and cadmium tetradecanoate (≥4 equiv.) to 240 ˚C results in complete conversion of Cd(S(2)PPh(2))(2) to cadmium sulfide nanocrystals with tetradecanoate surface termination. The nanocrystals have a narrow size distribution (d = 3.8-4.1 nm, σ < 10%) that is evident from the linewidth of the lowest energy absorption feature (λ = 412 - 422 nm, fwhm = 0.17 eV) and display bright photoluminescence (PLQY(band edge + trap) = 36%). Interestingly, the final diameter is insensitive to the reaction conditions, including the total concentration of precursors and initial cadmium to sulfur ratio. Monitoring the reaction with (31)P NMR, UV-Visible, and infrared absorption spectroscopies shows that the production of cadmium diphenylphosphinate (Cd(O(2)PPh(2))(2)) and tetradecanoic anhydride co-products is coupled with the formation of cadmium sulfide. From these measurements we propose a balanced chemical equation for the conversion reaction and use it to optimize a synthesis that affords CdS nanocrystals in quantitative yield. In light of these results we discuss the importance of well-defined precursor reactivity to reproducible conversion kinetics and the synthesis of nanocrystals with unambiguous chemical composition.
Mark P Hendricks; Brandi M Cossairt; Jonathan S Owen
Publication Detail:
Type:  JOURNAL ARTICLE     Date:  2012-10-8
Journal Detail:
Title:  ACS nano     Volume:  -     ISSN:  1936-086X     ISO Abbreviation:  ACS Nano     Publication Date:  2012 Oct 
Date Detail:
Created Date:  2012-10-9     Completed Date:  -     Revised Date:  -    
Medline Journal Info:
Nlm Unique ID:  101313589     Medline TA:  ACS Nano     Country:  -    
Other Details:
Languages:  ENG     Pagination:  -     Citation Subset:  -    
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