Mendeleev Commun., 2016, 26, 231–234 – 231 – Mendeleev Communications © 2016 Mendeleev Communications. Published by ELSEVIER B.V. on behalf of the N. D. Zelinsky Institute of Organic Chemistry of the Russian Academy of Sciences. Graphene is currently the most intensively studied material for a wide range of applications including electronics, solar energy, batteries and sensors. 1–4 It is biocompatible and seems to have superior properties compared to other sensor materials. 3,5 In particular, graphene-based materials have unique chemical and physical properties which make them very promising for applica- tions in biology and, particularly, for surface-enhanced Raman spectroscopy (SERS) in medical diagnostics. 2,3,6–11 Graphene oxide (GO) is a convenient construction block for building and self-assembling nanocomposites including GO–metal nanoparticles materials. 6–20 The GO precursor offers the unique advantage of tunable physical and chemical properties which can be achieved simply by oxidizing or reducing GO. This can drastically change the types and amounts of functional groups and defects associated with GO. 12,13 A usual way to create a GO–metal nanocomposite includes a separate synthesis of noble metal nanoparticles and their binding to the surface of GO using electrostatic forces or chemical interactions with thiols or amines. 6–11 Only in few works, nucleation and growth of plasmonic nanoparticles in the presence of GO is suggested by soft chemistry methods. 10,15–20 Aerosol spray pyrolysis (ASP) is an effective streaming and scalable method based on spraying of micrometre-sized droplets of precursor solutions and their fast nonequilibrium transforma- tion at high temperatures into solid phases and nanostructured materials. 11,21–23 The droplets play the role of microreactors often providing such nanostructuring. 21 Unfortunately, applica- tion of this technique with respect to GO and noble metal nanocomposites is limited at the moment and focused on gold nanoparticles mostly. 11 At the same time, GO itself can serve as either a reducing or anchoring agent specifically for silver ions; therefore, Ag@GO nanocomposites would benefit from these properties. In this work, the ASP method was applied for the first time to produce effectively and in one step Ag@GO nanostruc- tures with tuned nanoparticle load, sizes and an overall specific area of the nanocomposite and also graphene oxide mediated SERS substrates. Both the routes for the nanoparticles and the substrates are basically same and include a new effective and scalable streaming procedure based on diamminesilver hydroxide self-reduction on the surface of GO flakes. [Ag(NH 3 ) 2 ] + derivatives are suitable precursors for the preparation of pure silver nano- particles even without an application of additional reagents thus providing new possibilities for Ag-based biocompatible SERS material formation. 21,22 The colloidal GO was prepared by the modified Hammers method of oxidation of graphite powder (TIMCAL TIMREX ® KS4, 99.9%). 12 In brief, graphite powder was mixed with sodium nitrate and 98% sulfuric acid inside an ice bath and then KMnO 4 was slowly added under magnetic stirring at temperature lower than 70 °C. The obtained brownish mixture was accurately diluted with distilled water, then remained KMnO 4 and MnO 2 were reduced and dissolved using 3% H 2 O 2 , while the color of the mixture turned into yellow. The suspension of graphene oxide was left to stay overnight to complete all the reduction processes and then it was centrifuged and washed with distilled water for at least three times. To prepare the Ag@GO nanocomposites, a precursor suspen- sion of GO was mixed with 0.01 M [Ag(NH 3 ) 2 ]OH aqueous solution in volumetric ratios of 1:1, 10:1 and 100:1, respectively, while the original concentration of GO was fixed at about 3.9×10 –2 M. Diamminesilver solution was simply prepared by dissolution of silver nitrate in pure water, precipitation of silver(I) oxide with 0.5 M sodium hydroxide, washing and adding aqueous ammonia as described. 21,22 After that, the precursor mixture was transformed into an aerosol stream by an ultrasonic nebulizer and decomposed in a hot zone of a tubular furnace (600–800 °C) followed by collecting the resulting powder onto a porous glass filter. To form the GO mediated SERS substrates, the 1:1 precursor mixture of colloidal One-pot preparation of SERS nanocomposites of silver and graphene oxide with tunable properties Mariia O. Volodina, a Alexander Yu. Polyakov, b Alexander V. Sidorov, b,c Anastasia V. Grigorieva, b Elena A. Eremina, a,b Serguei V. Savilov a and Eugene A. Goodilin* a,b,d a Department of Chemistry, M. V. Lomonosov Moscow State University, 119991 Moscow, Russian Federation. Fax: +7 495 939 0998; e-mail: goodilin@yandex.ru, goodilin@inorg.chem.msu.ru b Department of Materials Science, M. V. Lomonosov Moscow State University, 119991 Moscow, Russian Federation c National Research Centre ‘Kurchatov Institute’, 123098 Moscow, Russian Federation d N. S. Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences, 119991 Moscow, Russian Federation DOI: 10.1016/j.mencom.2016.05.003 Surface-enhanced Raman spectroscopy-active nanocom- posites of silver and graphene oxide were obtained by ultra- sonic aerosol spray pyrolysis of graphene oxide suspension in diamminesilver(I) hydroxide aqueous solution thus allowing one to tune silver nanoparticle load, size and an overall specific area of the nanocomposite.