najoNanosystems: Physics, Chemistry, MathematicsНаносистемы: физика, химия, математика2220-80542305-7971Университет ИТМО10.17586/2220-8054-2017-8-4-512-522najo-749Research ArticleCHEMISTRY AND MATERIALS SCIENCEХИМИЯ И НАУКА О МАТЕРИАЛАХSizes and size distributions of nanoparticles: Causes of differences in results obtained by transmission electron microscopy and small angle X-ray scatteringSizes and size distributions of nanoparticles: Causes of differences in results obtained by transmission electron microscopy and small angle X-ray scatteringShvedchenkoD. O.ShvedchenkoD. O.

119333; Leninsky pr., 59; Moscow

119333; Leninsky pr., 59; Moscow

dmitrymephi@gmail.comVolkovV. V.VolkovV. V.

119333; Leninsky pr., 59; Moscow

119333; Leninsky pr., 59; Moscow

vvo@ns.crys.ras.ruSuvorovaE. I.SuvorovaE. I.

119333; Leninsky pr., 59; Moscow

119333; Leninsky pr., 59; Moscow

suvorova@ns.crys.ras.ruA. V. Shubnikov Institute of Crystallography of Russian Academy of SciencesA. V. Shubnikov Institute of Crystallography of Russian Academy of Sciences20171308202584512522Copyright © Shvedchenko D.O., Volkov V.V., Suvorova E.I., 20252025Shvedchenko D.O., Volkov V.V., Suvorova E.I.Shvedchenko D.O., Volkov V.V., Suvorova E.I.Данная работа распространяется под лицензией Creative Commons Attribution 4.0.This work is licensed under a Creative Commons Attribution 4.0 License.https://nanojournal.ifmo.ru/jour/article/view/749

   Comparative size and structure characterization of silver and selenium nanoparticles obtained and stabilized in different polymer solutions was performed by transmission electron microscopy (TEM) and small-angle X-ray scattering (SAXS). Effects of instrumental properties, nature of the samples, data collecting and data processing on accuracy of measurements are highlighted and summarized. Numerical differences in the mode diameter values derived from the TEM and SAXS data were found to have different sources. The SAXS results can be misleading in case of small particles (2–4 nm), for instance, Ag nanoparticles formed and stabilized in some aqueous polymer solutions due to instrumental limits, while TEM can provide sufficient statistics on such nanoparticles. SAXS is efficient in characterization of size distributions for soft Se-polymer composite particles of 20 to 100 nm in diameter. TEM is mandatory for investigating the chemical and phase composition of particles in mixtures, and their formation mechanism.

   Comparative size and structure characterization of silver and selenium nanoparticles obtained and stabilized in different polymer solutions was performed by transmission electron microscopy (TEM) and small-angle X-ray scattering (SAXS). Effects of instrumental properties, nature of the samples, data collecting and data processing on accuracy of measurements are highlighted and summarized. Numerical differences in the mode diameter values derived from the TEM and SAXS data were found to have different sources. The SAXS results can be misleading in case of small particles (2–4 nm), for instance, Ag nanoparticles formed and stabilized in some aqueous polymer solutions due to instrumental limits, while TEM can provide sufficient statistics on such nanoparticles. SAXS is efficient in characterization of size distributions for soft Se-polymer composite particles of 20 to 100 nm in diameter. TEM is mandatory for investigating the chemical and phase composition of particles in mixtures, and their formation mechanism.

nanoparticlesseleniumsilvertransmission electron microscopysmall-angle X-ray scatteringsize distributionnanoparticlesseleniumsilvertransmission electron microscopysmall-angle X-ray scatteringsize distribution.ReferencesChu B., Liu T. Characterization of nanoparticles by scattering techniques. J. Nanopart. Res., 2000, 2, P. 29–41.Chu B., Liu T. Characterization of nanoparticles by scattering techniques. J. Nanopart. Res., 2000, 2, P. 29–41.Pedersen J.S. Analysis of small-angle scattering data from colloids and polymer solutions: modeling and least-squares fitting. Adv. Colloid. Interfac., 1997, 70, P. 171–210.Pedersen J.S. Analysis of small-angle scattering data from colloids and polymer solutions: modeling and least-squares fitting. Adv. Colloid. Interfac., 1997, 70, P. 171–210.Shvedchenko D.O., Suvorova E.I. A novel method of automated statistical analysis of polymer stabilized metal nanoparticles in electron microscopy images. Crystallogr. Rep.+, 2017, 62(5), P. 802–808.Shvedchenko D.O., Suvorova E.I. A novel method of automated statistical analysis of polymer stabilized metal nanoparticles in electron microscopy images. Crystallogr. Rep.+, 2017, 62(5), P. 802–808.Svergun D.I., Konarev P.V., Volkov V.V., Koch M.H.J., Sager W.F.C., Smeets J., Blokhuis E.M. A small angle x–ray scattering study of the droplet–cylinder transition in oil–rich sodium bis(2–ethylhexyl) sulfosuccinatemicroemulsions. J. Chem. Phys., 2000, 113, P. 1651–1665.Svergun D.I., Konarev P.V., Volkov V.V., Koch M.H.J., Sager W.F.C., Smeets J., Blokhuis E.M. A small angle x–ray scattering study of the droplet–cylinder transition in oil–rich sodium bis(2–ethylhexyl) sulfosuccinatemicroemulsions. J. Chem. Phys., 2000, 113, P. 1651–1665.Svergun D.I. Small-angle scattering studies of macromolecular solutions. J. Appl.Cryst., 2007, 40, P. s10–s17.Svergun D.I. Small-angle scattering studies of macromolecular solutions. J. Appl.Cryst., 2007, 40, P. s10–s17.Percus J.K., Yevick G.J. Analysis of Classical Statistical Mechanics by Means of Collective Coordinates. Phys. Rev., 1958, 110, P. 1–13.Percus J.K., Yevick G.J. Analysis of Classical Statistical Mechanics by Means of Collective Coordinates. Phys. Rev., 1958, 110, P. 1–13.Williams D.B., Carter C.B. Transmission Electron Microscopy. Plenum Press, New York, 1996, 729 pp.Williams D.B., Carter C.B. Transmission Electron Microscopy. Plenum Press, New York, 1996, 729 pp.Nekrasova T.N., Zolotova Y.I., Nazarova O.V., Levit M.L., Suvorova E.I., Sirotkin A.K., Baklagina Y.G., Didenko E.V., Pautov V.D.,Panarin E.F. Silver nanocomposites based on (Co)polymers of 2-deoxy-2-methacrylamido-D-glucose, N-vinylamides, and aminoacrylates. Dokl. Chem., 2013, 446, P. 212–214.Nekrasova T.N., Zolotova Y.I., Nazarova O.V., Levit M.L., Suvorova E.I., Sirotkin A.K., Baklagina Y.G., Didenko E.V., Pautov V.D.,Panarin E.F. Silver nanocomposites based on (Co)polymers of 2-deoxy-2-methacrylamido-D-glucose, N-vinylamides, and aminoacrylates. Dokl. Chem., 2013, 446, P. 212–214.Shvedchenko D.O., Nekrasova T.N., Nazarova O.V., Buffat P.A., Suvorova E.I. Mechanism of formation of silver nanoparticles in MAG–DMAEMA copolymer aqueous solutions. J. Nanopart. Res., 2015, 17, P. 275.Shvedchenko D.O., Nekrasova T.N., Nazarova O.V., Buffat P.A., Suvorova E.I. Mechanism of formation of silver nanoparticles in MAG–DMAEMA copolymer aqueous solutions. J. Nanopart. Res., 2015, 17, P. 275.Valueva S.V., Kopeikin V.V., Kipper A.I., Filippov A.P., Shishkina G.V., Khlebosolova E.N., Rumyantseva N.V., Nazarkina Y.I., Borovikova L.N. Formation of Zero-Valence Selenium Nanoparticles in Polyampholyte Aqueous Solutions in the Presence of Redox Systems. Polym. Sci. Ser. B+, 2005, 47, P. 143–146.Valueva S.V., Kopeikin V.V., Kipper A.I., Filippov A.P., Shishkina G.V., Khlebosolova E.N., Rumyantseva N.V., Nazarkina Y.I., Borovikova L.N. Formation of Zero-Valence Selenium Nanoparticles in Polyampholyte Aqueous Solutions in the Presence of Redox Systems. Polym. Sci. Ser. B+, 2005, 47, P. 143–146.Valueva S.V., Kipper A.I., Kopeikin V.V., Borovikova L.N., Lavrent’ev V.K., Ivanov D.A., Filippov A.P. Formation and Morphological Characteristics of Selenium-Containing Nanostructures Based on Rigid-Chain Cellulose Derivatives. Polym. Sci. Ser. A+, 2006, 48, P. 803–810.Valueva S.V., Kipper A.I., Kopeikin V.V., Borovikova L.N., Lavrent’ev V.K., Ivanov D.A., Filippov A.P. Formation and Morphological Characteristics of Selenium-Containing Nanostructures Based on Rigid-Chain Cellulose Derivatives. Polym. Sci. Ser. A+, 2006, 48, P. 803–810.Mogilevsky L.Yu., Dembo A.T., Svergun D.I., Feigin L.A. Small-angle scattering diffractometer with single coordinates detector. Crystallogr. Rep.+, 1984, 29, P. 587–591.Mogilevsky L.Yu., Dembo A.T., Svergun D.I., Feigin L.A. Small-angle scattering diffractometer with single coordinates detector. Crystallogr. Rep.+, 1984, 29, P. 587–591.Konarev P.V., Volkov V.V., Sokolova A.V., Koch M.H.J., Svergun, D.I. PRIMUS: a Windows PC-based system for small-angle scattering data analysis. J. App.Cryst., 2003, 36, P. 1277–1282.Konarev P.V., Volkov V.V., Sokolova A.V., Koch M.H.J., Svergun, D.I. PRIMUS: a Windows PC-based system for small-angle scattering data analysis. J. App.Cryst., 2003, 36, P. 1277–1282.Feigin L.A., Svergun D.I. Structure Analysis by Small-Angle X-Ray and Neutron Scattering. Plenum Press, New York, 1987, 335 pp.Feigin L.A., Svergun D.I. Structure Analysis by Small-Angle X-Ray and Neutron Scattering. Plenum Press, New York, 1987, 335 pp.Suvorova E.I., Klechkovskaya V.V. Effect of polymer matrix on structure of Se particles formed in aqueous solutions during redox process. Crystallogr. Rep.+, 2010, 55, P. 1116–1121.Suvorova E.I., Klechkovskaya V.V. Effect of polymer matrix on structure of Se particles formed in aqueous solutions during redox process. Crystallogr. Rep.+, 2010, 55, P. 1116–1121.

The authors declare that there are no conflicts of interest present.