Ten-gram-scale preparation of PTMS-based monodisperse ORMOSIL nano- and microparticles and conversion to silica particles

  • Jung Soo Kim
  • Gyu Il Jung
  • Soo Jung Kim
  • Sang Man Koo
Research Paper


Monodisperse organically modified silica (ORMOSIL) particles, with an average diameter ranging from 550 nm to 4.2 μm, were prepared at low temperature at a scale of about 10 g/batch by a simple one-step self-emulsion process. The reaction mixture was composed only of water, phenyltrimethoxysilane (PTMS), and a base catalyst, without any surfactants. The size control of the particles and the monodispersity of resultant particles were achieved through the controlled supply of hydrolyzed PTMS monomer molecules, which was enabled by manipulating the reaction parameters, such as monomer concentration, type and amount of base catalyst, stirring rate, and reaction temperature. PTMS-based ORMOSIL particles were converted into silica particles by employing either a wet chemical reaction with an oleum-sulfuric acid mixture or thermal treatment above 650 °C. Complete removal of organic groups from the ORMOSIL particles was achieved by the thermal treatment while ~ 74% removal was done by the chemical process used.

Graphical abstract


Phenyltrimethoxysilane ORMOSIL Nanoparticle Microparticle Self-emulsion process Conversion to silica 


Funding information

This work was supported by the Technology Innovation Program (10052730, Rutile TiO2 Powder Manufacturing Technology by TiCl4 Oxidation) funded by the Ministry of Trade, Industry and Energy (MI, Korea).

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest

Supplementary material

11051_2018_4186_MOESM1_ESM.docx (2.2 mb)
ESM 1 (DOCX 2246 kb)


  1. Argyo C, Weiss V, Bräuchle C, Bein T (2014) Multifunctional mesoporous silica nanoparticles as a universal platform for drug delivery. Chem Mater 26(1):435–451. CrossRefGoogle Scholar
  2. Bogush GH, Tracy MA, Zukoski CF IV (1988) Preparation of monodisperse silica particles: control of size and mass fraction. J Non-Cryst Solids 104(1):95–106. CrossRefGoogle Scholar
  3. Chai GS, Shin IS, Yu J (2004) Synthesis of ordered, uniform, macroporous carbons with mesoporous walls templated by aggregates of polystyrene spheres and silica particles for us as catalyst supports in direct methanol fuel cells. Adv Mater 16(22):2057–2061. CrossRefGoogle Scholar
  4. Cheong WJ (2014) Porous silica particles as chromatographic separation media: a review. Bull Kor Chem Soc 35(12):3465–3474. CrossRefGoogle Scholar
  5. de Oliveira LF, Bouchmella K, Gonçalves KA, Bettini J, Kobarg J, Cardoso MB (2016) Functionalized silica nanoparticles as an alternative platform for targeted drug-delivery of water insoluble drugs. Langmuir 32(13):3217–3225. CrossRefGoogle Scholar
  6. Genorio B, Pirnat K, Cerc-Korosec R, Dominko R, Gaberscek M (2010) Electroactive organic molecules immobilized onto solid nanoparticles as a cathode material for lithium-ion batteries. Angew Chem Int Ed 49(40):7222–7224. CrossRefGoogle Scholar
  7. Ha JM, Jung GI, Kim JS, Kim JW, Jeon SJ, Koo SM (2015) Synthesis of hyperbranched poly(amidoamine) conjugated silica (HBPcS) particles and their application to colorimetric detection of cadmium ion. Colloid Polym Sci 293(8):2331–2339. CrossRefGoogle Scholar
  8. Jung CY, Kim JS, Kim HY, Ha JM, Kim YH, Koo SM (2012) One-pot synthesis and surface modifications of organically modified silica (ORMOSIL) particles having multiple functional groups. J Colloid Interface Sci 367(1):67–73. CrossRefGoogle Scholar
  9. Kim P, Kim H, Joo JB, Kim W, Song IK, Yi J (2005) Preparation and application of nanoporous carbon templated by silica particle for use as a catalyst support for direct methanol fuel cell. J Power Sources 145(2):139–146. CrossRefGoogle Scholar
  10. Kondoh S, Kawada S, Takahashi R, Tajima E (2011) 2.7 inch QVGA type FLC-device for SLM. Ferroelectrics 246(1):121–129. CrossRefGoogle Scholar
  11. Lei X, Yu B, Cong H, Tian C, Wang Y, Wang Q, Liu C (2014) Synthesis of monodisperse silica microspheres by a modified Stöber method. Integr Ferroelectr 154(1):142–146. CrossRefGoogle Scholar
  12. Nagao D, Osuzu H, Yamada A, Mine E, Kobayashi Y, Konno M (2004) Particle formation in the hydrolysis of tetraethyl orthosilicate in pH buffer solution. J Colloid Interface Sci 279(1):143–149. CrossRefGoogle Scholar
  13. Quan B, Lee C, Yoo JS, Piao Y (2017) Facile scalable synthesis of highly monodisperse small silica nanoparticles using alkaline buffer solution and their application for efficient sentinel lymph node mapping. J Mater Chem B 5(3):586–594. CrossRefGoogle Scholar
  14. Roy I, Kumar P, Kumar R, Ohulchanskyy TY, Yong K, Prasad PN (2014) ORMOSIL nanoparticles as a sustained-release drug delivery vehicle. RSC Adv 4(96):53498–53504. CrossRefGoogle Scholar
  15. Santra S, Bagwe RP, Dutta D, Stanley JT, Walter GA, Tan W, Moudgil BM, Mericle RA (2005) Synthesis and characterization of fluorescent, radio-opaque, and paramagnetic silica nanoparticles for multimodal bioimaging applications. Adv Mater 17(18):2165–2169. CrossRefGoogle Scholar
  16. Stöber W, Fink A, Bohn E (1968) Controlled growth of monodisperse silica spheres in the micron size range. J Colloid Interface Sci 26(1):62–69. CrossRefGoogle Scholar
  17. Swihart MT (2003) Vapor-phase synthesis of nanoparticles. Curr Opin Colloid Interface Sci 8(1):127–133. CrossRefGoogle Scholar
  18. Tan CG, Bowen BD, Epstein N (1987) Production of monodisperse colloidal silica spheres: effect of temperature. J Colloid Interface Sci 118(1):290–293. CrossRefGoogle Scholar
  19. Wang X, Shen Z, Sang T, Cheng X, Li M, Chen L, Wang Z (2010) Preparation of spherical silica particles by Stöber process with high concentration of tetra-ethyl-orthosilicate. J Colloid Interface Sci 341(1):23–29. CrossRefGoogle Scholar
  20. Wang R, Zhang M, Liu F, Bao S, Wu T, Jiang X, Zhang Q, Zhu M (2015) Investigation on the physical-mechanical properties of dental resin composites reinforced with novel bimodal silica nanostructures. Mater Sci Eng C 50:266–273. CrossRefGoogle Scholar
  21. Yan F, Jiang J, Chen X, Tian S, Li K (2014) Synthesis and characterization of silica nanoparticles preparing by low-temperature vapor-phase hydrolysis of SiCl4. Ind Eng Chem Res 53(30):11884–11890. CrossRefGoogle Scholar
  22. Yuan J, Zhou S, You B, Wu L (2005) Organic pigment particles coated with colloidal nano-silica particles via layer-by-layer assembly. Chem Mater 17(14):3587–3594. CrossRefGoogle Scholar
  23. Zhang J, Raphael AP, Yang Y, Popat A, Prow TW, Yu C (2014) Nanodispersed UV blockers in skin-friendly silica vesicles with superior UV-attenuating efficiency. J Mater Chem B 2(44):7673–7678. CrossRefGoogle Scholar
  24. Zhao B, Tian C, Zhang Y, Tang T, Wang F (2011) Size control of monodisperse nonporous silica particles by seed particle growth. Particuology 9(3):314–317. CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media B.V., part of Springer Nature 2018

Authors and Affiliations

  1. 1.Department of Chemical EngineeringHanyang UniversitySeoulSouth Korea

Personalised recommendations