Designer poly(urea-siloxane) microspheres with controlled modulus and size: Synthesis, morphology, and nanoscale stiffness by AFM

Hubert Gojzewski*, Jagoda Obszarska, Agnes Harlay, Mark A. Hempenius, G. Julius Vancso (Corresponding Author)

*Corresponding author for this work

Research output: Contribution to journalArticleAcademicpeer-review

2 Citations (Scopus)
1 Downloads (Pure)

Abstract

Crosslinked poly(urea-siloxane) (PUS) copolymer microspheres with diameters ranging from 0.8 to 1.8 μm with diameter polydispersity indices between 1.15 and 1.60 were synthesized in one-step precipitation polymerization in water-acetone solvent mixtures at room temperature. The spheres were obtained using aminopropyl-terminated siloxanes, isophorone diisocyanate and a tetrafunctional isocyanate crosslinker, employing a systematically varied molar ratio. The length of the siloxanes was controlled to obtain spheres with pre-determined Young's modulus values. Phase separation between soft disiloxane/poly(dimethylsiloxane) segments and hard isophorone bisurea units was observed with an excellent spatial resolution of ∼5 nm using atomic force microscopy (AFM). AFM mapping of the Young's modulus was achieved utilizing the PeakForce Quantitative Nanomechanical Mapping (QNM) mode. This AFM method allowed us to also measure the values of elasticity moduli of individual microspheres, ranging from 200 to 900 MPa. The microspheres can be used as filler to fine-tune the properties of composite materials, particularly with regard to elasticity. The hydrophobicity was also varied as indicated by water contact angle values between 122° - 132°. These features open the possibility of preparing designer composites for a range of applications from coatings to the biomedical field.

Original languageEnglish
Pages (from-to)289-300
Number of pages12
JournalPolymer (United Kingdom)
Volume150
DOIs
Publication statusPublished - 15 Aug 2018

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Siloxanes
Microspheres
Urea
Atomic force microscopy
Stiffness
Elasticity
Elastic moduli
Isocyanates
Water
Composite materials
Polydispersity
Polydimethylsiloxane
Hydrophobicity
Acetone
Phase separation
Contact angle
Fillers
Copolymers
Polymerization
Coatings

Keywords

  • Atomic force microscopy
  • Copolymer
  • Heterogeneous polymer
  • PeakForce tapping
  • Poly(urea-siloxane)
  • Precipitation polymerization
  • Spheres
  • Structure-property relationships

Cite this

@article{212b8717d2394fa887767d91de7d6a71,
title = "Designer poly(urea-siloxane) microspheres with controlled modulus and size: Synthesis, morphology, and nanoscale stiffness by AFM",
abstract = "Crosslinked poly(urea-siloxane) (PUS) copolymer microspheres with diameters ranging from 0.8 to 1.8 μm with diameter polydispersity indices between 1.15 and 1.60 were synthesized in one-step precipitation polymerization in water-acetone solvent mixtures at room temperature. The spheres were obtained using aminopropyl-terminated siloxanes, isophorone diisocyanate and a tetrafunctional isocyanate crosslinker, employing a systematically varied molar ratio. The length of the siloxanes was controlled to obtain spheres with pre-determined Young's modulus values. Phase separation between soft disiloxane/poly(dimethylsiloxane) segments and hard isophorone bisurea units was observed with an excellent spatial resolution of ∼5 nm using atomic force microscopy (AFM). AFM mapping of the Young's modulus was achieved utilizing the PeakForce Quantitative Nanomechanical Mapping (QNM) mode. This AFM method allowed us to also measure the values of elasticity moduli of individual microspheres, ranging from 200 to 900 MPa. The microspheres can be used as filler to fine-tune the properties of composite materials, particularly with regard to elasticity. The hydrophobicity was also varied as indicated by water contact angle values between 122° - 132°. These features open the possibility of preparing designer composites for a range of applications from coatings to the biomedical field.",
keywords = "Atomic force microscopy, Copolymer, Heterogeneous polymer, PeakForce tapping, Poly(urea-siloxane), Precipitation polymerization, Spheres, Structure-property relationships",
author = "Hubert Gojzewski and Jagoda Obszarska and Agnes Harlay and Hempenius, {Mark A.} and Vancso, {G. Julius}",
year = "2018",
month = "8",
day = "15",
doi = "10.1016/j.polymer.2018.07.034",
language = "English",
volume = "150",
pages = "289--300",
journal = "Polymer",
issn = "0032-3861",
publisher = "Elsevier",

}

Designer poly(urea-siloxane) microspheres with controlled modulus and size : Synthesis, morphology, and nanoscale stiffness by AFM. / Gojzewski, Hubert; Obszarska, Jagoda; Harlay, Agnes; Hempenius, Mark A.; Vancso, G. Julius (Corresponding Author).

In: Polymer (United Kingdom), Vol. 150, 15.08.2018, p. 289-300.

Research output: Contribution to journalArticleAcademicpeer-review

TY - JOUR

T1 - Designer poly(urea-siloxane) microspheres with controlled modulus and size

T2 - Synthesis, morphology, and nanoscale stiffness by AFM

AU - Gojzewski, Hubert

AU - Obszarska, Jagoda

AU - Harlay, Agnes

AU - Hempenius, Mark A.

AU - Vancso, G. Julius

PY - 2018/8/15

Y1 - 2018/8/15

N2 - Crosslinked poly(urea-siloxane) (PUS) copolymer microspheres with diameters ranging from 0.8 to 1.8 μm with diameter polydispersity indices between 1.15 and 1.60 were synthesized in one-step precipitation polymerization in water-acetone solvent mixtures at room temperature. The spheres were obtained using aminopropyl-terminated siloxanes, isophorone diisocyanate and a tetrafunctional isocyanate crosslinker, employing a systematically varied molar ratio. The length of the siloxanes was controlled to obtain spheres with pre-determined Young's modulus values. Phase separation between soft disiloxane/poly(dimethylsiloxane) segments and hard isophorone bisurea units was observed with an excellent spatial resolution of ∼5 nm using atomic force microscopy (AFM). AFM mapping of the Young's modulus was achieved utilizing the PeakForce Quantitative Nanomechanical Mapping (QNM) mode. This AFM method allowed us to also measure the values of elasticity moduli of individual microspheres, ranging from 200 to 900 MPa. The microspheres can be used as filler to fine-tune the properties of composite materials, particularly with regard to elasticity. The hydrophobicity was also varied as indicated by water contact angle values between 122° - 132°. These features open the possibility of preparing designer composites for a range of applications from coatings to the biomedical field.

AB - Crosslinked poly(urea-siloxane) (PUS) copolymer microspheres with diameters ranging from 0.8 to 1.8 μm with diameter polydispersity indices between 1.15 and 1.60 were synthesized in one-step precipitation polymerization in water-acetone solvent mixtures at room temperature. The spheres were obtained using aminopropyl-terminated siloxanes, isophorone diisocyanate and a tetrafunctional isocyanate crosslinker, employing a systematically varied molar ratio. The length of the siloxanes was controlled to obtain spheres with pre-determined Young's modulus values. Phase separation between soft disiloxane/poly(dimethylsiloxane) segments and hard isophorone bisurea units was observed with an excellent spatial resolution of ∼5 nm using atomic force microscopy (AFM). AFM mapping of the Young's modulus was achieved utilizing the PeakForce Quantitative Nanomechanical Mapping (QNM) mode. This AFM method allowed us to also measure the values of elasticity moduli of individual microspheres, ranging from 200 to 900 MPa. The microspheres can be used as filler to fine-tune the properties of composite materials, particularly with regard to elasticity. The hydrophobicity was also varied as indicated by water contact angle values between 122° - 132°. These features open the possibility of preparing designer composites for a range of applications from coatings to the biomedical field.

KW - Atomic force microscopy

KW - Copolymer

KW - Heterogeneous polymer

KW - PeakForce tapping

KW - Poly(urea-siloxane)

KW - Precipitation polymerization

KW - Spheres

KW - Structure-property relationships

U2 - 10.1016/j.polymer.2018.07.034

DO - 10.1016/j.polymer.2018.07.034

M3 - Article

AN - SCOPUS:85053103578

VL - 150

SP - 289

EP - 300

JO - Polymer

JF - Polymer

SN - 0032-3861

ER -