Publication detail

Controlling the surface silanol density in capillary columns and planar silicon via the self-limiting, gas-phase deposition of tris(dimethylamino) methylsilane, and quantification of surface silanols after silanization by low energy ion scattering

Moeini, B. Pinder, JW. Avval, TG. Jacobsen, C. Brongersma, HH. Prusa, S. Bábik, P. Vanicková, E. Argyle, MD. Strohmeier, BR. Jones, B. Shollenberger, D. Bell, DS. Linford, MR.

Original Title

Controlling the surface silanol density in capillary columns and planar silicon via the self-limiting, gas-phase deposition of tris(dimethylamino) methylsilane, and quantification of surface silanols after silanization by low energy ion scattering

Type

journal article in Web of Science

Language

English

Original Abstract

Surface silanols (Si-OH) play a vital role on fused silica surfaces in chromatography. Here, we used an atmospheric-pressure, gas-phase reactor to modify the inner surface of a gas chromatography, fused silica capillary column (0.53 mm ID) with a small, reactive silane (tris(dimethylamino)methylsilane, TDMAMS). The deposition of TDMAMS on planar witness samples around the capillary was confirmed with X-ray photoelectron spectroscopy (XPS), ex situ spectroscopic ellipsometry (SE), and wetting. The number of surface silanols on unmodified and TDMAMS-modified native oxide-terminated silicon were quantified by tagging with dime-thylzinc (DMZ) via atomic layer deposition (ALD) and counting the resulting zinc atoms with high sensitivity-low energy ion scattering (HS-LEIS). A bare, clean native oxide - terminated silicon wafer has 3.66 OH/nm2, which agrees with density functional theory (DFT) calculations from the literature. After TDMAMS modification of native oxide-terminated silicon, the number of surface silanols decreases by a factor of ca. 10 (to 0.31 OH/nm2). Intermediate surface testing (IST) was used to characterize the surface activities of functionalized capillaries. It suggested a significant deactivation/passivation of the capillary with some surface silanols remaining; the modified capillary shows significant deactivation compared to the native/unmodified fused silica tubing. We believe that this methodology for determining the number of residual silanols on silanized fused silica will be enabling for chromatography.

Keywords

Capillary column; Fused silica; Silane; Surface silanol; Low energy ion scattering; Tag-and-Count; Dimethylzinc; Atomic layer deposition

Authors

Moeini, B.; Pinder, JW.; Avval, TG.; Jacobsen, C.; Brongersma, HH.; Prusa, S.; Bábik, P.; Vanicková, E.; Argyle, MD.; Strohmeier, BR.; Jones, B.; Shollenberger, D.; Bell, DS.; Linford, MR.

Released

27. 9. 2023

Publisher

ELSEVIER

Location

AMSTERDAM

ISBN

1873-3778

Periodical

JOURNAL OF CHROMATOGRAPHY A

Year of study

1707

Number

464248

State

Kingdom of the Netherlands

Pages count

9

URL

https://www.sciencedirect.com/science/article/pii/S0021967323004739?via%3Dihub

BibTex

@article{BUT187337,
  author="Moeini, B. and Pinder, JW. and Avval, TG. and Jacobsen, C. and Brongersma, HH. and Prusa, S. and Bábik, P. and Vanicková, E. and Argyle, MD. and Strohmeier, BR. and Jones, B. and Shollenberger, D. and Bell, DS. and Linford, MR.",
  title="Controlling the surface silanol density in capillary columns and planar silicon via the self-limiting, gas-phase deposition of tris(dimethylamino) methylsilane, and quantification of surface silanols after silanization by low energy ion scattering",
  journal="JOURNAL OF CHROMATOGRAPHY A",
  year="2023",
  volume="1707",
  number="464248",
  pages="9",
  doi="10.1016/j.chroma.2023.464248",
  issn="1873-3778",
  url="https://www.sciencedirect.com/science/article/pii/S0021967323004739?via%3Dihub"
}