Nanoparticle metrology of silica colloids and super-resolution studies using the ADOTA fluorophore

Hazel L Stewart, Philip Yip, Martin Rosenberg, Thomas Just Sørensen, Bo W Laursen, Alex E Knight, David J S Birch

Research output: Contribution to journalArticle

4 Citations (Scopus)

Abstract

We describe how a new fluorescent dye, methyl ADOTA (N-methyl-azadioxatriangulenium tetrafluoroborate), is an improvement on dyes reported previously for measuring silica nanoparticle size in sols using the decay of fluorescence anisotropy. Me(thyl)-ADOTA possesses the unusual combination of having a red emission and a long fluorescence lifetime of ~ 20 ns, leaving it better-placed to reveal particle sizes at the upper end of the 1-10 nm measurement range. For stable LUDOX colloids, Me-ADOTA is shown to offer higher measurement precision in ≤ 1/30th of the measurement time required for dyes previously used. In measurement times of only ~ 20 mins nanoparticle radii for LUDOX SM-AS, AM and AS-40 of 4.6 ± 0.3 nm, 5.9 ± 0.2 nm and 11.1 ± 1.1 nm, are in good agreement with two of the manufacturer’s values of 3.5 nm, 6 nm and 11 nm respectively. Unlike the Si-ADOTA (N-(4-(triethoxysilylethyl)urea-phenyl-) ADOTA tetrafluoroborate) derivative containing a reactive trimetoxysilane group, Me-ADOTA is shown to not induce aggregation of colloidal silica. Measurements on nanoparticles growing in an acidic silica hydrogel at pH 0.94, prior to the gel time of ~ 50 hr, reveals an average nanoparticle size up to ~ 6.3 nm, significantly larger than the 4.5 nm reported previously. The difference is most certainly due to the longer fluorescence lifetime of Me-ADOTA (~ 20 ns) revealing the presence of larger particles. Studies of growing silica clusters in an alcogel of tetraethyl orthosilicate (TEOS) were able to resolve a monotonically increasing average radius of 1.42 ± 0.10 nm to 1.81 ± 0.14 nm over a period of 48 hr. We have also assessed a carboxylic acid derivative of ADOTA (N-(3-carboxypropylene)-ADOTA tetrafluoroborate - Acid-ADOTA) using dSTORM super-resolution microscopy. Although demonstrating high photochemical stability and blinking, its lower brightness and relative propensity to aggregate limits Acid-ADOTA’s use for dSTORM.
LanguageEnglish
Article number045007
Number of pages12
JournalMeasurement Science and Technology
Volume27
Issue number4
DOIs
Publication statusPublished - 14 Mar 2016

Fingerprint

Fluorophores
Super-resolution
Colloids
Metrology
Silica
metrology
Nanoparticles
colloids
silicon dioxide
nanoparticles
Dyes
dyes
Fluorescence
Fluorescence Lifetime
Time measurement
fluorescence
time measurement
Derivatives
blinking
tetraethyl orthosilicate

Keywords

  • fluorescence lifetime
  • super-resolution microscopy
  • dSTORM
  • ADOTA
  • silica sol-gel
  • nanoparticle metrology
  • fluorescence anisotropy

Cite this

Stewart, Hazel L ; Yip, Philip ; Rosenberg, Martin ; Sørensen, Thomas Just ; Laursen, Bo W ; Knight, Alex E ; Birch, David J S. / Nanoparticle metrology of silica colloids and super-resolution studies using the ADOTA fluorophore. In: Measurement Science and Technology. 2016 ; Vol. 27, No. 4.
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Nanoparticle metrology of silica colloids and super-resolution studies using the ADOTA fluorophore. / Stewart, Hazel L; Yip, Philip; Rosenberg, Martin; Sørensen, Thomas Just; Laursen, Bo W; Knight, Alex E; Birch, David J S.

In: Measurement Science and Technology, Vol. 27, No. 4, 045007, 14.03.2016.

Research output: Contribution to journalArticle

TY - JOUR

T1 - Nanoparticle metrology of silica colloids and super-resolution studies using the ADOTA fluorophore

AU - Stewart, Hazel L

AU - Yip, Philip

AU - Rosenberg, Martin

AU - Sørensen, Thomas Just

AU - Laursen, Bo W

AU - Knight, Alex E

AU - Birch, David J S

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AB - We describe how a new fluorescent dye, methyl ADOTA (N-methyl-azadioxatriangulenium tetrafluoroborate), is an improvement on dyes reported previously for measuring silica nanoparticle size in sols using the decay of fluorescence anisotropy. Me(thyl)-ADOTA possesses the unusual combination of having a red emission and a long fluorescence lifetime of ~ 20 ns, leaving it better-placed to reveal particle sizes at the upper end of the 1-10 nm measurement range. For stable LUDOX colloids, Me-ADOTA is shown to offer higher measurement precision in ≤ 1/30th of the measurement time required for dyes previously used. In measurement times of only ~ 20 mins nanoparticle radii for LUDOX SM-AS, AM and AS-40 of 4.6 ± 0.3 nm, 5.9 ± 0.2 nm and 11.1 ± 1.1 nm, are in good agreement with two of the manufacturer’s values of 3.5 nm, 6 nm and 11 nm respectively. Unlike the Si-ADOTA (N-(4-(triethoxysilylethyl)urea-phenyl-) ADOTA tetrafluoroborate) derivative containing a reactive trimetoxysilane group, Me-ADOTA is shown to not induce aggregation of colloidal silica. Measurements on nanoparticles growing in an acidic silica hydrogel at pH 0.94, prior to the gel time of ~ 50 hr, reveals an average nanoparticle size up to ~ 6.3 nm, significantly larger than the 4.5 nm reported previously. The difference is most certainly due to the longer fluorescence lifetime of Me-ADOTA (~ 20 ns) revealing the presence of larger particles. Studies of growing silica clusters in an alcogel of tetraethyl orthosilicate (TEOS) were able to resolve a monotonically increasing average radius of 1.42 ± 0.10 nm to 1.81 ± 0.14 nm over a period of 48 hr. We have also assessed a carboxylic acid derivative of ADOTA (N-(3-carboxypropylene)-ADOTA tetrafluoroborate - Acid-ADOTA) using dSTORM super-resolution microscopy. Although demonstrating high photochemical stability and blinking, its lower brightness and relative propensity to aggregate limits Acid-ADOTA’s use for dSTORM.

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KW - super-resolution microscopy

KW - dSTORM

KW - ADOTA

KW - silica sol-gel

KW - nanoparticle metrology

KW - fluorescence anisotropy

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