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

Hazel L. Stewart; Philip Yip; Martin Rosenberg; Thomas Just Sørensen; Bo Wegge Laursen; Alex E. Knight; David J. S.  Birch

doi:10.1088/0957-0233/27/4/045007

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

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

Department of Chemistry

5 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 min 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 h, 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 h. 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.

Original language	English
Article number	045007
Journal	Measurement Science and Technology
Volume	27
Number of pages	12
ISSN	0957-0233
DOIs	https://doi.org/10.1088/0957-0233/27/4/045007
Publication status	Published - 14 Mar 2016

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title = "Nanoparticle metrology of silica colloids and super-resolution studies using the ADOTA fluorophore",

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 min 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 h, 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 h. 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.",

author = "Stewart, {Hazel L.} and Philip Yip and Martin Rosenberg and S{\o}rensen, {Thomas Just} and Laursen, {Bo Wegge} and Knight, {Alex E.} and Birch, {David J. S.}",

year = "2016",

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doi = "10.1088/0957-0233/27/4/045007",

language = "English",

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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 Wegge

AU - Knight, Alex E.

AU - Birch, David J. S.

PY - 2016/3/14

Y1 - 2016/3/14

N2 - 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 min 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 h, 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 h. 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.

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 min 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 h, 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 h. 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.

U2 - 10.1088/0957-0233/27/4/045007

DO - 10.1088/0957-0233/27/4/045007

M3 - Journal article

SN - 0957-0233

VL - 27

JO - Measurement Science and Technology

JF - Measurement Science and Technology

M1 - 045007

ER -

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

Abstract

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