Determination of surface area and porosity of small, nanometer-thick films by quartz crystal microbalance measurement of gas adsorption

Yoshitaka Aoki, Mineo Hashizume, Shinya Onoue, Toyoki Kunitake

Research output: Contribution to journalArticle

3 Citations (Scopus)

Abstract

The Brunauer-Emmett-Teller (BET) surface area of 15 nm-thick films made of TiO2/polyelectrolyte bilayer was determined by quartz crystal microbalance (QCM) measurement of N2 and Ar adsorption isotherms at 77 K. The measurements were carried out using a home-built vacuum chamber that includes built-in 9 MHz QCM and cryostat units. As little as 1 ng of the adsorbed gas could be detected, and the BET surface area of a flat Au film (ca. 0.5 cm2) on an oscillator was determined within an experimental error of ±5%. The titania/polymer composite film gives N2 and Ar adsorption isotherms consisting of a less-pronounced type-I curve and a break at around p/p0) = 0.7. This behavior is ascribed to the presence of irregular micropores and 6 nm φ-mesopores in the composite film. An analysis of the isotherms shows that the porosity of the composite film is about 12%, which is much smaller than that of bulk titania gel powder. The greater density appears to be related to the reported superior properties (robustness and resistance to electrical breakdown) of the organic/inorganic multilayer film. We conclude that the QCM-based, high-precision measurement of gas adsorption is a powerful tool for investigation of the detailed morphology of nanometer-thick films.

Original languageEnglish
Pages (from-to)14578-14582
Number of pages5
JournalJournal of Physical Chemistry B
Volume112
Issue number46
DOIs
Publication statusPublished - Nov 20 2008
Externally publishedYes

Fingerprint

Quartz Crystal Microbalance Techniques
Gas adsorption
Quartz crystal microbalances
Porosity
Composite films
quartz crystals
Thick films
microbalances
Adsorption
thick films
Gases
porosity
Adsorption isotherms
adsorption
Titanium
gases
isotherms
Cryostats
Multilayer films
composite materials

All Science Journal Classification (ASJC) codes

  • Physical and Theoretical Chemistry
  • Surfaces, Coatings and Films
  • Materials Chemistry

Cite this

Determination of surface area and porosity of small, nanometer-thick films by quartz crystal microbalance measurement of gas adsorption. / Aoki, Yoshitaka; Hashizume, Mineo; Onoue, Shinya; Kunitake, Toyoki.

In: Journal of Physical Chemistry B, Vol. 112, No. 46, 20.11.2008, p. 14578-14582.

Research output: Contribution to journalArticle

Aoki, Yoshitaka ; Hashizume, Mineo ; Onoue, Shinya ; Kunitake, Toyoki. / Determination of surface area and porosity of small, nanometer-thick films by quartz crystal microbalance measurement of gas adsorption. In: Journal of Physical Chemistry B. 2008 ; Vol. 112, No. 46. pp. 14578-14582.
@article{7d7df9f6f51946308cce2bb69e6336d2,
title = "Determination of surface area and porosity of small, nanometer-thick films by quartz crystal microbalance measurement of gas adsorption",
abstract = "The Brunauer-Emmett-Teller (BET) surface area of 15 nm-thick films made of TiO2/polyelectrolyte bilayer was determined by quartz crystal microbalance (QCM) measurement of N2 and Ar adsorption isotherms at 77 K. The measurements were carried out using a home-built vacuum chamber that includes built-in 9 MHz QCM and cryostat units. As little as 1 ng of the adsorbed gas could be detected, and the BET surface area of a flat Au film (ca. 0.5 cm2) on an oscillator was determined within an experimental error of ±5{\%}. The titania/polymer composite film gives N2 and Ar adsorption isotherms consisting of a less-pronounced type-I curve and a break at around p/p0) = 0.7. This behavior is ascribed to the presence of irregular micropores and 6 nm φ-mesopores in the composite film. An analysis of the isotherms shows that the porosity of the composite film is about 12{\%}, which is much smaller than that of bulk titania gel powder. The greater density appears to be related to the reported superior properties (robustness and resistance to electrical breakdown) of the organic/inorganic multilayer film. We conclude that the QCM-based, high-precision measurement of gas adsorption is a powerful tool for investigation of the detailed morphology of nanometer-thick films.",
author = "Yoshitaka Aoki and Mineo Hashizume and Shinya Onoue and Toyoki Kunitake",
year = "2008",
month = "11",
day = "20",
doi = "10.1021/jp801919h",
language = "English",
volume = "112",
pages = "14578--14582",
journal = "Journal of Physical Chemistry B Materials",
issn = "1520-6106",
publisher = "American Chemical Society",
number = "46",

}

TY - JOUR

T1 - Determination of surface area and porosity of small, nanometer-thick films by quartz crystal microbalance measurement of gas adsorption

AU - Aoki, Yoshitaka

AU - Hashizume, Mineo

AU - Onoue, Shinya

AU - Kunitake, Toyoki

PY - 2008/11/20

Y1 - 2008/11/20

N2 - The Brunauer-Emmett-Teller (BET) surface area of 15 nm-thick films made of TiO2/polyelectrolyte bilayer was determined by quartz crystal microbalance (QCM) measurement of N2 and Ar adsorption isotherms at 77 K. The measurements were carried out using a home-built vacuum chamber that includes built-in 9 MHz QCM and cryostat units. As little as 1 ng of the adsorbed gas could be detected, and the BET surface area of a flat Au film (ca. 0.5 cm2) on an oscillator was determined within an experimental error of ±5%. The titania/polymer composite film gives N2 and Ar adsorption isotherms consisting of a less-pronounced type-I curve and a break at around p/p0) = 0.7. This behavior is ascribed to the presence of irregular micropores and 6 nm φ-mesopores in the composite film. An analysis of the isotherms shows that the porosity of the composite film is about 12%, which is much smaller than that of bulk titania gel powder. The greater density appears to be related to the reported superior properties (robustness and resistance to electrical breakdown) of the organic/inorganic multilayer film. We conclude that the QCM-based, high-precision measurement of gas adsorption is a powerful tool for investigation of the detailed morphology of nanometer-thick films.

AB - The Brunauer-Emmett-Teller (BET) surface area of 15 nm-thick films made of TiO2/polyelectrolyte bilayer was determined by quartz crystal microbalance (QCM) measurement of N2 and Ar adsorption isotherms at 77 K. The measurements were carried out using a home-built vacuum chamber that includes built-in 9 MHz QCM and cryostat units. As little as 1 ng of the adsorbed gas could be detected, and the BET surface area of a flat Au film (ca. 0.5 cm2) on an oscillator was determined within an experimental error of ±5%. The titania/polymer composite film gives N2 and Ar adsorption isotherms consisting of a less-pronounced type-I curve and a break at around p/p0) = 0.7. This behavior is ascribed to the presence of irregular micropores and 6 nm φ-mesopores in the composite film. An analysis of the isotherms shows that the porosity of the composite film is about 12%, which is much smaller than that of bulk titania gel powder. The greater density appears to be related to the reported superior properties (robustness and resistance to electrical breakdown) of the organic/inorganic multilayer film. We conclude that the QCM-based, high-precision measurement of gas adsorption is a powerful tool for investigation of the detailed morphology of nanometer-thick films.

UR - http://www.scopus.com/inward/record.url?scp=57249087436&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=57249087436&partnerID=8YFLogxK

U2 - 10.1021/jp801919h

DO - 10.1021/jp801919h

M3 - Article

C2 - 18590322

AN - SCOPUS:57249087436

VL - 112

SP - 14578

EP - 14582

JO - Journal of Physical Chemistry B Materials

JF - Journal of Physical Chemistry B Materials

SN - 1520-6106

IS - 46

ER -