An ultrahigh vacuum chamber for simultaneous Fourier transform infrared spectroscopy and microgravimetric measurements

Guorong Zhuang, Gary Chottiner, In Tae Bae, Euijin Hwang, Daniel Alberto Scherson

Research output: Contribution to journalArticle

4 Citations (Scopus)

Abstract

A small UHV chamber that fits in the sample compartment of a commercial Fourier transform infrared spectrometer (IBM-98, Brucker) has been designed and constructed to acquire reflection/absorption spectra of species adsorbed and/or condensed on metal films vapor deposited in situ on the surface of a quartz-crystal microbalance (QCM). The QCM is mounted on a variable-temperature Au-plated Cu block, which houses a second (reference) QCM, attached in turn to a liquid-He cold finger. The unique capabilities of this apparatus make it possible to correlate quantitatively various spectral characteristics, including peak widths and intensities, with the absolute mass of adsorbed and/or condensed material per unit area m, or coverage, over a wide range of m and temperatures. Results obtained using tetrahydrofuran (THF) condensed on freshly vapor deposited gold films have shown that the sensitivity of the instrument is sufficient to detect mTHF on the order of a single monolayer. Plots of the intensity of the most prominent THF peak at 1064 cm-1 as a function of mTHF were found to deviate significantly from linearity in the range 0.1<mTHF<2.8 μg/cm2. In addition, the relative intensities of the most prominent THF peaks for even the largest mTHF examined differed markedly from those of bulk-like THF, an effect that can be attributed to a preferential orientation of THF microcrystals with respect to the underlying substrate. In the case of coverages on the order of one monolayer, such spectral behavior may arise from specific adsorbate/substrate interactions, which can cause a lowering in the molecular symmetry and/or distortions in the structure of the adsorbate. Evidence in support of a Au-induced THF activation was obtained from independent temperature programmed desorption (TPD) measurements involving perdeuterated THF (TDF) performed in a separate UHV system. In particular, for exposures of about 1.5 L, the TPD spectra for the largest m/e features, i.e., 80, 48, and 30, revealed the presence of a peak centered at a higher temperature (∼180 K) than that found for much larger exposures (120 K).

Original languageEnglish
Pages (from-to)2494-2499
Number of pages6
JournalReview of Scientific Instruments
Volume65
Issue number8
DOIs
Publication statusPublished - 1994 Dec 1
Externally publishedYes

Fingerprint

Quartz crystal microbalances
Ultrahigh vacuum
vacuum chambers
tetrahydrofuran
ultrahigh vacuum
Fourier transform infrared spectroscopy
infrared spectroscopy
Adsorbates
Temperature programmed desorption
Monolayers
Vapors
quartz crystals
Microcrystals
microbalances
Infrared spectrometers
Substrates
Crystal orientation
Temperature
Absorption spectra
Fourier transforms

ASJC Scopus subject areas

  • Instrumentation

Cite this

An ultrahigh vacuum chamber for simultaneous Fourier transform infrared spectroscopy and microgravimetric measurements. / Zhuang, Guorong; Chottiner, Gary; Bae, In Tae; Hwang, Euijin; Scherson, Daniel Alberto.

In: Review of Scientific Instruments, Vol. 65, No. 8, 01.12.1994, p. 2494-2499.

Research output: Contribution to journalArticle

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