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Journal of Applied Physics

Method for characterizing self-assembled monolayers as antirelaxation wall coatings for alkali vapor cells

Youngwoo Yi, H. G. Robinson, Svenja A. Knappe, Joseph E. Maclennan, C. D. Jones, Chenhui Zhu, Noel A. Clark, John E. Kitching

Published Jul 15, 2008• 75 citations
Publisher

Abstract

We describe a method for characterizing self-assembled monolayers (SAMs) in terms of their performance as antirelaxation wall coatings for alkali atom vapor cells. A combination of initial surface analysis and subsequent laser spectroscopy is used to provide insight into the quality of the coating, as well as its performance under the exposure to alkalis as it occurs, for example, when used in applications such as atomic magnetometers or clocks. Fused silica plates coated with octadecyltrichlorosilane SAMs were used to make cubic R87b gas cells. The surface was characterized by x-ray diffraction, contact angle measurements, and atomic force microscopy. Measurements of hyperfine resonance linewidths and frequency shifts show that the rubidium vapor atoms collide up to 40 times with the walls of the cells before their coherence relaxes and their adsorption energy is around 0.065 eV. Chemical analysis of the cell indicates some weak reactions between the coating and the rubidium atoms.

DOI
10.1063/1.2958329

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Applied Physics Letters•Jan 26, 2009•26 citations
We describe a method for characterizing self-assembled monolayers (SAMs) in terms of their performance as antirelaxation wall coatings for alkali atom vapor cells. A combination of initial surface analysis and subsequent laser spectroscopy is used to provide insight into the quality of the coating, as well as its performance under the exposure to alkalis as it occurs, for example, when used in applications such as atomic magnetometers or clocks. Fused silica plates coated with octadecyltrichlorosilane SAMs were used to make cubic R87b gas cells. The surface was characterized by x-ray diffraction, contact angle measurements, and atomic force microscopy. Measurements of hyperfine resonance linewidths and frequency shifts show that the rubidium vapor atoms collide up to 40 times with the walls of the cells before their coherence relaxes and their adsorption energy is around 0.065 eV. Chemical analysis of the cell indicates some weak reactions between the coating and the rubidium atoms.
Antirelaxation surface coatings allow long spin relaxation times in alkali-metal cells without buffer gas, enabling faster diffusion of the alkali atoms throughout the cell and giving larger signals due to narrower optical linewidths. Effective coatings were previously unavailable for operation at temperatures above 80 °C. We demonstrate that octadecyltrichlorosilane (OTS) can allow potassium or rubidium atoms to experience hundreds of collisions with the cell surface before depolarizing, and that an OTS coating remains effective up to about 170 °C for both potassium and rubidium. We consider the experimental concerns of operating without buffer gas and with minimal quenching gas at high vapor density, studying the stricter need for effective quenching of excited atoms and deriving the optical rotation signal shape for atoms with resolved hyperfine structure in the spin-temperature regime. As an example of a high-temperature application of antirelaxation coated alkali vapor cells, we operate a spin-exchange relaxation-free atomic magnetometer with sensitivity of 6 fT/Hz and magnetic linewidth as narrow as 2 Hz.
An alkene-based antirelaxation coating for alkali-metal vapor cells exhibiting Zeeman relaxation times up to 77 s was recently identified by Balabas et al. The long relaxation times, two orders of magnitude longer than in paraffin- (alkane-) coated cells, motivate revisiting the question of what the mechanism is underlying wall-collision-induced relaxation and renew interest in applications of alkali-metal vapor cells to secondary frequency standards. We measure the width and frequency shift of the ground-state hyperfine $m{}_{F}=0\ensuremath{\rightarrow}m{}_{F}^{\ensuremath{'}}=0$ transition (clock resonance) in vapor cells with 85{}^{85}85Rb and 87{}^{87}87Rb atoms, with an alkene antirelaxation coating. We find that the frequency shift is slightly larger than for paraffin-coated cells and that the Zeeman linewidth scales linearly with the hyperfine frequency shift.
We present a microfabricated alkali vapor cell equipped with an anti-relaxation wall coating. The anti-relaxation coating used is octadecyltrichlorosilane and the cell was sealed by thin-film indium-bonding at a low temperature of 140 °C. The cell body is made of silicon and Pyrex and features a double-chamber design. Depolarizing properties due to liquid Rb droplets are avoided by confining the Rb droplets to one chamber only. Optical and microwave spectroscopy performed on this wall-coated cell are used to evaluate the cell's relaxation properties and a potential gas contamination. Double-resonance signals obtained from the cell show an intrinsic linewidth that is significantly lower than the linewidth that would be expected in case the cell had no wall coating but only contained a buffer-gas contamination on the level measured by optical spectroscopy. Combined with further experimental evidence this proves the presence of a working anti-relaxation wall coating in the cell. Such cells are of interest for applications in miniature atomic clocks, magnetometers, and other quantum sensors.
Many technologies based on cells containing alkali-metal atomic vapor benefit from the use of antirelaxation surface coatings in order to preserve atomic spin polarization. In particular, paraffin has been used for this purpose for several decades and has been demonstrated to allow an atom to experience up to 10 000 collisions with the walls of its container without depolarizing, but the details of its operation remain poorly understood. We apply modern surface and bulk techniques to the study of paraffin coatings in order to characterize the properties that enable the effective preservation of alkali spin polarization. These methods include Fourier transform infrared spectroscopy, differential scanning calorimetry, atomic force microscopy, near-edge x-ray absorption fine structure spectroscopy, and x-ray photoelectron spectroscopy. We also compare the light-induced atomic desorption yields of several different paraffin materials. Experimental results include the determination that crystallinity of the coating material is unnecessary, and the detection of C[Double Bond]C double bonds present within a particular class of effective paraffin coatings. Further study should lead to the development of more robust paraffin antirelaxation coatings, as well as the design and synthesis of new classes of coating materials.
I studied the effect of wall collisions on the electron paramagnetic resonance (EPR) of gas phase alkali metal atoms (87Rb). Two types of walls were studied: antirelaxation-coated walls and RbH-coated walls. I measured the dwell times of spin polarized Rb atoms on the two most common antirelaxation coatings, octadecyltrichlorosilane (OTS)- and paraffin. I found that at a cell temperature of 72 C the dwell times for OTS- and paraffin-coated walls are 0.9 ± 0.1 μs and 1.8 ± 0.2 μs, respectively. The implication of these dwell times, which are much longer than what was previously reported in the literature, is discussed in connection with the relaxing property of these coatings. In cells coated with RbH salt I made the first observation of the EPR frequency shift of the gas phase 87Rb atoms. Due to collisions with the RbH salt, which was nuclear spin polarized by spin exchange with optically pumped Rb vapor. The measured EPR frequency shifts are of the order of several hundred Hz in a millimeter-sized cell. By measuring the dependence of the EPR frequency shifts on cell length and by comparing the EPR frequency shifts in RbH-coated cells with those in OTS-coated cells, I provided convincing evidence that the observed EPR frequency shifts are due to collisions with RbH-coated walls, and not due to gas phase processes. The EPR frequency shift is due to the Fermi contact interaction between the s-electron of the adsorbed 87Rb atom and the polarized nucleus on the salt surface. The measured EPR frequency shifts allowed me to calculate the ensemble-averaged phase shift experienced by the Rb atom while adsorbed on the walls. Under our experimental condition this is about 70 mrad. My experiment opens up the possibility of studying surface NMR using gas phase EPR. The phase shift is proportional to the surface nuclear polarization, thus provides an interesting method for measuring the surface nuclear polarization using gas phase EPR. My observation will alert the high precision miniature atomic magnetometry community that collisions with cell walls may cause a systematic error and line broadening in the magnetic resonance frequency.
Surface relaxation rates differ for spin-polarized alkali atoms interacting with monolayer or bilayer octadecyltrichlorosilane (OTS) coatings. The morphology and composition of Rb vapor-exposed films of OTS have been studied with atomic force microscopy (AFM) and x-ray photoelectron spectroscopy (XPS). On OTS monolayers, numerous small (<500 nm wide) Rb containing islands nucleate at the boundaries of the ∼1–2 μm wide organic domains. On OTS bilayers, singular large (∼3 μm wide) Rb containing islands were found. Alkali island formation mediated by surface structure could affect the antirelaxation behavior of organic coatings used in atomic magnetometer cells.