Detection of CO<sub>2</sub> and O<sub>2</sub> by iron loaded LTL zeolite films

doi:10.1007/s11705-017-1692-5

Front. Chem. Sci. Eng.

2018, Vol. 12

Issue (1) : 94-102 https://doi.org/10.1007/s11705-017-1692-5

RESEARCH ARTICLE

Detection of CO₂ and O₂ by iron loaded LTL zeolite films

Veselina Georgieva¹, Richard Retoux², Valerie Ruaux¹, Valentin Valtchev¹, Svetlana Mintova¹(

)

¹. Laboratoire Catalyse et Spectrochimie (LCS), ENSICAEN, CNRS, Normandy University, 14000 Caen, France
². Laboratoire de Cristallographie et Sciences des Matériaux (CRISMAT), ENSICAEN, CNRS, Normandy University, 14000 Caen, France

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Abstract

Detection of oxygen and carbon dioxide is important in the field of chemical and biosensors for atmosphere and biosystem monitoring and fermentation processes. The present study reports on the preparation of zeolite films doped with iron nanoparticles for detection of CO₂ and O₂ in gas phase. Pure nanosized LTL type zeolite with monomodal particle size distribution loaded with iron (Fe-LTL) was prepared under hydrothermal condition from colloidal precursor suspensions. The zeolite was loaded with iron to different levels by ion exchange. The Fe-LTL suspensions were used for preparation of thin films on silicon wafers via spin coating method. The reduction of the iron in the zeolite films was carried out under H₂ flow (50% H₂ in Ar) at 300 °C. The presence of iron nanoparticles is proved by in situ ultra-violet-visible spectroscopy. The properties of the films including surface roughness, thickness, porosity, and mechanical stability were studied. In addition, the loading and distribution of iron in the zeolite films were investigated. The Fe-LTL zeolite films were used to detect O₂ and CO₂ in a concentration dependent mode, followed by IR spectroscopy. The changes in the IR bands at 855 and 642 cm⁻¹ (Fe–O–H and Fe–O bending vibrations) and at 2363 and 2333 cm⁻¹ (CO₂ asymmetric stretching) corresponding to the presence of O₂ and CO₂, respectively, were evaluated. The response to O₂ and CO₂ was instant, which was attributed to great accessibility of the iron in the nanosized zeolite crystals. The saturation of the Fe-LTL films with CO₂ and O₂ at each concentration was reached within less than a minute. The Fe-LTL films detected both oxygen and carbon dioxide in contrast, to the pure LTL zeolite film.

Keywords zeolite films detection of CO₂ and O₂ adsorption

Corresponding Author(s): Svetlana Mintova

Just Accepted Date: 30 October 2017 Online First Date: 19 January 2018 Issue Date: 26 February 2018

Cite this article:

Veselina Georgieva,Richard Retoux,Valerie Ruaux, et al. Detection of CO₂ and O₂ by iron loaded LTL zeolite films[J]. Front. Chem. Sci. Eng., 2018, 12(1): 94-102.

URL:

https://academic.hep.com.cn/fcse/EN/10.1007/s11705-017-1692-5
https://academic.hep.com.cn/fcse/EN/Y2018/V12/I1/94

Fig.1 XRD patterns of nanosized (a) Fe-LTL zeolite samples and (b) pure LTL in the regions of 2q = 5°?80°

Tab.1 Chemical composition of pure LTL and Fe-LTL zeolite samples

Fig.2 Optical photographs of (a) pure LTL and (b) Fe-LTL zeolite suspensions (solid concentration of 5 wt-%)

Fig.3 (A) DLS and (B) zeta potential curves of (a) pure LTL and (b) Fe-LTL zeolite suspensions

Fig.4 Nitrogen adsorption-desorption isotherms of (a) pure LTL and (b) Fe-LTL zeolite samples

Tab.2 Results from the nitrogen sorption measurements for pure LTL and Fe-LTL zeolite samples

Fig.5 HRTEM images of (a, b) pure LTL and (c, d, e) Fe-LTL zeolite nanoparticles. Elemental composition of (f) Fe-LTL crystals (measured by EDX-HRTEM (carbon comes from the carbon film of the sample holder). Iron particles are pointed out by red arrows

Fig.6 UV-Vis spectra of the Fe-LTL zeolite sample: (a) as-prepared, (b) after reduction in 50 vol-% H₂ in Ar for 3 h at 300 °C, and after (c) oxidation in 100 vol-% O₂ in Ar at 25 °C for 12 h

Fig.7 SEM surface and side-view micrographs of (a, c) pure LTL and (b, d) Fe-LTL zeolite films

Fig.8 SEM photographs of (a, c) pure LTL and (b, d) Fe-LTL zeolites films after adhesive testing

Fig.9 FTIR spectra of CO₂ adsorbed on (A) pure LTL, (B) Fe-LTL zeolites films after outgassing under vacuum at 300 °C, and (C) CO₂ adsorption isotherms of LTL and Fe-LTL. CO₂ concentration increased in small doses as follow: (a) 0, (b) 7, (c) 20, (d) 70, (e) 100, (f) 150, (g) 200, (h) 250, (i) 300, (j) 350, (k) 400, (l) 450 mg?L^?¹

Fig.10 FTIR spectra of O₂ adsorbed on (A) pure LTL, (B) Fe-LTL zeolite films after outgassing under vacuum at 300 °C, and (C) O₂ adsorption isotherms of LTL and Fe-LTL. O₂ concentration increased in small doses as follow: (a) 0, (b) 10, (c) 60, (d) 120, (e) 200, (f) 300, (g) 400 mg?L^?¹. Insert in (B) enlargement of the peak at 863 cm^?¹ with an increase of the oxygen concentration

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