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
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.
. [J]. Frontiers of Chemical Science and Engineering, 2018, 12(1): 94-102.
Veselina Georgieva, Richard Retoux, Valerie Ruaux, Valentin Valtchev, Svetlana Mintova. Detection of CO2 and O2 by iron loaded LTL zeolite films. Front. Chem. Sci. Eng., 2018, 12(1): 94-102.
Diamond D. Principles of chemical and biological sensors. Michigan: Wiley, 1998, 220–290
2
Bein T. Synthesis and applications of molecular sieve layers and membranes. Chemistry of Materials, 1996, 8(8): 1636–1653 https://doi.org/10.1021/cm960148a
3
Mintova S, Mo S, Bein T. Humidity sensing with ultrathin LTA-type molecular sieve films grown on piezoelectric devices. Chemistry of Materials, 2001, 13(3): 901–905 https://doi.org/10.1021/cm000671w
4
Yang P, Lau C, Liang J Y, Lu J Z, Liu X. Zeolite-based cataluminescence sensor for the selective detection of acetaldehyde. Luminescence, 2007, 22(5): 473–479 https://doi.org/10.1002/bio.987
5
Mintova S, Jaber M, Valtchev V. Nanosized microporous crystals: Emerging applications. Chemical Society Reviews, 2015, 44(20): 7207–7233 https://doi.org/10.1039/C5CS00210A
6
Bein T, Mintova S. Zeolites and ordered mesoporous materials: Progress and prospects. Studies in Surface Science and Catalysis, 2005, 157: 263–288 https://doi.org/10.1016/S0167-2991(05)80015-1
Leite E, Babeva T, Ng E P, Toal V, Mintova S, Naydenova I. Optical properties of photopolymer layers doped with aluminophosphate nanocrystals. Journal of Physical Chemistry C, 2010, 114(39): 16767–16775 https://doi.org/10.1021/jp1060073
9
Valtchev V, Tosheva L. Porous nanosized particles: Preparation, properties, and applications. Chemical Reviews, 2013, 113(8): 6734–6760 https://doi.org/10.1021/cr300439k
10
Yasuda K E, Visser J E, Bein T. Molecular sieve catalysts on microcalorimeter chips for selective chemical sensing. Microporous and Mesoporous Materials, 2009, 119(1-3): 356–359 https://doi.org/10.1016/j.micromeso.2008.11.009
11
Xu X, Wang J, Long Y. Zeolite-based materials for gas sensors. Sensors (Basel), 2006, 6(12): 1751–1764 https://doi.org/10.3390/s6121751
12
Lakiss L, Kecht J, De Waele V, Mintova S. Copper-containing nanoporous films. Superlattices and Microstructures, 2008, 44(4-5): 617–625 https://doi.org/10.1016/j.spmi.2007.10.009
13
Thomas S, Bazin P, Lakiss L, De Waele V, Mintova S. In situ infrared molecular detection using palladium-containing zeolite films. Langmuir, 2011, 27(23): 14689–14695 https://doi.org/10.1021/la203075m
14
Huang H, Zhou J, Chen S, Zeng L, Huang Y. A highly sensitive QCM sensor coated with Ag+-ZSM-5 film for medical diagnosis. Sensors and Actuators. B, Chemical, 2004, 101(3): 316–321 https://doi.org/10.1016/j.snb.2004.04.001
15
Dubbe A. The effect of platinum clusters in the zeolite micropores of a zeolite-based potentiometric hydrocarbon gas sensor. Sensors and Actuators. B, Chemical, 2009, 137(1): 205–208 https://doi.org/10.1016/j.snb.2008.11.039
16
Wales D J, Grand J, Ting V P, Burke R D, Edler K J, Bowen C R, Mintova S, Burrows A D. Gas sensing using porous materials for automotive applications. Chemical Society Reviews, 2015, 44(13): 4290–4321 https://doi.org/10.1039/C5CS00040H
17
Fine G F, Cavanagh L M, Afonja A, Binions R. Metal oxide semi-conductor gas sensors in environmental monitoring. Sensors (Basel), 2010, 10(6): 5469–5502 https://doi.org/10.3390/s100605469
18
Mohan N, Cindrella L. Mater. Direct synthesis of Fe-ZSM-5 zeolite and its prospects as efficient electrode material in methanol fuel cell. Materials Science in Semiconductor Processing, 2015, 40: 361–368 https://doi.org/10.1016/j.mssp.2015.06.087
19
Yue Y, Liu H, Yuan P, Yu C, Bao X. One-pot synthesis of hierarchical FeZSM-5 zeolites from natural aluminosilicates for selective catalytic reduction of NO by NH3. Scientific Reports, 2015, 5(9270): 1–10
20
Luo L, Dai C, Zhang A, Wang J, Liu M, Song C, Guo X. Facile synthesis of zeolite-encapsulated iron oxide nanoparticles as superior catalysts for phenol oxidation. RSC Advances, 2015, 5(37): 29509–29512 https://doi.org/10.1039/C5RA02194D
21
Bouazizi N, Ouargli R, Nousir S, Slama R B, Azzouz A. Properties of SBA-15 modified by iron nanoparticles as potential hydrogen adsorbents and sensors. Journal of Physics and Chemistry of Solids, 2015, 77: 172–177 https://doi.org/10.1016/j.jpcs.2014.10.011
22
Georgieva V, Anfray C, Retoux R, Valtchev V, Valable S, Mintova S. Iron loaded EMT nanosized zeolite with high affinity towards CO2 and NO. Microporous and Mesoporous Materials, 2016, 232: 256–263 https://doi.org/10.1016/j.micromeso.2016.06.015
23
Suri K, Annapoorni S, Sarkar A K, Tandon R P. Gas and humidity sensors based on iron oxide-polypyrrole nanocomposites. Sensors and Actuators. B, Chemical, 2002, 81(2-3): 277–282 https://doi.org/10.1016/S0925-4005(01)00966-2
24
Mcdonagh C M, Shields M, Mcevoy K, Maccraith B D, Gouin J F. Optical sol-gel-based dissolved oxygen sensor: Progress towards a commercial instrument. Journal of Sol-Gel Science and Technology, 1998, 13(1-3): 207–211 https://doi.org/10.1023/A:1008608901645
25
Ishiji T, Chipman D W, Takahashi T, Takahashi K. Amperometric sensor for monitoring of dissolved carbon dioxide in seawater. Sensors and Actuators. B, Chemical, 2001, 76(1-3): 265–269 https://doi.org/10.1016/S0925-4005(01)00580-9
26
Guéguen C, Tortell P D. High-resolution measurement of southern ocean CO2 and O2/Ar by membrane inlet mass spectrometry. Marine Chemistry, 2008, 108(3-4): 184–194 https://doi.org/10.1016/j.marchem.2007.11.007
27
Higgins C, Wencel D, Burke C S, MacCraith B D, McDonagh C. Novel hybrid optical sensor materials for in-breath O(2) analysis. Analyst (London), 2008, 133(2): 241–247 https://doi.org/10.1039/B716197B
28
Hoelper B M, Alessandri B, Heimann A, Behr R, Kempski O. Brain oxygen monitoring: In-vitro accuracy, long-term drift and response-time of Licox- and Neurotrend sensors. Acta Neurochirurgica, 2005, 147(7): 767–774 https://doi.org/10.1007/s00701-005-0512-8
29
Baldini F, Falai A, De Gaudio R, Landi D, Lueger A, Mencaglia A, Scherr D, Trettnak W. Continuous monitoring of gastric carbon dioxide with optical fibres. Sensors and Actuators. B, Chemical, 2003, 90(1-3): 132–138 https://doi.org/10.1016/S0925-4005(03)00042-X
30
Čajlaković M, Bizzarri A, Ribitsch V. Luminescence lifetime-based carbon dioxide optical sensor for clinical applications. Analytica Chimica Acta, 2006, 573-574: 57–64 https://doi.org/10.1016/j.aca.2006.05.085
31
Wolfbeis O S, Klimant I, Werner T, Huber C, Kosch U, Krause C, Neurauter G, Dürkop A. Set of luminescence decay time based chemical sensors for clinical applications. Sensors and Actuators. B, Chemical, 1998, 51(1-3): 17–24 https://doi.org/10.1016/S0925-4005(98)00181-6
32
Mills A. Oxygen indicators and intelligent inks for packaging food. Chemical Society Reviews, 2005, 34(12): 1003–1011 https://doi.org/10.1039/b503997p
33
Chaix E, Guillaume C, Guillard V. Oxygen and carbon dioxide solubility and diffusivity in solid food matrices: A review of past and current knowledge. Comprehensive Reviews in Food Science and Food Safety, 2014, 13(3): 261–286 https://doi.org/10.1111/1541-4337.12058
34
Ge X, Hanson M, Shen H, Kostov Y, Brorson K, Frey D D, Moreira A R, Rao G. Validation of an optical sensor-based high-throughput bioreactor system for mammalian cell culture. Journal of Biotechnology, 2006, 122(3): 293–306 https://doi.org/10.1016/j.jbiotec.2005.12.009
35
Ge X, Kostov Y, Rao G. Low-cost noninvasive optical CO2 sensing system for fermentation and cell culture. Biotechnology and Bioengineering, 2005, 89(3): 329–334 https://doi.org/10.1002/bit.20337
36
Mulrooney J, Clifford J, Fitzpatrick C, Lewis E. Detection of carbon dioxide emissions from a diesel engine using a mid-infrared optical fibre based sensor. Sensors and Actuators. A, Physical, 2007, 136(1): 104–110 https://doi.org/10.1016/j.sna.2006.11.016
37
Litzelman S J, Rothschild A, Tuller H L. The electrical properties and stability of SrTi0.65Fe0.35O3-δ thin films for automotive oxygen sensor applications. Sensors and Actuators. B, Chemical, 2005, 108(1-2): 231–237 https://doi.org/10.1016/j.snb.2004.10.040
38
Souici A, Wong K L, De Waele V, Marignier J L, Metzger T H, Keghouche N, Mintova S, Mostafavi M. Capturing the formation of sub-nanometer sized CdS clusters in LTL zeolite. Journal of Physical Chemistry C, 2014, 118(12): 6324–6334 https://doi.org/10.1021/jp500185m
39
Hölzl M, Mintova S, Bein T. Colloidal LTL zeolite synthesized under microwave irradiation. Studies in Surface Science and Catalysis, 2005, 158(5): 11–18 https://doi.org/10.1016/S0167-2991(05)80316-7
40
Lakiss L, Yordanov I, Majano G, Metzger T, Mintova S. Effect of stabilizing binder and dispersion media on spin-on zeolite thin films. Thin Solid Films, 2010, 518(8): 2241–2246 https://doi.org/10.1016/j.tsf.2009.07.179
41
Lowell S. Characterization of Porous Solids and Powders: Surface Area, Pore Size and Density. Netherlands: Springer, 2004, 58–81
42
Sing K S W. Reporting physisorption data for gas/solid systems with special reference to the determination of surface area and porosity. Pure and Applied Chemistry, 1985, 57(4): 603–619 https://doi.org/10.1351/pac198557040603
43
Das D, Ravichandran G, Chakrabarty D K, Piramanayagam S N, Shringi S N. Selective synthesis of light alkenes from carbon monoxide and hydrogen on silicalite supported iron-manganese catalysts. Applied Catalysis A, General, 1993, 107(1): 73–81 https://doi.org/10.1016/0926-860X(93)85116-7
44
Guo L, Huang Q, Li X, Yang S. Iron nanoparticles: Synthesis and applications in surface enhanced Raman scattering and electrocatalysis. Physical Chemistry Chemical Physics, 2001, 3(9): 1661–1665 https://doi.org/10.1039/b009951l
45
Bordiga S, Buzzoni R, Geobaldo F, Lamberti C, Giamello E, Zecchina A, Leofanti G, Petrini G, Tozzola G, Vlaic G. Structure and reactivity of framework and extraframework iron in Fe-silicalite as investigated by spectroscopic and physicochemical methods. Journal of Catalysis, 1996, 158(2): 486–501 https://doi.org/10.1006/jcat.1996.0048
46
Pérez-Ramírez J, Groen J C, Brückner A, Kumar M S, Bentrup U, Debbagh M N, Villaescusa L A. Evolution of isomorphously substituted iron zeolites during activation: Comparison of Fe-beta and Fe-ZSM-5. Journal of Catalysis, 2005, 232(2): 318–334 https://doi.org/10.1016/j.jcat.2005.03.018
Andrews L, Chertihin G V, Citra A, Neurock M. Reactions of laser-ablated iron atoms with N2O, NO, and O2 in condensing nitrogen. Infrared spectra and density functional calculations of ternary iron nitride oxide molecules. Journal of Physical Chemistry, 1996, 100(27): 11235–11241 https://doi.org/10.1021/jp960674p
50
Reiff W M, Baker W A, Erickson N E. Binuclear, oxygen-bridged complexes of iron(III). New iron (III)-2,2′,2"-terpyridine complexes. Journal of the American Chemical Society, 1968, 90(18): 4794–4800 https://doi.org/10.1021/ja01020a008
51
Dalla Betta R A, Garten R L, Boudart M. Infrared examination of the reversible oxidation of ferrous ions in Y zeolite. Journal of Catalysis, 1976, 41(1): 40–45 https://doi.org/10.1016/0021-9517(76)90198-6
