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The multisensor array Based on Grown-On-Chip Zinc Oxide Nanorod Network for Selective Discrimination of Alcohol Vapors at Sub-ppm Range

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SENSORS 2019年第19期19卷 4265-4265页

作者： Bobkov, Anton Varezhnikov, Alexey Plugin, Ilya Fedorov, Fedor S. Trouillet, Vanessa Geckle, Udo Sommer, Martin Goffman, Vladimir Moshnikov, Vyacheslav Sysoev, Victor St Petersburg Electrotech Univ LETI Dept Micro & Nanoelect St Petersburg 197022 Russia Yuri Gagarin State Tech Univ Saratov Physicotech Inst 77 Polytech Skaya Str Saratov 410054 Russia Skolkovo Innovat Ctr Skolkovo Inst Sci & Technol 3 Nobel Str Moscow 121205 Russia Karlsruhe Inst Technol Inst Appl Mat Hermann von Helmholtz Pl 1 D-76344 Eggenstein Leopoldshafen Germany Karlsruhe Inst Technol Karlsruhe Nano Micro Facil Hermann von Helmholtz Pl 1 D-76344 Eggenstein Leopoldshafen Germany Karlsruhe Inst Technol Inst Microstruct Technol Hermann von Helmholtz Pl 1 D-76344 Eggenstein Leopoldshafen Germany

We discuss the fabrication of gas-analytical multisensor arrays based on ZnO nanorods grown via a hydrothermal route directly on a multielectrode chip. The protocol to deposit the nanorods over the chip includes the primary formation of ZnO nano-clusters over the surface and secondly the oxide hydrothermal growth in a solution that facilitates the appearance of ZnO nanorods in the high aspect ratio which comprise a network. We have tested the proof-of-concept prototype of the ZnO nanorod network-based chip heated up to 400 degrees C versus three alcohol vapors, ethanol, isopropanol and butanol, at approx. 0.2-5 ppm concentrations when mixed with dry air. The results indicate that the developed chip is highly sensitive to these analytes with a detection limit down to the sub-ppm range. Due to the pristine differences in ZnO nanorod network density the chip yields a vector signal which enables the discrimination of various alcohols at a reasonable degree via processing by linear discriminant analysis even at a sub-ppm concentration range suitable for practical applications.

关键词： zinc oxide nanorod gas sensor multisensor array selectivity sensitivity ethanol isopropanol butanol

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The Potentiodynamic Bottom-up Growth of the Tin Oxide Nanostructured Layer for Gas-Analytical multisensor array Chips

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SENSORS 2017年第8期17卷 1908-1908页

作者： Fedorov, Fedor S. Podgainov, Dmitry Varezhnikov, Alexey Lashkov, Andrey Gorshenkov, Michail Burmistrov, Igor Sommer, Martin Sysoev, Victor Skolkovo Innovat Ctr Lab Nanomat Skolkovo Inst Sci & Technol 3 Nobel Str Moscow 143026 Russia Yuri Gagarin State Tech Univ Saratov Lab Sensors & Microsyst 77 Polytech Skaya Str Saratov 410054 Russia Natl Univ Sci & Technol MISiS 4 Leninskiy Pr Moscow 119991 Russia Karlsruhe Inst Technol Inst Microstruct Technol 1 Hermann von Helmholtz Pl D-76344 Eggenstein Leopoldshafen Germany

We report a deposition of the tin oxide/hydroxide nanostructured layer by the potentiodynamic method from acidic nitrate solutions directly over the substrate, equipped with multiple strip electrodes which is employed as a gas-analyticalmultisensor array chip. The electrochemical synthesis is set to favor the growth of the tin oxide/hydroxide phase, while the appearance ofmetallic Sn is suppressed by cycling. The as-synthesized tin oxide/hydroxide layer is characterized by mesoporous morphology with grains, 250-300 nm diameter, which are further crystallized into fine SnO2 poly-nanocrystals following heating to 300 degrees C for 24 h just on the chip. The fabricated layer exhibits chemiresistive properties under exposure to organic vapors, which allows the generation of a multisensor vector signal capable of selectively distinguishing various vapors.

关键词： electrochemical deposition gas sensor multisensor array tin oxide cyclic voltammetry

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Toward On-Chip multisensor arrays for Selective Methanol and Ethanol Detection at Room Temperature: Capitalizing the Graphene Carbonylation

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ACS APPLIED MATERIALS & INTERFACES 2023年第23期15卷 28370-28386页

作者： Rabchinskii, Maxim K. Sysoev, Victor V. Varezhnikov, Alexey S. Solomatin, Maksim A. Struchkov, Nikolai S. Stolyarova, Dina Yu. Ryzhkov, Sergei A. Antonov, Grigorii A. Gabrelian, Vladimir S. Cherviakova, Polina D. Baidakova, Marina V. Krasnova, Anna O. Brzhezinskaya, Maria Pavlov, Sergei I. Kirilenko, Demid A. Kislenko, Vitaliy A. Pavlov, Sergey V. Kislenko, Sergey A. Brunkov, Pavel N. Ioffe Inst St Petersburg 194021 Russia Yuri Gagarin State Tech Univ Saratov Saratov 410054 Russia Natl Res Univ Elect Technol Moscow 124498 Russia NRC Kurchatov Inst Akad Kurchatova pl 1 Moscow 123182 Russia Zent Berlin Mat & Energie Hahn Meitner Pl 1 D-14109 Berlin Germany Skolkovo Inst Sci & Technol Skoltech Moscow 121205 Russia Joint Inst High Temp RAS 13-2 Izhorskaya St Moscow 125412 Russia

Theartificial olfaction units (or e-noses) capable ofroom-temperatureoperation are highly demanded to meet the requests of society in numerousvital applications and developing Internet-of-Things. Derivatized2D crystals are considered as sensing elements of choice in this regard,unlocking the potential of the advanced e-nose technologies limitedby the current semiconductor technologies. Herein, we consider fabricationand gas-sensing properties of On-chip multisensor arrays based ona hole-matrixed carbonylated (C-ny) graphene film with a graduallychanged thickness and concentration of ketone groups of up to 12.5at.%. The enhanced chemiresistive response of C-ny graphene towardmethanol and ethanol, of hundred ppm concentration when mixing withair to match permissible exposure OSHA limits, at room-temperatureoperation is signified. Following thorough characterization via core-leveltechniques and density functional theory, the predominant role ofthe C-ny graphene-perforated structure and abundance of ketone groupsin advancing the chemiresistive effect is established. Advancing practiceapplications, selective discrimination of the studied alcohols isapproached by linear discriminant analysis employing a multisensorarray's vector signal, and the fabricated chip's long-termperformance is shown.

关键词： 2D materials functionalized graphene graphenederivatives e-nose multisensor array gas sensors alcohols DFT calculations

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Bottom-up designing nanostructured oxide libraries under a lab-on-chip paradigm towards a low-cost highly-selective E-nose

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ANALYTICA CHIMICA ACTA 2025年 1333卷 343387页

作者： Solomatin, Maksim A. Fedorov, Fedor S. Kirilenko, Demid A. Trouillet, Vanessa Varezhnikov, Alexey S. Kiselev, Ilia, V Geckle, Udo Sommer, Martin Bainyashev, Alexey M. Artemov, Vasily Ushakov, Nikolay M. Goffman, Vladimir G. Rabchinskii, Maxim K. Nasibulin, Albert G. Sysoev, Victor V. Yuri Gagarin State Tech Univ Saratov 77 Polytechn St Saratov 410054 Russia RAS Saratov Branch Kotelnikov Inst Radioengn & Elect Zelenaya St 38 Saratov 410019 Russia Skolkovo Inst Sci & Technol Bolshoy Blvd 30Bld 1 Moscow 121205 Russia Ioffe Inst 26 Politekhn St St Petersburg 194021 Russia Karlsruhe Inst Technol Inst Appl Mat IAM Hermann Von Helmholtz Pl 1 D-76344 Eggenstein Leopoldshafen Germany Karlsruhe Inst Technol Karlsruhe Nano Micro Facil KNMFi Hermann Helmholtz Pl 1 D-76344 Eggenstein Leopoldshafen Germany Breitmeier Messtechn GmbH Englerstr 27 D-76275 Ettlingen Germany Karlsruhe Inst Technol KIT Inst Microstruct Technol Hermann Von Helmholtz Pl 1 D-76344 Eggenstein Leopoldshafen Germany Ecole Polytech Fed Lausanne EPFL Inst Bioengn CH-1015 Lausanne Switzerland Saratov NG Chernyshevskii State Univ Astrakhanskaya Str 83 Saratov 410012 Russia

Background: The multisensor concept has been developed as a powerful alternative to well-known gas-analytical instrumentation for applications where a fast but accurate and reliable assessment of the environment is required. The concept follows a biology-inspired approach where the selectivity towards various gases/odors is attained via pattern recognition of multisensory signal vectors. Herein, we discuss how to design a selective multisensor library based on various metal oxide nanostructures like a lab-on-chip using a simple but efficient bottom-up growth of materials over the multi-electrode chip under robust dc electrochemical protocols. Results: In addition to a conventional growth of oxide layers over the metal electrodes, we show that the fine nanowall-like oxide structures appear as a quasi-matrixed percolation film over the SiO2 substrate surface in the inter-electrode gaps to constitute a chemiresistive film. We have tested two directions while applying the technique to grow Co, Ni, Mn, and Zn oxides to develop on-chip sensor arrays of, (i) monoxide type employing the oxide films with gradual change of growth time, and (ii) multi-oxide type based on the four oxides. The materials were thoroughly characterized by electron microscopy, X-ray diffraction, thermogravimetric analysis, and X-ray photoelectron spectroscopy/mapping to prove the composition and structure. Among tested oxides, ZnO readily appears not only at the electric potential-targeted chip zone but also in other areas to dope the films for yielding heterojunctions with other oxides that enhances a variability of functional properties in the on-chip sensor array. The gas-sensing performance of the chips has been tested versus various chemically akin alcohol vapors at the sub- and low ppm range of concentrations in a mixture with air. Significance: We show that the grown oxide nanostructures exhibit a high-sensitive chemiresistive signal which allows one to build a multisensor vector signal, sele

关键词： Electronic nose multisensor array Gas sensor Nanowall Electrochemical deposition

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SnO2 Nanobelts as a Chemiresistive Platform for an On-Chip multisensory "Spectrometer" to Selectively Gauge Ions of Inert Gases

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ACS APPLIED NANO MATERIALS 2024年第19期7卷 22942-22952页

作者： Sysoev, Victor V. Petrunin, Alexander A. Plugin, Ilya A. Varezhnikov, Alexey S. Glukhova, Olga E. Yuri Gagarin State Tech Univ Saratov Dept Phys Saratov 410054 Russia Saratov NG Chernyshevskii State Univ Inst Phys Saratov 410012 Russia IM Sechenov First Moscow State Med Univ Inst Bion Technol & Engn Moscow 119991 Russia

The detection of inert gases presents a challenging task because these molecules do not react with most known sensor-based units aimed at environment monitoring. Here, we ionize these molecules in a low-potential discharge mode to force their interaction with semiconducting SnO2 single-crystal nanobelts (NBs) deposited as a mat over a multielectrode chip and show the ion-induced resistivity changes similar to a conventional operation of the metal oxide sensor. In particular, the conductance of the percolating NB mats is significantly enhanced under irradiation with He+, Ne+, and Ar+ ions at a low-pressure oxygen background. The phenomenon is well explained via ab initio calculations performed in the framework of density functional theory (DFT), which clarify the interaction of various ions with SnO2 nanocrystals related primarily to the appearance of electronic states and redistribution of their density dependent on the kind of ions. The differences in ion interaction with the SnO2 surface is the background for options to distinguish the inert gases with a SnO2 NB-based multisensor array as a low-cost selective detector via transferring the variations in a charge exchange at the adsorbate/adsorbent interface into a varied chemiresistive vector signal like a (mass) spectrometer performs.

关键词： metal oxide ion detector densityfunctionaltheory electronic nose multisensor array

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Multiplexed Gas Sensor: Fabrication Strategies, Recent Progress, and Challenges

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ACS SENSORS 2023年第9期8卷 3320-3337页

作者： Verma, Gulshan Gokarna, Anisha Kadiri, Hind Nomenyo, Komla Lerondel, Gilles Gupta, Ankur Indian Inst Technol Dept Mech Engn Jodhpur 342030 India Univ Technol CNRS UMR 6281 L2n F-10004 Troyes France

Due to miscellaneous toxic gases in the vicinity, thereis a burgeoningneed for advancement in the existing gas sensing technology not onlyfor the survival of mankind but also for the industries based in variousfields such as beverage, forestry, health care, environmental monitoring,agriculture, and military security. A gas sensor must be highly selectivetoward a specific gas in order to avoid incorrect signals while respondingto nontarget gases. This may lead to complex scenarios depicting sensordefects, such as low selectivity and cross-sensitivity. Therefore,a multiplex gas sensor is required to address the problems of crossselectivity by combining different gas sensors, signal processing,and pattern recognition techniques along with the currently employedgas sensing technologies. The different sensing materials used inthese sensor arrays will produce a unique response signal for developinga set of identifiers as the input that can be used to recognize aspecific gas by its "fingerprint". This review providesa comprehensive review of chemiresistive-based multiplex gas sensors,including various fabrication strategies from expensive to low-costtechniques, advances in sensing materials, and a gist of various patternrecognition techniques used for both rigid and flexible gas sensorapplications. Finally, the review assesses the current state-of-the-artin multiplex gas sensor technology and discusses various challengesfor future research in this direction.

关键词： chemiresistive sensors multisensor array gas sensor pattern recognition cross selectivity toxic gas interdigitated electrodes microsystem

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Guiding Graphene Derivatization for the On-Chip multisensor arrays: From the Synthesis to the Theoretical Background

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ADVANCED MATERIALS TECHNOLOGIES 2022年第7期7卷

作者： Rabchinskii, Maxim K. Sysoev, Victor V. Glukhova, Olga E. Brzhezinskaya, Maria Stolyarova, Dina Yu Varezhnikov, Alexey S. Solomatin, Maksim A. Barkov, Pavel, V Kirilenko, Demid A. Pavlov, Sergei, I Baidakova, Marina, V Shnitov, Vladimir V. Struchkov, Nikolai S. Nefedov, Denis Yu Antonenko, Anastasiia O. Cai, P. Liu, Z. Brunkov, Pavel N. Ioffe Inst Politekh Skaya St 26 St Petersburg 194021 Russia Yuri Gagarin State Tech Univ Saratov 77 Polytech Skaya St Saratov 410054 Russia Saratov NG Chernyshevskii State Univ Astrakhanskaya St 83 Saratov 410012 Russia IM Sechenov First Moscow State Med Univ Bolshaya Pirogovskaya St 2-4 Moscow 119991 Russia Helmholtz Zentrum Berlin Mat & Energie Hahn Meitner Pl 1 D-14109 Berlin Germany Kurchatov Inst NRC Akad Kurchatova Pl 1 Moscow 123182 Russia Natl Res Univ Elect Technol Bld 1Shokin Sq Moscow 124498 Russia St Petersburg State Univ Univ Skaya Nab 7-9 St Petersburg 199034 Russia China Jiliang Univ 258 Xueyuan St Hangzhou 310018 Zhejiang Peoples R China

Engineering the physics and chemistry of 2D materials is a key to unlock the potential of the advanced e-nose technologies limited by the current semiconductor technologies. Herein, the adjustment of the graphene's morphology, physics, and gas sensing properties upon its carboxylation via the developed photochemical method is demonstrated. Formation of matrices of nanoscale holes yet with the retention of the lamellar structure of the graphene layer is signified upon the introduction of up to 9.5 at% of carboxyl groups. The impact of the applied carboxylation on the conduction mechanism and electronic structure is demonstrated. The appearance of a set of the localized states in the valence band is revealed, originating from the molecular orbitals of carboxyls as is signified by the proposed approach for the identification of electronic states in graphene chemical derivatives. Given holey structure, predominance of highly affine carboxyls, and lateral inhomogeneity, the enhanced detection and discrimination of various alcohols, acetone, and ammonia vapors at room temperature is demonstrated. The opposite chemiresistive response toward ammonia in the humid air is also experimentally revealed and justified by the performed density functional theory modeling on the effect of ammonia, water, and their mix on electronic structure, and resistivity of the carboxylated graphene.

关键词： 2D material density functional theory calculations derivatization e-nose electronic structure gas sensor multisensor array

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Smart Diaper Based on Integrated Multiplex Carbon Nanotube-Coated Electrode array Sensors for In Situ Urine Monitoring

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ACS APPLIED NANO MATERIALS 2022年第4期5卷 4767-4778页

作者： Li, Xiangling Zhan, Changyuan Huang, Qiqi He, Mengyi Yang, Cheng Yang, Chengduan Huang, Xinshuo Chen, Meiwan Xie, Xi Chen, Hui-Jiuan Sun Yat Sen Univ Sch Elect & Informat Technol State Key Lab Optoelect Mat & Technol Guangzhou 510080 Peoples R China Sun Yat Sen Univ Guangdong Prov Key Lab Display Mat & Technol Guangzhou 510080 Peoples R China Sun Yat Sen Univ Sch Biomed Engn Guangzhou 528406 Peoples R China Univ Macau Inst Chinese Med Sci Taipa 999078 Macao Peoples R China

Wearable sensor technology is essential to achieve personalized health management via continuous monitoring of individual health status. Although diaper-based biosensors have been developed, multiplex strategies for biomolecular sensing of urine in situ are still rarely investigated, which limits a comprehensive assessment of the wearer's health information from urine. In this study, we present a mechanically flexible and smart diaper based on integrated multiplex electrochemical sensors (MECSs) for in situ urinalysis that simultaneously and selectively measures urinary metabolites (e.g., glucose, reactive oxygen species with H2O2 as an example, and uric acid) and electrolytes, including sodium and potassium ions. The sensor electrode arrays were modified with carbon nanotube coatings and chemical substances (ion-selective membranes, enzymes, or Pt nanoparticles) to achieve highly selective and sensitive monitoring of target biomarkers associated with urine status. The MECSs could be further prepared into a prototype that integrates a biosensor module, flexible circuit board, and Bluetooth signal transmitter to provide a promising substitute for monitoring for bedside patients, infants, and senior citizens.

关键词： urine monitoring CNT-coated electrode smart diaper sensing system multisensor array wearable device

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Alcohol Vapor Sensor Based on Quasi-2D Nb2O5 Derived from Oxidized Nb2CTz MXenes

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SENSORS 2024年第1期24卷 38页

作者： Pazniak, Hanna Plugin, Ilya A. Sheverdyaeva, Polina M. Rapenne, Laetitia Varezhnikov, Alexey S. Agresti, Antonio Pescetelli, Sara Moras, Paolo Kostin, Konstantin B. Gorokhovsky, Alexander V. Ouisse, Thierry Sysoev, Victor V. Univ Grenoble Alpes Inst Polytech Grenoble Ctr Natl Rech Sci Lab Mat & Genie PhysCS 50257 F-38016 Grenoble 1 France Yuri Gagarin State Tech Univ Saratov PhysicoTech Inst ul Polytech Skaya 77 Saratov 410054 Russia Ist Struttura Mat CNR ISM CNR SS 14Km 163-5 I-34149 Trieste Italy Univ Roma Tor Vergata Ctr Hybrid & Organ Solar Energy Elect Engn Dept I-00133 Rome Italy

MXenes are two-dimensional (2D) materials with a great potential for sensor applications due to their high aspect ratio and fully functionalized surface that can be tuned for specific gas adsorption. Here, we demonstrate that the Nb2CTz-based sensor exhibits high performance towards alcohol vapors at temperatures up to 300-350 degrees C, with the best sensitivity towards ethanol. We attribute the observed remarkable chemiresistive effect of this material to the formation of quasi-2D Nb2O5 sheets as the result of the oxidation of Nb-based MXenes. These findings are supported by synchrotron X-ray photoelectron spectroscopy studies together with X-ray diffraction and electron microscopy observations. For analyte selectivity, we employ a multisensor approach where the gas recognition is achieved by linear discriminant analysis of the vector response of the on-chip sensor array. The reported protocol demonstrates that MXene layers are efficient precursors for the derivation of 2D oxide architectures, which are suitable for developing gas sensors and sensor arrays.

关键词： MXene gas sensor niobium oxide X-ray photoelectron spectroscopy multisensor array

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Sol-gel derived ZnO film as a gas sensor: Influence of UV processing versus a thermal annealing

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SENSORS AND ACTUATORS A-PHYSICAL 2024年 377卷

作者： Pronin, Igor A. Plugin, Ilia A. Kolosov, Dmitry A. Karmanov, Andrey A. Yakushova, Nadezhda D. Varezhnikov, Alexey S. Komolov, Alexey S. Lazneva, Eleonora F. V. Koroleva, Aleksandra Moshnikov, Vyacheslav A. Kondratev, Valeriy M. Glukhova, Olga E. Korotcenkov, Gennadii Sysoev, Victor V. Penza State Univ Dept Nano & Microelect Penza 440026 Russia Yuri Gagarin State Tech Univ Saratov Dept Phys Saratov 410054 Russia Saratov NG Chernyshevskii State Univ Dept Radio Engn & Electrodynam Saratov 410012 Russia St Petersburg State Univ Dept Phys St Petersburg 199034 Russia St Petersburg State Univ Res Pk St Petersburg 199034 Russia St Petersburg Electrotech Univ LETI Dept Micro & Nanoelect St Petersburg 197022 Russia Alferov Univ Ctr Nanotechnol St Petersburg 194021 Russia Moscow Ctr Adv Studies Moscow 123592 Russia Moldova State Univ Dept Phys & Engn Kishinev 2009 Moldova IM Sechenov First Moscow State Med Univ Inst Bion Technol & Engn Moscow 119991 Russia

While preparing oxide layers as gas sensors by a sol-gel approach, a high-temperature annealing makes a challenge to apply in numerous applications like flexible electronics with a heavy influence on the oxide microstructure. Therefore, its replacing by UV irradiation combined with a mild heating as "photo-annealing" paves the way to develop soft protocols when designing oxide-based gas sensors bearing a fine nanocrystallinity. Herein, we consider hierarchical sol-gel derived ZnO films which were a subject of conventional annealing and photoannealing to compare their gas-sensor performance when exposed to alcohol vapors. It is found that films obtained by photoannealing have an X-ray amorphous character, in contrast to ones being thermally annealed;although, the hierarchical organization of both samples revealed by SEM is almost identical. The DFTB modeling performed for ZnO crystal exposed to alcohol molecules and water has indicated the chemiresistive effect to be enhanced with a molecular weight of analytes. These observations were validated in experiment with sol-gel ZnO layers which exhibited an alcohol response in sub-ppm concentration range down to 10 ppb. To selectively compare the impact of various alcohols, we successfully applied a linear-discriminant analysis to the vector signal of the on-chip multisensor array.

关键词： Sol -gel technology Epidermal electronics Zinc oxide UV irradiation multisensor array DFT

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