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\n  \n 2025\n \n \n (1)\n \n \n
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\n \n\n \n \n \n \n \n \n Fast and Sensitive Hydrogen Detection Using Nanostructured Black Palladium Thin Films Prepared by Pulsed Laser Deposition.\n \n \n \n \n\n\n \n Hruska, M.; Kejzlar, J.; Irimiciuc, S., A.; Premysl, F.; Vrnata, M.; Bouvet, M.; and Lancok, J.\n\n\n \n\n\n\n Barrande-Vltava 2025, 14th French-Czech Chemistry Meeting, Pardubice, Czech Republic. 8 2025.\n \n\n\n\n
\n\n\n\n \n \n \"FastPaper\n  \n \n\n \n\n \n link\n  \n \n\n bibtex\n \n\n \n  \n \n abstract \n \n\n \n\n \n \n \n \n \n \n \n\n  \n \n \n\n\n\n
\n 
@article{\n title = {Fast and Sensitive Hydrogen Detection Using Nanostructured Black Palladium Thin Films Prepared by Pulsed Laser Deposition},\n type = {article},\n year = {2025},\n month = {8},\n day = {31},\n id = {f6be4fc9-652f-3144-84b8-f4607c5a861b},\n created = {2025-08-31T19:56:36.437Z},\n file_attached = {true},\n profile_id = {d93fd8e4-0fb0-3e3d-a377-1ecd109e9ef5},\n group_id = {79dcc08f-a69a-38df-be65-84478e4db9b9},\n last_modified = {2025-09-03T14:30:44.870Z},\n read = {false},\n starred = {false},\n authored = {false},\n confirmed = {false},\n hidden = {false},\n private_publication = {false},\n abstract = {Hydrogen sensing is a crucial topic for many industrial and environmental applications, particularly in the context of the Green Deal and the adoption of hydrogen as a next-generation energy vector [1]. Consequently, various approaches are being explored to develop sensitive, reliable, and cost-effective devices for hydrogen detection—especially in the critical range below and near 4%, but also down to the ppm level [2].\nRecent sensor research has increasingly focused on exploiting the unique properties of nanomaterials and nanostructured thin films, particularly their high surface-to-volume ratio, to improve sensitivity. One such material is highly nanostructured metallic films, commonly referred to as black metals (BMs) due to their fine, fractal-like morphology, which gives them a black appearance and black-body behaviour. Although these materials have been known for decades, their application in gas sensing has only recently gained attention. [3, 4] We have successfully used evaporated black gold layers to detect hydrogen at concentrations below 1% [5].\nIn this study, we investigated the hydrogen sensing capabilities of black palladium. Low density Pd films were deposited in relatively high fluence conditions. The extreme growth conditions are optimum for foam-/fractal-like growth. Pulsed laser deposition technique offers superior control over the foam properties copmared with other classical approaches, whilst not being dependent on the physical and chemical properties of the target. The sensor performance is evaluated through calibration curves in the sub-4% hydrogen concentration range, alongside analysis of the sensor kinetics. Both pristine and thermally annealed (300 °C, 12 h) samples are studied and compared to optimise response dynamics and achieve a fast and sensitive hydrogen detection device.\n\nThis work was supported by the Agence Nationale de la Recherche through the ANR project Por4Sens ANR-22-CE06-0039-01 as well as by the Operational Programme Johannes Amos Comenius financed by European Structural and Investment Funds and the Czech Ministry of Education, Youth and Sports (Project No. SENDISO - CZ.02.01.01/00/22_008/0004596).\n\n1. Z. Abdin et al., Renew. Sustain. Energy Rev. 2020, 120, 109620. 2. T. Hübert et al., Sens. Actuators B: Chem. 2011, 157(2), 329–352. 3. M. Hruška et al., Nanomaterials 2022, 12(23), 4297. 4. J. Kejzlar et al., Mater. Adv. 2025, 6(10), 3280–3292. 5. M. Hruška et al., Appl. Surf. Sci. 2024, 647, 158618.},\n bibtype = {article},\n author = {Hruska, Martin and Kejzlar, Jan and Irimiciuc, Stefan Andrei and Premysl, Fitl and Vrnata, Martin and Bouvet, Marcel and Lancok, Jan},\n journal = {Barrande-Vltava 2025, 14th French-Czech Chemistry Meeting, Pardubice, Czech Republic}\n}
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\n Hydrogen sensing is a crucial topic for many industrial and environmental applications, particularly in the context of the Green Deal and the adoption of hydrogen as a next-generation energy vector [1]. Consequently, various approaches are being explored to develop sensitive, reliable, and cost-effective devices for hydrogen detection—especially in the critical range below and near 4%, but also down to the ppm level [2].\nRecent sensor research has increasingly focused on exploiting the unique properties of nanomaterials and nanostructured thin films, particularly their high surface-to-volume ratio, to improve sensitivity. One such material is highly nanostructured metallic films, commonly referred to as black metals (BMs) due to their fine, fractal-like morphology, which gives them a black appearance and black-body behaviour. Although these materials have been known for decades, their application in gas sensing has only recently gained attention. [3, 4] We have successfully used evaporated black gold layers to detect hydrogen at concentrations below 1% [5].\nIn this study, we investigated the hydrogen sensing capabilities of black palladium. Low density Pd films were deposited in relatively high fluence conditions. The extreme growth conditions are optimum for foam-/fractal-like growth. Pulsed laser deposition technique offers superior control over the foam properties copmared with other classical approaches, whilst not being dependent on the physical and chemical properties of the target. The sensor performance is evaluated through calibration curves in the sub-4% hydrogen concentration range, alongside analysis of the sensor kinetics. Both pristine and thermally annealed (300 °C, 12 h) samples are studied and compared to optimise response dynamics and achieve a fast and sensitive hydrogen detection device.\n\nThis work was supported by the Agence Nationale de la Recherche through the ANR project Por4Sens ANR-22-CE06-0039-01 as well as by the Operational Programme Johannes Amos Comenius financed by European Structural and Investment Funds and the Czech Ministry of Education, Youth and Sports (Project No. SENDISO - CZ.02.01.01/00/22_008/0004596).\n\n1. Z. Abdin et al., Renew. Sustain. Energy Rev. 2020, 120, 109620. 2. T. Hübert et al., Sens. Actuators B: Chem. 2011, 157(2), 329–352. 3. M. Hruška et al., Nanomaterials 2022, 12(23), 4297. 4. J. Kejzlar et al., Mater. Adv. 2025, 6(10), 3280–3292. 5. M. Hruška et al., Appl. Surf. Sci. 2024, 647, 158618.\n
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\n  \n 2024\n \n \n (1)\n \n \n
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\n \n\n \n \n \n \n \n \n In-Situ QCM Impedance Analysis of Nanostructured Thin Film Growth.\n \n \n \n \n\n\n \n Hruška, M.; Kejzlar, J.; Otta, J.; Fitl, P.; Novotný, M.; Kiba, T.; Kawamura, M.; and Vrňata, M.\n\n\n \n\n\n\n ISSP2024, The 17th International Symposium on Sputtering & Plasma Processes. 7 2024.\n \n\n\n\n
\n\n\n\n \n \n \"In-SituPaper\n  \n \n\n \n\n \n link\n  \n \n\n bibtex\n \n\n \n  \n \n abstract \n \n\n \n\n \n \n \n \n \n \n \n\n  \n \n \n\n\n\n
\n 
@article{\n title = {In-Situ QCM Impedance Analysis of Nanostructured Thin Film Growth},\n type = {article},\n year = {2024},\n month = {7},\n id = {830ed1ab-8ad9-36aa-af1e-88203fa1d944},\n created = {2024-07-04T00:54:05.149Z},\n file_attached = {true},\n profile_id = {d93fd8e4-0fb0-3e3d-a377-1ecd109e9ef5},\n group_id = {79dcc08f-a69a-38df-be65-84478e4db9b9},\n last_modified = {2024-07-04T07:53:54.765Z},\n read = {false},\n starred = {false},\n authored = {false},\n confirmed = {false},\n hidden = {false},\n private_publication = {false},\n abstract = {A comprehensive understanding of thin film growth is pivotal for enhancing the performance of thin film sensors, especially those composed of highly nanostructured materials where uniformity in density across the film thickness is often lacking. Investigating the growth of these films, particularly through in-situ methods during deposition processes such as thermal evaporation or magnetron sputtering, is thus of great benefit. In this study, we explore the growth mechanisms of highly nanostructured black metals (BMs), particularly black gold (BAu) and black aluminum (BAl) prepared by thermal evaporation and magnetron sputtering using an in-situ Quartz Crystal Microbalance with Impedance Analysis (QCM-IA). By employing an advanced Butterworth-Van Dyke (BVD) fitting algorithm [1] for real-time measurements, we provide new insights into the complex processes that control thin film formation as well as their interactions with surrounding gaseous environment, by loading the vacuum apparatus with inert gases (He, N2, Ar), providing insights into subsequent sensor applications. Prepared films were characterized by SEM and AFM, confirming their nanostructured morphology. Additionally, these films were tested for their potential use as active layers for QCM sensors, showcasing their applicability in sensor technology. This approach not only provides a deeper understanding of the nanostructured film growth process but also emphasizes the integration of advanced characterization techniques for the enhancement of sensor functionalities. Building upon our previous studies of black metals [2, 3], this work extends our knowledge on nanostructured film growth and possibly also introduces methodology for in-depth investigations.\n[1]\tMartin Hruska (2024). QCM_BvD_Fitting_Toolbox, MATLAB Central File Exchange. Retrieved February 29, 2024. (https://www.mathworks.com/matlabcentral/fileexchange/136079-qcm_bvd_fitting_toolbox)\n[2]\tHruška, M., More-Chevalier, J., Fitl, P., Novotný, M., Hruška, P., Prokop, D., Pokorný, P., Kejzlar, J., Gadenne, V., Patrone, L., Vrňata, M., Lančok, J., Nanomaterials MDPI, 12 (23), (2023) 4297\n[3]\tHruška, M., Kejzlar, J., Otta, J., Fitl, P., Novotný, M., Čížek, J., Melikhova, O., Mičušík, M., Machata, P., Vrňata, M., Applied Surface Science, 647, (2024) 158618.},\n bibtype = {article},\n author = {Hruška, Martin and Kejzlar, Jan and Otta, Jaroslav and Fitl, Přemysl and Novotný, Michal and Kiba, Takayuki and Kawamura, Midori and Vrňata, Martin},\n journal = {ISSP2024, The 17th International Symposium on Sputtering & Plasma Processes}\n}
\n
\n\n\n
\n A comprehensive understanding of thin film growth is pivotal for enhancing the performance of thin film sensors, especially those composed of highly nanostructured materials where uniformity in density across the film thickness is often lacking. Investigating the growth of these films, particularly through in-situ methods during deposition processes such as thermal evaporation or magnetron sputtering, is thus of great benefit. In this study, we explore the growth mechanisms of highly nanostructured black metals (BMs), particularly black gold (BAu) and black aluminum (BAl) prepared by thermal evaporation and magnetron sputtering using an in-situ Quartz Crystal Microbalance with Impedance Analysis (QCM-IA). By employing an advanced Butterworth-Van Dyke (BVD) fitting algorithm [1] for real-time measurements, we provide new insights into the complex processes that control thin film formation as well as their interactions with surrounding gaseous environment, by loading the vacuum apparatus with inert gases (He, N2, Ar), providing insights into subsequent sensor applications. Prepared films were characterized by SEM and AFM, confirming their nanostructured morphology. Additionally, these films were tested for their potential use as active layers for QCM sensors, showcasing their applicability in sensor technology. This approach not only provides a deeper understanding of the nanostructured film growth process but also emphasizes the integration of advanced characterization techniques for the enhancement of sensor functionalities. Building upon our previous studies of black metals [2, 3], this work extends our knowledge on nanostructured film growth and possibly also introduces methodology for in-depth investigations.\n[1]\tMartin Hruska (2024). QCM_BvD_Fitting_Toolbox, MATLAB Central File Exchange. Retrieved February 29, 2024. (https://www.mathworks.com/matlabcentral/fileexchange/136079-qcm_bvd_fitting_toolbox)\n[2]\tHruška, M., More-Chevalier, J., Fitl, P., Novotný, M., Hruška, P., Prokop, D., Pokorný, P., Kejzlar, J., Gadenne, V., Patrone, L., Vrňata, M., Lančok, J., Nanomaterials MDPI, 12 (23), (2023) 4297\n[3]\tHruška, M., Kejzlar, J., Otta, J., Fitl, P., Novotný, M., Čížek, J., Melikhova, O., Mičušík, M., Machata, P., Vrňata, M., Applied Surface Science, 647, (2024) 158618.\n
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\n  \n 2023\n \n \n (1)\n \n \n
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\n \n\n \n \n \n \n \n \n Quartz Crystal Microbalance Sensors with Nanoporous Coatings: An Impedance Analysis Study.\n \n \n \n \n\n\n \n Hruška, M.; Iino, H.; Kudo, S.; Kejzlar, J.; Otta, J.; Fitl, P.; Novotný, M.; Kiba, T.; Kawamura, M.; and Vrňata, M.\n\n\n \n\n\n\n IMEKO TC8, TC11 and TC24 Conference. 2023.\n \n\n\n\n
\n\n\n\n \n \n \"QuartzPaper\n  \n \n\n \n\n \n link\n  \n \n\n bibtex\n \n\n \n  \n \n abstract \n \n\n \n\n \n \n \n \n \n \n \n\n  \n \n \n\n\n\n
\n 
@article{\n title = {Quartz Crystal Microbalance Sensors with Nanoporous Coatings: An Impedance Analysis Study},\n type = {article},\n year = {2023},\n city = {Funchal, Madeira, Portugal},\n id = {89dd6fc2-d94a-35bc-8f8b-788e8b7567cb},\n created = {2024-07-04T00:48:41.481Z},\n file_attached = {true},\n profile_id = {d93fd8e4-0fb0-3e3d-a377-1ecd109e9ef5},\n group_id = {79dcc08f-a69a-38df-be65-84478e4db9b9},\n last_modified = {2024-07-04T07:55:31.971Z},\n read = {false},\n starred = {false},\n authored = {false},\n confirmed = {false},\n hidden = {false},\n private_publication = {false},\n abstract = {Quartz crystal microbalance sensors (QCM) are characterized by many potential applications. They are widely used as biosensors, for combustion control, environmental pollution monitoring, or gas sensors. Regardless of the specific application, the recognition resolution of QCMs is determined and restricted according to the Sauerbray equation. This fact is crucial mainly for gas sensor applications where low concentrations need to be detected, and the mass of adsorbed analytes does not usually lead to a sufficient sensor response. Yet, there are some possibilities for how to enhance the QCM sensor properties and amplify their sensitivity, for instance by increasing the specific surface area and thus providing more bonding sites for the analytes. One such approach is the use of highly nanoporous metal layers, namely black metals (BMs), due to their fractal surface and high surface-to-volume ratio. However, BMs also show lower rigidity and impaired viscoelastic properties with respect to QCM oscillations, and thus they can cause damping as shown by the lower quality factor. For these reasons, proper investigation of those processes is necessary to optimise the black metal preparation conditions and utilisation of black metal based QCM sensors. Herein we present a detailed study of QCM sensors with nanoporous black metal coatings using impedance analysis. The influence of the thickness of the black metal layer and the preparation method on the quality factor of the QCM is compared and discussed. Also, a novel impedance data fitting method for the Butterworth-van Dyke equivalent circuit model is presented.},\n bibtype = {article},\n author = {Hruška, Martin and Iino, Hiroumi and Kudo, Sodai and Kejzlar, Jan and Otta, Jaroslav and Fitl, Přemysl and Novotný, Michal and Kiba, Takayuki and Kawamura, Midori and Vrňata, Martin},\n journal = {IMEKO TC8, TC11 and TC24 Conference}\n}
\n
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\n Quartz crystal microbalance sensors (QCM) are characterized by many potential applications. They are widely used as biosensors, for combustion control, environmental pollution monitoring, or gas sensors. Regardless of the specific application, the recognition resolution of QCMs is determined and restricted according to the Sauerbray equation. This fact is crucial mainly for gas sensor applications where low concentrations need to be detected, and the mass of adsorbed analytes does not usually lead to a sufficient sensor response. Yet, there are some possibilities for how to enhance the QCM sensor properties and amplify their sensitivity, for instance by increasing the specific surface area and thus providing more bonding sites for the analytes. One such approach is the use of highly nanoporous metal layers, namely black metals (BMs), due to their fractal surface and high surface-to-volume ratio. However, BMs also show lower rigidity and impaired viscoelastic properties with respect to QCM oscillations, and thus they can cause damping as shown by the lower quality factor. For these reasons, proper investigation of those processes is necessary to optimise the black metal preparation conditions and utilisation of black metal based QCM sensors. Herein we present a detailed study of QCM sensors with nanoporous black metal coatings using impedance analysis. The influence of the thickness of the black metal layer and the preparation method on the quality factor of the QCM is compared and discussed. Also, a novel impedance data fitting method for the Butterworth-van Dyke equivalent circuit model is presented.\n
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\n  \n 2019\n \n \n (1)\n \n \n
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\n \n\n \n \n \n \n \n \n Photoregeneration and improvement of chemical sensors.\n \n \n \n \n\n\n \n Hruška, M.; Tomeček, D.; Fitl, P.; Vlček, J.; Havlová, Š.; Fara, J.; Otta, J.; Marešová, E.; and Vrňata, M.\n\n\n \n\n\n\n MultiComp Autumn Prague Meeting. 9 2019.\n \n\n\n\n
\n\n\n\n \n \n \"PhotoregenerationPaper\n  \n \n\n \n\n \n link\n  \n \n\n bibtex\n \n\n \n  \n \n abstract \n \n\n \n\n \n \n \n \n \n \n \n\n  \n \n \n\n\n\n
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@article{\n title = {Photoregeneration and improvement of chemical sensors},\n type = {article},\n year = {2019},\n month = {9},\n city = {Prague},\n id = {a009128a-af04-3da5-9061-c4921982f78f},\n created = {2024-07-25T14:05:44.408Z},\n file_attached = {true},\n profile_id = {d93fd8e4-0fb0-3e3d-a377-1ecd109e9ef5},\n group_id = {79dcc08f-a69a-38df-be65-84478e4db9b9},\n last_modified = {2024-07-25T14:08:16.353Z},\n read = {false},\n starred = {false},\n authored = {false},\n confirmed = {false},\n hidden = {false},\n private_publication = {false},\n abstract = {Photoregeneration is a soft and economic method for desorption of adsorbed analytes from thin gas sensor layers (= for sensor regeneration). It is based on the illumination of the sensor by specific light at a precise wavelength and intensity [1].\nThis method of regeneration is appropriate especially for thin organic or inorganic layers that suffer from long recovery times and baseline shifts. Or there where temperature regeneration is undesirable due to possible morphological changes of the active layer.\nThe main aim of our work is focused on the optimization of photoregeneration method for phthalocyanine chemiresistors and quartz crystal microbalance (QCM) sensors sensitive to NO2.\nPart of our work also focuses on the improvement of sensing properties of QCM sensors by the use of metal-blacks (MBs) MBs are highly nanoporous and nanostructured materials that have a large specific surface area. This large surface provides more binding sites for analytes and, hence, increase the response of the QCM sensor.\nIn the future, we would like to combine these two principles together and prepare high-sensitive and simply regenerable QCM sensors sensitive to NO2 or other analytes depending on the used active layer.\n\nReferences\n\n[1] – Tomeček, D.; Hruška, M.; Fitl, P.; et al. Phthalocyanine Photoregeneration for Low Power Consumption Chemiresistors. ACS Sensors 2018, 3 (12), 2558–2565.},\n bibtype = {article},\n author = {Hruška, Martin and Tomeček, David and Fitl, Přemysl and Vlček, Jan and Havlová, Šárka and Fara, Jan and Otta, Jaroslav and Marešová, Eva and Vrňata, Martin},\n journal = {MultiComp Autumn Prague Meeting}\n}
\n
\n\n\n
\n Photoregeneration is a soft and economic method for desorption of adsorbed analytes from thin gas sensor layers (= for sensor regeneration). It is based on the illumination of the sensor by specific light at a precise wavelength and intensity [1].\nThis method of regeneration is appropriate especially for thin organic or inorganic layers that suffer from long recovery times and baseline shifts. Or there where temperature regeneration is undesirable due to possible morphological changes of the active layer.\nThe main aim of our work is focused on the optimization of photoregeneration method for phthalocyanine chemiresistors and quartz crystal microbalance (QCM) sensors sensitive to NO2.\nPart of our work also focuses on the improvement of sensing properties of QCM sensors by the use of metal-blacks (MBs) MBs are highly nanoporous and nanostructured materials that have a large specific surface area. This large surface provides more binding sites for analytes and, hence, increase the response of the QCM sensor.\nIn the future, we would like to combine these two principles together and prepare high-sensitive and simply regenerable QCM sensors sensitive to NO2 or other analytes depending on the used active layer.\n\nReferences\n\n[1] – Tomeček, D.; Hruška, M.; Fitl, P.; et al. Phthalocyanine Photoregeneration for Low Power Consumption Chemiresistors. ACS Sensors 2018, 3 (12), 2558–2565.\n
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