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1

Comparison of Field Effect Transistor with C-nPd gate and resistive C-nPd film sensing properties toward hydrogen

Krawczyk Sławomir, Czerwosz Elżbieta, Wronka Halina, Firek Piotr, Sochacki Mariusz, Szmidt Jan

Przegląd Elektrotechniczny

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2022

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R. 98, nr 9

311--313

EN

As a result of the implementation of the POIG project (UDI-POiG.01.03.01-14-071/08-00), the research network Łukasiewicz, the Teleand Radio Institute and the Warsaw University of Technology, developed resistance hydrogen sensors using changes in nanocomposite resistance. Carbon-Palladium films (C-nPd) were obtained by PVD method, followed by transistor sensors (FET) with a gate covered with a previously developed nanocomposite C-nPd film. In this article, we show differences in a sensing properties and reaction of discussed resistance for the transistor sensors with a C-nPd film and resistive sensors built of C-nPd film deposited on ceramic substrate. For both types of sensors we performed sensing characterization in a research set-up prepared especially for this purpose during the implementation of the project. We found that transistor sensor is much more sensitive toward hydrogen than resistive sensor.

PL

W wyniku realizacji projektu POIG (UDA-POIG.01.03.01-14-071/08-00) realizowanego w latach 2009-2015 . Sieć Badawcza Łukasiewicz Instytut Tele- i Radiotechniczny oraz Politechnika Warszawską opracowały oporowe sensory wodoru wykorzystujący zmiany rezystancji nanokompozytowych warstw węglowo-palladowych (C-nPd) otrzymywanych metodą PVD, a następnie sensory tranzystorowe (FET) z bramką wykonaną z opracowanej wcześniej nanokompozytowej warstwy C-nPd. W tym artykule zostały pokazane różnice we właściwościach sensorycznych i ich reakcjach na wodór dla obu typów sensorów tranzystorowego i oporowego w postaci warstwy C-nPd osadzonej na podłożu ceramicznym. Dla obu typów sensorów badania sensorowe były prowadzone na specjalnie do tego celu zbudowanym stanowisku badawczym.

2

Hydrogen sensor based on field effect transistor with C–Pd layer

Firek Piotr, Krawczyk Sławomir, Wronka Halina, Czerwosz Elżbieta, Szmidt Jan

Metrology and Measurement Systems

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2020

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Vol. 27, nr 2

313--321

EN

ISFET (Ion Sensitive Field Effect Transistors) microsensors are widely used for pH measurements as well as analytical and biomedical applications. At the same time, ISFET is a good candidate for testing various materials for their applications in sensitive membranes. For example, hydrogen sensitive carbonaceous films containing Pd nanocrystallites (C-Pd) make this material very interesting for sensor applications. A cost effective silicon technology was selected to fabricate n-channel transistors. The structures were coupled to specially designed double-sided PCB (Printed Circuit Board) holder. The holder enables assembly of the structure as part of an automatic stand. The last step of production of MIS structures was deposition of the C-Pd layer. The C-Pd films were fabricated by the Physical Vapor Deposition (PVD) method in which C60 and palladium acetate were evaporated. Electrical resistance of structures with C-Pd films was measured during their interaction with hydrogen. Finally, a new type of highly sensitive FET hydrogen sensor with C-Pd layer was demonstrated and characterized.

3

Cross-sensitivity of hydrogen sensors to relative humidity

Majewski J.

Przegląd Elektrotechniczny

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2018

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R. 94, nr 7

128--131

EN

The influence of the relative humidity of hydrogen-air mixture on the most commonly used types of hydrogen sensors, based on catalytic combustion, metal oxide semiconductor, and thermal conductivity is discussed, and compared. The cross-sensitivity of these types of hydrogen sensors to relative humidity is discribed and exemplified with experimental data, as well as approaches to mitigate that cross-sensitivity are characterised.

PL

Przedstawiono i porównano wpływ wilgotności względnej mieszaniny wodór-powietrze na najbardziej rozpowszechnione typy sensorów wodoru: katalityczne, półprzewodnikowe z tlenków metali, i termokonduktancyjne. Opisano czułość skrośną tych typów sensorów wodoru na wilgotność względną i podano przykłady jej wyznaczania, oraz scharakteryzowano sposoby zmniejszania tej czułości.

4

Badania nanokompozytowych materiałów węglowych

Diduszko R., Kozłowski M., Krawczyk S., Rymarczyk J., Stępińska I., Czerwosz E.

Elektronika : konstrukcje, technologie, zastosowania

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2016

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Vol. 57, nr 6

32--38

PL

W artykule przedstawiono niektóre metody badań właściwości nanokompozytowych materiałów węglowych zbudowanych z różnych odmian alotropowych węgla i nanoziaren palladu lub niklu. Właściwości tych nanometeriałow zbadane zostały przy zastosowaniu wielu metod takich jak: skaningowa mikroskopia elektronowa wraz ze spektroskopią dyspersji energii, spektroskopia w podczerwieni z transformacją Fouriera, dyfrakcja rentgenowska. Pokazano również wyniki badań takich właściwości tych nanomateriałów jak emisja polowa i zmiany rezystancji pod wpływem zmian otoczenia gazowego. Wszystkie prezentowane badania były prowadzone w Zakładzie Nanotechnologii ITR.

EN

The results of studies of some properties of nanocomposite materials compose of many allotropic form of carbon and nickel or palladium nanograins are presented. The properties of such materials were studied with: Scanning Electron Microscopy, Fourier Transform Infrared Spectroscopy, X-Ray Diffraction. The results of field emission studies and resistance changes due gas influencestudies are also shown. All presented investigations were performed in Nanotechnology Department of ITR.

5

Hydrogen Sensor Of TiO2-Based Nanomaterials

Łysoń-Sypień B., Zakrzewska K., Gajewska M., Radecka M.

Archives of Metallurgy and Materials

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2015

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Vol. 60, iss. 2A

935--940

EN

The aim of this research was to examine gas sensing properties of TiO2 based nanomaterials. Nanopowders of Cr doped TiO2 with constant Specific Surface Area, SSA, were obtained using Flame Spray Synthesis technique, FSS. Nanomaterials were characterized by Brunauer – Emmett – Teller adsorption isotherms, BET, X – ray diffraction, XRD, Transmission Electron Microscopy, TEM, optical spectrometry UV – vis with the use of an integrating sphere as well as impedance spectroscopy. Detection of hydrogen was carried out over the concentration range of 50 - 3000 ppm at the temperatures extending from 200 to 400°C and synthetic air working as a reference atmosphere. As a result of experiments it appeared that incorporation of 5 at.% of Cr into TiO2 improved hydrogen sensing features due to small crystallite size and predominance of rutile polymorphic phase.

PL

Przedmiotem pracy są nanomateriały na bazie TiO2 do zastosowań sensorowych. Nanoproszki TiO2 domieszkowane chromem o stałej powierzchni właściwej SSA (ang. Specific Surface Area) otrzymano przy pomocy techniki syntezy w płomieniu FSS (ang. Flame Spray Synthesis). Materiały poddano charakteryzacji z wykorzystaniem: izoterm adsorpcyjnych Brunauer – Emmett – Teller, BET, dyfraktometrii rentgenowskiej, XRD, transmisyjnej mikroskopii elektronowej, TEM, spektroskopii optycznej UV – vis oraz spektroskopii impedancyjnej. Pomiar własności sensorowych został przeprowadzony dla koncentracji H2 w zakresie 50-3000 ppm w przedziale temperatur 200-400°C. Wykazano, że najlepiej na wodór odpowiada próbka TiO2: 5 at.% Cr charakteryzująca się małym rozmiarem krystalitów oraz przewagą fazy rutylu.

6

Infiuence of Hydrogen on the Properties of Nanostructured C-Pd Films for Sensing Applications

Kamińska A., Diduszko R., Krawczyk S., Czerwosz E., Sobczak K.

Polish Journal of Chemical Technology

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2014

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Vol. 16, nr 2

77--81

EN

In this paper we present the results of the investigations of nanostructured C-Pd films for hydrogen sensing applications. These C-Pd films were prepared by physical vapor deposition and then annealed in an argon flow at the temperature of 500°C. The structure and morphology of the prepared C-Pd films were investigated using transmission electron microscopy and energy dispersive X-ray spectroscopy. We studied the infiuence of hydrogen on the electrical properties and crystal structure of C-Pd films. It was shown that film resistance changes depended on hydrogen concentration. At lower hydrogen concentration (up to 2 vol.%), the films response increased proportionally to [H2], while above 2 vol.% H2, it was almost constant. This is connected with the formation of a solid solution of hydrogen in palladium at lower H2 concentration and the creation of palladium hydride at higher H2 concentration. X-ray diffraction was used to confirm the formation of Pd-H solid solution and palladium hydride.

7

Czujnik wodoru do zastosowań w podwyższonej temperaturze i wilgotności

Czerwosz E., Kamińska A., Kowalska E., Kozłowski M., Krawczyk S., Radomska J., Wronka H.

Elektronika : konstrukcje, technologie, zastosowania

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2014

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Vol. 55, nr 7

120-123

PL

Ze względu na silny rozwój technologii wodorowych wzrasta zainteresowanie urządzeniami i materiałami pozwalającymi gromadzić i wykrywać wodór. W szczególności czujniki wodoru mogą znaleźć zastosowanie w wielu dziedzinach życia i techniki. W tej pracy przedstawiamy rezultaty kilkuletniej pracy nad opracowaniem czujnika wodoru nowej generacji wykorzystującego jako element aktywny warstwy węglowo-palladowe. Ten innowacyjny, rezystancyjny czujnik wodoru może pracować w warunkach podwyższonej temperatury i wilgotności. Czujnik taki jest selektywny, charakteryzuje się szybką odpowiedzią i daje wyraźny sygnał nawet dla bardzo niskich koncentracji wodoru.

EN

Rapid development of hydrogen technology caused interest in devices and materials allowing for storage and detection of hydrogen. Especially, hydrogen sensors could be applied in many areas of daily life and technics. In this paper we present results of our studies on a elaboration of construction and material technology for new generation of hydrogen sensor based on carbonaceous-palladium films. This innovative, resistive hydrogen sensor can operated at higher than normal temperature and humidity. This sensor is selective, shows fast response and gives strong signal even at very low concentration of hydrogen.

8

Influence of palladium chemical structure on hydrogen sensing properties of carbonaceous–palladium thin films

Kaminska A., Krawczyk S., Kozlowski C.

Optica Applicata

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2013

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Vol. 43, nr 4

633--640

EN

In this work we investigate nanocomposite carbonaceous–palladium (C–Pd) films prepared by physical vapor deposition. Such films are promising materials for hydrogen sensor applications. This is related to the highly selective hydrogen absorption by palladium nanocrystallites. The C–Pd films obtained in various technological conditions differ in structure and electrical properties. These films were characterized by SEM, EDS and FTIR spectroscopy. FTIR spec-troscopy was used to determine the amount of palladium acetate and fullerene, incompletely decomposed during the deposition process. FTIR spectra enabled us to explain the differences in C–Pd films resistance based on palladium chemical structure. The possibility of the application of C–Pd films as active layers in hydrogen sensors was also studied. The results showed that synthesized C–Pd films containing palladium nanograins could be used for hydrogen sensing.

9

The sensibility of resistance sensor structures with graphene to the action of selected gaseous media

Pustelny T., Setkiewicz M., Drewniak S., Maciak E., Stolarczyk A., Urbańczyk M., Procek M., Gut K., Opilski Z., Pasternak I., Strupinski W.

Bulletin of the Polish Academy of Sciences. Technical Sciences

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2013

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Vol. 61, nr 2

293--300

EN

The paper presents resistance sensor structures with a graphene sensing layer. The structures were tested concerning their sensitivity to the affects of hydrogen, nitrogen dioxide and steam in an atmosphere of a synthetic air. Investigations have proved that resistance structures with a graphene layer are sensitive to the presence of the tested gases. The resistance of the structures amounted to about 10Ω, whereas changes in the resistances affected by the external gaseous medium were contained within the range of a several mΩ. The investigations confirmed that the resistance structures with graphene exposed to the affect of hydrogen in atmosphere of synthetic air change their resistances practically at once (within the order of only a few seconds). This indicates that such structures might be practically applied in sensors of hydrogen ensuring a short time of response.

10

Badania zmian oporności warstw C-Pd zachodzących pod wpływem wodoru i metanu

Kamińska A., Krawczyk S., Czerwosz E.

Elektronika : konstrukcje, technologie, zastosowania

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2012

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Vol. 53, nr 8

31-33

PL

W pracy badano możliwość zastosowania warstw C-Pd, jako czujników wodoru oraz metanu. Warstwy C-Pd otrzymywano dwuetapową metodą PVD/CVD. Wyniki przeprowadzonych badań pokazują, iż uzyskane warstwy reagują zarówno na obecność wodoru, jak i metanu.

EN

The paper presents the results of investigations of the possibility of using C-Pd films as hydrogen and methane sensors. C-Pd films were prepared in a two-step PVD/CVD method. The obtained results show that the films respond both to the presence of hydrogen and methane in the surrounding atmosphere.

11

Badania struktury molekuralnej i nanokrystalicznej warstw Pd-C do zastosowań w detektorach wodorowych

Suchańska M., Czerwosz E., Diduszko R., Dłużewski P., Kęczkowska J., Kowalska E., Rymarczyk J.

Elektronika : konstrukcje, technologie, zastosowania

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2010

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Vol. 51, nr 6

54-57

PL

Prezentowane są wyniki charakteryzacji właściwości fizyko-chemicznych nanostrukturalnych warstw węglowo-palladowych (Pd-C), które mogą być wykorzystane jako warstwy aktywne w detektorach wodoru i/lub związków gazowych wodoru. Warstwy Pd-C zostały wytworzone metodą dwuetapową, gdzie jako pierwszy etap zastosowano technologie PVD, zaś drugim etapem byta metoda CVD. Badano topografię warstw metodą mikroskopii sił atomowych (AFM). Struktura warstw była badana na poziomie subatomowym metodą transmisyjnej mikroskopii elektronowej (TEM), w skali molekularnej metodą spektroskopii ramanowskiej (RS), a w skali mikro metodą dyfrakcji rentgenowskiej (XRD).

EN

Pd-C films are known as very promising materials for hydrogen sensors and storage. We present results of characterization of Pd-C films composed of carbon and palladium nanograins and obtained in two steps method. The film obtained in the first step exhibits multiphase structure composed of fullerene nanograins, amorphous carbon and palladium nanocrystals. This film is modified in CVD process. The final films has porous carbonaceous structure. The films topography was studied using Atomie Force Microscopy (AFM). The films structure was investigated using the following methods: Transmission Electron Microscopy (TEM) on subatomic level, Raman Spectroscopy (RS) in molecular scale and X-ray Diffraction (XRD) in micro scale.

12

Hydrogen Sensor with Palladium and Metal-Free Phthalocyanine Bilayer Structures in Surface Phthalocyanine Bilayer Structures in Surface Acoustic Wave Attenaution on Ferrofluid

Jakubik W.

Molecular and Quantum Acoustics

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2003

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Vol. 24

81-87

EN

Presented here are the results concerning a hydrogen sensor based on a novel bilayer structure in a Surface Acoustic Wave dual-delay line and electric systems. The sensor material consists of two layers produced in two different vapour deposition processes. The first one is a metal-free pthalocyanine (H2Pc) layer, whereas the second is a ~20 nm thin palladium (Pd) film. This structure was simultaneously formed in a one of the SAW dual delay lines and on the interdigital electrodes of the glass substrate for electric measurements. In such a bilayer structure detection of hydrogen in a medium concentration range (from 1% to 4 % in nitrogen) is possible, even at room temperature. Preliminary measurements of this two bilayer structures has been performed simultaneously in the same chamber for this same measurements conditions. A good correlation of results between these structures has been observed.

13

Surface Acoustic Wave Hydrogen Sensor with Nickel Phtalocyyanine and Palladium Thin Layers

Jakubik W., Urbańczyk M., Kochowski S., Bodzenta J.

Molecular and Quantum Acoustics

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2002

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Vol. 23

473-482

EN

Presented here are the results concerning a hydrogen sensor based on a novel bilayer structure in a Surface Acoustic Wave dual-delay line system. The sensor material consists of two layers produced in two different vapour deposition processes.The first one is a 230 nm nickel phtalocyanine (NiPc) layer, whereas the second is a 20 nm thin palladium (Pd) film. This structure was formed in one of the dual delay line systems on a LiNbO3 Y-cut Z-propagation substrate, while the other serves as a reference, permitting an easy detection of the arising differential frequency ?f. This frequency, depending on the operating frequency modes, is in range of 20 to 30 kHz, whereas he oscillator frequencies are in the range of 43.6MHz. The wavelenghts is 80um. In such a bilayer structure detection of hdrogen in a medium concentration range (from 1% to 4% in nitrogen) is possible, even at room temperature. For the investigated structure the interaction response depends on temperature. For the structure an interesting "interaction jump" has beeen detected, which is connected wht the phase trasition in the palladium film. At hidher temeperatures thisinteraction jump shifts in the direction of higher hydrogen concentrations.

14

Surface Acousic Wave Sensor for Hydrogen Detection with a Two-Layered Structure

Jakubik W., Urbańczyk M., Kochowski S., Nadolski M.

Molecular and Quantum Acoustics

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2001

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Vol. 22

123-131

EN

Result concerning a hydrogen sensor based on a two-layer structure in a Surface Acousic Wave dual-delay line sustem are presented. The sensor material consist of two layeds performed in two different vapor deposition processes. The first one is a 720nm CuPc (or 110nm H2Pc) layer, the other one - a 20 nm thin palladium film. This structure was formed in a one of the dual-delay line system on a LiNbO3 Y-cut Z-propagation substrate. In such a multilayer structure can detect hydrogen in a medium concentration range (from 0.25% to 3% in nitrogen), even at room temperature. The sensor has a very good sensitivity, stability and is entirely reversible. The responce and recovery times are very short (-200s 0 800s), which is very important from the practical point fo view.

15

Optical and Resistance Sensors for Hydrogen Detection in Gas Mixture and Transformer Oil

Bodzenta J., Burak B., Jakubik W., Kochowski S., Urbańczyk M.

Molecular and Quantum Acoustics

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2001

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Vol. 22

29-36

EN

Results of the investigation of thin Pd layers as hydrogen sensors are presented. Two types of sensors are examined - resistance and optical sensors. Changes in measured signal as a function of hyfrogen concentration in hydrogen-nitrogen mixture are registered. The sensor is exposed either directly to the gas mixture or to the transformer oil, through wich the gas mixture passes. The hydrogen concentration in the mixture changes from 0.5% to 4%. Investigated sensors are sensituve enough in this concentration range, in both media. Changes of Pd film properties caused by hydrogen absorption are reversible except a few first exposures to the mixture. Obtained results confirm the possibility of developing simple sensor for detection of hydrogen gas in dissolved in the transformer oil.