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1

Influence of modulation frequency on the synthesis of thin films in pulsed magnetron sputtering processes

Strzelecki G. W., Nowakowska-Langier K., Chodun R., Okrasa S., Wicher B., Zdunek K.

Materials Science Poland

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2018

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Vol. 36, No. 4

697--703

EN

The research on the influence of modulation frequency on the properties of films synthesized using a unique pulsed power supply combined with a standard unbalanced circular magnetron was conducted in the process of pulsed magnetron sputtering (PMS). It was shown that by using different levels of modulation, the composition of plasma (measured by optical emission spectroscopy, OES) as well as film growth rate and morphology (observed with scanning electron microscope, SEM), can be changed. The impact of modulation is related to the used materials and gases and can vary significantly. It was concluded that modulation frequency can greatly influence the synthesis of materials and can be used as an additional parameter in PMS. Specific relations between modulation frequency and synthesized material require further investigation.

2

Structure and Electrical Resistivity Dependence of Molybdenum Thin Films Deposited by DC Modulated Pulsed Magnetron Sputtering

Wicher B., Chodun R., Nowakowska-Langier K., Okrasa S., Król K., Minikayev R., Strzelecki G., Zdunek K.

Archives of Metallurgy and Materials

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2018

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Vol. 63, iss. 3

1339--1344

EN

This work reports the results of a study of Mo thin films synthesis by DC Pulsed Magnetron Sputtering method (PMS), operating at pulse main frequency of 100 kHz and modulated by the additional modulation frequency, driving in the range of 5-1000 Hz (modulated Pulse Magnetron Sputtering – mPMS). We have studied the influence of mPMS on plasma chemical reactions and mechanisms of layer growth using optical emission spectroscopy technique. Our experiment showed strong influence of mPMS method, on the morphology (scanning electron microscopy), phase composition (X-ray diffractometry) and electric properties (4-point probes method) of nanocrystalline and amorphous Mo films. From the utilitarian point of view, low value of resistivity – 43,2 μΩcm of synthesized Mo films predestines them as back contacts for thin solar cells CIGS. Our results revealed that additional modulation frequency should be considered as an important factor for optimization of films synthesis by means of PMS-based methods.

3

Multi-sided metallization of textile fibres by using magnetron system with grounded cathode

Chodun R., Wicher B., Skowroński Ł., Nowakowska-Langier K., Okrasa S., Grabowski A., Minikayev R., Zdunek K.

Materials Science Poland

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2017

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Vol. 35, No. 3

639--646

EN

The synthesis of coatings on textiles fibers enables functionalization of their properties e.g.: changing the reaction on IR radiation. In our experiment, a magnetron with a grounded cathode and positively biased anode was used as a source of plasma. A ring anode was positioned at 8 cm distance from the cathode. Samples of glass and cotton textile were placed at the plane of the anode. Ti and TiN coatings were deposited by sputtering of titanium target in Ar or Ar+ N2 atmosphere. SEM studies showed that, using the magnetron system described above, the textile fibers were covered by the 2 μm to 3 μm thick coatings. Unexpectedly, the coatings were deposited at both sides of the samples: the front side was exposed to glow discharge plasma and the backside was completely shaded from the plasma. IR optical investigation exhibited significant change in reflectance and transmittance of the coated textiles. The using of standard magnetron system (grounded anode and cathode at negative potential) resulted in a coating deposition at the textile side exposed to the plasma action only. We believe that the multi-sided deposition of coatings observed during the process run with magnetron with grounded cathode is a result of an ambipolar diffusion mechanism in the anodic potential drop region.

4

The role of magnetic energy on plasma localization during the glow discharge under reduced pressure

Chodun R., Nowakowska-Langier K., Zdunek K., Okrasa S.

Nukleonika

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2016

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Vol. 61, No. 2

191--194

EN

In this work, we present the first results of our research on the synergy of fields, electric and magnetic, in the initiation and development of glow discharge under reduced pressure. In the two-electrode system under reduced pressure, the breakdown voltage characterizes a minimum energy input of the electric field to initiate and sustain the glow discharge. The glow discharge enhanced by the magnetic field applied just above the surface of the cathode influences the breakdown voltage decreasing its value. The idea of the experiment was to verify whether the contribution of potential energy of the magnetic field applied around the cathode is sufficiently effective to locate the plasma of glow discharge to the grounded cathode, which, in fact, is the part of a vacuum chamber wall (the anode is positively biased in this case). In our studies, we used the grounded magnetron unit with positively biased anode in order to achieve favorable conditions for the deposition of thin films on fibrous substrates such as fabrics for metallization, assuming that locally applied magnetic field can effectively locate plasma. The results of our studies (Paschen curve with the participation of the magnetic field) seem to confirm the validity of the research assumption. What is the most spectacular – the glow discharge was initiated between introduced into the chamber anode and the grounded cathode of magnetron ‘assisted’ by the magnetic field (discharge did not include the area of the anode, which is a part of the magnetron construction).

5

Research on interactions of plasma streams with CFC targets in the Rod Plasma Injector facility

Zaloga D. R., Kwiatkowski R., Skladnik-Sadowska E., Sadowski M. J., Nowakowska-Langier K.

Nukleonika

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2016

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Vol. 61, No. 2

179--183

EN

This paper present results of optical spectroscopy studies of interactions of intense plasma streams with a solid target made of carbon fibre composite (CFC). The experiments were carried out within the Rod Plasma Injector (RPI) IBIS facility. The optical measurements were performed first for a freely propagating plasma stream in order to determine the optimal operational parameters of this facility. Optical emission spectra (OES) were recorded for different operational modes of the RPI IBIS device, and spectral lines were identified originating from the working gas (deuterium) as well as some lines from the electrode material (molybdenum). Subsequently, optical measurements of plasma interacting with the CFC target were performed. In the optical spectra recorded with the irradiated CFC samples, in addition to deuterium and molybdenum lines, many carbon lines, which enabled to estimate erosion of the investigated targets, were recorded. In order to study changes in the irradiated CFC samples, their surfaces were analysed (before and after several plasma discharges) by means of scanning electron microscope (SEM) and energy dispersive spectroscopy (EDS) techniques. The analysis of the obtained SEM images showed that the plasma irradiation induces noticeable changes in the surface morphology, for example vaporisation of some carbon fi bres and formation of microcracks. The obtained EDS images showed that upon the irradiated target surface, some impurity ions are also deposited, particularly molybdenum ions from the applied electrodes.

6

Titanium nitride coatings synthesized by IPD method with eliminated current oscillations

Chodun R., Nowakowska-Langier K., Zdunek K.

Materials Science Poland

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2016

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Vol. 34, No. 3

523--528

EN

This paper presents the effects of elimination of current oscillations within the coaxial plasma accelerator during IPD deposition process on the morphology, phase structure and properties of synthesized TiN coatings. Current observations of waveforms have been made by use of an oscilloscope. As a test material for experiments, titanium nitride TiN coatings synthesized on silicon and high-speed steel substrates were used. The coatings morphology, phase composition and wear resistance properties were determined. The character of current waveforms in the plasma accelerator electric circuit plays a crucial role during the coatings synthesis process. Elimination of the current oscillations leads to obtaining an ultrafine grained structure of titanium nitride coatings and to disappearance of the tendency to structure columnarization. The coatings obtained during processes of a non-oscillating character are distinguished by better wear-resistance properties.

7

The application of magnetic self-filter to optimization of AIN film growth process during the impulse plasma deposition synthesis

Chodun R., Nowakowska-Langier K., Okrasa S., Zdunek K.

Materials Science Poland

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2016

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Vol. 34, No. 1

126--131

EN

This work presents the very first results of the application of plasma magnetic filtering achieved by a coil coupled with an electrical circuit of a coaxial accelerator during the synthesis of AlN thin films by use of Impulse Plasma Deposition method (IPD). The uniqueness of this technical solution lies in the fact that the filter is not supplied, controlled and synchronized from any external device. Our solution uses the energy from the electrical circuit of plasma accelerator. The plasma state was described on the basis of OES studies. Estimation of the effects of plasma filtering on the film quality was carried out on the basis of characterization of structure morphology (SEM), phase and chemical composition (vibrational spectroscopy). Our work has shown that the use of the developed magnetic self-filter improved the structure of the AlN coatings synthesized under the condition of impulse plasma, especially by the minimization of the tendency to deposit metallic aluminum droplets and columnar growth.

8

Novel GIMS technique for deposition of colored Ti/TiO2 coatings on industrial scale

Zdunek K., Skowronski L., Chodun R., Nowakowska-Langier K., Grabowski A., Wachowiak W., Okrasa S., Wachowiak A., Strauss O., Wronkowski A., Domanowski P.

Materials Science Poland

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2016

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Vol. 34, No. 1

137--141

EN

The aim of the present paper has been to verify the effectiveness and usefulness of a novel deposition process named GIMS (Gas Injection Magnetron Sputtering) used for the first time for deposition of Ti/TiO2 coatings on large area glass substrates covered in the condition of industrial scale production. The Ti/TiO2 coatings were deposited in an industrial system utilizing a set of linear magnetrons with the length of 2400 mm each for covering the 2000 x 3000 mm glasses. Taking into account the specific course of the GIMS (multipoint gas injection along the magnetron length) and the scale of the industrial facility, the optical coating uniformity was the most important goal to check. The experiments on Ti/TiO2 coatings deposited by the use of GIMS were conducted on substrates in the form of glass plates located at the key points along the magnetrons and intentionally non-heated during any stage of the process. Measurements of the coatings properties showed that the thickness and optical uniformity of the 150 nm thick coatings deposited by GIMS in the industrial facility (the thickness differences on the large plates with 2000 mm width did not exceed 20 nm) is fully acceptable form the point of view of expected applications e.g. for architectural glazing.

9

Synthesis of multicomponent metallic layers during impulse plasma deposition

Nowakowska-Langier K., Chodun R., Zdunek K.

Materials Science Poland

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2015

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Vol. 33, No. 4

841--846

EN

Pulsed plasma in the impulse plasma deposition (IPD) synthesis is generated in a coaxial accelerator by strong periodic electrical pulses, and it is distributed in a form of energetic plasma packets. A nearly complete ionization of gas, in these conditions of plasma generation, favors the nucleation of new phase of ions and synthesis of metastable materials in a form of coatings which are characterized by amorphous and/or nanocrystalline structure. In this work, the Fe-Cu alloy, which is immiscible in the state of equilibrium, was selected as a model system to study the possibility of formation of a non-equilibrium phase during the IPD synthesis. Structural characterization of the layers was done by means of X-ray diffraction and conversion-electron Mossbauer spectroscopy. It was found that supersaturated solid solutions were created as a result of mixing and/or alloying effects between the layer components delivered to the substrate independently and separately in time. Therefore, the solubility in the Fe-Cu system was largely extended in relation to the equilibrium conditions, as described by the equilibrium phase diagram in the solid state.

10

Structure of AlN films deposited by magnetron sputtering method

Nowakowska-Langier K., Chodun R., Zdunek K., Minikayev R., Nietubyć R.

Materials Science Poland

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2015

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Vol. 33, No. 3

639--643

EN

AlN films on a Si substrate were synthesized by magnetron sputtering method. A dual magnetron system operating in AC mode was used in the experiment. Processes of synthesis were carried out in the atmosphere of a mixture of Ar/N2. Morphology and phase structure of the AlN films were investigated at different pressures. Structural characterizations were performed by means of SEM and X-ray diffraction methods. Our results show that the use of magnetron sputtering method in a dual magnetron sputtering system is an effective way to produce AlN layers which are characterized by a good adhesion to the silicon substrate. The morphology of the films is strongly dependent on the Ar/N2 gas mixture pressure. An increase of the mixture pressure is accompanied by a columnar growth of the layers. The films obtained at the pressure below 1 Pa are characterized by finer and compacter structure. The AlN films are characterized by a polycrystalline hexagonal (wurtzite) structure in which the crystallographic orientation depends on the gas mixture pressure.

11

Methods of optimization of reactive sputtering conditions of Al target during AlN films deposition

Chodun R., Nowakowska-Langier K., Zdunek K.

Materials Science Poland

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2015

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Vol. 33, No. 4

894--901

EN

Encouraged by recent studies and considering the well-documented problems occurring during AlN synthesis, we have chosen two diagnostic methods which would enable us to fully control the process of synthesis and characterize the synthesized aluminum nitride films. In our experiment we have compared the results coming from OES measurements of plasma and circulating power characteristics of the power supply with basic features of the deposited layers. The dual magnetron system operating in AC mode was used in our studies. Processes of aluminum target sputtering were carried out in an atmosphere of a mixture of argon and nitrogen. The plasma emission spectra were measured with the use of a monochromator device. Analyses were made by comparing the positions and intensities of spectral lines of the plasma components. The results obtained allowed us to characterize the sputtering process under various conditions of gas mixture compositions as well as power distribution more precisely, which is reported in this work. The measured spectra were related to the deposition rate, the structure morphology of the films and chemical composition. Our work proved that the use of plasma OES and circulating power measurements make possible to control the process of sputtering and synthesis of deposited films in situ.

12

Optimization of gas injection conditions during deposition of AlN layers by novel reactive GIMS method

Zdunek K., Nowakowska-Langier K., Chodun R., Dora J., Okrasa S, Talik E.

Materials Science Poland

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2014

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Vol. 32, No. 2

171—175

EN

In 2011, we proposed a novel magnetron sputtering method. It involved the use of pulsed injection of working gas for the initiation and control of gas discharge during reactive sputtering of an AlN layer (Gas Injection Magnetron Sputtering – GIMS). Unfortunately, the presence of Al–Al bonds was found in XPS spectra of the AlN layers deposited by GIMS onto Si substrate. Our studies reported in this paper proved that the synchronization of time duration of the pulses of both gas injection and applied voltage, resulted in the elimination of Al–Al bonds in the AlN layer material, which was confirmed by the XPS studies. In our opinion the most probable reason of Al–Al bonds in the AlN layers deposited by the GIMS was the self-sputtering of the Al target in the final stage of the pulsed discharge.

13

Zastosowanie metody IPD do syntezy warstw c-AlN

Chodun R., Nowakowska-Langier K., Okrasa S., Firek P., Szmidt J., Zdunek K.

Elektronika : konstrukcje, technologie, zastosowania

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2014

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Vol. 55, nr 10

11-13

PL

Azotek aluminium otrzymywany w postaci warstw wzbudza duże zainteresowanie ze względu na swoje właściwości dielektryczne. Typowym produktem syntezy warstw AlN metodami inżynierii powierzchni jest odmiana stabilna h-AlN. Ostatnio zwraca się uwagę na warstwy AlN syntetyzowane w odmianie kubicznej. W artykule opisane zostały badania dotyczące wykorzystania metody IPD do wytwarzania cienkich warstw azotku. Metodą tą uprzednio syntetyzowane były takie materiały, jak: DLC, czy e-BN. Na podstawie badań XRD oraz spektroskopii ramanowskiej warstw AlN wytwarzanych w pracy metodą IPD wykazano, że produktem syntezy jest odmiana kubiczna azotku.

EN

Recently, aluminum nitride (AlN) has attracted much attention due to its electric properties. Typically the AlN that is obtained by using the plasma surface engineering method crystallizes in stable, hexagonal structure. However, it can also be grown in cubic structure. The article describes the research concerning the use of the IPD method to synthesis of thin nitride layers. This method was previously used to synthesis of layers materials such as DLC or e-BN. On the basis of the X-ray diffraction and Raman spectroscopy of the AlN layers produced by the IPD method we demonstrated that, a cubic AlN was synthesized.

14

Optical emission spectroscopy of plasma produced from tungsten target irradiated within RPI - IBIS facility

Skladnik-Sadowska E., Malinowski K., Sadowski M. J., Nowakowska-Langier K., Ladygina M. S., Garkusha I. E.

Nukleonika

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2012

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Vol. 57, No. 2

193-196

EN

The paper presents recent research on characteristics of deuterium plasma streams generated within an RPI-IBIS (multi-rod plasma injector) facility, and optical spectra of plasma produced during the interaction of these streams with a tungsten target placed at a distance of 20 cm from the electrode outlets. Distinct WI- and WII-lines were recorded and the noticeable erosion of the W-target was observed for shots delivering more than 4 J/cm2 on the target surface.

15

Struktura i właściwości elektroniczne warstw AIN wytwarzanych w reaktywnym procesie rozpylania magnetronowego

Nowakowska-Langier K., Chodun R., Firek P., Waśkiewicz M., Zdunek K., Szmidt J.

Elektronika : konstrukcje, technologie, zastosowania

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2011

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Vol. 52, nr 11

43-45

PL

W artykule przedstawione zostaly wyniki badań dotyczące struktury i właściwości elektronicznych warstw AIN otrzymywanych w procesie pulsacyjnego reaktywnego rozpylania magnetronowego. Przeprowadzone badania pokazały, że zastosowanie metody rozpylania magnetronowego w układzie "gemini" jest skutecznym sposobem wytworzenia w temperaturze otoczenia (RT) cienkich, transparentnych warstw AIN odznaczających się wystarczającą adhezją do podloży krzemowych. Otrzymywane przez nas warstwy azotku glinu, wzrastające w kierunku <002> odznaczały się nanokrystaliczną strukturą heksagonalnego AIN o parametrze sieci zgodnym z danymi literaturowymi, wartością energetycznej przerwy wzbronionej ok. 5 ... 6 eV oraz wartością napięcia przebicia ok. 3,5...4,4 MV/cm. Z badań autorów wynika, że szczególnie korzystnym zespołem cech strukturalnych oraz właściwości elektronicznych odznaczały się warstwy wytwarzane przy ciśnieniu mieszaniny gazów Ar+N₂, w zakresie 1 ... 2 Pa. Warstwy takie wydają się szczególnie predestynowane do wykorzystania, jako dielektryk bramkowy w strukturze tranzystorów MISFET.

EN

In the present paper we show the results of our investigation concerning a structure and the electrical properties of the AIN layers produced by the non-reactive magnetron sputtering process. Our results show that application of magnetron sputtering in "Gemini" mode allows for effective and room-temperature (RT) deposition on thin, transparent AIN films with good adhesion to Si substrates. Obtained films, growing in <002> crystallographic orientation have nanocrystalline structure of hexagonal AIN with crystallographic parameters staying in agreement with data published so far, the dielectric constant value (εri) equal from 5 to 6.5 and and critical electric field intensity (ΕBR) from 3.6 to 4.4 MV cm⁻¹. The results show that the promising morphology, phase composition and good electrical properties have the films deposited in Ar/N₂, pressure range from 1 to 2 Pa. It makes those deposited material suitable for application in novel microelectronic devices like MISFET transistor.

16

Materiałowe skutki zastosowania zaworu impulsowego w urządzeniu IPD

Zdunek K., Nowakowska-Langier K., Chodun R., Dora J.

Elektronika : konstrukcje, technologie, zastosowania

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2009

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Vol. 50, nr 9

40-42

PL

W pracy zaprezentowane zostały pierwsze wyniki obserwacji skutków materiałowych zastosowania zaworu impulsowego dozującego gaz do koaksjalnego akceleratora plazmy impulsowej w metodzie IPD. Wynika z nich, że produktem syntezy jest materiał warstwy zbudowany z nanokrystalicznych graniastych ziarn, co sugeruje heterogeniczny mechanizm zarodkowania.

EN

In the paper were described the very first observations of the material effects of the impulse valve using for gas injection to the coaxial accelerator during the impulse plasma deposition. Coatings deposited in such conditions were nanocrystalline with grains morphology characteristic for coatings nucleated heterogenically on the substrate surface.

17

‘Plasma alloying’ during impulse plasma deposition of Fe-Ti alloy layers

Nowakowska-Langier K., Wierzbiński E., Zdunek K.

Polish Journal of Applied Chemistry

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2005

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Vol. 49, nr 4

291-295

EN

This paper presents a study of synthesis of Fe-Ti alloy layers under conditions of impulse mass and energy transport. The Impulse Plasma Deposition method (IPD) was used. The synthesis processes were conducted in a device equipped with two independent and alternately working accelerators of impulse plasma. The layer morphology using the Scanning Electron Microscopy (SEM) and the Atomic Force Microscopy in a Tapping Mode (TM AFM) techniques was investigated. The results proved the mechanism of a layer growth which proceeds by the local diffusion of clusters and their anisotropic incomplete coalescence.

18

Subtelne efekty strukturalne w warstwach wytwarzanych metodą impulsowo-plazmową (IPD)

Nowakowska-Langier K., Zdunek K.

Elektronika : konstrukcje, technologie, zastosowania

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2005

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Vol. 46, nr 6

13-14

PL

Opisane zostały wyniki badań subtelnej struktury warstw stopowych Fe-Ti, otrzymywanych metodą IPD z wykorzystaniem dwóch niezależnie i niewspółbieżnie pracujących koaksjalnych akceleratorów plazmy impulsowej. W ramach badań materiałowych obserwowana była morfologia strukturalna warstw oraz określana zależność magnetooporu od wartości i kierunku zewnętrznego pola magnetycznego. Ustalono, że morfologia warstw zależy od sposobu rozmieszczenia podłoży względem strumienia plazmy impulsowej oraz, że w przypadku niektórych wariantów technologicznych wytwarzania warstw otrzymuje się niesymetryczne charakterystyki magnetooporu.

EN

Effects of examinations of the subtle structure of Fe-Ti layers produced by the IPD method were described in the paper. The layers were deposited by the use of two irrespective and alternatively working impulse plasma coaxial accelerators fitted with internal electrodes made from the iron and titanium. Structural morphology and the magnetoresistance effect of the layers were studied within the confines of material examinations. Results of these examinations showed that morphology of layers as well as the unsymmetrical of magnetoresistance characteristics are depended on the position of layer substrates in comparison to the direction of impulse plasma distribution. The results confirmed our previous observations about the influence of potential fields connected with the impulse plasma itself on subtle structure of the layer material synthesized by the IPD method.

19

Kondensacja warstwy w warunkach impulsowego dostarczania masy i energii

Nowakowska-Langier K., Wierzbiński E., Zdunek K., Kopcewicz M.

Elektronika : konstrukcje, technologie, zastosowania

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2003

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Vol. 44, nr 11

35-36

PL

W artykule opisane zostały badania nad syntezą warstw w warunkach impulsowego dostarczania masy i energii. Do tego celu została wykorzystana metoda IPD. Procesy syntezy prowadzone byty w urządzeniu wyposażonym w dwa niezależnie i niewspółbieżnie (naprzemiennie) pracujące akceleratory plazmy impulsowej. Źródłem żelaza i tytanu byty wewnętrzne elektrody akceleratorów. Gazem plazmotwórczym byt argon. Warstwy nanoszone byty na podłoża krzemowe. Materiałem syntetyzowanym w prezentowanym eksperymencie byt stop Fe-Ti.

EN

This paper presents a study of synthesis layers in conditions of impulse mass and energy transport. In this case we used Impulse Plasma Deposition method (IPD). The synthesis processes were conducted in a device equipped with two independent and alternately working accelerators of impulse plasma. The sources of Fe and Ti were the internal electrodes of these impulse plasma accelerators, made of titanium and iron. The plasma-generating gas was argon. The layers were deposited on silicon substrates. The material synthesized in the present experiment was an Fe-Ti alloy.