Katarzyna Nowakowska-Langier

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

Abstract 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 flrst 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 × 3000 mm glasses. Taking into account the speciflc 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.

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

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.

On coating adhesion during impulse plasma deposition

The impulse plasma deposition (IPD) technique is the only method of plasma surface engineering (among plasma-based technologies) that allows a synthesis of layers upon a cold unheated substrate and which ensures a good adhesion. This paper presents a study of plasma impacts upon a copper substrate surface during the IPD process. The substrate was exposed to pulsed N2/Al plasma streams during the synthesis of AlN layers. For plasma–material interaction diagnostics, the optical emission spectroscopy method was used. Our results show that interactions of plasma lead to sputtering of the substrate material. It seems that the obtained adhesion of the layers is the result of a complex surface mechanism combined with the effects of pulsed plasma energy impacts upon the unheated substrate. An example of such a result is the value of the critical load for the Al2O3 layer, which was measured by the scratch-test method to be above 40 N.

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

Abstract 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).

Synthesis of multicomponent metallic layers during impulse plasma deposition

Abstract 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 Mössbauer 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.

Computational modelling of discharges within the impulse plasma deposition accelerator with a gas valve

The paper presents computational studies of working medium dynamics during the impulse plasma deposition (IPD) process when the electric discharge in an interelectrode region is initiated by a gas introduced through a fast-acting valve. During the computational simulations the influence of different discharge parameters on the plasma dynamics was studied. The optimization of the device includes the calculation of the current sheath movement and the sensibility analysis of its dynamics to geometrical and operational parameters. It was found that gas injection can be considered as a useful tool in optimization of the coatings obtained with the IPD technique. Computer simulation results indicate the direction of changes in the development and application of the analysed surface engineering method.

Titanium nitride coatings synthesized by IPD method with eliminated current oscillations

Abstract 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.

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

Abstract 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.

Characterization of sp 3 bond content of carbon films deposited by high power gas injection magnetron sputtering method by UV and VIS Raman spectroscopy

This paper presents the results of investigations of carbon films deposited by a modified version of the magnetron sputtering method - HiPGIMS (High Power Gas Injection Magnetron Sputtering). In this experiment, the magnetron system with inversely polarized electrodes (sputtered cathode at ground potential and positively biased, spatially separated anode) was used. This arrangement allowed us to conduct the experiment using voltages ranging from 1 to 2kV and a power supply system equipped with 25/50μF capacitor battery. Carbon films were investigated by VIS/UV Raman spectroscopy. Sp3/sp2 bonding ratio was evaluated basing the elementary components of registered spectra. Our investigation showed that sp3 bond content increases with discharge power but up to specific value only. In extreme conditions of generating plasma impulses, we detected a reversed relation of the sp3/sp2 ratio. In our opinion, a energy of plasma pulse favors nucleation of a sp3 phase because of a relatively higher ionization state but in extreme cases the influence of energy is reversed.

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

Abstract 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.