The paper presents investigation results of properties of the sintered tool materials: cemented carbides, cermets and Al2O3 type oxide tool ceramics with gradient (Ti,Al)N and Ti(C,N) coatings deposited with the cathodic arc evaporation CAE-PVD method.
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The article presents a model technical solution for modular vacuum chamber and a technological instrumentation for different experimental performance of PVD (Physical Vapour Deposition) coating processes with use of thin surface layers. A structure of the research stand is presented with main construction elements. Reconfiguration of the effector and control modules allows performing a research and development of introducing novelty technologies for physical deposition of coating from the gas phase. All those configuration possibilities allow performing the technological processes with use of arc and magentron sources. A developed chamber structure includes different connection ports and allows performing an analysis of the pyrometric measurement of temperatures processes and spectral analysis of the deposited layers in situ composition. The chamber uses novelty solution for protection of the AEGD (Arc-Enhanced Glow Discharge) electrode against harmful deposition of the products of PVD. A similar solution is used to protect materials against evaporation and impurities among substances in the plasma stream.
Vitreous floaters are one of the most common complain of ophthalmological patients. The aetiology of floaters includes pathological process (vitreous haemorrhages, injuries, diabetics or uveitis) and also natural age-related changes in vitreous body. Diagnosis and treatment depends on the severity of the symptoms. Process of posterior vitreous detachment requires particularly careful monitoring, because of potential complications such as retinal tears or retinal detachment. Supplementation with anti-glycation and antioxidant substances allows to reduce complains of patients with vitreous floaters.
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In this study, palladium-modified nickel foam substrate was applied to examine ethanol oxidation reaction (EOR) in 0.1 M NaOH supporting solution. An EOR catalyst was prepared by physical vapour deposition (PVD) of palladium onto Ni foam material. Temperature-dependent kinetics of the EOR were studied over the temperature range: 20-60°C by means of a.c. impedance spectroscopy and cyclic voltammetry techniques. Deposition of a noble metal additive was clearly exposed through scanning electron microscopy: SEM/EDX-supported analysis. Most importantly, this work investigated the effect of pre-deposited fullerene on nickel foam, on the catalytic (EOR) properties of such-produced Ni foam/Pd composite material.
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Carbon nanotubes films have been studied with SEM and TEM. The studied films were obtained using a two step method: PVD process and CVD process. Strongly defected and curled carbon nanotubes containing Ni nanoparticles formed the film with thickness of about 300–400 nm. Observed carbon nanotubes were of lengths from 100 nm to 300 nm and did not stick to each other.
W pracy przedstawiono wyniki badań powłok Ti-Si-C wytworzonych na podłożu stalowym (AISI 316L) metodą dwuwiązkową IBAD. Proces prowadzono w próżni, stosując węglik tytanowo-krzemowy Ti3SiC2 jako substancję rozpylaną (target), bombardowaną wiązką jonów Ar+ o energii 15 keV. Charakterystyki otrzymanych powłok dokonano za pomocą rentgenowskiej analizy dyfrakcyjnej (XRD), konfokalnej dyspersyjnej mikrospektroskopii ramanowskiej, metod mikroskopii elektronowej skaningowej i transmisyjnej (SEM, EDS, TEM). Na podstawie przeprowadzonych badań stwierdzono, że zastosowane parametry procesu IBAD pozwoliły uformować jednorodne, ciągłe powłoki o grubości poniżej 0,9 um. Stwierdzono wielofazową budowę powłok składających się z amorficznej osnowy (o stosunku zawartości 70% mas. Si/ 30% mas. Ti) oraz wydzieleń faz: Ti5Si3, Si2Ti oraz Ti6C3,75. Widma ramanowskie zarejestrowane dla uformowanych powłok w trybie wysokiej zdolności rozdzielczej (HR) wskazały na piki opisane funkcją typu Gauss-Lorentza, odpowiadające liczbom falowym 152 cm-1, (159 cm-1), 216 cm-1, (226 cm-1), 278 cm-1, (279 cm-1), 311 cm-1, (301 cm-1), 378 cm-1, (379 cm-1), 608 cm-1, 625 cm-1, 691 cm-1, (675 cm-1), odpowiadającym liczbom falowym rejestrowanym dla Ti3SiC2. Twardość HIT (od 2,7 GPa do 5,3 GPa) oraz zredukowany moduł Younga EIT (160 GPa), wyznaczone zostały metodą Oliver & Pharr'a na podstawie pomiaru nanotwardości pokrytych podłoży.
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Ti-Si-C coatings were formed at room temperature on AISI 316L steel substrates by dual beam ion assisted deposition technique from single compound Ti3SiC2 target. Scanning and transmission electron microcopy method were used to examine as-deposited coatings. Their morphology was smooth and dense and their thickness was in the range from 100 nm up to 1 ?m. Raman spectra of coated substrates were collected up with five peaks at 152 cm-1, (159 cm-1), 216 cm-1, (226 cm-1), 278 cm-1, (279 cm-1), 311 cm-1, (301 cm-1), 378 cm-1, (379 cm-1), 608 cm-1, 625 cm-1, 691 cm-1, (675 cm-1), the same positions as for Ti3SiC2 compound target. TEM and HRTEM examinations, accompanied by SAED analyses revealed that deposited films were amorphous. Nanoindentation tests were provided on coated and uncoated substrates and hardness HIT and reduced elastic modulus EIT were calculated using the Oliver & Pharr method.
Praca przedstawia nową, 2-stopniową metodę (PVD/CVD) wytwarzania nanoporowatych warstw węglowo-palladowych opracowaną w Instytucie Tele- i Radiotechnicznym oraz wpływ różnych parametrów procesu wytwarzania na strukturę uzyskanego materiału. Przedstawiono wyniki elektronomikroskopowych badań (SEM, TEM) powstałych w różnych warunkach termodynamicznych i na różnych podłożach nanoporowatych warstw zawierających węgiel i pallad. Badania pokazały, że stopień rozwinięcia powierzchni materiału porowatego silnie zależy od takich czynników jak wielkość i rozkład nanokrystalitów Pd w warstwie wyjściowej, otrzymanej metodą PVD oraz od temperatury i szybkości przepływu argonu w procesie CVD.
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This article we present new, 2-steps PVD/CVD technological method of nanoporous C-Pd film preparation. Method developed in Tele & Radio Research Institute allows for obtaining of films with various structures. SEM and TEM studies of nanoporous films prepared in different thermodynamical and chemical conditions on different substrates are presented. Our studies show, that materials nanoporosity depend such factors as: size and distribution of Pd nanocrystals in PVD films, temperature and rate of Arflow in CVD process.
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Purpose: Investigation of the Al2O3+TiC type oxide tool ceramics and cemented carbides with the multicomponent (Ti, Al)N and gradient Ti(C, N) coatings deposited with use of the cathodic arc evaporation CAE-PVD method. Design/methodology/approach: SEM, confocal microscopy, X-ray qualitative microanalysis of elements, X-ray qualitative phase analysis. Findings: It was stated that investigated materials have a dense, compact structure and their fracture surface topography attests their high brittleness, characteristic especially for the oxide ceramic materials. The coatings were put down uniformly onto the investigated substrate materials. They have a columnar, fine-graded structure. Practical implications: Pro-ecological dry cutting processes without the use of the cutting fluids and in the "Near-Net-Shape" technology. Originality/value: Application of multicomponent (Ti, Al)N and gradient Ti(C, N) types of coatings onto sintered tool materials in order to improve cutting properties of the tools.
W pracy przedstawiono wyniki badań struktury, własności mechanicznych oraz odporności korozyjnej nanokrystalicznych i nanokompozytowych powłok naniesionych w procesie PVD na podłoże ze stali narzędziowej do pracy na gorąco X40CrMoV5-1. Badania wykonano na powłokach TiAI- SiN, CrAlSiN oraz AlTiCrN. Stwierdzono, że struktura powłok złożona jest z drobnych krystalitów, a ich średnia wielkość wynosi 9 ... 25 nm w zależności od rodzaju powłoki. Badane powłoki wykazują strukturę kolumnową, jak również dobrą przyczepność do podłoża, wysoką twardość (>4000 HV) oraz odporność korozyjną.
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This paper presents the research results on the structure, mechanical properties and corrosion resistance of nanocrystalline and nanocomposite coatings deposited by PVD process on the X40CrMoV5-1 hot work tool steel substrates. The tests were carried out on TiAlSiN, CrAlSiN and AlTiCrN coatings. It was found that the structure of the PVD coatings consisted of line crystallites, while their average size fitted within the ranga of 9 ... 25 nm, depending on the coating type. The coatings demonstrated columnar structure as well as good adhesion to the substrate, a high hardness (>4000 HV) and corrosion resistance.
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W artykule przedstawiono chemiczne i fizyczne metody modyfikowania warstwy wierzchniej materiałów polimerowych, mające na celu przygotowanie ich powierzchni do metalizowania. Opisano także metodę chemicznego metalizowania bezprądowego, metalizowanie bezpośrednie oraz fizyczne (PVD) i chemiczne (CVD) metody osadzania warstwy metalu na powierzchni tworzyw polimerowych.
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Chemical and physical methods of modification of the surface layer of polymeric materials used in process of metallization are reported. Electroless plating, direct metallization, physical vapour deposition (PVD) and chemical vapour deposition (CVD) are discussed.
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Purpose: The X-Ray Photoelectron Spectrometry (XPS) and Auger Electrons Spectroscopy (AES) analysis of PVD coatings were performed for samples, made from cemented carbides, cermets and composite gradient tool materials. Design/methodology/approach: The Ti(C,N) gradient coating was investigated by XPS and AES method with multifunctional PHI 5700/660 spectrometer. The characteristic of surface region coating were determined from XPS depth profile. The transition region between Ti(C,N) coating and substrate was analyzed by AES method as line profile. Findings: The coating consists mainly of TiC and TiN compound. The oxygen impurities of investigated coating is below 2%. The "fresh" surface of Ti(C,N) coating is covered by thin films TiO₂. There was observed homogeneous distribution of carbon, titanium and nitrogen elements in the surface region. The ratio of C/N obtained for surface region is characteristic for deposited coating. The transition region is also homogeneous between coating and cermet substrate. Practical implications: PVD deposition techniques making it possible to obtain surface layers with the varying thickness values, respectively, with the structure changing across the layer depth along with the change of its chemical or phase compositions for improvement of its properties, and especially for the advantageous combination of the very high abrasion wear resistance of the surface along with the relatively high ductility of the core of materials used for, respectively, blanking tools and for hot working, profile cutting tools with ductility high enough and for the heavy duty very high speed cutting tools. Originality/value: Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS) are an excellent tools for performing surface analysis and for determining elemental composition as a function of depth. AES or XPS analyzes the residual surface left after a certain sputtering time with rare gas ions. In this way composition depth profiles can be obtained that provide a powerful means for analyzing worked layers, modified layers, thin films, multiple-layered coatings, lubricants, reaction film products, transferred films, and their interfaces.
W pracy przedstawiono wyniki badań struktury i właściwości mechanicznych dwuwarstwowych powłok hybrydowych (gradientowa/wieloskładnikowa) naniesionych techniką PVD (odparowanie łukiem elektrycznym) na podłoże ze stopów magnezu Mg-Al i aluminium Al-Si-Cu. Badania wykonano na powłokach typu TiCN/CrN, CrN/CrN. Strukturę wytworzonych powłok obserwowano za pomocą skaningowej mikroskopii elektronowej. Zmiany stężenia chemicznego składników powłok oceniono na podstawie badań w spektrometrze optycznym wyładowania jarzeniowego. Struktura powłok PVD jest złożona z drobnych krystalitów, a ich średnia wielkość zawiera się w przedziale 15÷20 nm w zależności od rodzaju powłoki. Badane powłoki wykazują zwartą budową, bez widocznych rozwarstwień i defektów, są równomiernie nałożone i szczelnie przylegają do podłoża. Morfologia przełomu powłok charakteryzuje się brakiem struktury kolumnowej. Obserwacje przełomów potwierdzają, że powłoka TiCN/CrN wykazuje budowę warstwową z wyraźnie zaznaczoną strefą przejścia pomiędzy powłoką gradientową TiCN a powłoką przeciwzużyciową CrN, uzyskiwanych w wyniku stosowania oddzielnych źródeł par metali.
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In this work there are presented the investigation results concerning microstructure and mechanical properties of bilayer coatings (gradient/multicompound) coated using the PVD method (electric arc evaporation) onto a magnesium Mg-Al and aluminium alloys Al-Si-Cu substrate. Investigations of the TiCN/CrN and CrN/CrN coating type were performed. The microstructure of the achieved layers was observed using scanning electron microscope. Change of the chemical composition was measured on the basis of the glow discharge optical emission spectrometer (GDOS). The structure of the PVD coatings is composed of small crystallites with the average size in the range between 15÷20 nm, depending on the coating type. The investigated coatings reveal a compact structure, without visible defoliations and defects, it is coated uniformly and tightly bound to the substrate. The fracture morphology is characterised with a lack of columnar structures. Investigations confirm also that the TiCN/CrN coating reveals a clearly visible transition zone between the gradient TiCN layer and the wear resistant CrN layer, achieved as a result of separately applied metal vapour sources.
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Purpose: Comprehensive structure and properties investigation results of the multilayer, multi-component, gradient PVD and CVD coatings developed on the Si3N4 nitride tool ceramics substrate are presented in the paper. Design/methodology/approach: The detailed results are presented of examinations carried out on the transmission and scanning electron microscopes, as well as of the mechanical properties and tribological tests of the investigated coatings. Findings: The research carried out proved that depositing the hard, anti wear, multilayer coatings based on the Al2O3 and TiN layers onto the Si3N4 nitride tool ceramics with the PVD method results in obtaining better functional properties like extension of the cutting tool life, than in case of the uncoated nitride ceramics or coated with the PVD coatings and some CVD ones. Research limitations/implications: Pro-ecological dry cutting processes without the use of the cutting fluids and in the "Near-Net-Shape" technology. Originality /value: In the paper the research coatings deposited in the PVD and CVD methods on sintered tool materials carried out in order to improve the tool cutting properties.
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Purpose: Investigation of structure and properties of the Al2O3 based Al2O3+ZrO2, Al2O3+TiC and Al2O3+SiC(w) type based oxide tool ceramics coated with the anti-wear mono- and multilayers of the TiN, TiAlN, TiN+TiAlSiN+TiN, TiN+multiAiAlSiN+TiN and TiN+TiAlSiN+AlSiTiN types in the cathode arc evaporation CAE-PVD and with the multilayers of the TiCN+TiN and TiN+Al2O3 types obtained in the chemical deposition from the gas phase CVD process. Design/methodology/approach: The investigations were carried out on the multi-point inserts made from the Al2O3+ZrO2, Al2O3+TiC, Al2O3+SiC(W) ceramics uncoated, coated in the PVD and CVD processes with thin coatings; observations of the investigated coatings' structures were carried out on the transverse fractures on the scanning electron microscope; the diffraction examinations and examinations of thin foils were made on the transmission electron microscope; the measurements of textures and phase composition were made; the macro-stress values were calculated; tribological tests were carried out on the "pin-on-disk" tester; the microhardness and adhesion tests of coatings were made; cutting ability of the investigated materials was determined basing on the technological continuous cutting tests. Findings: It has been demonstrated that the creation of the developed coatings by the use of the PVD and CVD methods on oxide ceramic tool materials causes the increase of coatings hardness and allows to improve application features of multi point cutting tools for high speed machining, tools for fine cutting coated with them and dry cutting without using the cutting fluids in comparison to the multi point cutting tools produced from the same uncoated materials. Practical implications: Putting down the anti-wear coatings onto the oxide ceramic tool materials is justified and the composite tool materials developed in this way may have the important application significance in the industry for cutting tools. Originality/value: Comparison of the wide range of modern oxide tool ceramics with wide unique set of PVD and CVD coatings.
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Nanostrukturalne/porowate warstwy węglowo-palladowe (C-Pd) wykazują właściwości świadczące o możliwości zastosowania ich w czujnikach wodoru i/lub związków wodoru. Warstwy C-Pd otrzymuje się w ITR metodą dwuetapową stosując proces fizycznego naparowania w próżni (PVD – I etap) a następnie modyfikując warstwę z I etapu w procesie chemicznego osadzania z par ksylenu (CVD - II etap). W pracy przedstawiamy wyniki badań zmian przewodnictwa elektrycznego nanostrukturalnych warstw C-Pd o różnej budowie (topografii i morfologii) zachodzące pod wpływem mieszanki gazowej zawierającej węglowodory CxHX o różnej koncentracji.
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Nanostructural/porous carbonaceous – palladium (C-Pd) films can be applied as active layers in hydrogen and/or hydrogen compounds sensor applications. The C-Pd films were obtained in Radio&TeleResearch Institute in two stages method using physical vapor deposition process (PVD) as a first stage and chemical vapor deposition process (CVD) as a second one. In this paper we present results of studies of electrical conductivity changes in nanostructural C-Pd films with different topography and morphology due to mixture of gases containing hydrocarbons CxHx with different concentration.
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Purpose: The paper presents investigation results of structure and properties of steel matrix composites (SMC) uncoated and coated with hard (Ti,Al)N gradient coatings with use of physical vapour deposition process. Design/methodology/approach: Powder Metallurgy, PVD, TEM, SEM, XRD, GDOES, Microhardness tests, Scratch test. Findings: Depositing of gradient (Ti,Al)N coatings onto SMC materials meets the requirements connected with hybrid technology of production, joining powder metallurgy and physical vapour deposition techniques, in area of producing modern composite gradient tool materials. Sintered steel matrix composites reinforced with hard carbide phases and deposited with gradient PVD coatings can be widely employed in industry for tools, especially for machining and plastic forming processes. Practical implications: Tool materials used especially for tools employed especially in machining and plastic forming processes. Originality/value: Modern methods of powders’ forming application make possible to achieve gradient structure of tool, which is very advantageous in respect of mechanical properties. Employed compositions of technologies joining powder metallurgy and physical vapour deposition techniques give the possibility to achieve high properties characteristic of cemented carbides with the high ductility characteristic of steels.
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W pracy przedstawiono wyniki badań porównawczych wpływu warstwy powierzchniowej jednorodnej z TiN i CrN oraz o strukturze pasmowej TiN - stal 46Cr2 i CrN - stal 46Cr2 na próbce pierścieniowej na warunki tarcia w parze ciernej, w warunkach smarowania obszaru tarcia olejami silnikowymi Lotos Syntetyk 5W/40 i Castrol Magnatec 5W/40. W parze ciernej przeciwpróbka została wykonana ze stopu łożyskowego AlSn20. Badania przeprowadzono na testerze trybologicznym T-05. Wyniki badań potwierdziły możliwość zastosowania warstw powierzchniowych o strukturze pasmowej w parach ślizgowych, które pracują w warunkach tarcia mieszanego. Badania wykazały, że siła tarcia, temperatura w obszarze tarcia i zużycie materiału łożyskowego zależą od warunków tarcia i kompozycji współpracujących warstw powierzchniowych pary ciernej. Zaobserwowano korzystne parametry tarcia w parach ciernych z próbkami z warstwy powierzchniowej o strukturze pasmowej CrN - stal 46Cr2 i jednorodnej CrN.
EN
The study has determined influence of coatings (TiN, CrN) and surface layers with ring structure (TiN and 46Cr2 steel, CrN and 46Cr2 steel) on parameters of friction in sliding pairs. During the research ring samples worked with segment of bearing sleeve made of AlSn20 alloy. The kinematics pair lubricated motor oils lotos syntetyk 5W-40 and castrol magnatec 5W/40. The research performed on test machine T-05. Change of moment of friction was individual for investigated sliding. The researches showed that moment of friction had the lowest values for pairs with surface layer CrN. Values of friction forces of pair with surface layer TiN was the highest, by only during lubrication lotos oil. The researches showed that friction force and temperature of contact area and wear depended on load condition and structure of sliding. On base of experiences one ascertained influence formed surface layers on wear of bearing alloy. Cooperation surface layer CrN-46Cr2 steel and ion nitriding surface layer characterized least wear bearing alloys. Instead greatest wear registered for pairs with coating TiN. The researches showed profitable influence of motor oil castrol GTX magnatec 5W/40 in relation to oil lotus synthetic 5W/40 on decrease of wear of bearing alloy.
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Purpose: This paper presents investigation of gradient coating of (Ti,Al,Si)N deposited on the Al2O3+SiC(w) oxide ceramics substrate deposited with the PVD process. Design/methodology/approach: Structure of substrate and coating was investigated with use of scanning electron microscopy (SEM); The X-Ray Photoelectron Spectrometry (XPS) and Auger Electron Spectrometry (AES) examinations was carried out for proving the gradient character of the (Ti,Al,Si)N coating. The investigation includes also microhardness and roughness tests of the deposited coating and used substrate. Scratch test results was analysed to introduce adherence of the investigated coating. Findings: Gradient structure and main properties of the investigated materials were introduced. It has been stated, that properties of the coated with gradient (Ti,Al,Si)N coating oxide tool ceramic increase in comparison with uncoated material. Practical implications: Depositing the wear resistant gradient coating onto the Al2O3+SiC(w) oxide tool ceramic results in a significant increase of the surface layer microhardness, contributing most probably in this way in machining to the decrease of the wear intensity of cutting tools’ flanks made from the Al2O3+SiC(w) oxide tool ceramic. Originality/value: Gradient coatings are an innovative idea. The composition, microstructure and properties of gradient materials change continuously from the surface to the interior of the material.
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Purpose: The main aim of researches was investigation of structure and properties of the (Ti, Al, Si)N gradient wear resistant coatings. Design/methodology/approach: The structural investigations include the metallographic analysis on the transmission and scanning electron microscope. Examinations of the chemical compositions of the deposited coatings were carried out using the X-ray energy dispersive spectrograph EDS, glow-discharge optical emission spectroscope GDOES, auger electron spectroscope (AES) and using the X-ray diffractometer. The investigations include also analysis of the mechanical and functional properties of the materials: substrate hardness tests and microhardness tests of the deposited coatings, surface roughness tests, evaluation of the adhesion of the deposited coatings as well as cutting properties. Findings: Deposition of the multicomponent gradient coatings with the PVD method, based on the Al and Si solid secondary solution in the TiN titanium nitride, isomorphous with the alternating pure titanium nitride TiN, on tools made from oxide, nitride ceramics and tool cermets, results in the increase of mechanical properties in comparison with uncoated tool materials, deciding thus the improvement of their working properties. Practical implications: Deposition of (Ti, Al, Si)N nanocrystalline coatings by the use of PVD method causes the increase of cutting properties of tools made of cermets for ca. 300% and of Al2O3+ZrO2 for ca. 100% comparing to adequately uncoated tools. Originality/value: Comparison of the wide range of modern sintered tool materials with wide unique set of PVD coatings.
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Purpose: The paper presents investigation results of structure and properties of the multilayer and gradient TiN+(Ti,Al,Si)N+TiN nanocrystalline coatings deposited with the PVD method (CAE -Cathodic Arc Evaporation process) and in the combination of Al2O3 and TiN coatings in the CVD process on the substrate of cemented carbides,cermets, Al2O3+ZrO2, Al2O3+TiC, Al2O3+SiC(w) oxide ceramics and Si3N4 nitride ceramics. Design/methodology/approach: The structural investigation includes the metallographic analysis on thetransmission and scanning electron microscope, confocal microscope. Examinations of the chemicalcompositions of the deposited coatings were carried out using the X-ray energy dispersive spectrograph EDS, glow-discharge optical emission spectroscope GDOS, and using the X-ray diffractometer. The investigation includes also analysis of the mechanical and functional properties of the material: substrate hardness tests and microhardness tests of the deposited coatings, surface roughness tests, evaluation of the adhesion of the deposited coatings, cutting properties of the investigated materials. Findings: Deposition of the multicomponent gradient coatings with the PVD method, based on the Al and Si solid secondary solution in the TiN titanium nitride, isomorphous with the alternating pure titanium nitride TiN, on tools made from oxide, nitride ceramics and tool cermets, results in the increase of mechanical properties in comparison with uncoated tool materials, deciding thus the improvement of their working properties. Practical implications: Deposition of (Ti,Al,Si)N nanocrystalline coatings by the use of PVD method causes the increase of cutting properties of tools made of cermets for ca. 300% and of Al2O3+ZrO2 for ca. 100% comparing to adequately uncoated tools. Originality/value: Comparison of the wide range of modern sintered tool materials with wide unique set of PVD coatings.
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