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1

Abrasion Resistance Test of the Modified Ti13Nb13Zr Alloy Surface

Lisoń-Kubica Julia, Taratuta Anna, Antonowicz Magdalena, Basiaga Marcin

Tribologia

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2023

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nr 2

55--64

EN

The research describes an atomic layer deposition (ALD) coating method and its application on a new generation of titanium alloy (Ti13Nb13Zr) for biomedical applications. The study aimed to assess the physicochemical properties and mechanics of a titanium alloy coated with titanium oxide (TiO2) or aluminium oxide (Al2O3) using the ALD method. The physicochemical properties of the surface coatings were evaluated through microscopic observations, potentiodynamic tests, surface wettability tests, optical profilometry scratch tests, and abrasion tests. Based on the data obtained, different physicochemical properties of the alloy with titanium nitride and titanium oxide coatings were found. Such differences were dependent on the number of cycles used and the temperature of the manufacturing process. The coatings have reduced the abrasion coefficient, thus improving the abrasion resistance of the Ti13Nb13Zr alloy, which enables their use within the skeletal system. These findings are of practical importance for applying this type of surface modification to various types of miniaturised implants used in the skeletal system.

PL

Badania polegają na opisaniu metody osadzania powłok atomowych i możliwości jej zastosowania na stopie tytanu nowej generacji do zastosowań biomedycznych. Celem pracy jest ocena wpływu właściwości fizyko chemicznych i mechanicznych zmodyfikowanego stopu Ti13Nb13Zr powłoką tlenku tytanu (TiO2) oraz tlenku glinu (Al2O3) przy użyciu metody ALD. W ramach oceny własności fizykochemicznych tak powstałych powłok powierzchniowych przeprowadzono obserwacje mikroskopowe (SEM), badania potencjodynamiczne, badania zwilżalności powierzchni, profilometrię optyczną, scratch test oraz badania ścieralności powłok. Na podstawie uzyskanych danych stwierdzono zróżnicowane własności fizykochemiczne stopu z powłokami tlenku glinu oraz tlenku tytanu w zależności od zastosowanej ilości cykli oraz temperatury procesu wytwarzania. Powłoki mają obniżony współczynnik ścieralności, poprawiając tym samym odporność na ścieranie stopu Ti13Nb13Zr, co umożliwia ich zastosowanie w układzie kostnym. Uzyskana na tej podstawie wiedza ma znaczenie praktyczne dla zastosowania tego typu modyfikacji powierzchni dla różnych rodzajów zminiaturyzowanych implantów znajdujących swoje zastosowanie w układzie kostnym.

2

Properties of Al2O3 Ceramic Coatings Applied by ALD Method on 100Cr6 Steel

Radoń-Kobus Krystyna, Madej Monika

Tribologia

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2022

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nr 2

45--53

EN

The purpose of the paper was to assess the morphology, chemical composition, geometric surface structure and contact angle, as well as to analyse the tribological properties of Al2O3 coatings deposited on 100Cr6 steel using the technique of atomic layers ALD. Al2O3 coatings were selected due to their tribological properties, adhesion to the substrate and hardness. Tribological tests were performed in a reciprocating motion in a ballon-disc combination, with a counter-specimen of 100Cr6 steel, under the conditions of technically dry friction. Surface morphology was observed under a scanning microscope, and an EDS analyser enabled the performance of an analysis of the chemical composition of the samples. Wetting of the surface of the Al2O3 coating was determined by means of an optical strain gauge. The geometric surface structure before and after the tribological tests was analysed by means of a confocal microscope with an interferometric mode. The tests proved that during technically dry friction, the average coefficient of friction for the Al2O3 coating is lower by approximately 30% than for 100Cr6 steel. The tested coatings are characterised by hydrophobicity.

PL

Celem pracy była ocena morfologii, składu chemicznego, struktury geometrycznej powierzchni, kąta zwilżania oraz analiza właściwości tribologicznych powłok Al2O3 osadzanych na stali 100Cr6 techniką warstw atomowych ALD. Powłoki Al2O3 wytypowano ze względu na ich właściwości tribologiczne, adhezję do podłoża oraz twardość. Testy tribologiczne przeprowadzono w ruchu posuwisto-zwrotnym w skojarzeniu kula–tarcza z przeciwpróbką ze stali 100Cr6 w warunkach tarcia technicznie suchego. Na mikroskopie skaningowym obserwowano morfologię powierzchni, a analizator EDS umożliwił przeprowadzenie analizy składu chemicznego próbek. Przy pomocy tensjometru optycznego określono zwilżalność powierzchni powłoki Al2O3. Strukturę geometryczną powierzchni przed i po testach tribologicznych analizowano za pomocą mikroskopu konfokalnego z trybem interferometrycznym. Testy wykazały, że podczas tarcia technicznie suchego średni współczynnik tarcia dla powłoki Al2O3 jest około 30% mniejszy niż dla stali 100Cr<6. Badane powłoki charakteryzują się hydrofobowością.

3

Microstructure and antibacterial properties of a ZnO coating on a biomaterial surface

Basiaga Marcin, Paszenda Zbigniew, Lisoń Julia, Taratuta Anna, Kazek-Kęsik Alicja, Krok-Borkowicz Małgorzata, Nuckowski Paweł, Szindler Magdalena, Staszuk Marcin, Major Łukasz, Major Roman, Barabaszová Karla Čech, Dyner Marcin

Archives of Civil and Mechanical Engineering

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2022

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Vol. 22, no. 2

art. no. e93, 1--18

EN

A promising strategy for fighting the bacterial biofilm on the surface of biomaterials involves modification of their surface with the use of bactericidal and bacteriostatic coatings. Ongoing studies concentrate on the development of material that can limit bacterial colonisation and is safe for the human organism. Therefore, the current research focuses on the conditions related to implant coating to limit biofilm formation. However, previous outcomes in this area have not been satisfactory. Accordingly, the main goal of the carried out tests was to study the impact of the physicochemical properties of the surface layers on the course of processes taking place on the surface of implants made of metallic biomaterials used in the bone system. The surface of the analysed biomaterial -316LVM steel - was modified using such processes as grinding, electrochemical polishing, sandblasting, application of a ZnO layer using low-temperature Atomic Layer Deposition (ALD), and medical sterilisation. Initial assessments involved the chemical composition, phase composition, and the microstructure of the surface layer. The last stage involved microbiological studies, including an assessment of the adhesion of Gram-positive and Gram-negative bacteria to the modified surface, proliferation of MG-63 osteoblast-like cells and cytotoxicity tests. The analysis of adhesion of S. aureus and E. coli colonies confirmed that the ZnO coating is effective in reducing bacterial adhesion to the 316LVM steel substrate, regardless of the number of cycles, process temperature and surface treatment method.

4

A study on the physicochemical properties of surface modified Ti13Nb13Zr alloy for skeletal implants

Lisoń Julia, Taratuta Anna, Paszenda Zbigniew, Dyner Marcin, Basiaga Marcin

Acta of Bioengineering and Biomechanics

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2022

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Vol. 24, no. 1

39--47

EN

As it is widely stated in the literature, biofilms are responsible for most chronic infections, which have grown exponentially over the past three decades. The use of so-called alloys, as a new generation of materials, enables us to find the golden mean in the arena widely known as implantology. The use of the surface layer, using the chosen Atomic Layer Deposition method, is to be the basis for minimizing the risk of an organism reactions. Therefore, the primary objective of this study was to observe the impact of physicochemical properties of the surface layers (bactericidal) on the processes that occur on the implants surface made of titanium biomaterials used in bone structures. The study also attempted to evaluate the physicochemical properties of the ZnO coatings, deposited on the substrate of one of the new generation Ti13Nb13Zr alloys, using the ALD method. Included in the assessment of the physicochemical properties of the surface layers formed in this manner, we perform pitting corrosion resistance tests, scratch tests, tribological tests and surface wettability tests. Based on the obtained data, the differing physicochemical properties of the alloy with ZnO coatings are found to be dependent on the applied surface modification. For the conducted tests, differences are determined for the tests on the corrosion resistance, surface wettability and the abrasion resistance for samples with and without the ZnO coating. In addition, tests show that the coating applied to the alloy, which is previously subjected to the sand-blasted process, is characterized by improved adhesion.

5

Atomic layer deposited ZnO films on stainless steel for biomedical applications

Basiaga Marcin, Walke Witold, Kajzer Wojciech, Sambok-Kiełbowicz Agata, Szewczenko Janusz, Simka Wojciech, Szindler Marek, Ziębowicz Bogusław, Lubenets Vira

Archives of Civil and Mechanical Engineering

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2021

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Vol. 21, no. 1

1--15

EN

The main goal of carried out tests were the impact of physicochemical properties of surface layers on the course of processes taking place on the surface of implants made of metallic biomaterials used in the bone system. As a precursor of ZnO, diethylzinc (DEZ) has been used, which reacted with water enabling the deposition of thin films. The chamber temperature was as follows—T = 200°–300 °C. The number of cycles was 500, 1000, and 1500. In the first stage, pitting corrosion test was carried out. Corrosion resistance has been tested under conditions simulating tissue environment. Moreover, the created layers were tested using electrochemical impedance spectroscopy (EIS). The conducted electrochemical tests showed the beneficial effect of the ZnO layer on the substrate made of 316 LVM steel, as evidenced by the obtained parameters describing the corrosion resistance. Furthermore, tests were performed on mechanical properties (scratch test), surface morphology (SEM and AFM method), and physical properties (wettability and thickness layers) for samples with different surface treatments. The investigations of the surface morphology of the applied ZnO layer using the ALD method showed a tendency to inherit the substrate independently of the used application parameters. On the other hand, the tests of adhesion to the substrate showed that the number of cycles of the application process has a fundamental impact on the adhesion of the applied layer to the substrate. Summarizing tests have clearly shown that the number of cycles and temperature in the case of the ZnO coating is significant and positively influences the increase of electrochemical, mechanical, and physical properties of layers.

6

Adhesion of SiO2 layers deposited by means of sol-gel and ALD methods on 316LVM steel

Basiaga M., Walke W., Kajzer A., Kajzer W., Staszuk M., Kurtyka P.

Engineering of Biomaterials

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2016

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Vol. 19, no. 138 spec. iss.

114

7

Potentiostatic, Potentiodynamic and Impedance Study of TiO2 Layers Deposited of 316 LVM Steel Used for Coronary Stents

Basiaga M., Staszuk M., Walke W., Tański T., Kajzer W.

Archives of Metallurgy and Materials

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2016

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Vol. 61, iss. 2A

821--824

EN

The objective of the study is assessment of suitability of the ALD method for application of a TiO2 layer on surface of 316LVM steel used for production of vessel stents. Selection of the appropriate process parameters for application of the layer affects its electrochemical properties, which largely determine resistance of the biomaterial to corrosion in the blood environment, thus affecting its hemocompatibility. To assess resistance of the AISI 316LVM steel with modified surface to corrosion, voltammetric and impedance measurements were conducted. The proposed variant of surface processing allows safe deformation of the TiO2 layer without its delamination.

8

Influence of Surface Modification on Properties of Stainless Steel Used for Implants

Basiaga M., Jendruś R., Walke W., Paszenda Z., Kaczmarek M., Popczyk M.

Archives of Metallurgy and Materials

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2015

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Vol. 60, iss. 4

2965--2970

EN

The aim of the study was assessment of the influence of stainless steel 316 LVM surface modification on its functional properties. The analyzed steel undergone a surface treatment consisting of the following processes: mechanical polishing, chemical passivation and deposition of Al2O3 layers by Atomic Layer Deposition method. The proposed variant of surface treatment will undoubtedly contribute to improving the functional properties of stainless steel intended for implants. In order to assess functional properties of the steel, electrochemical studies, adhesion (scratch test), wetting angle tests and topography of surface (AFM method) were performed. The obtained results of the study showed clearly that the proposed by the authors way of surface treatment including: mechanical polishing, chemical passivation and deposition of Al2O3 layer by means of the ALD method effectively improves the corrosion resistance of stainless steel.

PL

Celem pracy była ocena wpływu modyfikacji powierzchni stali nierdzewnej 316 LVM na jej właściwości funkcjonalne. Obróbka powierzchni składała się z następujących procesów: polerowanie mechaniczne, chemiczna pasywacja i naniesienie warstw Al2O3 metodą ALD (Atomic Layer Deposition). Zaroponowany wariant obróbki powierzchni niewątpliwie przyczyni się do poprawy właściwości funkcjonalnych stali przeznaczonej na implanty. W celu oceny właściwości funkcjonalnych stali przeprowadzono badania elektrochemiczne, badania adhezji warstw (scratch test), oraz badania zwilżalności (kąt zwilżania i badania topografii powierzchni metodą AFM). Uzyskane wyniki badań wykazały wyraźnie, że zaproponowany przez autorów sposób obróbki powierzchni, w tym: polerowanie mechaniczne, pasywacja chemiczna i naniesienie warstw Al2O3 metodą ALD skutecznie poprawia odporność na korozję stali nierdzewnej.