ICMCTF2012 Session B4-3: Properties and Characterization of Hard Coatings and Surfaces

Wednesday, April 25, 2012 1:50 PM in Room Royal Palm 4-6

Wednesday Afternoon

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1:50 PM B4-3-1 Structure and composition of TiSiCN coatings synthesized by reactive arc evaporation: implications for cutting tool applications.
Emmanuelle Göthelid, Leif Löwenberg, Axel Genvald, Björn Ericsson, Mats Ahlgren (Sandvik Tooling, Sweden)
Developing the ultimate all around tool has become some sort of Holly Grail for machining industries. Such a tool should be tough, with good flank and crater wear resistance, a combination which is not easy to achieve. Insert performance can be dramatically improved with the help of an appropriate coating. We present here a novel route for depositing TiSiCN coating on WC-Co substrates. A reactive mixture of trimethyl-silane (TMS- (CH3)3-SiH) and N2 is used as Si, C and N source while arcing Ti at different substrate bias. Thanks to this approach, the Si to Ti and C to N ratios may be tuned at will. The samples structure was analyzed by XRD and SEM, their chemical composition by EDS and XPS. Hardness and E modulus were also determined. Interesting samples were then performance tested in a turning application. The results show that the Si content plays a crucial role for the texture of the film and the outcoming performances. The best variant at ca 6-10 at % Si exhibited a good combination of flank and crater wear resistance. These results will be discussed in the light of the physical data acquired.
2:10 PM B4-3-2 Influence of Process Parameters on the Properties of Low Temperature (Cr1-xAlx)N Coatings Deposited via Hybrid PVD DC-MSIP/HPPMS
Kirsten Bobzin, Nazlim Bagcivan, Mara Ewering, RicardoHenrique Brugnara (Surface Engineering Institute - RWTH Aachen University, Germany)

Ternary nitrides find widespread application as hard protective coating on cutting tools and as corrosion and wear resistant coatings on mechanical components. Concerning to this, ternary nitride such (Cr1‑xAlx)N deposited via PVD (Physical Vapour Deposition) show outstanding tribological, mechanical and chemical properties. The combination of these properties makes (Cr1-xAlx)N coatings suitable for many applications. For an effective protection of coated parts a uniform layer of coating material is also required. In this regard, the HPPMS (high power pulse magnetron sputtering) technology offers possibilities to improve coating thickness uniformity as well as to enhance mechanical properties. The present work deals with the investigation of the influence of process parameters on the (Cr1-xAlx)N coating properties deposited at 200 °C via combination of DC-MSIP and HPPMS technology. The aluminum content of the (Cr1-xAlx)N was varied between 22 at‑% and 88 at‑%. Further, the deposition pressure was varied in the range of 475 mPa and 525 mPa. Subsequently, the bias voltage was varied from 0 up to -200 V in order to analyze the coating thickness distribution on surfaces parallel and perpendicular to cathode. Mechanical properties, morphology and phase composition were analyzed by means of Nanoindentation, SEM (Scanning Electron Microscopy) and XRD (X‑Ray diffraction) measurements. The results show that the coating with 31 at-% Al displays higher hardness (20 GPa) and more favorable Young’s modulus (370 GPa) compared to the other coatings. The increase of the deposition pressure from 475 mPa to 525 mPa leads to a decrease of the hardness to 7 GPa. With increasing bias voltage a preferred 200 grain orientation and denser crystalline morphology are indentified. Regarding coating thickness uniformity, the coating deposited with -150 V shows the lowest deposition rate difference between the surface parallel and perpendicular to cathode. In addition, optical emission spectroscopy (OES) was used to investigate the effect of bias voltage and deposition pressure on intensity of Cr (357 nm) and Cr+ (283 nm) close to substrate during the coating process. In the studied parameter range, the change of the bias voltage shows a light effect on the Cr and Cr+ signal. The increasing of bias voltage from 0 V up to -150 V leads to decrease especially of non-ionized Cr. This effect can also be observed with increasing deposition pressure.

2:30 PM B4-3-3 Development of a new type micro slurry-jet erosion (MSE) test method for evaluation of surface strength of hard thin coatings
Yoshiro Iwai (University of Fukui, Japan); Toru Matsubara (Palmeso Co., ltd, Japan); Kenji Yamamoto (Kobe Steel Ltd., Japan)

Versatile and reliable techniques for evaluation of hard thin coatings are necessary for the development and tribological assessment of new coatings. Several different experimental techniques such as a nano-indentation, scratch and wear tests are normally used. However, most of the tests cannot assess properties of coating, substrate and interface independently.

We have proposed a new type of Micro Slurry-jet Erosion test (MSE), i.e. a solid particle impact erosion test for swift evaluation of coatings. In this study, the potential of our developed MSE test is demonstrated for the evaluation of different kind of vapor deposited coatings including PVD or CVD-TiN, TiC, TiAlN, CrN and DLC. Slurry containing 1.2 μm alumina particles was mixed with compressed air in the nozzle and eventually impacted on test materials at high velocity up to 100 m/s. The cross-section of the nozzle exit was a square of 1 x 1 to 3 x 3 mm2 . The impingement angle was 90 degrees. Wear progressions in depth profiles of the wear scar were measured. The wear depths vs. the amount of impacting particles or test time curves show the individual behavior depending on the properties of coatings, substrate and interface. Their wear rates show a huge difference in the various coatings. The new MSE test generates highly reproducible results and is very sensitive to the quality of the coatings.

So our conclusion is that MSE tests can evaluate (1) coatings and substrate strength, (2) strength or property distribution in the direction of depth from the surface, (3) coating thickness based on strength or functional aspect, (4) interface layer or zone strength, (5) change of substrate properties according to deposition process. Consequently, the MSE test is highly suitable as a screening test when evaluating single and multi-layered coatings, thin coatings with gradients, coating/substrate interfaces, etc.

3:10 PM B4-3-5 Investigation of structural ,mechanical and tribological properties of TiAlN/CrN multilayer films deposited by CFUBMS technique
Cinar Laloglu (Turkey); Özlem Baran (Erzincan University, Turkey); Yasar Totik, İhsan Efeoglu (Turkey)

TiAlN and CrN are using widely in many industrial applications. In this work, TiAlN/CrN multilayer films deposited onto M2 high-speed steel and were examined by closed field-unbalanced magnetron sputtering (CFUBMS). Process parameters of coatings were determined according to Taguchi L4 (32) method. The structural properties of coatings have been analyzed by scanning electron microscopy (SEM), X-ray diffraction (XRD) and energy dispersive spectrometry (EDS). Besides, the mechanical and tribological properties were determined by using microhardness tester and pin-on-disc test, respectively. Experimental results showed that TiAlN/CrN multilayer films improved noticeably tribological properties of cutting tools.

3:30 PM B4-3-6 The Phase Transition and Corrosion Resistance of ZrO2(N) Thin Films on AISI 304 Stainless Steel Deposited by Ion Plating
Jia-Hong Huang, Po-Hua Huang, Ge-Ping Yu (National Tsing Hua University, Taiwan)

ZrO2(N) thin films were deposited on AISI 304 stainless steel substrate using hallow cathode discharge ion-plating (HCD-IP). Our previous study [1] indicated that the adhesion of ZrO2 thin film on stainless steel was poor due to low wettability. The objectives of the present study were to understand the phase transition of ZrO2(N) thin films with increasing nitrogen contents and to provide a feasible approach to manufacture ZrO2(N) coatings on stainless steel with excellent corrosion resistance and good adhesion. By maintaining oxygen flow rate at 10 sccm and adjusting nitrogen flow rate, ranging from 0 to 12 sccm, the compositions and phase ratios of the ZrO2(N) thin films can be controlled. With increasing nitrogen flow rate, the XRD patterns showed that the phase content of c-ZrO2 increased while that of m-ZrO2 decreased, and then ZrN phase increased. The N solubility limit in ZrO2 for the formation of ZrN was 8.8 at% for the as-deposited thin film. After annealing in vacuum, different phase transitions were found for the specimens. At higher nitrogen content, phase separation of ZrN from c-ZrO2 occurred in the specimens. The corrosion resistance of the ZrO2(N)-coated stainless steel specimens was evaluated by potentiodynamic scan in both 5% NaCl and in 1N H2SO4 solutions, and salt spray test was employed to assess the durability of the films. Corrosion resistance was associated with film packing density and major phases. The results showed that the HCD-IP method can effectively overcome the surface wetting problem of ZrO2 on stainless steel, and hence the ZrO2(N) coating on stainless steel possesses excellent adhesion and corrosion resistance. ZrO2(N) thin films containing ZrN ranging from 14.4 % to 28.8 % were found to have better corrosion resistance than pure ZrO2 thin films.

[1] Jia-Hong Huang, Tzu-Chun Lin, Ge-Ping Yu, Surf. Coat. Technol.,206(2011)107.

4:10 PM B4-3-8 Hardness Percolation in Plasma Enhanced Chemical Vapor Deposited a-SiC:H Thin Films
Sean King (Intel Corporation, US)

Plasma Enhanced Chemically Vapor Deposited a-SiC:H thin films are compelling materials for both semiconductor nano-electronic and MEMS/NEMS technologies due to the extreme chemical inertness of this material and the ability to tune a variety of material properties across an extreme range of values. As one example of the latter, we demonstrate that the hardness of a-SiC:H thin films can be varied from 0.5 to 40 GPa. Utilizing Fourier Infrared-Transform Spectroscopy, we additionally show that this remarkable range in materials properties is achieved primarily via the incorporation of terminal hydrogen groups which lowers the overal connectivity of the Si-C network bonding. We find that once the average network coordination number for Si and C falls below 2.6, the Si-C network becomes under constrained and there is a loss of rigidity percolating through the system. This rigidity limit constrains the range of materials properties that can be achieved in the Si-C system.

4:30 PM B4-3-9 Tungsten-modified hydrogenated amorphous carbon coatings providing tailored friction properties
Harald Hetzner, Stephan Tremmel, Sandro Wartzack (Friedrich-Alexander-University Erlangen-Nuremberg, Germany)

In comparison to pure hydrogenated amorphous carbon coatings (a-C:H), the metal-modified variants (a-C:H:Me) are known to have better adhesion to the substrate due to lower residual stresses and more stable friction in dry sliding against steel. For this reason, particularly in higher loaded applications, a-C:H:Me is usually preferred over a‑C:H, even though hardness and hence abrasion protection tends to be lower. Dependent on the deposition parameters, the properties of a‑C:H:Me can be varied over wide ranges: From metal-like and carbide-like to amorphous-carbon-like. On the one hand this allows to a certain extent the adaption of the coating’s mechanical properties to the load-carrying and overload capability required by the targeted application. On the other hand, this offers the opportunity to use these coatings for the realization of tailored friction properties.

In the present study, tungsten-modified hydrogenated amorphous carbon coatings (a‑C:H:W) were deposited on hardened and tempered tool steel using an industrial scale coating machine. The applied coating technique was reactive magnetron sputtering of a tungsten carbide (WC) target in argon-acetylene atmosphere. To improve the adhesion to the substrate, a thin chromium layer and a WC intermediate layer were deposited by arc evaporation and magnetron sputtering, respectively. For the deposition of the a‑C:H:W functional layer, four process parameters, namely cathode power, bias voltage, process gas pressure and argon-to-acetylene flow ratio were varied according to a 24 factorial design.

The coated samples were characterized in terms of structural, mechanical and tribological properties: Micro structure and thickness were evaluated by scanning electron microscopy. Surface roughness was measured using a profilometer. Hardness and Young’s modulus were determined by instrumented indentation tests. Rockwell C indentation and scratch tests provided information on cracking resistance and adhesion to the substrate. Friction and wear of the coatings were studied in ball-on-disk tests over a sliding distance of 1,000 meters (13,263 rotations). In dry sliding against 100Cr6 balls, coefficients of friction in the range of 0.10 to 0.43 were determined for the respective coatings. Under oil lubrication, the respective friction coefficient was found to be between 0.05 and 0.11. For almost any of the tested coatings, the observed friction behavior was also sufficiently stable. This proves the potential of providing tailored friction properties by proper choice of the deposition parameters of a‑C:H:W coatings.
4:50 PM B4-3-10 Characterization of Plasma Electrolytic Oxidation (PEO) Coatings on 6082 Aluminium Alloy
Alan Jarvis, Aleksey Yerokhin (University of Sheffield, UK); Pavel Shashkov (Cambridge Nanolytic, Ltd., UK); Allan Matthews (University of Sheffield, UK)
This research characterizes two sets of PEO alumina coatings obtained on BS 6082 series aluminium alloy substrates. One was produced using the more common electrolyte containing silicates, and the other was made without silicates. The coatings were characterized using a variety of methods and their relative wear resistance was evaluated with a reciprocating wear tester. The wear resistance of the coating made using the advanced method is significantly higher than the reference coating. The greater wear resistance of this coating appears to be due to the difference in wear modes: mostly transverse fracture cracks that lead to a gradual loss of material. The silicate containing coating suffers a more severe wear mode of both transverse as well as lateral cracks leading to spalling. The difference in wear resistance appears to be due to both higher micro-scale Vickers indentation hardness, as well as its greater indentation toughness that indicates the resistance to the formation of lateral cracks, and thus spalling. The reasons for this difference in toughness were not determined. The greater hardness of the new coating is likely due to lower porosity. Nanoindentation hardness measurements were used to evaluate the hardness and elastic modulus at a nano scale and tend to support the difference in alpha and gamma alumina phase content found using XRD measurements. Several other coating characteristics were investigated and appeared to have no correlation with wear resistance. The residual stresses in the coatings were measured using two methods: XRD and an optical fluorescence method (piezo-spectroscopic) which both showed the same trends. An attempt was made to quantify the amount of amorphous alumina in the coatings using a quantitative Rietveld method, however the results were inconclusive due to the difficulty in determining the exact gamma alumina phase crystal structure, thought to be a defect spinel structure.
5:10 PM B4-3-11 The microstructure and mechanical properties of Cr-Si-Ti-Al-N coatings
Yu-Chu Kuo (National Taiwan University of Science and Technology, Taiwan); Jyh-Wei Lee, Chaur-Jeng Wang (Ming Chi University of Technology, Taiwan)
The Cr-Si-Ti-Al-N thin films with various silicon contents were fabricated by a co-sputtering process with three targets. The influences of silicon contents on the microstructure, mechanical and tribological properties of Cr-Si-Ti-Al-N films were investigated in this work. The phase structures of the coatings were determined by a glancing angle X-ray diffractometer (GA-XRD). The microstructures of thin films were evaluated by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), respectively. The hardness and elastic modulus were examined by a nanoindentation. The scratch test, Rockwell-C adhesion and pin-on-disk wear tests were used to evaluate the adhesion quality and tribological properties of thin films. It was found that the column structure was transformed to a dense structure when the silicon contents were higher than 10 at.%. The hardness and tribological properties were also strongly influenced by the silicon concentration of the Cr-Si-Ti-Al-N coatings.
Time Period WeA Sessions | Abstract Timeline | Topic B Sessions | Time Periods | Topics | ICMCTF2012 Schedule