ICMCTF2007 Session B4: Laser-Assisted and Ion Beam Coatings and Technologies

Wednesday, April 25, 2007 8:00 AM in Room Royal Palm 1-3

Wednesday Morning

Time Period WeM Sessions | Abstract Timeline | Topic B Sessions | Time Periods | Topics | ICMCTF2007 Schedule

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8:00 AM B4-1 Ion and Laser Beam Assisted Deposition and Modification of Multilayered Coatings
C. Bundesmann, J. Dienelt, F. Frost, J.W. Gerlach, T. Höche, H. Neumann, D. Ruthe, F. Scholze, E. Schubert, K. Zimmer, B. Rauschenbach (Institut für Oberflächenmodifizierung e.V., Germany)

Recent results of thin film deposition by means of ion beam sputtering or UV laser beam ablation of solid targets for depositing multilayered coatings for x-ray, EUV, and optical applications are summarized. In particular, the large area deposition of Mo/Si multilayers for EUV lithography masks by ion beam sputter deposition using a new ion beam sputter deposition tool are reviewed. The concept ideas of the tool to fulfill the requirements of homogeneity and low particle generation are pointed out and the selected results of the multilayer characterization are mentioned. The influence of the deposition parameters on the film properties are discussed in terms of the film properties, e.g. the film stress. Further examples concern the deposition of Ni/C and Cu/C multilayers by PLD and oxidic multilayers by IBS.

Finally, the interaction of these multilayers with ultrashort laser pulses are presented. The basics of laser-matter interactions of such thin film multilayers with ultrashort pulses are discussed and measurements on the damage threshold of optical multilayers presented.

8:40 AM B4-3 Plasma Diagnostics of Laser Ablation, Magnetron Sputtering, and Cathodic Arc using In Situ Optical Spectroscopy
J.G. Jones (Air Force Research Laboratory); C. Muratore (UTC/Air Force Research Laboratory); A.R. Waite, A.A. Voevodin (Air Force Research Laboratory)
Optical Spectroscopy was used to monitor laser ablation, magnetron sputtering, magnetically filtered cathodic arc, and plasma treatments. Combinations of these processes were used to deposit novel nanocomposite thin-films having an amorphous metal matrix and nanocrystalline grains of hard wear resistant materials for tribological applications. These combined plumes were monitored using a high fidelity mutli-channel analyzer that collected spectra at small integration times to determine laser plume chemical evolution during individual laser and magnetron pulses; longer integration times showing cumulative optical emissions were also examined. Alternatively, an inexpensive spectrometer was used to monitor the plasmas using only long integration times for the purposes of determining atomic species and process drift over the course of deposition. Spectra collected throughout the course of a deposition will be presented to show process drift, identification of atomic species, and comparison of data from each system.
9:00 AM B4-4 A Correlation Between Field Emission Properties and Increasing Crystallinity in Lanthanum Monosulfide (LaS) Thin Films
S.B. Fairchild (Air Force Research Laboratory); P.T. Murray (University of Dayton); D.J. Lockwood, X. Wu, D. Poitras (Institute for Microstructural Sciences, NRC, Canada); V. Semet, V.T. Binh (University of Lyon, France); M. Cahay (University of Cincinnati)

Thin films of lanthanum monosulfide (LaS) have been successfully deposited on Si and MgO substrates by pulsed laser deposition. Films grown on Si substrates at room temperature in vacuum were mostly amorphous with small (5-10 nm) crystalline regions and exhibit very broad Raman features. Films grown on MgO at elevated substrate temperatures in a background gas of H2S were polycrystalline with varying grain size dependent on temperature and pressure. The Raman spectra of these LaS/MgO films are all similar and exhibit intensity variations from sample to sample consistent with changes in grain size. These spectra resemble that of polycrystalline bulk LaS showing a number of sharp and also broader features with the main peaks at 101, 148, 178, and 262 cm-1 due to disorder-induced first-order scattering from acoustic and optic phonons1. Spectroscopic ellipsometry1 shows a sharper optical band edge in the LaS/MgO films compared with LaS/Si films consistent with an increased crystallinity. Scanning anode field emission microscopy (SAFEM) reveals that an increase in film crystallinity leads to an increase in the total emitted current. The mostly amorphous La/Si films emit up to 0.5 µA for a cathode surface of 200 µm2 before a burnout occurs due to thermally induced phase change in the emitting nanocrystallites. A polycrystalline LaS/MgO film with a 40 nm grain size emits up to 40 µA /200 µm2 with no burnout, a result that is consistent with the patchwork field emission behavior of the LaS/Si films.2 LaS thin films could potentially be used for cathode materials in vacuum microelectronic devices.

1 M. Cahay, K. Garre, X. Wu, D. Poitras, D. J. Lockwood, and S. Fairchild, JOURNAL OF APPLIED PHYSICS 99, 123502 (2006)

2 V. Semet, M. Cahay, Vu Thien Binh, S. Fairchild, X.Wu , D.J. Lockwood, JOURNAL OF VACUUM SCIENCE AND TECHMOLOGY B 24(5), Sept/Oct 2006 .

9:20 AM B4-5 Investigation of MoS2/Metal Solid-Lubricant Thin Film Coatings Deposited by High-Power Ion Beam Ablation1
T.J. Renk, S.V. Prasad (Sandia National Laboratories)

Thin-film MoS2 coatings have been been studied for a number of years as a self-lubricating wear-resistant film for a number of applications.2 The addition of metals such as Ti has been observed to improve such tribological properties as friction and wear behavior. The metals have typically been added to sputtered coatings by either dual sputtering or by interlayering using alternate sputtering targets. We are investigating the microstructure, friction, and wear performance of MoS2/metal films formed by high-power ion beam ablation of one or more targets. These experiments are carried out on the 750 kV RHEPP-1 facility at Sandia National Laboratories. An intense ion beam of up to 10 J/cm2 fluence is used to ablate either a composite MoS2/metal target, or ablate alternately two discrete targets. The deposited layer from each pulse can be between 5-20 nm in thickness. Although Ti is the primary admixed metal, other metals such as Ni may be investigated. Due to the high-power nature of the process (similar to PLD), the film texturing is likely to be different from that formed by either RF or DC-magnetron sputtering. The pulsed nature may lead to new metastable phases due to the rapid quench, and with much higher deposition rates than PLD. We will form and investigate pure MoS2, MoS2/metal composite, and MoS2/interlayered metal films. Pin-on-disk testing, SEM, and XTEM of selected layers is planned.

1Sandia is a multiprogram laboratory operated by Sandia Corporation, a Lockheed Martin Co., under US DOE Contract DE-AC04-94AL85000.

2N.M. Renevier, J. Hampshire, V.C.Fox, J. Witts, T.Allen, D.G. Teer, Surf. Coat. Tech. 142-144 (2001) 67-77.

9:40 AM B4-6 Synthesis of Nanoparticle Coatings by Through Thin Film Ablation
P.T. Murray, E. Shin (University of Dayton); L. Dosser, K. Bailey (Mound Laser and Photonics Center)
Nanoparticle coatings of Fe, Si, and C have been formed by the process of Through Thin Film Ablation (TTFA). In the TTFA process, the target consists of a thin film of material that has been applied to an optically transparent support, which is usually fused silica. The thin film target is ablated in vacuum through the transparent support, and this produces a directional plume of nanoparticles. TEM analysis of the coatings indicates the deposition of nanoparticles that are not agglomerated and that typically have a most probable size of 2 nm; the size distribution is a function of target thickness and laser energy density at the target. Optical emission spectroscopy measurements have been carried out on the ablated plume, and time resolved optical emission measurements indicate the ablated nanoparticles are ejected with kinetic energies on the order of 5-10 eV. Ablation has been carried out with both ns and fs lasers, and a comparison of the two ablation regimes will be discussed. Finally, the results suggest that the nanoparticle formation mechanism involves an adiabatic expansion of the ablated material into vacuum.
10:00 AM B4-7 Hybrid Technology Hard Coating - Electron Beam Surface Hardening
R. Zenker, G. Sacher, A. Buchwalder (TU Bergakademie/IWT, Germany); J. Liebich (Ionbond Sachsen/Germany); A. Reiter (OC Oerlikon Balzers Coating AG, Liechtenstein); R. Haessler (BTC, Chemnitz, Germany)
Hard surface layers often cannot show to advantage their good hardness, strength and wear resistance on relatively soft material, so that an additional thermal treatment of the basic material before / or after coating is necessary. A good and modern alternative to the mostly used bulk heat treatment are surface treatment technologies with high energy beams (electron beam (EB) and laser beam (LB)). The energy deposition is precisely focused, so it is possible to limit the heat treatment to highly loaded areas and up to the depth where a transformation (hardening) is necessary. Therefore, the bulk material is not heated up to critical temperatures. The thermal load of the over-all component is minimized and distortion can be avoided that way also. The paper deals with current results of investigations on the combination of PVD hard protective coatings (based on TiN, TiCN, TiAlN, CrxNy and DLC) with EB surface hardening. Basic materials used for these investigations were different steels (unalloyed steel: C45; low alloyed tool steel: 100Cr6; high alloyed tool steel: X155CrVMo12-1). It is not only the sequence of treatments (beam hardening before or after coating) which has a considerable influence on treatment results, but also the parameters of energy beam surface treatment (energy density distribution, speed of treatment, atmosphere around the interaction area). It will be discussed the relations between treatment conditions, process parameters and surface deformation, layer structure and composition, structure and composition gradients, surface properties, properties gradients and transformation behavior of matrix material These modern combined technologies open up new fields of industrial application for local high loaded tools and components.
10:20 AM B4-8 Fluorine Laser Irradiation of Cubic Boron Nitride Films: Influence on Internal Stress and Microstructure
G. Reisse, F. Haehnel, D. Rost, S. Weissmantel (University of Applied Sciences Mittweida, Germany)
Cubic boron nitride films prepared by ion-assisted pulsed laser deposition on silicon substrates have been irradiated with fluorine laser pulses of 157 nm wavelength and 30 ns pulse duration. It will be presented that the high internal stress of the films of 10 - 12 GPa was at least partially released in consequence of the irradiation and that the extent of stress relaxation depends mainly on the fluence and the number of laser pulses used per area. Thereby, the portion of the cubic phase did not decrease significantly, which was established by comparing the infrared spectra taken before and after irradiation. The results of electron microscopic investigations will also be presented and finally some conclusions on possible mechanisms involved in the process will be discussed.
10:40 AM B4-9 Microstructuring of Superhard Pulsed Laser Deposited ta-C Films Using Excimer and Femtosecond Laser Pulses
S. Weissmantel, R. Boettcher, A. Engel, M. Nieher, G. Reisse, D. Rost, E. Weissmantel (University of Applied Sciences, Mittweida, Germany)
Several micrometer thick superhard tetrahedral amorphous carbon films prepared by pulsed laser deposition on polished steel and hard metal substrates have been microstructured using (1) excimer laser pulses of 248 nm wavelength and 30 ns pulse duration and (2) femtosecond laser pulses of 780 nm mean wavelength and 130 fs pulse duration. The aim was to investigate if and how microstructuring influences the tribological properties and the wear resistance of the films, which were measured using a tribometer. By using the excimer laser well defined gratings with the width and depth of the grooves as well as the grating space in the range of 0.5 to a few micrometer were produced. By using the femtosecond laser so-called ripple structures, which resemble gratings with a spacing of some 0.5 µm, were produced in the films. The formation mechanism of those ripples is not yet understood, but it can be used to microstructure swiftly relatively large film areas. The microstructures have been investigated with respect to their appearance and their dimensions by Scanning Electron and Laser Scanning Microscopy, the results of which will be shown. Moreover, the influence of the different microstructures on tribological and wear performance of the films under various conditions will be presented.
11:00 AM B4-10 Synthesis and Tribological Characterization of Mo -(W)- S -Se- (TE) Composite Coatings by Pulsed Laser Deposition
J.J. Hu (UTC Inc./Air Force Research Laboratory ((AFRL / MLBT)); J. Zabinski, J.E. Bultman, J.H. Sanders, A.A. Voevodin (Air Force Research Laboratory / MLBT)
Mo - W - S - Se and Mo - S - Te composite coatings were deposited on steel substrates at room temperature to 300°C in a high vacuum chamber. The plasma plumes were produced by direct laser ablation of a cold-pressed composite target with pulsed UV beams of 248 nm wavelength, 20 ns duration, 1~50 Hz rate, and 200~600 mJ energy. The coating chemistry and microstructure were characterized using X-ray photoelectron spectroscope (XPS), X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM). The Mo-S, Mo-Se and Mo-Te bonding and hexagonal crystal structure were verified in the coatings. The Se or Te replacements on S sites were proposed to explain a large expansion along the c-axis (spacing between basal planes) and the bending of S-Mo-S layers (i.e., basal planes). The tribological properties of the Mo - W - S - Se and Mo - S - Te coatings were measured in dry and humid conditions using a ball-on-disc tribometer, which showed a lower friction coefficient and much longer wear lifetime than pure MoS2 coatings in humid air tests. The wear scar surfaces and coating cross sections were studied using SEM, TEM and focused ion beam (FIB) microscopes, which also provided the information on chemical composition distributions in depth along with microstructure features. Micro Raman spectra and X-ray energy dispersive spectra collected inside wear scars demonstrated that the composite coatings had a significant high resistance to oxidation.
Time Period WeM Sessions | Abstract Timeline | Topic B Sessions | Time Periods | Topics | ICMCTF2007 Schedule