ICMCTF2010 Session D1: Boron Nitride, Carbon Nitride-Based Multifunctional Materials and Group-III (Al, Ga, In) Nitride Materials

Wednesday, April 28, 2010 1:30 PM in Room Pacific Salon 3

Wednesday Afternoon

Time Period WeA Sessions | Abstract Timeline | Topic D Sessions | Time Periods | Topics | ICMCTF2010 Schedule

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1:30 PM D1-1 A Novel Cubic Boron Nitride Coating Technology: Coating Design, Deposition, Analysis, and Performance in Turning Applications
Wenping Jiang (Duralor, LLC); Ajay Malshe (University of Arkansas and NanoMech, LLC)
A composite coating series based on nano‐ and micro‐sized cubic born nitride particulates and choice of application‐specific binders was developed for turning engineering materials. The coating series were produced via two‐step sequential processes: electrostatic spray coating of cubic boron nitride particles with size less than 2 μm for a conformal porous coating preform of designed thickness; chemical vapor infiltration of ceramic binder phase(s) at a temperature of around 1000 oC for a dense and well adherent composite coating. In this paper, the coating design in combination with insert edge preparation for different applications was discussed. As a study case, cubic boron nitride‐titanium nitride composite coating was characterized by use of different techniques for coating cross‐section, elemental composition, crystal phases, and adhesion strength. Characterization results indicated a composite coating with uniform coating thickness and evenly distributed cubic boron nitride particles in titanium nitride matrix. Additionally, the coating was tested for its machining performance in turning AISI 4340 hardened steels, AISI 4140 pre‐hardened steels, and ductile cast iron at representative application conditions, and compared to correspondingly industrial benchmarks. Testing results showed that the composite coating outperforms its industrial counterparts, polycrystalline cubic nitride, titanium aluminum nitride by physical vapor deposition, multi‐layer coating by chemical vapor deposition, and aluminum oxide bulk tools, in respective application.
2:10 PM D1-3 Comparative Study of Chemical Bonding Observed for Ion-Implanted BN, B4C and CNx Films With B-C-N Films
Erman Bengu, Mustafa Fatih Genisel (Bilkent University, Turkey)

The ternary compounds of the B-C-N phase diagram have attracted much attention because it is potentially possible to combine unique properties of different compounds into one and, synthesize new ones. Hence, there is still much effort to synthesize crystalline ternary compounds of B-C-N. However, deposited films were mostly either amorphous or a mixture of h-BN and C/CNx phases, even though there were numerous claims of hybrid films. In this study, in an effort to investigate chemical bonding and better document phase separation in B-C-N films, we have deposited h-BN, a-B4C and CNx thin films using reactive magnetron sputtering on Si (100) surfaces. Then, these films were subjected to ion-implantation by 40 keV C+, N2+ and N+ ions. After implantation, chemical bonding in these films were investigated using X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared (FT-IR) spectroscopy. Local variations in structure for these films were also investigated by high-resolution transmission electron microscopy (HR-TEM ) and electron energy loss spectroscopy (EELS) was employed to investigate chemical environment of boron, carbon and nitrogen in these films. Similar data gathered by XPS, FT-IR and TEM studies on sputter deposited B-C-N films were comparatively examined, as well. Results from these studies indicated boron-nitrogen bond to be preferred over carbon-nitrogen or boron-carbon over a wide range of process parameters for B-C-N films. Hence, carbon tends to phase-segregate in to carbon clusters rather than displaying a homogeneous distribution in the both the implanted and deposited films.

2:30 PM D1-4 Challenges in the Industrial-Scale Deposition of Thick Amorphous and Fullerene-Like Carbon Nitride Coatings
Esteban Broitman (Carnegie Mellon University); Lars Hultman (Linköping University)

During the last two decades, carbon-nitride (CNx) coatings have enjoyed a growing interest in several disciplines. Amorphous and fullerene-like films exhibit very attractive properties, such as low friction and wear, high hardness, good chemical stability, and high resiliency to deformation, which make them suitable for replacing diamond-like carbon (DLC) films. The first successful industrial application of this material has been the use of very thin (~2 nm) amorphous CNx films for the protection of hard disk drives. However, commercial use of thicker (1-5 µm) coatings on steel substrates has been difficult because of the development of high compressive intrinsic stresses during deposition, which causes delamination unless the coating/substrate adhesion can be improved.

In 2007, we reported a pretreatment using high power impulse magnetron sputtering (HIPIMS) technology that overcomes the adhesion issue. We thus demonstrated the possibility to deposit thick amorphous CNx coatings on steel substrates at low temperature (< 200oC) using an industrial mass-production chamber CemeCon CC800. In this presentation, different strategies to increase the adhesion of carbon-based coatings to steel substrates will be reviewed. Our novel approach, using two HIPIMS power supplies in a master-slave configuration (one to establish the discharge and one to produce a pulsed substrate bias), will be discussed. Plasma processes during our pretreatment leading to the formation of a Cr interface will be described. The structural, mechanical, and tribological properties of amorphous and fullerene-like CNx coatings deposited in both laboratory and industrial-scale systems will be compared by characterization techniques like HREM, SEM, XPS, ESR, nanoindentation, surface energy drop wetting angle, pin on disk, scratch and Daimler-Benz Rockwell-C tests. Finally, commercial applications of CNx coatings will be envisioned.
3:10 PM D1-6 Texture Development and Microstructure Characterization of Piezoelectric AlN Thin Films Fabricated by Pulsed Closed FieldUnbalanced Magnetron Sputtering
Masood Hasheminiasari, John J. Moore, Brajendra Mishra (Colorado School of Mines)

Piezoelectric aluminum nitride (AlN) thin films were synthesized by reactive sputtering of Al metal target in different nitrogen-argon gas ratio atmosphere using a pulsed closed field unbalanced magnetron sputtering system on various substrates with thin Cr electrodes. The texture, orientation and the microstructure of AlN films were characterized by means of X-ray diffraction and scanning electron microscopy. The mechanical properties of the coatings were studied using the XP nanoindenter. Impedance analyzer was used to characterize the piezoelectric properties of these films. It was found that reactive gas ratio, the pulsing frequency and the working pressure significantly affected the (002) orientation in AlN films. Strong (002) orientation has been achieved in the AlN thin films under various pulsing conditions, which can be correlated to the high ion energies associated with the pulsed magnetron sputtering.

3:30 PM D1-7 In-situ Stress Measurements During Growth of GaN(0001)/Al2O3(0001) by Reactive DC Magnetron Sputter Epitaxy
Muhammad Junaid, Per Sandström, Jens Birch (Linköping University, Sweden)

Growth of GaN by magnetron sputter epitaxy (MSE) has the potential to be used for high quality single crystalline epi-layer synthesis over large substrates at low temperatures. Development of growth stresses is a known issue in GaN epitaxy affect the material properties as well as devices performance and hence need to be controlled.

In-situ stress evolution during growth of GaN(0001) epilayers on (0001)-Al2O3 substrates has been studied during reactive MSE growth of 900 nm thick layers at different growth temperatures. A liquid Ga target was used and a working gas mixture of ultra pure Ar and N2 held at 2.5 and 2 mTorr partial pressures, respectively. The in-situ stress measurements were made by measuring the curvature induced to the substrate by the stress exerted by the growing film. The equipment used was a multi beam optical stress sensor (MOS), based on the deflection of multiple laser beams. The crystalline quality of the films was studied by using x-ray diffraction techniques.

At 750°C , we observed a continuous compressive stress evolution during the film growth, reaching a total film stress of ~200 MPa at the completion of the growth. The FWHM of HR-XRD rocking curves for these films are ~720 arc sec. which is indicates a high crystalline quality. In contrast to this result, a tensile stress of ~150MPa was observed in a film growing at 500°C. This film also has a comparatively low crystalline quality with a rocking curve FWHM of 1200 arc sec. After cooling down to room temperature all films are under compression due to the differences in thermal expansion coefficients between GaN and sapphire.

Our results are in contrast to in-situ stress studies on MOCVD-grown GaN(0001)/Al2O3(0001) where a tensile stress evolution to 200-400 MPa was observed during growth at 1000 °C. We attribute the origin of the compressive stresses in our films grown at 750 °C to atomic peening by energetic particle bombardment and/or coherency stresses due to a compressive substrate lattice mismatch. At 500°C, we conclude that tensile stresses due to cohesion over grain boundaries and annihilation of defects (caused by low adatom mobility) dominate over the effect of atomic peening.

Time Period WeA Sessions | Abstract Timeline | Topic D Sessions | Time Periods | Topics | ICMCTF2010 Schedule