ICMCTF2000 Session F1/E4-2: Mechanical Properties and Adhesion

Tuesday, April 11, 2000 1:30 PM in Room San Diego

Tuesday Afternoon

Time Period TuA Sessions | Abstract Timeline | Topic F Sessions | Time Periods | Topics | ICMCTF2000 Schedule

Start Invited? Item
1:30 PM F1/E4-2-1 Adhesion of Gold-Chrome Multilayer Films in Hybrid Microcircuits: Techniques for Assessing Thin Film Reliability
N.R. Moody (Sandia National Laboratories); A.A. Volinsky (University of Minnesota); D.P. Adams (Sandia National Laboratories); M.D. Kriese (Osmic, Inc.); W.W. Gerberich (University of Minnesota)
Interface structure and composition are two of the most important factors controlling the performance and reliability of thin films. They are especially important in gold-on-chrome hybrid microcircuits where the interfaces can change markedly during processing at elevated temperatures through diffusion and segregation. Nevertheless, the effect of these changes on durability is known only by relative comparisons. We have therefore begun a systematic study of how sputter deposition and exposure to elevated temperatures during post deposition processing affects susceptibility to fracture. Gold and gold-on-chrome films were sputter deposited following production procedures. Onto these films, a tantalum nitride overlayer was sputter deposited to apply a uniform compressive stress field. These stresses triggered interfacial delamination and blister formation in as-deposited films while additional stresses from nanoindentation were required to induce failure in the annealed films. From these blisters, fracture energies and interfacial bond strengths were obtained using the mechanics-based models modified for multilayer films. The results clearly showed that elevated temperature processing and the use of chrome interlayers enhanced adhesion. Furthermore, the results showed that adhesion is enhanced even when chrome is in solid solution. These results will be used in this presentation to show how interface composition affects film adhesion. They will also be used to show how small volume test techniques are being used to assess long term mechanical reliability of thin film systems. This work supported by U.S. DOE Contract DE-AC04-94AL85000.
2:10 PM F1/E4-2-3 Adhesion Strength of Electroplated Copper Films
C.H. Seah (Chartered Silicon Partners Pte Ltd, Republic of Singapore); S.B. Law, S. Mridha (Nanyang Technological University, Republic of Singapore); L.H. Chan (Chartered Semiconductor Manufacturing Ltd., Republic of Singapore)

In the rapidly expanding field of integrated circuits device fabrication, thin electroplated copper films are being deposited onto silicon wafer replacing the traditional aluminum as the interconnect material. As a result the adhesion of the copper film with the underlying seed and barrier layers have become of paramount importance. This study focused on the characterization of such films in term of scratch resistance and adhesion strength. Copper films were electroplated on thin layers of W/TiN/Si(100) and Cu/Ta/Si(100) substrates and the properties of these films were then characterized with a micro scratch tester using a diamond indenter of different sizes.

For the electroplated copper film on W seed, using a 200 µm tip, with an increased loading, minor delamination corresponding to damage along the sides of the scratch path was observed initially, followed by cracking at centre of the scratch. Finally a complete delamination of the film, causing tear of the film from the underlying substrate, was observed at a critical load of 16 N.

In the case of the film on Cu seed, no delamination was observed within the loading range up to 22 N under the 200 µm tip. When a 50 µm indenter was performed, a minor delamination was seen initially at a force of 4 N, and this delamination subsequently increased from 5 N onwards, however no full delamination was found within the loading range up to 22 N. The full delamination of the film on Cu seed occurred at 3 N when the scratch testing was performed using a 20 µm diamond tip. The failure phenomenon for the film on Cu seed is different from that on W seed. The initial failure caused by radial cracking in the film, which turned into chipping of the film as the loading force increased. The film then completely delaminated, causing substantial debris to be strewn along the scratch path.

2:30 PM F1/E4-2-4 Influence of Residual Stress Gradients on the Adhesion Strength of Sputtered Hard Coatings
H.K. Toenshoff, H. Seegers (University of Hannover, Germany)

Today's research activities covering the field of improving the properties of cutting tools are concentrated on optimizing manufacturing technologies and tool geometry as well as improved alloying of special cutting materials and coating of tools. Especially in the area of coated cutting inserts a high potential to enhance the wear resistance is still existing.

As a result of the reduced machinability of new cutting tool materials high mechanical and thermal loads during grinding influence the subsurface properties heavily. Hence, strong gradient residual stresses are induced in the subsurface of the tools during manufacturing. Even with optimized coating parameters deposited PVD-coatings fail due to insufficient subsurface properties of the substrates.

In this paper influences of residual stress distribution in subsurface layers on interface strength of PVD-coated carbides were investigated. The investigations were carried out with WC-based cemented carbides coated by PVD-deposited (TiAl)N layers. Considered topics are the influence of grinding and water peening on the subsurface residual stress state of the cemented carbide. Dependencies between stress distribution in subsurface layers and interface strength are highlighted.

X-ray measurements were carried out by using a new method for evaluating residual stress gradients. This stress gradients in the subsurface layers of the substrate were determined using the non-linear distribution of the diffraction angle versus the tilt angle in units of sin2Psi. Depth profiles of residual stress of ground and ground and waterpeened substrates before coating of the cemented carbide were determined. The results were compared with the well known sin2Psi-method using different lattice planes which correspond to different penetration depths. The adhesion and the wear behavior of the deposited coatings were analyzed in final cutting test during dry machining.

2:50 PM F1/E4-2-5 The influence of Er Doping of Al-N Sputtered Coatings on their Mechanical Properties
A. Cavaleiro, J.C. Oliveira, M.T. Vieira (ICEMS - FCT da Universidade de Coimbra, Portugal)
Thin films of AlN and AlN(Er) were deposited on M2 steel substrates using reactive magnetron sputtering starting from an aluminium target in Ar/N2 mixtures. AlN films with low nitrogen content show a f.c.c. Al structure while, near stoichiometry, crystalline and transparent AlN films were deposited. The deposition rate increases 1.5 times as the rf power is increased from 400 to 600 W. AlN(Er) films were deposited starting from the same aluminium target which was partially covered with erbium pieces. The incorporation of Er in Al-N films for N contents higher than 1.3 at. % leads to the amorphization of the structure. This study is part of a work which main objective is the development and optimisation of AlN(Er) thin films with luminescent properties suitable for use as sensors in the evaluation of the wear and the corrosion strength of mechanical components. For this purpose the mechanical properties of the AlN(Er) films are crucial since these films must be incorporated in the protective layers without disturbing the functional properties. The effect of nitrogen and erbium content on the hardness of the deposited films was studied by ultramicrohardness at a load of 50 nm. Scratch test was used to evaluate the adhesion/cohesion strength of the coatings.
3:30 PM F1/E4-2-7 Multi-pass Sub-critical Load Testing of Titanium Nitride Coatings
I. Efeoglu (Same, Turkey); R.D. Arnell (University of Salford, England)
TiN coatings deposited by closed field unbalanced magnetron sputter ion plating have been scratch tested in two modes. An initial conventional scratch test has been carried out to determine the critical load, and multiple scratches have been made over single tracks at different fractions of the critical load. It is shown that, even very high fractions of the critical load, the coatings do not fail adhesively or cohesively; rather, they simply become progressively thinner with successive passes of the diamond, Scanning electron microscopy of the worn surfaces has revealed a previously unobserved wear mechanism, and also shown that the coating adhesion can be truly described as perfect.
3:50 PM F1/E4-2-8 Evaluation of the Mechanical Properties and Tribological Behavior of the CrN Coating Deposited on Mild Steel Modified with Electroless Ni Interlayer
F.B. Wu, J.G. Duh (National Tsing Hua University, Taiwan)
Electroless nickel (EN) deposits are plated onto mild steel (MS) followed by the r.f. magnetron sputtered chromium nitride thin film. The tribological behavior and mechanical properties of coating assemblies including as-deposited EN, heat-treated EN, CrN and hybrid CrN/EN on mild steel are evaluated. A significant increase of the surface hardness of the CrN on mild steel (CrN/MS) assembly is achieved by the addition of the EN interlayer. The strengthening of the CrN/MS coating system by the modification of the Ni-P intermedia is further confirmed through the loading-unloading indentation analysis. For both scratch and wear test, cohesive failures are observed only in EN with higher phosphorous contents in the heat-treated EN/MS assembly. It is also revealed that the EN interlayer acts as a suitable buffer material underlaying the CrN film to provide required load-supporting function for CrN/MS assembly during the dry pin-on-disc sliding process. In addition, acoustic emission analysis is adopted to evaluate the failure modes in contact sliding process.
4:10 PM F1/E4-2-9 Study of Mechanical Behaviour of Thin PVD Coatings Using Several Instrumented Tribometers
Y. Gachon, C. Héau (HEF Research and Development, France)

Mechanical applications of Physical Vapour Deposited coatings are numerous. In many cases, the thickness of material deposited is not large enough to avoid transmission to the substrate of a significant part of applied stress during traditional tribological tests. The consequence is that coating removal generally corresponds to a failure of the substrate under the interface. It is therefore essential to investigate mechanical behaviour of the coating of its own.

To study damage mechanisms of the film a microtribometer was installed in the vacuum chamber of a scanning electron microscope. It was mainly used with ball on disc configuration but other are available like diamond on disc or cylinder on disc. During the tests friction coefficient is measured by strain gauges and recorded on a computer. A link can be directly established between this measure and mechanisms observed on the microscope screen. The image can be transmitted to a video recorder which allows afterward comparison of several tests. This technique equally allows to study friction behaviour of a coating under vacuum conditions.

During service life of a piece used for mechanical application, the superficial film generally encounters fatigue type sollicitation. It radically differs from regularly increasing load that is applied on classical scratch test apparatus. Using the sames hardness diamond indenters as on scratch test device, we performed tests on a pin on disc tribometer. During tests, the diamond undergo nearly no damage, which means that contact pressure remains constant. Another advantage is that the highest shear stress is located in the layer.

These techniques were tested on several types of hard layers produced by PVD (DLC, TiN, TiBN...) and brought numerous informations concerning their mechanical behaviour.

4:30 PM F1/E4-2-10 Tribological Behavior of Coated 8036 Steel with Ultrahard TiB2 by Using Pulsed Electrode Surfacing
M.H. Staia, A. Fragiel (Central University of Venezuela); B. Campillo (UNAM, Mexico); T.S. Sudarshan (Materials Modification Inc)
TiB2 has numerous exceptional properties including high hardness, high melting temperature and high electrical conductivity which make it an attractive candidate for technological application where wear and corrosion resistance at low and high temperature is required. The pulsed electrode surfacing (PES), which is a microwelding process, was adopted for depositing a sintered electrode of TiB2 with 2% Fe as a binder additive on 8036 steel substrate. Different coatings parameters (mode and the density current of the PES process) have been varied. Detailed characterization of the samples have been performed by using SEM, XRD and microhardness. Pin-on-disc tests were carried out to determine the friction and wear properties. The tests were performed under non-lubricated conditions in air with a relative humidity of 50±2% and an ambient temperature of 24±10C. Pins of 6 mm diameter, made from alumina, were loaded with a normal force of 5 N against the specimens and rotated with a sliding velocity of 0.1 m/s for a sliding distance of 1000 m. The depth profiles and the area of the wear tracks were evaluated by using profilometry. The evaluation of the wear resistance was conducted by calculating wear factor, k, considering that the wear volume is linearly proportional to the load and the sliding distance. Wear scars morphology were examined by using scanning electron microscopy technique (SEM). It was observed that although the friction coefficients did not varied with the deposition parameters ( µaverage = 0.5) the running-in values for the wear tests were different.
Time Period TuA Sessions | Abstract Timeline | Topic F Sessions | Time Periods | Topics | ICMCTF2000 Schedule