Oili M. E. Ylivaara

Microscratch testing method for systematic evaluation of the adhesion of atomic layer deposited thin films on silicon

The scratch test method is widely used for adhesion evaluation of thin films and coatings. Usual critical load criteria designed for scratch testing of coatings were not applicable to thin atomic layer deposition (ALD) films on silicon wafers. Thus, the bases for critical load evaluation were established and the critical loads suitable for ALD coating adhesion evaluation on silicon wafers were determined in this paper as LCSi1, LCSi2, LCALD1, and LCALD2, representing the failure points of the silicon substrate and the coating delamination points of the ALD coating. The adhesion performance of the ALD Al2O3, TiO2, TiN, and TaCN+Ru coatings with a thickness range between 20 and 600 nm and deposition temperature between 30 and 410 °C on silicon wafers was investigated. In addition, the impact of the annealing process after deposition on adhesion was evaluated for selected cases. The tests carried out using scratch and Scotch tape test showed that the coating deposition and annealing temperature, thickness of...

X-ray reflectivity characterization of atomic layer deposition Al2O3/TiO2 nanolaminates with ultrathin bilayers

Nanolaminate structures have many prospective uses in mechanical, electrical, and optical applications due to the wide selection of materials and precise control over layer thicknesses. In this work, ultrathin Al2O3/TiO2 nanolaminate structures deposited by atomic layer deposition from Me3Al, TiCl4, and H2O precursors with intended bilayer thicknesses ranging from 0.1 to 50 nm were characterized by x-ray reflectivity (XRR) measurements. The measurements were simulated to obtain values for thickness, density, and roughness of constituting layers. XRR analysis shows that the individual layers within the nanolaminate remain discrete for bilayers as thin as 0.8 nm. Further reduction in bilayer thickness produces a composite of the two materials.

Thermal conductivity of amorphous Al2O3/TiO2 nanolaminates deposited by atomic layer deposition

The thermophysical properties of Al2O3/TiO2 nanolaminates deposited by atomic layer deposition (ALD) are studied as a function of bilayer thickness and relative TiO2 content (0%-100%) while the total nominal thickness of the nanolaminates was kept at 100 nm. Cross-plane thermal conductivity of the nanolaminates is measured at room temperature using the nanosecond transient thermoreflectance method. Based on the measurements, the nanolaminates have reduced thermal conductivity as compared to the pure amorphous thin films, suggesting that interfaces have a non-negligible effect on thermal transport in amorphous nanolaminates. For a fixed number of interfaces, we find that approximately equal material content of Al2O3 and TiO2 produces the lowest value of thermal conductivity. The thermal conductivity reduces with increasing interface density up to 0.4 nm(-1), above which the thermal conductivity is found to be constant. The value of thermal interface resistance approximated by the use of diffuse mismatch model was found to be 0.45 m(2) K GW(-1), and a comparative study employing this value supports the interpretation of non-negligible interface resistance affecting the overall thermal conductivity also in the amorphous limit. Finally, no clear trend in thermal conductivity values was found for nanolaminates grown at different deposition temperatures, suggesting that the temperature in the ALD process has a non-trivial while modest effect on the overall thermal conductivity in amorphous nanolaminates.

Aluminum oxide/titanium dioxide nanolaminates grown by atomic layer deposition: Growth and mechanical properties

Atomic layer deposition (ALD) is based on self-limiting surface reactions. This and cyclic process enable the growth of conformal thin films with precise thickness control and sharp interfaces. A multilayered thin film, which is nanolaminate, can be grown using ALD with tuneable electrical and optical properties to be exploited, for example, in the microelectromechanical systems. In this work, the tunability of the residual stress, adhesion, and mechanical properties of the ALD nanolaminates composed of aluminum oxide (Al 2O3) and titanium dioxide (TiO2) films on silicon were explored as a function of growth temperature (110–300 °C), film thickness (20–300 nm), bilayer thickness (0.1–100 nm), and TiO2 content (0%–100%). Al 2O3 was grown from Me3 Al and H2O, and TiO2 from TiCl4 and H2O. According to wafer curvature measurements, Al 2O3/TiO2 nanolaminates were under tensile stress; bilayer thickness and growth temperature were the major parameters affecting the stress; the residual stress decreased with increasing bilayer thickness and ALD temperature. Hardness increased with increasing ALD temperature and decreased with increasing TiO2 fraction. Contact modulus remained approximately stable. The adhesion of the nanolaminate film was good on silicon.

Bonding of ALD Alumina for Advanced SOI Substrates

Silicon on insulator (SOI) substrates have become important starting materials for IC and MEMS fabrication. In some cases, it would be beneficial to add another buried material(s) or to replace the silicon dioxide film. By atomic layer deposition (ALD), various materials can be deposited with accurate thickness control as well as with high uniformity [1]. Amorphous ALD films are also generally sufficiently smooth to fulfill the requirements of direct wafer bonding. By using ALD films to deposit layers to be buried in SOI, the high-cost chemical–mechanical polishing step required to bond CVD thin films can be avoided.

Direct wafer bonding of atomic layer deposited TiO 2 and Al 2 O 3 thin films

In MEMS industry, silicon-on-insulator (SOI) wafers are gaining ground from blank silicon wafers as the main starting substrate. Tailored SOI wafers available in the market contain for example buried cavities or a buried gettering layer. Adding another layer in addition to the thermal SiO2 insulator, or replacing it with another material altogether, could be a way to tailor the properties of SOI wafers further. In this work, the direct wafer bonding of ALD TiO2, and Al2O3 for reference, is investigated, eventually in order to fabricate SOI wafers with other buried ALD oxides.

On the reliability of nanoindentation hardness of Al2O3 films grown on Si-wafer by atomic layer deposition

The interest in applying thin films on Si-wafer substrate for microelectromechanical systems devices by using atomic layer deposition (ALD) has raised the demand on reliable mechanical property data of the films. This study aims to find a quick method for obtaining nanoindentation hardness of thin films on silicon with improved reliability. This is achieved by ensuring that the film hardness is determined under the condition that no plastic deformation occurs in the substrate. In the study, ALD Al2O3 films having thickness varying from 10 to 600 nm were deposited on a single-side polished silicon wafer at 300 °C. A sharp cube-corner indenter was used for the nanoindentation measurements. A thorough study on the Si-wafer reference revealed that at a specific contact depth of about 8 nm the wafer deformation in loading transferred from elastic to elastic–plastic state. Furthermore, the occurrence of this transition was associated with a sharp increase of the power-law exponent, m, when the unloading data we...

Fracture properties of atomic layer deposited aluminum oxide free-standing membranes

The fracture strength of Al2O3 membranes deposited by atomic layer deposition at 110, 150, 200, and 300 °C was investigated. The fracture strength was found to be in the range of 2.25–3.00 GPa using Weibull statistics and nearly constant as a function of deposition temperature. This strength is superior to common microelectromechanical systems materials such as diamondlike carbon, SiO2, or SiC. As-deposited membranes sustained high cycling pressure loads >10 bar/s without fracture. Films featured, however, significant reduction in the resistance to failure after annealing (800 °C) or high humidity (95%, 60 °C) treatments.The fracture strength of Al2O3 membranes deposited by atomic layer deposition at 110, 150, 200, and 300 °C was investigated. The fracture strength was found to be in the range of 2.25–3.00 GPa using Weibull statistics and nearly constant as a function of deposition temperature. This strength is superior to common microelectromechanical systems materials such as diamondlike carbon, SiO2, or SiC. As-deposited membranes sustained high cycling pressure loads >10 bar/s without fracture. Films featured, however, significant reduction in the resistance to failure after annealing (800 °C) or high humidity (95%, 60 °C) treatments.

Tribological properties of thin films made by atomic layer deposition sliding against silicon

Interfacial phenomena, such as adhesion, friction, and wear, can dominate the performance and reliability of microelectromechanical (MEMS) devices. Here, thin films made by atomic layer deposition (ALD) were tested for their tribological properties. Tribological tests were carried out with silicon counterpart sliding against ALD thin films in order to simulate the contacts occurring in the MEMS devices. The counterpart was sliding in a linear reciprocating motion against the ALD films with the total sliding distances of 5 and 20 m. Al2O3 and TiO2 coatings with different deposition temperatures were investigated in addition to Al2O3-TiO2-nanolaminate, TiN, NbN, TiAlCN, a-C:H [diamondlike carbon (DLC)] coatings, and uncoated Si. The formation of the tribolayer in the contact area was the dominating phenomenon for friction and wear performance. Hardness, elastic modulus, and crystallinity of the materials were also investigated. The nitride coatings had the most favorable friction and wear performance of the...

Comparison of mechanical properties and composition of magnetron sputter and plasma enhanced atomic layer deposition aluminum nitride films

A comparative study of mechanical properties and elemental and structural composition was made for aluminum nitride thin films deposited with reactive magnetron sputtering and plasma enhanced atomic layer deposition (PEALD). The sputtered films were deposited on Si (100), Mo (110), and Al (111) oriented substrates to study the effect of substrate texture on film properties. For the PEALD trimethylaluminum–ammonia films, the effects of process parameters, such as temperature, bias voltage, and plasma gas (ammonia versus N2/H2), on the AlN properties were studied. All the AlN films had a nominal thickness of 100 nm. Time-of-flight elastic recoil detection analysis showed the sputtered films to have lower impurity concentration with an Al/N ratio of 0.95, while the Al/N ratio for the PEALD films was 0.81–0.90. The mass densities were ∼3.10 and ∼2.70 g/cm3 for sputtered and PEALD AlN, respectively. The sputtered films were found to have higher degrees of preferential crystallinity, whereas the PEALD films were more polycrystalline as determined by x-ray diffraction. Nanoindentation experiments showed the elastic modulus and hardness to be 250 and 22 GPa, respectively, for sputtered AlN on the (110) substrate, whereas with PEALD AlN, values of 180 and 19 GPa, respectively, were obtained. The sputtered films were under tensile residual stress (61–421 MPa), whereas the PEALD films had a residual stress ranging from tensile to compressive (846 to −47 MPa), and high plasma bias resulted in compressive films. The adhesion of both films was good on Si, although sputtered films showed more inconsistent critical load behavior. Also, the substrate underneath the sputtered AlN did not withstand high wear forces as with the PEALD AlN. The coefficient of friction was determined to be ∼0.2 for both AlN types, and their wear characteristics were almost identical.A comparative study of mechanical properties and elemental and structural composition was made for aluminum nitride thin films deposited with reactive magnetron sputtering and plasma enhanced atomic layer deposition (PEALD). The sputtered films were deposited on Si (100), Mo (110), and Al (111) oriented substrates to study the effect of substrate texture on film properties. For the PEALD trimethylaluminum–ammonia films, the effects of process parameters, such as temperature, bias voltage, and plasma gas (ammonia versus N2/H2), on the AlN properties were studied. All the AlN films had a nominal thickness of 100 nm. Time-of-flight elastic recoil detection analysis showed the sputtered films to have lower impurity concentration with an Al/N ratio of 0.95, while the Al/N ratio for the PEALD films was 0.81–0.90. The mass densities were ∼3.10 and ∼2.70 g/cm3 for sputtered and PEALD AlN, respectively. The sputtered films were found to have higher degrees of preferential crystallinity, whereas the PEALD films wer...