Origins of Residual Stress in Mo and Ta Films: the Role of Impurities, Microstructural Evolution, and Phase Transformations

1996 ◽  
Vol 436 ◽  
Author(s):  
L. J. Parfitt ◽  
O. P. Karpenko ◽  
Z. U. Rek ◽  
S. M. Yalisove ◽  
J. C. Bilello

AbstractBoth the sign and magnitude of residual stress can vary with the thickness of sputter deposited films. The origins of this behavior are not well understood. In this work, we consider the correlation between the residual stress behavior and the depth dependence of impurities in thin (2.5 nm - 150 nm) sputtered Mo and Ta films. We also consider the effects of phase transformations and microstructural changes on the stress behavior. Films were deposited onto Si substrates with native oxide. The residual stress observed in the Mo films varied from highly compressive at 2.5 nm film thickness to ∼ 0 ˜ 10 nm thickness. Ta films also exhibited a high compressive stress, which relaxed from highly compressive to tensile between 10 nm and 50 nm film thickness. Impurities in the films may originate from the sputtering targets, the background gases, and the substrate surfaces. Auger Electron Spectroscopy (AES) results showed the presence of O and C contamination near the film/Si interface; these impurities contributed to the compressive stresses in the thinner films. As anticipated, both Mo and Ta films exhibited grain growth as a function of film thickness, which may have contributed to the relaxation in the compressive stress. The Mo films were entirely bcc. The Ta films showed a transformation from the amorphous phase to the β crystalline phase between 2.5 nm and 20 nm film thickness, which contributed to the relaxation in stress observed in that thickness regime.

1996 ◽  
Vol 441 ◽  
Author(s):  
L. J. Parfitt ◽  
Z. U. Rek ◽  
S. M. Yalisove ◽  
J. C. Bilello

AbstractResidual stress changed substantially between 2.5 and 80 nm film thickness in very thin Mo and Ta coatings sputtered onto Si substrates with native oxide. For both Mo and Ta, the thinnest films had a high compressive stress on the order of 2 to 3 GPa, and the stress relaxed, or became slightly tensile, with increasing film thickness. The coatings were examined using a variety of advanced characterization techniques including Auger Electron Spectroscopy (AES), Grazing Incidence X-ray Scattering (GIXS), and High Resolution Transmission Electron Microscopy (HRTEM). AES showed the presence of 0 and C contamination at the interface between the substrate and the film; these impurities originated from the adsorbed species and the native oxide on the surface of the wafers. GIXS analysis of the Mo films showed that the lattice of the thinnest layers was considerably expanded compared to the interplanar spacing of bulk, pure Mo. This expansion was caused by incorporation of impurities from the substrate into interstitial sites, which caused the very high compressive stress. HRTEM showed that the sputter deposition process did not alter the thickness of the native oxide layer, suggesting that the Mo and Ta films interacted with only the adsorbed impurities and the top one or two layers of the SiO2. Mo films deposited onto clean W layers were tensile, which supported the hypothesis that impurities caused the high compressive stresses in the films deposited onto SiO2. Grain growth and phase transformations contributed to the relaxation in stress observed in the thicker films.


1995 ◽  
Vol 397 ◽  
Author(s):  
M. Barth ◽  
J. Knobloch ◽  
P. Hess

ABSTRACTThe growth of high quality amorphous hydrogenated semiconductor films was explored with different in situ spectroscopic methods. Nucleation of ArF laser-induced CVD of a-Ge:H on different substrates was investigated by real time ellipsometry, whereas the F2 laser (157nm) deposition of a-Si:H was monitored by FTIR transmission spectroscopy. The ellipsometric studies reveal a significant influence of the substrate surface on the nucleation stage, which in fact determines the electronic and mechanical properties of the bulk material. Coalescence of initial clusters occurs at a thickness of 16 Å for atomically smooth hydrogen-terminated c-Si substrates, whereas on native oxide covered c-Si substrates the bulk volume void fractions are not reached until 35 Å film thickness. For the first time we present a series of IR transmission spectra with monolayer resolution of the initial growth of a-Si:H. Hereby the film thickness was measured simultaneously using a quartz crystal microbalance with corresponding sensitivity. The results give evidence for cluster formation with a coalescence radius of about 20 Å. Difference spectra calculated for layers at different depths with definite thickness reveal that the hydrogen-rich interface layer stays at the substrate surface and does not move with the surface of the growing film. The decrease of the Urbach energy switching from native oxide to H-terminated substrates suggests a strong influence of the interface morphology on the bulk material quality.


1989 ◽  
Vol 168 ◽  
Author(s):  
S.-L. Zhang ◽  
R. Buchta ◽  
M. Östling

AbstractTungsten disilicide (WSi2 ) was formed by annealing 185 nm and 750 nm thick LPCVD-W films deposited on <100>-Si substrates. The thickness of the formed WSi2 was observed by Rutherford backscattering measurements (RBS) to increase parabolically with the annealing time. This agrees with the behavior reported in the literature for sputter deposited or evaporated W films. However, a higher stlicide growth rate was found in this work. An activation energy of 2.6 eV/atom was measured, which is smaller than those for sputter deposited or evaporated W films. The crystal structures of the formed WSi2 and the unreacted W films were analyzed using X-ray diffraction (XRD) technique. The thermal history of the samples was found to play an important role for the crystal structure of the unreacted W and formed WSi2. The as-deposited W films became more oriented to the <100> direction with increasing film thickness, while the unreacted W films on top of the formed WSi2, from the samples annealed at temperatures from 700 to 800°C, became more <100> direction dominated with decreasing W film thickness. The preferred orientation of the grown WSi2 films also varied with the silicidation conditions. These observations indicate that the simple method of determining W film thickness by comparing the W diffraction peak heights of the remaining W films after heat treatment to a reference sample will unavoidably introduce large errors. A compensation technique was suggested where both the W and WSi2 diffraction signals were used. A parameter x, a function of reacted W thickness, was introduced to fit the compensation procedure. The conclusion of this study is that attention should be paid to the orientation change of W and WSi2 films during heat treatment if XRD is employed to study the kinetics of WSi2 formation.


1997 ◽  
Vol 472 ◽  
Author(s):  
Tilo P. Drüsedau ◽  
Frank Klabunde ◽  
Mirko Lohmann ◽  
Thomas Hempel ◽  
Jurgen Bläsing

ABSTRACTThe crystallite size and orientation in molybdenum films prepared by magnetron sputtering at a low rate of typical 1 Å/s and a pressure of 0.45 Pa was investigated by X-ray diffraction and texture analysis. The surface topography was studied using atomic force microscopy. Increasing the film thickness from 20 nm to 3 μm, the films show a turnover from a (110) fiber texture to a (211) mosaic-like texture. In the early state of growth (20 nm thickness) the development of dome-like structures on the surface is observed. The number of these structures increases with film thickness, whereas their size is weakly influenced. The effect of texture turnover is reduced by increasing the deposition rate by a factor of six, and it is absent for samples mounted above the center of the magnetron source. The effect of texture turnover is related to the bombardment of the films with high energetic argon neutrals resulting from backscattering at the target under oblique angle and causing resputtering. Due to the narrow angular distribution of the reflected argon, bombardment of the substrate plane is inhomogeneous and only significant for regions close to the erosion zone of the magnetron.


Author(s):  
S. Yegnasubramanian ◽  
V.C. Kannan ◽  
R. Dutto ◽  
P.J. Sakach

Recent developments in the fabrication of high performance GaAs devices impose crucial requirements of low resistance ohmic contacts with excellent contact properties such as, thermal stability, contact resistivity, contact depth, Schottky barrier height etc. The nature of the interface plays an important role in the stability of the contacts due to problems associated with interdiffusion and compound formation at the interface during device fabrication. Contacts of pure metal thin films on GaAs are not desirable due to the presence of the native oxide and surface defects at the interface. Nickel has been used as a contact metal on GaAs and has been found to be reactive at low temperatures. Formation Of Ni2 GaAs at 200 - 350C is reported and is found to grow epitaxially on (001) and on (111) GaAs, but is shown to be unstable at 450C. This paper reports the investigations carried out to understand the microstructure, nature of the interface and composition of sputter deposited and annealed (at different temperatures) Ni-Sb ohmic contacts on GaAs by TEM. Attempts were made to correlate the electrical properties of the films such as the sheet resistance and contact resistance, with the microstructure. The observations are corroborated by Scanning Auger Microprobe (SAM) investigations.


Coatings ◽  
2020 ◽  
Vol 11 (1) ◽  
pp. 23
Author(s):  
Weiguang Zhang ◽  
Jijun Li ◽  
Yongming Xing ◽  
Xiaomeng Nie ◽  
Fengchao Lang ◽  
...  

SiO2 thin films are widely used in micro-electro-mechanical systems, integrated circuits and optical thin film devices. Tremendous efforts have been devoted to studying the preparation technology and optical properties of SiO2 thin films, but little attention has been paid to their mechanical properties. Herein, the surface morphology of the 500-nm-thick, 1000-nm-thick and 2000-nm-thick SiO2 thin films on the Si substrates was observed by atomic force microscopy. The hardnesses of the three SiO2 thin films with different thicknesses were investigated by nanoindentation technique, and the dependence of the hardness of the SiO2 thin film with its thickness was analyzed. The results showed that the average grain size of SiO2 thin film increased with increasing film thickness. For the three SiO2 thin films with different thicknesses, the same relative penetration depth range of ~0.4–0.5 existed, above which the intrinsic hardness without substrate influence can be determined. The average intrinsic hardness of the SiO2 thin film decreased with the increasing film thickness and average grain size, which showed the similar trend with the Hall-Petch type relationship.


1998 ◽  
Vol 541 ◽  
Author(s):  
S. Tirumala ◽  
S. O. Ryu ◽  
K. B. Lee ◽  
R. Vedula ◽  
S. B. Desu

AbstractThe effect of various electrode materials on the ferroelectric properties of SrBi2Ta2O9 (SBT) thin films has been investigated for non-volatile memory applications. Two sets of electrode structures, viz., Pt-Ir based and Pt-Rh based, were sputter deposited in-situ on Si substrates. SBT thin films were deposited on these electrodes using a metal-organic solution deposition technique followed by a post-deposition anneal at 750 °C in oxygen. Structural characterization revealed a polycrystalline nature with predominant perovskite phase in SBT thin films. Ferroelectric properties were studied in capacitor mode by depositing top electrodes, where the top electrode material is identical to that of the bottom electrode. Extensive analysis of the ferroelectric properties signify the important role played by the electrode material in establishing the device applicability is reported in this work.


1991 ◽  
Vol 226 ◽  
Author(s):  
Hideo Miura ◽  
Hiroshi Sakata ◽  
Shinji Sakata Merl

AbstractThe residual stress in silicon substrates after local thermal oxidation is discussed experimentally using microscopic Raman spectroscopy. The stress distribution in the silicon substrate is determined by three main factors: volume expansion of newly grown silicon–dioxide, deflection of the silicon–nitride film used as an oxidation barrier, and mismatch in thermal expansion coefficients between silicon and silicon dioxide.Tensile stress increases with the increase of oxide film thickness near the surface of the silicon substrate under the oxide film without nitride film on it. The tensile stress is sometimes more than 100 MPa. On the other hand, a complicated stress change is observed near the surface of the silicon substrate under the nitride film. The tensile stress increases initially, as it does in the area without nitride film on it. However, it decreases with the increase of oxide film thickness, then the compressive stress increases in the area up to 170 MPa. This stress change is explained by considering the drastic structural change of the oxide film under the nitride film edge during oxidation.


1993 ◽  
Vol 8 (10) ◽  
pp. 2608-2612 ◽  
Author(s):  
C. Spinella ◽  
F. Benyaïch ◽  
A. Cacciato ◽  
E. Rimini ◽  
G. Fallico ◽  
...  

The early stages of the thermally induced epitaxial realignment of undoped and As-doped polycrystalline Si films deposited onto crystalline Si substrates were monitored by transmission electron microscopy. Under the effect of the heat treatment, the native oxide film at the poly-Si/c-Si interface begins to agglomerate into spherical beads. The grain boundary terminations at the interface are the preferred sites for the triggering of the realignment transformation which starts by the formation of epitaxial protuberances at these sites. This feature, in conjunction with the microstructure of the films during the first instants of the heat treatment, explains the occurrence of two different realignment modes. In undoped films the epitaxial protuberances, due to the fine grain structure, are closely distributed and grow together forming a rough interface moving toward the film's surface. For As-doped films, the larger grain size leaves a reduced density of realignment sites. Due to As doping some of these sites grow fast and form epitaxial columns that further grow laterally at the expense of the surrounding polycrystalline grains.


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