Intrinsic stress of magnetron-sputtered niobium films

The stresses in niobium films were studied and the following preliminary results were obtained. (1) Niobium films can be prepared in any stress state (tensile, stress free or compressive) by varying the argon sputtering pressure. (2) As the bias voltage increases, more argon is incorporated into the film; both T_c and R/R₀ decrease; and the stress becomes more compressive and seems to saturate at about 1.5 × 10¹⁰ dyn cm^?2 at higher bias voltages (at an argon sputtering pressure of 1.9 Pa). (3) The lattice parameters show a close relation to the film stresses. (4) Lowering the sputtering rate results in a higher argon content in the bias-sputtered films. (5) The as-deposited film surface is smoother when deposited at lower pressures; the film has a columnar structure and intercolumnar gaps at higher pressures. (6) The film prepared at a higher bias voltage has a smoother as-deposited surface and a much smaller column size.From this study of the behavior of the stresses in niobium films, it appears that the stress is determined mainly by the microstructure and the energetic particle bombardment. Energetic particle bombardment may promote compressive stress by the incorporation of argon, by the formation of a more dense microstructure and by a “shot-peening” action.     

Evolutions of residual stress and microstructure in ZrO2 thin films deposited at different temperatures and rates

The residual stress in ZrO₂ thin films prepared by electron beam evaporation was measured by viewing the substrate deformation using an optical interferometer. The influences of deposition temperature and deposition rate on the residual stress have been studied. The results show that residual stress in ZrO₂ thin films varies from tensile to compressive depending on deposition temperature and deposition rate, respectively. The value of compressive stress increases with the increasing of deposition temperature and deposition rate. At the same time, X-ray diffraction measurement was carried out in order to examine the crystallization behavior of the ZrO₂ thin films as a function of deposition temperature and deposition rate. The relationship between the residual stress and the microstructure has also been discussed.     

Effect of substrate temperature and bias voltage on the crystallite orientation in RF magnetron sputtered AlN thin films

The crystal orientation and residual stress of AlN thin films were investigated using X-ray diffraction and substrate curvature method. The AlN films were deposited on Si(100) by RF magnetron sputtering in a mixed plasma of argon and nitrogen under various substrate negative bias V_s (up to − 100 V) and deposition temperature T_s up to 800 °C. The results show that lower temperature and moderate bias favor the formation of (002) plane parallel to the substrate surface. On the contrary, strong biasing beyond − 75 V and deposition temperature higher than 400 °C lead to the growth of (100) plane. At the same time nanoindentation hardness and compressive stress measured by substrate curvature method showed significant enhancement with substrate bias and temperature. The biased samples develop compressive stress while unbiased samples exhibit tensile or compressive stress depending on plasma power and temperature. The relationships between deposition conditions and crystallographic orientation of the films are discussed in terms of surface energy minimization and ion bombardment effects.     

Effect of lattice-mismatch strain on the structural and dielectric properties of (Pb,Sr)TiO3 thin films grown by pulsed laser deposition

Pb_0.35Sr_0.65TiO₃ (PST) thin films have been fabricated on LaAlO₃ (LAO) and MgO substrates using the pulsed laser deposition technique. The microstructure characteristics of the films were examined by means of X-ray diffraction, atomic force microscopy, scanning electron microscopy and Raman spectroscopy, and the results indicate that the films are epitaxially grown and show good crystallinity. The dielectric constant dependence on DC bias voltage and temperature were measured in a planar capacitor configuration for these films. Compared to the PST thin film grown on LAO, the film grown on MgO showed a higher temperature of the capacitance maximum and a higher dielectric constant at zero bias. We explain the results by taking into account the lattice-mismatch strain between the substrate and the film. In contrast to the in-plane compressive strain induced by the LAO substrate, the in-plane tensile strain induced by the MgO substrate enlarges the unit cell of PST and enhances the magnitude of dipole moments, which increases the dielectric constant. These results indicate that a reasonable in-plane tensile strain could improve the dielectric properties of PST thin films.     

交替频率PECVD方法沉积低应力氮化硅薄膜及其性质研究

用ＰＥＣＶＤ方法制备氮化硅薄膜,研究了射频频率对氮化硅薄膜的沉积和性质的影响。结果表明,在低频下（１００ＫＨｚ）制备的氮化硅薄膜密度较大,具有８ｘ１０９Ｐａ左右的压应力和较小的刻蚀速率;而高频（１３．５６ＭＨｚ）沉积的氮化硅薄膜密度较小,具体约２ｘ１０９Ｐａ的张应力,刻蚀速率较大。红外光谱表明,薄膜性质同薄膜中的氢原子成键情况有关。实验中利用高、低频交替沉积的方法,成功地制备了低应力（１０７Ｐａ）氮化硅薄膜。当加热到５００Ｃ时,应力较大的氮化硅薄膜会发生开裂（张应力）或拱起（压应力）。低应力的氮化硅薄膜能够承受７００Ｃ的温度,温度更高时,薄膜的完整性因氢溢出而破坏。     

Mechanical and thermal properties of physical vapour deposited alumina films Part I Thermal stability

Thermal stability of non-reactive physical vapour deposited alumina films of varying thickness on Al₂O₃-TiC and Si substrates, deposited at two different substrate biases, is examined. Substrate curvature measurements were used to determine the deposition stress and stress development during thermal cycling and annealing. Thermal cycling experiments revealed that the films deposited on Al₂O₃-TiC substrates become irreversibly more compressive on heating and annealing while films deposited on Si substrates become irreversibly more tensile. The deposition stress was found to be independent of film thickness, substrate material, and substrate bias during deposition. The thermal stability was independent of film thickness and substrate bias during deposition.     

Magnetron sputter deposition of low-stress, carbon-containing cubic boron nitride films using Ar―N2―CH4 gas mixtures

Cubic boron nitride (c-BN) films produced by PVD and plasma-assisted CVD techniques typically exhibit undesired high compressive stresses. One of the effective and feasible methods to reduce stress and hence improve film adhesion has been a controlled addition of a third element into the film during deposition. In the present study, BN films were grown on to silicon substrates using reactive magnetron sputtering with a hexagonal BN target. An auxiliary flow of methane was mixed into argon and nitrogen as the working gas. The deposition was conducted at various methane flow rates at 400 °C substrate temperature, 0.2 Pa total working pressure, and − 250 V r.f. substrate bias. The microstructure of the deposited films was then examined in dependence of the methane flow rate. With increasing methane flow rate from 0 to approx. 2.0 sccm, the fraction of the cubic BN phase in the deposited films decreased gradually down to approx. 75 vol.%, whereas the film stress was reduced much more rapidly and almost linearly in relation to the methane flow rate. At 2.1 sccm methane, the stress became approx. 3 times reduced. Owing to the significantly decreased film stress, adherent, micrometer thick, cubic-phase dominant films can be allowed to form on silicon substrate. The microstructure of the films will be illustrated through FTIR and XRR.     

Stress evolution in magnetron sputtered Ti-Zr-N and Ti-Ta-N films studied by in situ wafer curvature: Role of energetic particles

Stress evolution during reactive magnetron sputtering of binary TiN, ZrN and TaN thin films as well as ternary Ti-Zr-N and Ti-Ta-N solid-solutions was studied using real-time wafer curvature measurements. The energy of the incoming particles (sputtered atoms, backscattered Ar, ions) was tuned by changing either the metal target (M_Ti = 47.9, M_Zr = 91.2 and M_Ta = 180.9 g/mol), the plasma conditions (effect of pressure, substrate bias or magnetron configuration) for a given target or by combining different metal targets during co-sputtering. Experimental results were discussed using the average energy of the incoming species, as calculated using Monte-Carlo simulations (SRIM code). In the early stage of growth, a rapid evolution to compressive stress states is noticed for all films. A reversal towards tensile stress is observed with increasing thickness at low energetic deposition conditions, revealing the presence of stress gradients. The tensile stress is ascribed to the development of a ‘zone T’ columnar growth with intercolumnar voids and rough surface. At higher energetic deposition conditions, the atomic peening mechanism is predominant: the stress remains largely compressive and dense films with more globular microstructure and smooth surface are obtained.     

Measurement of the noibium/sapphire interface toughness via delamination

Niobium films were deposited on sapphire substrates using both physical vapor deposition (PVD) and ion beam assisted deposition (IBAD) at an ion energy of 1000 eV and an ion-to-atom arrival rate ratio of 0.4. The interface between the niobium film and the sapphire substrate was doped with up to 7.6 monolayers of silver. The films were patterned into fine lines using photolithography. During the photolithography process, curling and buckling were observed. The curling indicated a stress gradient in which the top of the film is tensile with respect to the bottom of the film, while buckling demonstrated that a portion of the film thickness must have been in compression. An analysis of the delamination showed that the critical energy release rate for the interface was on the order of 1 J m^–2, and that the compressive stress is of the order 1 GPa. The higher energy release rate of the IBAD samples confirmed that the stronger interface is due either to the orientation relationship between the ion beam textured niobium film and the (0001) sapphire surface or the interface mixing caused by ion bombardment.     

Deposition and characterization of reactive magnetron sputtered aluminum nitride thin films for film bulk acoustic wave resonator

This work studies the relationship between the deposition process parameters and the properties of sputtered c-axis-oriented aluminum nitride (AlN) thin films. AlN films were deposited on a Pt electrode by reactive magnetron sputtering under various deposition conditions. The films were characterized by X-ray diffraction (XRD) and field-emission scanning electron microscopy (FESEM). A polycrystalline AlN film with highly c-axis-preferred orientation was achieved. The XRD rocking curve was 2.7°. The FESEM photographs also show that the AlN film has a dense hexagonal surface texture with uniform grain size and a highly ordered column structure.     

Stress behavior of FCC metallic thin films during thermal evaporation

The development of stress in metallic thin films, monitored by in-situ curvature measurements during deposition, is analyzed. Three distinct stress regions including initial compressive, broad tensile, and incremental compressive stress were reported in terms of the film thickness (deposition time) by F. Spaepen. An experimental set-up was assembled for the in-situ curvature measurements utilizing vacuum thermal evaporation and multi-beam laser reflection points arrayed in x- and y-axis. The change in the spacing of laser reflected points was converted to the curvature of specimen, in turn, to instantaneous stress levels in the growing films using Stoney's formula. To investigate the effect on the distinct stress regions, the flux of the depositing metallic atoms was used as an experimental variable in this study. For the lowest flux cases for Cu and Ag, an additional second compressive stress stages after tensile maximum stress was observed in this study. Initial compressive part and tensile maximum stress regions appeared in shorter period of time for the thin films deposited at higher flux of atoms. Thus the flux of depositing atoms may affect the mechanisms of each stage. The initial compressive stress is conjectured to stem from the state of thin film surfaces; dynamic and relaxed surface. A broad tensile region is reported from the fact that the reduction of excess volume associated with grain boundaries and/or the coalescence of grains for high mobility materials. The incremental compressive stress region may be related to surface state and atomic mobilities.     

Residual stress on nanocrystalline silicon thin films deposited under energetic ion bombardment by using internal ICP-CVD

Nano/microcrystalline silicon thin films were deposited using an internal-type, inductively coupled, plasma-chemical vapor deposition (ICP-CVD) at room temperature by varying the bias power to the substrate. The structural characteristics of the deposited thin film were investigated. The deposition rate was increased by the application of a small RF bias power of 30 W (12.56 MHz), but was then decreased as the bias power was increased above 30 W. In addition, the application of bias power generally increased the residual compressive stress, which was attributed to the increased defect formation in the thin film due to the formation of interstitial atoms. The crystalline volume fraction was also decreased with increasing bias power. However, in the low bias power range of 0-60 W, the compressive stress in the deposited thin film was in the range of − 34 to − 77 MPa, which was lower than the residual stress in the range of − 150 to − 1050 MPa that is observed for the nano/microcrystalline silicon thin films deposited by capacitively coupled plasma.     

Mechanical properties of amorphous and microcrystalline silicon films

Hydrogen-free amorphous silicon (a-Si) films with thickness of 4.5-6.5 μm were prepared by magnetron sputtering of pure silicon. Mechanical properties (hardness, intrinsic stress, elastic modulus), and film structure (Raman spectra, electron diffraction) were investigated in dependence on the substrate bias and temperature. The increasing negative substrate bias or Ar pressure results in simultaneous reducing compressive stress, the film hardness and elastic modulus. Vacuum annealing or deposition of a-Si films at temperatures up to 600 °C saving amorphous character of the films, results in reducing compressive stress and increasing the hardness and elastic modulus. The latter value was always lower than that for monocrystalline Si(111). The crystalline structure (c-Si) starts to be formed at deposition temperature of ∼ 700 °C. The hardness and elastic modulus of c-Si films were very close to monocrystalline Si(111). Phase transformations observed in the samples at indentation depend not only on the load and loading rate but also on the initial phase of silicon. However, the film hardness is not too sensitive to the presence of phase transformations.     

The measurement of thin film stress using phase shifting interferometry

Abstract

A new technique for determining the stress of thin films is described. This technique combines digital phase shifting interferometry with image-processing software. A circular disc polished on one side is used as the coated substrate during film deposition. The average stress in thin films can be derived by comparing the deflection of the substrate before and after film deposition. The deflection of the substrate by the deposited film is obtained by the phase map. Using the Zernike polynomial fitting algorithm, a three-dimensional contour map is generated from the polynomial coefficients to visualize the deformation of the thin film and to examine the tensile or compressive stress after film deposition. Four oxide films prepared by ionbeam sputter deposition are investigated for their film stresses. The experimental results show that the stress values are concordant with measurements using other methods.     

Substrate biasing effects on the microstructure of magnetron-sputtered AlN films investigated by in situ reflectance interferometry

In situ reflectance interferometry (RI) at 400 nm wavelength was used to investigate the effect of the substrate negative bias on the microstructure of aluminium nitride (AlN) films deposited at room temperature on Si substrates by magnetron sputtering. Their surface reflectance recorded during film deposition promptly yields real-time information on the microstructures developed under oxygen contamination and bias change. Specifically, the refractive index n and the extinction coefficient k are deduced from reflectance using appropriate multilayer optical models and validated by spectroscopic ellipsometry. These optical constants correlate appreciably with the microstructure that evolves between columnar-crystallized and purely amorphous phases including in-between amorphous states containing dispersed nano-AlN grains. These microstructures were identified using ex situ energy dispersive X-ray spectroscopy, transmission electron microscopy and diffraction, X-ray diffraction and Auger electron spectroscopy. The simple and cost-effective in situ RI thus appears a powerful tool in controlling the microstructures of thin AlN films for desired applications.     

Effect of Nitrogen Content on Microstructures and Mechanical Properties of WB_2(N) Films Deposited by Reactive Magnetron Sputtering

In the present study,WB_2(N) films are fabricated on silicon and YG8 substrates at different N_2 pressures by reactive magnetron sputtering.The influence of N_2 partial pressure(P_(N2)) on the film microstructure and characteristics is studied systematically,including the chemical composition,crystalline structure,residual stress,surface roughness as well as the surface and the cross-section morphology.Meanwhile,nano-indentation and ball-on-disk tribometer are performed to analyze the mechanical and tribological properties of the films.The results show that the addition of nitrogen apparently leads to the change of the structure from(1 0 1) to(0 0 1) orientation then to the amorphous structure with the formation of BN phase.And the addition of nitrogen can greatly refine the grain size and microstructure of the films.Furthermore,the residual stress of the film is also found to change from tensile to compressive stress as a function of P_(N2),and the compressive stress increases with P_(N2),The WB_2(N) films with small nitrogen content,which are deposited at P_(N2) of 0.004 and 0.006 Pa,exhibit better mechanical,tribological and corrosion properties than those of other films.Further increase of nitrogen content accelerates the formation of BN phase and fast decreases the film hardness.In addition,the large N_2 partial pressure gives rise to the target poisoning accompanied by the increase of the target voltage and the decrease of the deposition rate.     

Ion beam sputter deposited Permalloy thin films

Ni₈₀Fe₂₀ thin films were deposited using a wide range of process parameters in a dual source ion beam sputter deposition system. The films were characterized structurally, chemically, and magnetically. Two modes of deposition were investigated; the first permitted concurrent second source bombardment during film deposition but was limited in net deposition rate to about 300 Å/m; the second provided deposition rates in excess of 1000 Å/m, but did not allow for concurrent ion bombardment from the second ion source. Depending on specific conditions film stress varied from slightly tensile to highly compressive in both deposition modes. This, combined with small variations in magnetostriction, resulted in films with vertical anisotropy and stripe domain patterns as well as conditions where well-formed closure domain patterns were observed in yoke shaped structures. For monolithic films, easy axis coercivities <0.7 Oe, anisotropy fields ≃5Oe and hard axis coercivities of <0.5 Oe were obtained     

基于AlN基板的不同Al组分的AlGaN材料生长

采用脉冲法生长了200nm厚的AlN薄膜,其XRD摇摆曲线的半高宽为130aresec,表面粗糙度为2.021nm.以此AIN层为基板生长了不同Al组分的AlGaN薄膜,高分辨率XRD测试发现,随Al组分的增加,AlN基板层对AlGaN薄膜施加的压应力增大,同时,AlGaN薄膜在生长合并过程中产生的张应力也增大.在Al组分为0.67时,发现这两种应力处于一种平衡的状态,此时的AlGaN薄膜有最优的结晶质量.     

Mechanical properties of SiNxCx ceramic films prepared by plasma CVD

The mechanical properties of Si₃N₄-SiC, SiN_x and SiC_y films prepared at a low temperature of 400 °C by plasma chemical vapour deposition are reported. Microhardness, internal stress of the film and adhesive strength between the film and glass or stainless steel substrate were evaluated as principal mechanical properties. Microhardness was measured to be about 10 to 20 G Pa dependent on the film composition in each system. Internal stress of the films on borosilicate glass substrates extensively varied from tensile to compressive with the film composition change from Si₃N₄ to SiC. Adhesive strength, as ascertained by the scratch test, was about 580 to 800 MPa for crown glass substrates, and about 210 to 310 M Pa for 316 stainless steel substrates. It is pointed out that tensile stress in these films brought about more abrupt decreases of the adhesive strength than did compressive stress.