Mechanical testing and microstructural characterisation of TiN thin films

1997 ◽  
Vol 505 ◽  
Author(s):  
A. Karimi ◽  
O. R. Shojaei ◽  
J. L. Martin

ABSTRACTMechanical properties of titanium nitride (TiNx) thin films have been investigated using the bulge test and the depth sensing nanoindentation measurements. The bulge test was performed on the square free standing membranes made by means of standard micromachining of silicon wafers, while the nanoindentation was conducted on the films adhered to their supporting substrate. Thin layeres of titanium nitride (t = 300 – 1000 nm) were deposited in a r. f. magnetron sputtering system on the Si(100) wafers containing a layer of low stress LPCVD silicon nitride (SiNy). The bulge test was first conducted on the silicon nitride film to determine its proper residual stress and Young's modulus. Then, the composite membrane made of TiNx together with underlying silicon nitride was bulged and the related load-displacement variation was measured. Finally, using a simple rule of mixture formula the elastic mechanical properties of TiNx coatings were calculated. Both the Young's modulus and residual stress showed increasing values with negative bias voltage and nitrogen to titanium ratio, but the substrate temperature between 50–570°C was found less significant as compared to the other parameters. Nanoindentation data extracted from dynamically loading-unloading of TiN films converged to the bulge test measurements for compact coatings, but diverged from the bulge test data for porous coatings. Scanning electron microscopy observation of the cross sectioned specimens showed that TiN films first grow by formation of the nanocrystallites of size mostly between 10 – 15 nm. These nanocrystallites give rise to the columnar morphology beyond a thickness of 50–100 nm. The columns change their aspect with deposition parameters, but remain nearly perpendicular to the film surface. Relationship between microstructural evolution of columns and mechanical properties of coatings are discussed in terms of deposition parameters.

2007 ◽  
Vol 329 ◽  
pp. 545-550 ◽  
Author(s):  
Dao Hui Xiang ◽  
Ming Chen ◽  
Y.P. Ma ◽  
Fang Hong Sun

Despite great advancements in diamond thin film growth and deposition techniques, determination of the residual stress and Young’s modulus for diamond films has continued to be a challenge. The bulge test is a potentially powerful tool for characterizing the mechanical properties of diamond film. In a bulge tester, pressure is applied on a thin membrane and the out-of-plane deflection of the membrane center is measured. The Young’s Modulus and the residual stress are simultaneously determined by using the load-deflection behavior of a membrane. By means of electron-enhanced hot filament chemical vapor deposition (HFCVD), a diamond film was deposited on silicon slice (100), and the free-standing window sample of diamond thin films was fabricated by means of photolithography and anisotropic wet etching. The deflection of the membranes is measured using a laser interferometry system. The elastic modulus and residual stress were measured using a self-designed bulge equipment. In addition, the distortion of diamond thin films under different pressure was simulated using finite element analysis and the contrast was made with experimental data. The research indicated that the Young’s Modulus of diamond thin films is 937.8GPa and the residual stress is -10.53MPa. The elastic modulus and the residual stress coincide with the report in the literature and the value tested by X-ray diffraction, respectively. This method uses a simple apparatus, and the fabrication of samples is very easy, and it has provided an effective means for precise measure the mechanical properties of other thin films.


1999 ◽  
Vol 594 ◽  
Author(s):  
T. Y. Zhang ◽  
Y. J. Su ◽  
C. F. Qian ◽  
M. H. Zhao ◽  
L. Q. Chen

AbstractThe present work proposes a novel microbridge testing method to simultaneously evaluate the Young's modulus, residual stress of thin films under small deformation. Theoretic analysis and finite element calculation are conducted on microbridge deformation to provide a closed formula of deflection versus load, considering both substrate deformation and residual stress in the film. Silicon nitride films fabricated by low pressure chemical vapor deposition on silicon substrates are tested to demonstrate the proposed method. The results show that the Young's modulus and residual stress for the annealed silicon nitride film are respectively 202 GPa and 334.9 MPa.


Micromachines ◽  
2019 ◽  
Vol 10 (12) ◽  
pp. 801 ◽  
Author(s):  
Jaweb Ben Messaoud ◽  
Jean-François Michaud ◽  
Dominique Certon ◽  
Massimo Camarda ◽  
Nicolò Piluso ◽  
...  

The stress state is a crucial parameter for the design of innovative microelectromechanical systems based on silicon carbide (SiC) material. Hence, mechanical properties of such structures highly depend on the fabrication process. Despite significant progresses in thin-film growth and fabrication process, monitoring the strain of the suspended SiC thin-films is still challenging. However, 3C-SiC membranes on silicon (Si) substrates have been demonstrated, but due to the low quality of the SiC/Si heteroepitaxy, high levels of residual strains were always observed. In order to achieve promising self-standing films with low residual stress, an alternative micromachining technique based on electrochemical etching of high quality homoepitaxy 4H-SiC layers was evaluated. This work is dedicated to the determination of their mechanical properties and more specifically, to the characterization of a 4H-SiC freestanding film with a circular shape. An inverse problem method was implemented, where experimental results obtained from bulge test are fitted with theoretical static load-deflection curves of the stressed membrane. To assess data validity, the dynamic behavior of the membrane was also investigated: Experimentally, by means of laser Doppler vibrometry (LDV) and theoretically, by means of finite element computations. The two methods provided very similar results since one obtained a Young’s modulus of 410 GPa and a residual stress value of 41 MPa from bulge test against 400 GPa and 30 MPa for the LDV analysis. The determined Young’s modulus is in good agreement with literature values. Moreover, residual stress values demonstrate that the fabrication of low-stressed SiC films is achievable thanks to the micromachining process developed.


2003 ◽  
Vol 16 (2) ◽  
pp. 46-54 ◽  
Author(s):  
Jay S. Mitchell ◽  
Christian A. Zorman ◽  
Thomas Kicher ◽  
Shuvo Roy ◽  
Mehran Mehregany

2003 ◽  
Vol 782 ◽  
Author(s):  
Wen-Hsien Chuang ◽  
Thomas Luger ◽  
Rainer K. Fettig ◽  
Reza Ghodssi

ABSTRACTMechanical properties of micro-electro-mechanical systems (MEMS) materials at cryogenic temperatures are investigated to extend MEMS devices into space applications. A helium-cooled measurement setup mimicking the outer space environment is developed and installed inside a focused-ion-beam (FIB) system. T-shape, low-stress LPCVD silicon nitride cantilevers suspended on a silicon substrate are fabricated as the test structures using bulk micromachining technique. A lead-zirconate-titanate (PZT) translator and a silicon diode are utilized as an actuator and a temperature sensor in the measurement setup, respectively. The resonant frequencies of an identical cantilever with different “milling masses” are measured to obtain the thickness and the Young's modulus. Additionally, a bending test is performed to determine the fracture strength. From the experiments, the Young's modulus of LPCVD silicon nitride thin films varies from 260.5 GPa ± 5.4 GPa at room temperature (298 K) to 266.6 GPa ± 4.1 GPa at 30 K, while the fracture strength ranges from 6.9 GPa ± 0.6 GPa at room temperature to 7.9 GPa ± 0.7 GPa at 30 K.


2008 ◽  
Vol 33-37 ◽  
pp. 969-974 ◽  
Author(s):  
Bong Bu Jung ◽  
Seong Hyun Ko ◽  
Hun Kee Lee ◽  
Hyun Chul Park

This paper will discuss two different techniques to measure mechanical properties of thin film, bulge test and nano-indentation test. In the bulge test, uniform pressure applies to one side of thin film. Measurement of the membrane deflection as a function of the applied pressure allows one to determine the mechanical properties such as the elastic modulus and the residual stress. Nano-indentation measurements are accomplished by pushing the indenter tip into a sample and then withdrawing it, recording the force required as a function of position. . In this study, modified King’s model can be used to estimate the mechanical properties of the thin film in order to avoid the effect of substrates. Both techniques can be used to determine Young’s modulus or Poisson’s ratio, but in both cases knowledge of the other variables is needed. However, the mathematical relationship between the modulus and Poisson's ratio is different for the two experimental techniques. Hence, achieving agreement between the techniques means that the modulus and Poisson’s ratio and Young’s modulus of thin films can be determined with no a priori knowledge of either.


2000 ◽  
Vol 657 ◽  
Author(s):  
C.-F. Qian ◽  
Y.-J. Su ◽  
M.-H. Zhao ◽  
T.-Y. Zhang

ABSTRACTThe present work further develops the microbridge testing method to characterize mechanical properties of bilayer thin films. A closed-form formula for deflection versus load under small deflection is derived with consideration of the substrate deformation and residual stress in each layer. The analysis shows that the solution for bending a bilayer beam is equivalent to that for bending a single-layer beam with an equivalent bending stiffness, an equivalent residual force and a residual moment. One can estimate the Young's modulus and residual stress in a layer if the corresponding values in the other layer are known. The analytic results are confirmed by finite element calculations. The microbridge tests are conducted on low-temperature-silicon oxide (LTO)/silicon nitride bilayer films as well as on silicon nitride single-layer films. All microbridge specimens are prepared by the microfabricating technique. The tests on the single-layer films provide the material properties of the silicon nitride films. Then, applying the proposed method for bilayer films under small deflection yields the Young's modulus of 37 GPa and the residual stress of -148 MPa for LTO films.


2015 ◽  
Vol 742 ◽  
pp. 773-777
Author(s):  
Qun Feng Yang ◽  
Jian Yi Zheng ◽  
Jun Qing Wang ◽  
Jun Hui Lin ◽  
Xue Nan Zhao ◽  
...  

The purpose of this work is to study the mechanical characteristics of the silicon nitride(SiNx) thin films prepared by PECVD technique, some researches as follows were carried out. First, the SiNx thin films were deposited on the two different substrates. Then, the atomic force microscope (AFM) was adopted to test the surface quality of the SiNxfilms, and the scanning electron microscope (SEM) was used to test the section morphology of the SiNxthin films. Finally, the rotating beam structures was applied to measure the residual stress in the SiNx films. The SiNxthin films with low stress can be fabricated through PECVD, in which the surface roughness values(Ra) are 1.261 nm and 2.383nm, and the residual stress is 43.5 kPa. Therefore, the SiNxthin films deposited by PECVD are suitable for the preparation of device dielectric films in MEMS.


2005 ◽  
Vol 297-300 ◽  
pp. 574-580 ◽  
Author(s):  
Takahiro Namazu ◽  
Shozo Inoue ◽  
Daisuke Ano ◽  
Keiji Koterazawa

This paper focuses on investigating mechanical properties of micron-thick polycrystalline titanium nitride (TiN) films. We propose a new technique that can directly measure lateral strain of microscale crystalline specimen by X-ray diffraction (XRD) during tensile test. The XRD tensile test can provide not only Young’s modulus but also Poisson’s ratio of TiN films. Micron-thick TiN films were deposited onto both surfaces of single crystal silicon (Si) specimen by r.f. reactive magnetron sputtering. Young’s modulus and Poisson’s ratio of Si specimen obtained by XRD tensile tests were in good agreement with analytical values. TiN films deposited at Ar partial pressure of 0.7Pa had the average values of 290GPa and 0.36 for Young’s modulus and Poisson’s ratio. The elastic mechanical properties of TiN films gradually decreased down to 220GPa and 0.29 with increasing Ar partial pressure up to 1.0Pa, regardless of film thickness. The change in the film properties with Ar partial pressure would be attributed to the change in the film density.


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