Measurement of Elastic Modulus and Residual Stress of Diamond Thin Films

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.

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.


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

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.


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.


Micromachines ◽  
2021 ◽  
Vol 12 (9) ◽  
pp. 1072
Author(s):  
Sergio Sapienza ◽  
Matteo Ferri ◽  
Luca Belsito ◽  
Diego Marini ◽  
Marcin Zielinski ◽  
...  

3C-SiC is an emerging material for MEMS systems thanks to its outstanding mechanical properties (high Young’s modulus and low density) that allow the device to be operated for a given geometry at higher frequency. The mechanical properties of this material depend strongly on the material quality, the defect density, and the stress. For this reason, the use of SiC in Si-based microelectromechanical system (MEMS) fabrication techniques has been very limited. In this work, the complete characterization of Young’s modulus and residual stress of monocrystalline 3C-SiC layers with different doping types grown on <100> and <111> oriented silicon substrates is reported, using a combination of resonance frequency of double clamped beams and strain gauge. In this way, both the residual stress and the residual strain can be measured independently, and Young’s modulus can be obtained by Hooke’s law. From these measurements, it has been observed that Young’s modulus depends on the thickness of the layer, the orientation, the doping, and the stress. Very good values of Young’s modulus were obtained in this work, even for very thin layers (thinner than 1 mm), and this can give the opportunity to realize very sensitive strain sensors.


2009 ◽  
Vol 24 (9) ◽  
pp. 2974-2985 ◽  
Author(s):  
Erik G. Herbert ◽  
Warren C. Oliver ◽  
Maarten P. de Boer ◽  
George M. Pharr

A new method is proposed to determine the elastic modulus and residual stress of freestanding thin films based on nanoindentation techniques. The experimentally measured stiffness-displacement response is applied to a simple membrane model that assumes the film deformation is dominated by stretching as opposed to bending. Dimensional analysis is used to identify appropriate limitations of the proposed model. Experimental verification of the method is demonstrated for Al/0.5 wt% Cu films nominally 22 µm wide, 0.55 µm thick, and 150, 300, and 500 µm long. The estimated modulus for the four freestanding films match the value measured by electrostatic techniques to within 2%, and the residual stress to within 19.1%. The difference in residual stress can be completely accounted for by thermal expansion and a modest change in temperature of 3 °C. Numerous experimental pitfalls are identified and discussed. Collectively, these data and the technique used to generate them should help future investigators make more accurate and precise measurements of the mechanical properties of freestanding thin films using nanoindentation.


2014 ◽  
Vol 875-877 ◽  
pp. 1642-1646
Author(s):  
Jing Zhang

Alumina and zirconia are important materials for energy and optical applications. In this study, the effect of thermal cycling on grain size and residual stress was reported. Residual stress was measured using X-ray diffraction (XRD) sin2ψ method for the as-received and the samples after thermal cycling up to 900 cycles. For alumina, the measured residual stress is approximately 96 MPa in tensile for the as-received material, and increases to its highest value of 480 MPa after 650 thermal cycles. The residual stress decreases from 480 MPa to 96 MPa in tensile with increased thermal cycling from 650 to 900 cycles. The crystallized grain size calculated from the diffraction pattern shows that the mean crystallized grain size is about 93 nm for the as-received and increases to 232 nm after 650 thermal cycles. This result is consistent with the enlarged grain size observed by scanning electron microscopy for the alumina after 650 thermal cycles reported earlier. With continued thermal cycling up to 900 cycles, the crystallized grain size is greatly reduced to 104 nm. It suggests that evolution of the crystallized grain size is correlated with the residual stress. For yttria-stabilized tetragonal zirconia (Y-TZP), the mechanical properties at room temperature, are consistent with the property values provided by the manufacturer. The Young’s modulus of shows a non-linear inverse relationship with increasing temperature. The degradation of the Young’s modulus mostly occurs prior to 400 °C and to a less extent in the temperature range of 400 °C up to 850 °C. The Vickers hardness number for the as-received Y-TZP material decreases to a very small extent after 560 thermal cycles and increases approximately 2%, after 1200 thermal cycles. This is consistent with the trend of the Young’s modulus for thermal-cycled specimens.


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