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(1) Freestanding thin films, small dimensional foils (Fig. 1(a)) and thin wires (Fig. 1(b)).
(2) Thin films confined by a substrate (Fig. 1(c)).
Irrespective of any type of these materials at least one dimension of the material should be in the range from
micrometers to nanometers [11].
(c) Substrate.
Fig.1. Schematic of the small-scale materials (a) freestanding thin foils/films, (b) fine
wires and (c) thin films confined by a substrate.
Nowadays, higher integration density in micro/nano systems is leading to material dimensions
(microstructural and geometrical dimensions) shrinking toward the submicrometer and nanometer scale.
Very few researches on mechanical characterization of micro-and nano-components were published
before the 1980s, but since, seems the micro-electromechanical systems MEMS, the number has become
significantly in increased. Numerous fatigue testing techniques for material specimens with characteristic size
ranging from few nanometers to several hundred micrometers, have been reported, investigated, developed,
described, and employed for determining mechanical fatigue testing techniques such as Uniaxial tension-tension,
Dynamic bending, Resonant vibration, Uniaxial tension-compression and Thermal-cyclic.
In this review we classify, describe, summarize, and compare all of these techniques that are currently
available. We prove what are the most used, why they are so popular, and what the actual vogue is. Furthermore,
we characterize the most studied materials and how the attention in them when changed with time.
2. Fatigue testing techniques and evaluation methods for small scale materials
Material mechanical properties are the basic input parameters for structural design of micro/ nano devices. The
accuracy of numerical modeling and simulation results depends on the accuracy of the material properties
provided as input. That is why, throughout the recent years several appropriate techniques are developed to
enhance the measuring accuracy or to increase the amount of the calculable mechanical quantities. We have a
tendency to present a classification of those techniques in Fig.2.
Fig.2. Classification of the fatigue testing techniques for materials at micro- and nano- scales.
To decrease the dimensions of materials into the micrometer nanometer scale. Some of new experimental
method investigated to measure fatigue properties, which is proposed that some of factors should be considered.
As shown below:
1- Ultra-low force load cell, closed-loop high resolution displacement actuator and PC-controlled data
acquisition system.
2- Reliable clamping method that can overcome the difficulty in mounting thin films without damaging.
3- Application of a simple and homogenous stress state which makes extraction of fatigue data and
comparison with bulk materials easier.
4- It is also anticipated to in-situ observe the fatigue damage process, such as fatigue crack initiation and
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Fig.4. Plot of maximum cyclic stress against the number of cycles to failure (S-N plot) for electron-beamevaporated copper thin-film specimens [16].
The experimental setup was a piezoelectric driven uniaxial stress-strain measurement system to
estimate fatigue properties of thin Ni films. The force calibration was linear over 0-1.50 N with a resolution of
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0.2 mN. The displacement range of the closed-loop piezoelectric actuator in the test apparatus was 0-90 m, with
a displacement measurement resolution of 1.8 nm. The frequency response of the piezoelectric actuator was up
to 103 Hz, which is enough to do the fatigue test. To simplify grip specimen, three-axis micro positioning system
and a CCD with remote microscope were used to locate designed of glass grip appropriately. Thus, a micro
electromechanical system (MEMS) was the based devices that used to manage the fatigue testing of very small
specimens (20m) for that attaching the specimen to the test equipment became very important.
While the tensiontension fatigue behavior of carbon nanotube wires have been studied by H.E. Misak
et al [18] and his coworker they conclude that the Three versions of CNT wires (30-, 60-, and 100-yarn) in the as
usual condition were tested to investigate their tensiontension fatigue behavior. Electrical conductivity of CNT
wires was also measured during fatigue tests. In order to establish fatigue-life diagrams (SN curves), fatigue
tests were conducted at different stress levels (35%, 50%, 60%, 75% and 80%) of ultimate tensile strengths and
at 0.1 Hz and R of 0.1. The applied stress versus cycles to failure data showed a linear correlation on the semilog diagram then resulted equations are shown below in Fig. 5.
Fig.5. Applied stress vs. number of cycle relationships of 100-, 60-, and 30- yarns CNT wires [18].
Fatigue life was reduced signicantly with an increasing number of yarns in the CNT wires. The major
damage under fatigue was caused by the formation of kink bands and tearing and breakage of strands in the wire.
These damage modes were caused by low resistance to shear force due to weak lateral bonds (van der Waals
forces, frictional forces, and mechanical interlocking) between CNTs. Electrical conductivity of CNT wires
increased with the increase in fatigue load and number of applied fatigue cycles. Micro CT density
measurements provided evidence that the increase in conductivity was due to the reduction of micro/nano voids
between and inside the yarns [19-22].
2.2 Dynamic bending
Instead of uniaxial tension-tension tests, mechanical properties of materials at micro/nanoscales can be
found from bending tests, which were sometimes preferred over tension tests, since they need smaller forces and
produce grander displacements. In this situation, micro-cantilever beams were affected by dynamic bending
under constant amplitude load control supplied by repeated indentation [23, 24].
Then, developed the fatigue machine for small-scale materials as shown in Fig.3 (b). Fatigue crack
growth tests were achieved by using a newly developed fatigue testing machine for micro sized specimens as
,where
) of 2mN and stress ratios
shown in Fig.6.Under constant amplitude load (
(
, where
is the minimum load and
is the maximum load applied over the
fatigue cycle) of 0.1, 0.3and 0.5. The fatigue machine has a displacement of 5nm and a load of 10m. the
machine can used different waveforms for frequencies and cyclic loading up to 100 Hz. And used two types of
cantilever beam micro sized specimens with different breadth were all set from an electroless plated Ni-P
amorphous alloy thin film by focused ion beam machining as shown in Fig 7.
After seeing the striations on the fatigue fracture surfaces and fatigue crack propagation rates were
evaluated by a careful measurement of the striation spacing. Found the fatigue crack growth rates at stress ratios
of 0.3 and 0.5 were almost similar, but the fatigue crack growth rate at a stress ratio of 0.1 were lower compared
to the others at a given value of K as shown in Fig. 8, and Fig. 9. Shown the fatigue crack growth resistance
was depending on the breadth of specimen [23].
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Fig.6. Block diagram of fatigue testing machine for micro sized specimens[23].
Fig.7. Two types of micro sized cantilever beam specimens with different breadth (B) prepared by focused ion
beam machining. (a) B=10mm and (b) B=30mm [23].
Fig.8. Fatigue crack growth resistance curves for micro sized Ni-P amorphous alloy specimens with a B
of 10m tested at different stress ratios [23].
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Fig.9. Fatigue crack growth resistance curves for micro size Ni-P amorphous alloy specimens with different B
tested at a stress ratio of 0.5 [23].
On the other hand, the cyclic loading of a free standing Ni-P amorphous alloy and SUS304 stainless
steel foils was carried out in[24] by consuming dynamic bending of micro cantilever beam. Before testing, the
diamond tip of the indenture was precisely located at the loading point of the micro beam by the repeated
calibrations using the CCD camera, and then the micro cantilever beam was dynamically bent under constant
load amplitude control. Based on the elastic beam theory, when the beam was deflected dynamically, the top
surface at the fixed end of the micro beam would be subjected to a tension-tension stress and the back surface of
the micro beam to a compression-compression stress. During dynamic bending tests, the micro beam stiffness
was recorded automatically. The fatigue life of the free standing small samples was determined based on the
variation of the micro beam stiffness during dynamic bending because crack initiation would cause a decrease in
the stiffness. While Fig. 10. Shown a process to manner cyclic tension-compression loading of thin Ag films
deposited onto a SiO2 substrate was projected by [25] out of a nanoindenter with a function of continuous
stiffness measurement, The dynamically elastic bending of the film/SiO 2 substrate composite causes cyclic
tension-compression loading to the thin Ag film at the top of the substrate. Fatigue failure of the Ag film was
controlled by the variation of the stiffness of the microbeam.
Fig.10. Schematic of the bilayer Ag-SiO2 beam deflection experiment. The indenter tip was used to deflect the
beam [25].
2.3 Uniaxial tension-compression
The most common tests involve uniaxial cyclic loading. The tension-compression cyclic loading tests
can also be studied on thin free-standing films. The new fatigue testing method over applying a uniaxial load to
metal films placed on a compliant substrate with a high elasticity and mechanical stability, as shown in Fig. 11
(a). The film/substrate-composite was strained by turn On/Off tensile load while the film was deformed
elastically and plastically by turning On/Off tension and in compression load, respectively. Additionally, to
estimate the applied plastic strain range, the cyclic stress-strain curves of the specimens were measured in
normal by X-ray diffraction goniometer, as shown in Fig. 11 (b). The advantages of this method are [26]:
1. A cyclic tension-compression load could be applied to the very small thickness metal films even less
than 10 nm.
2. The bulk-like fatigue sample of metal film/substrate composite simply invented and fixed to the fatigue
machine relatively large clamps.
3. Fatigue tests could be controlled via constant load range or total strain range.
4. By using conventional preparation methods can easily to get the samples for Transmission Electron
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Fig.11. (a) Schematic of the Cu lm/polyimide substrate composite for fatigue testing, (b) film stress x as a
function of substrate strain during the second and tenth cycle of the test on a 0.7 lm thick copper lm. The
arrows indicate the development of the lm stresses during loading and unloading [26].
The molecular dynamics (MD) simulations were utilized to realize the yield behavior of Nano
crystalline Ni and Cu with grain sizes 10 nm at high strain rates. The propos calculation flow stress values at a
strain rate of (109 s-1) an asymmetry in the strength values in tension and compression for the Nano crystalline
metal more powerful in compression than in tension. Nevertheless, the tensioncompression strength asymmetry
was detected to reduce as the grain size decreases to a size of 4 nm, after which, a further reduction in grain size
resulted to rise in the strength asymmetry values. The higher asymmetry at size of 2 nm was consistent with the
mechanical behavior observed in metallic glasses and can be referred to the amorphous nature of the Nano
crystalline metal. The effect of strain rate on the yield behavior of Nano crystalline metals as obtained from
molecular dynamics (MD) simulations was debated and compared with that informed in the literature obtained
by molecular statics simulations for quasi-static loading conditions [27].
Also, for enough small grain sizes with diameters 20 nm (reliant to the material) molecular dynamics
simulations (MD) and latest experimental researches had shown that inter-grain processes typically dominate
deformation. These processes can result in weakening of a metal with reducing the grain size. Nanocrystalline
metals with grain sizes in the inverse HallPetch regime had gained considerable attention due to their increased
strengths during deformation at high strain rates [28]. Whilst there had important progress in understanding
mechanisms of plastic deformation in Nano crystalline metals, understanding the effect of grain size and strain
rate on macroscopic deformation behavior at high strain rates was still in its infancy.
On the other hand, the influence of loading mode and strain amplitude on fatigue crack growth from
microscopic observations and analysis by comparing the micro-mechanisms of fatigue crack initiation and
propagation behaviors of an unnotched solid polycrystalline copper specimen under cyclic tensioncompression
and torsion loadings were investigated [29]. The greatest significant finding displayed that the connection
between the matrix and persistent slip bands (PSBs) on the surface in crystalline materials is the favored location
for fatigue cracking [30-32]. This can be attributed to the plastic strain localization and high stress
engrossment in intrusions and extrusion initiated by cyclic slip irreversibility [32,33]. Moreover, the grain
boundaries (GBs) were furthermore significant sites for the fatigue crack initiation. Zhang et al. [34-37]
systematically examined the probability of the appearance of diverse grain boundaries (GBs) cracking, and
discovered that the intergranular fatigue cracking strongly depended on the interactions of persistent slip bands
(PSBs) with grain boundaries (GBs) in fatigued bicrystals instead of the grain boundaries (GBs) structure itself.
The SEM-ECC method was utilized to monitor styles of disintegration of the fatigued specimens. From
a great deal of observations, the most widespread dislocation patterns of coarse-grained copper after cyclic
tensioncompression loadings with an matching effective usual strain amplitude were shown in Fig. 12.
Displayed the dislocation patterns in the interior grains and specimen surface under tensioncompression fatigue,
respectively [29].
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Fig.12. Dislocation patterns of coarse-grained copper after cyclic deformation with equivalent effective normal
strain amplitude, (a) the internal area of tensioncompression fatigue sample, (b) the external area of tension
compression fatigue sample [29].
Fatigue cracks on the surface of polycrystalline copper under cyclic tensioncompression and torsion
loadings with equivalent effective normal strain amplitude as shown in Figs13. And explained by the Slip band
(SB) Grain boundaries (GB) damage mechanism [29].
Fig.13. Fatigue crack initiation and early propagation of coarse-grained copper during tensioncompression
fatigue tests [29].
Hence, this method appears to be the most suitable one for fatigue realizations of thin films at room
temperature. Following such an approach, a number of fatigue behaviors investigations of thin metal films and
metallic multilayers are proceed.
Table.1: Methods of fatigue testing of small-scale materials.
Shape of
Method
Material
Limitation
specimen
Uniaxial
Free-standing
-The transition from high cycle to low cycle fatigue
Cu, Ni,
thin wires, dogtensionhappen at around
Carbon
tension [12bone shaped
5000 cycles.
nanotube(CNT)
- Stress decrease from 0.75 % to 0.5%.
foils,
22].
Ni-P
Machine parameters:
Dynamic
amorphous
Micro-sized
- Displacement =5nm.
bending
alloys.
cantilever
- Load= 10m.
[23-25]
Stainless steel.
beam
- Frequency= 100 Hz
Silver.
(a) A cyclic tension-compression load could be
applied to the very small thickness metal films even
less than 10 nm.
(b) The bulk-like fatigue sample of metal
Uniaxial
Dog-bone shaped film/substrate composite simply invented and fixed
tensionto the fatigue machine relatively large clamps.
Cu/ Polyimide films confined by
compression
(c) Fatigue tests could be controlled via constant
a substrate
[26-37]
load range or total strain range.
(d) By using conventional preparation methods can
easily to get the samples for Transmission Electron
Microscopy (TEM) from fatigued specimens.
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22.
23.
24.
25.
26.
27.
28.
29.
30.
31.
32.
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