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Appl Phys A (2011) 103: 285–291

DOI 10.1007/s00339-010-6050-0

Small-span bending test for determination of elastic-plastic


properties of ultrathin Pt wires
Hironori Tohmyoh · M.A. Salam Akanda ·
Masumi Saka

Received: 6 April 2010 / Accepted: 8 September 2010 / Published online: 23 September 2010
© Springer-Verlag 2010

Abstract A mechanical testing methodology for determina- may show brittle characteristic compared with their bulk
tion of elastic-plastic properties of very thin metallic wires materials. For example, because the sufficient atoms and
using small-span bending under lateral load is described. their arrangements are needed for inducing plastic defor-
Sufficient strain is locally developed in the tested section mation, the atomic-scale, metallic wire may show no plas-
of wire by unsymmetrical bending with two opposite probes tic deformation. Brittle behavior of materials is sometimes
where one end of the wire is fixed on a substrate with rigid unsuitable for structural components because the fracture
joint by Joule heat welding. From the load-displacement re- occurs suddenly and sufficient time to prevent the fracture
lationships obtained experimentally, Young’s modulus is de- is hardly to be kept. Moreover, the fracture strength varies
termined by analytical formulation. Moreover, yield stress depending on their crystalline structure or geometrical fea-
and hardening modulus of the wire are identified using an tures, and therefore, the fracture of brittle materials includ-
optimization strategy with finite-element analyses. The thin ing the random factors is unpredictable. As reliable small-
Pt wires with a nominal diameter of about 625 nm are exam- scaled materials, proper plastic deformation ability of mate-
ined by the testing scheme and the wires are found to have rial must be indispensable in addition to higher and stable
higher yield stress compared to bulk Pt. strength. Larger plastic deformation of materials is also im-
portant for absorbing the shock energy. The very thin metal-
lic wires with the diameter range of 100–1000 nm are ex-
1 Introduction pected to have both higher strength and sufficient plastic
properties and these must be indispensable structural ele-
Various kinds of small-scaled materials such as nanowires or ments in NEMS/MEMS.
whiskers have been expected to be used as key components, To verify and understand the material functionality and
e.g., structural, electrical, optical and thermal elements, in application domains of the above range of wires and to con-
nanoelectromechanical systems (NEMS) or microelectro- trol their behavior, the elastic-plastic properties of the wires
mechanical systems (MEMS) due to their excellent physi- should be accurately determined. However, it is not an easy
cal properties. Generally, small-scaled materials are known task to realize it in the present state. In evaluating the prop-
to have pure crystalline structures without defects and such erties of thin metallic wires, testing by scanning tunneling
highly-ordered materials show higher strength compared microscope (STM) [9] or atomic force microscope (AFM)
with bulk materials [1–5]. On the other hand, because the [1–3, 10, 11] and nanoindentation [12] are well reported. Es-
plastic deformation occurs in the results of movement of pecially, the AFM is now a most promising way to obtain the
dislocations [1, 5–8], small-scaled materials without defects mechanical properties of materials because it can detect very
small force. Usually in AFM based (tensile or bending) tests
[1–3, 10], the samples are fixed on AFM tip or substrate.
H. Tohmyoh () · M.A.S. Akanda · M. Saka However, it is hard to develop a suitable setup for testing due
Department of Nanomechanics, Tohoku University, Aoba 6-6-01, to the difficulty in handling the small-scaled objects. More-
Aramaki, Aoba-ku, Sendai 980-8579, Japan
e-mail: tohmyoh@ism.mech.tohoku.ac.jp
over, in the AFM based technique, the deformation shape is
Fax: +81-22-7956893 difficult to be monitored during testing. The in-situ observa-
286 H. Tohmyoh et al.

tion of small-scaled objects during testing may give us more


valuable information for understanding nanomechanics of
small-scaled materials.
In the present paper, we report a testing methodology for
determining the elastic-plastic properties of very thin metal-
lic wires with the diameter of less than 1 µm. The cutting and
welding techniques for thin wires using Joule heating [13–
15] are used in handling the thin wire samples, and the ex-
perimental setup suitable for asymmetric, small-span bend-
ing with the visualization of a high-resolution digital micro-
scope is constructed. The higher stress field is locally devel-
oped in the wire with the closely-coupled force probes and
the load-displacement relationships of the ultrathin Pt wire
for various probe distances are recorded. From the relation-
ships, Young’s modulus of the Pt thin wire is determined an-
alytically. Moreover, by fitting the experimentally obtained
load-displacement relationship and that obtained by nonlin-
ear finite-element analysis (FEA), yield stress and harden-
ing modulus of thin wire are successfully determined. Ex-
amined ultrathin Pt wires with the diameters in the range
of 615 to 770 nm clearly show work hardening effects and
higher yield stress as compared with reported bulk Pt.

Fig. 1 Concept of testing methodology. (a) Schematic of local


2 Testing scheme small-span bending configuration. (b) Assumed distribution of yield
stress along diameter of the wire at yield point. (c) Equivalent plastic
strain at top fiber as a function of span ratio (a/b) and deformation (δ)
The tested material is assumed to be linear hardening elastic- of the wire. Here l is fixed at 60 µm and a is varying in the range of 6
plastic material. The relationship between stress, σ , and to 15 µm
strain, ε, for the material can be expressed as
σ
ε= , for σ ≤ σY , (1)
E the loading is considered close to a fixed support C and far
and from the fixed end A, higher stress field due to large bending
occurs locally across the loading probe B and this eliminates
σY σ − σY
ε= + , for σ > σY , (2) the problem of failure at the root of the sample.
E E
The load-displacement relationship obtained by the bend-
where E, σY and E  are Young’s modulus, yield stress and ing test contains the elastic and elastic-plastic regions. The
hardening modulus, respectively, and these three parameters property, E can be obtained from the load-displacement re-
should be decided for describing the elastic-plastic proper- lation in the elastic zone as
ties of the material.
The tensile test may be the simplest one and the mechan- P b3 P b4 (2l + a)2
ical properties of materials can be directly determined from E= − , (3)
3I δ 12l 3 I δ
the stress-strain relationship. However, in case of thin wire
specimens, they are likely to be broken at the grips due to
where P is the load applied by the probe at B, δ the dis-
unacceptable scratch and the stress concentration at these
placement at the loading point in the loading direction, b
regions. Moreover, the very thin wires prepared by vapor-
the distance between the fixed end (A) and the loading point
liquid-solid [16], spattering [17], or atomic diffusion [18]
techniques are usually on the substrate and one end of the (B), a the distance between the loading point (B) and the
wires is rigidly fixed. Therefore, the bending tests are the simply-supported end (C), and l the total span length. The
best choice to determine the mechanical properties of small- symbol I is for the moment of inertia of area of the sample
scaled objects. The configuration of the proposed testing is and is given by πd 4 /64 for wire, where d is the diameter of
illustrated in Fig. 1(a). A one-end-fixed sample is consid- the wire. If we consider the whole cross-sectional area of the
ered for bending at its free end by two opposite probes. As wire yielded as shown in Fig. 1(b), the moment at the yield-
Small-span bending test for determination of elastic-plastic properties of ultrathin Pt wires 287

ing point corresponding to yield load, PY , can be described


as
 3
4 d PY ab2
M = σY = (2l + a). (4)
3 2 2l 3
From (4), yield stress σY is given by

3PY ab2
σY = (2l + a). (5)
l3d 3
The remaining parameter, E  is difficult to be determined
analytically because it is a nonlinear problem. The distri-
bution of yield stress as considered (Fig. 1(b)) is valid for
fully plastic behavior of materials. Therefore, for accurate
estimation of σY and E  we employ elastic-plastic FEA. In
this case, the value for σY obtained from (5) is taken as the
initial guess for FEA. By searching the best fitting of the
load-displacement relationship obtained by FEA with the
experimental one [19], the parameters σY and E  are deter-
mined. Here, to improve the accuracy level of fitting, mod-
erate strain around the loading region should effectively be
induced for a required range of displacement. Figure 1(c)
shows the distributions of equivalent plastic strain against
the ratio a/b for various values of δ obtained by FEA. The
data used for this analysis were; d = 800 nm, l = 60 µm and Fig. 2 (a) The TEM image of the cross-section of the examined ultra-
a = 6–15 µm. It is clear that the smaller a gives effective thin Pt wire. (b) SEM micrographs for Pt-In joint. A magnified view of
increase in plastic deformation with increase in δ, and there- the joint is inserted
fore, the testing configuration presented in Fig. 1(a) is effi-
ciently used to induce sufficient plastic strain locally around To obtain the one-end-fixed beam structure on a suitable
the loading point. substrate for Pt wire as a testing sample, we adopted the
welding and cutting techniques utilizing Joule heating [13–
15, 21]. Indium (In) wire of diameter 500 µm was taken as
3 Experiment and analysis
substrate material. To make a joint with Pt the In wire is
prepared to have a very sharp tip end. The In substrate and
3.1 Sample preparation
the Pt sample were individually placed on two nanomanipu-
Extremely thin Pt wires with the nominal diameter of lators via Cu electrodes and they were aligned in line and
625 nm were examined. The ultrathin wires were Ag-coated brought in tip to tip contact. After that a conducting mi-
with the overall diameter of about 75 µm. This type of wire croprobe placed on a separate nanomanipulator brought in
is known as Wollaston wire [20]. The Wollaston wires were lateral contact with the Pt wire and electric current was sup-
cut into 10 mm lengths. The Ag coatings around the tips of plied through the contact of Pt and In by making a suitable
the cut pieces were removed by HNO3 to expose Pt. Fig- circuit having a controlled current source. Due to Joule heat
ure 2(a) shows a transmission electron microscope (TEM) dissimilar metal weld joint at the contact of Pt and In was
micrograph of the length-wise cross-section of an examined obtained. To avoid the change in property of the Pt sample
Pt wire together with the selected area diffraction (SADIFF) due to Joule heating, the length of the Pt wire for conducting
patterns obtained at the points S1 and S2 along the length of electric current was kept minimum (around 5 µm). After the
the section and the nano-beam electron diffraction (NBD) welding, the Pt wire was cut to form a cantilever on the In
patterns obtained at the points N1 to N3 along the diameter substrate with a length of about 200 µm. The details of cut-
of the wire. No clear grain boundary was observed in the ting the Pt wire at any point can be seen in reference [21].
TEM image and the SADIFF patterns on the wire showed Figure 2(b) shows a scanning electron microscope (SEM)
the same orientation. The facts indicated that the wire had micrograph of a typical weld joint between the Pt wire and
an elongated grain structure. The different NBD patterns the In substrate. The weld joint was found to be rigid. In
demonstrated that the examined Pt wire was covered with the bending experiment, the welded end of the Pt wire is,
very thin polycrystalline layer. therefore, considered as the fixed end of the testing sample.
288 H. Tohmyoh et al.

to 25 µm, and the maximum load as sensor capacity was


27.5 µN. It was experimentally confirmed that the measure-
ment uncertainty level of this type of force sensor was found
within 0.4% of maximum load. The resolution of the present
force sensor was about 10 nN.

3.3 Finite-element analysis

The FEA is performed considering finite deformation of the


bending problem. For FEA using MARC software [23], the
wire is assumed as circular cross-section with uniform di-
ameter along the length. The measured force-displacement
relation consists of two parts, i.e., a linear elastic part and
nonlinear elastic-plastic part. From the linear elastic part the
value of E is determined by using (3). Elastic-plastic FEA
is performed using the evaluated E and assumed values for
σY and E  . In the repeated simulations, suitable values for
σY and E  are looked into for which the best matching be-
tween FEA and experimental P –δ relations is obtained. In
the optimization strategy, at first assuming a small value for
Fig. 3 (a) Photograph of the testing setup. (b) Digital microscope im- E  the value of σY is adjusted by matching the FEA and
age of loading configuration. (c) Compact force sensor used experimental P –δ relations up to the first point of nonlin-
earity. Then E  is adjusted by matching the rest of the P –δ
3.2 Testing apparatus relations. It should be noted that in FEA the wire-probe fric-
tion coefficient is assumed to be 0.2 as the two cylindrical
In the test setup, a force sensor, a piezo stage and two surfaces make a smooth contact.
manipulators (one carrying the sample and the other car-
rying the piezo stage), were set on a single platform, see
Fig. 3(a). The sample was taken on a carrier and by using 4 Results and discussions
manual manipulation, the sample was placed just touching
the fixed probe with desired flexural length and the load- Figure 4(a) shows an example of the experimental force-
ing probe of the force sensor was placed against the sam- displacement (P –δ) relationship obtained under the condi-
ple as shown in Fig. 3(b). The deformation in sample and tion of l = 60 µm and a = 10 µm. Also the deformation pat-
the corresponding load for the testing were recorded in a terns of the wire corresponding to the loading states A, B
computer directly. The deformation pattern was also mon- and C as shown in Fig. 4(a) are shown in Figs. 4(b), (c) and
itored by a high-resolution digital microscope. The load- (d), respectively, and the pattern after unloading is shown
displacement relationships for bending the ultrathin Pt wires in Fig. 4(e). From the bending patterns, it was clear that
were recorded under the various combinations of l and a. less bending occurred at the root of the wire and maximum
The loading probes were made of hard material W. Using bending took place across the tip of loading probe. After
focused-ion-beam machining the tip part of each probe was unloading, the root region of the wire returned to its orig-
made as 5 µm diameter cylindrical surface for smooth con- inal shape whereas a permanent bending remained at the
tact with the Pt wire sample. loading point; see Fig. 4(e). This confirmed that sufficient
The force sensor was composed of a cantilever and a ca- plastic deformation in the wire was successfully achieved
pacitive (CP) sensor [22], see Fig. 3(c). This compact, in- across the closely-coupled loading probes without affecting
tegrated force sensor was designed to use with the combi- the root of the wire. This is also analogous to the analyti-
nation of various types of microscopes. The deformation of cal predictions. As shown in Fig. 1(a), the ratio of bending
the Pt wire is given by δ = δS − δC , where δS is the dis- moments of loading point B (MB ) and root A (MA ) analyti-
placement of piezo stage and δC the deflection of the can- cally can be expressed in terms of span ratio (a/ l) for small
tilever. The cross-sectional area of the cantilever beam was deflection as MB /MA = (1 − a/ l)(2 + a/ l)/(1 + a/ l). For
0.54 ×0.05 mm, and the beam length was 29.5 mm. The small a/ l ratio, this clearly shows that the bending moment
force acting on the wire is given by P = kδC , where k is at loading point B is higher than that of root A. As for ex-
the spring constant of cantilever and that of the cantilever amples, MB /MA = 1.59 at a/ l = 0.15 and MB /MA = 1.37
used was 1.1 N/m. The range for CP sensor used was up at a/ l = 0.24. In P –δ relationships for all conditions, we
Small-span bending test for determination of elastic-plastic properties of ultrathin Pt wires 289

Fig. 5 (a) The P –δ relations for various combination of l and a to-


gether with the results of FEA after nonlinear fitting. The distributions
of (b) stress and (c) plastic strain of the wire along diameter at the
location of bending are obtained by FEA

nonlinear fitting. The results of FEA are in good agreement


with their corresponding experimental measurements, and
Fig. 4 (a) An example of the load-displacement relationship the facts indicated that the nonlinear fittings up to a large de-
(l = 60 µm, a = 10 µm). The deformation images of the wire at the
states A to C in (a) are respectively, shown in (b)–(d), and that after
formation range were successfully achieved. In other words,
unloading is shown in (e). Note that the wire was yielded under the (1) and (2) were valid for describing the mechanical behav-
condition of the point B ior of the examined Pt wires. In P –δ relation as shown in
Fig. 5(a), the point A indicates the first point of nonlinearity,
which is considered here as the yield point and the point B
could clearly observe the proportional limit like point B as indicates a state of large plastic loading. The distributions
shown in Fig. 4(a), from which the nonlinear behavior for of axial stress along the diameter parallel to the direction
P –δ relations started. The nonlinear relationship for P and of loading for the two states A and B were determined by
δ is found to be due to the plastic deformation of the wire FEA and they are presented in Fig. 5(b). The stress distri-
and the geometric nonlinearity, i.e., movement of the speci- bution in the wire at the yield point has slight difference
men into the bending span. with that considered for determining σY analytically; see
Figure 5(a) shows the P –δ relations for various com- Fig. 1(b). Therefore, without using FEA, the value of σY de-
bination of l and a together with the results of FEA after termined from (5) will be rough and it is found around 14%
290 H. Tohmyoh et al.

was found as 17.6 ± 2.5 GPa. In the present experiments,


the values of E and E  did not vary depending on the sam-
ple. From these experimental facts, we concluded that the
difference of σY for each group was clear difference among
the samples and this might be brought by the difference in
the crystalline structure of the samples. Although the bulk
Pt is usually show perfectly plastic behavior, the examined
ultrathin Pt wire showed work hardening effect. This may be
due to the special crystalline structure of the Pt wire, i.e., the
bamboo structure. Few grain boundaries were existed in the
testing section on the wire and this attributed higher resis-
tance for movement of atoms. As mentioned earlier, in the
nonlinear FEA the probe-sample friction coefficient was as-
sumed to be 0.2. If the friction coefficient is changed from
0.2 to 0.3, only about 10% decrease in the values of σY and
E  is observed for getting best fit of FEA data to the exper-
imental data points. Therefore, the value of E  as evaluated
(17.6 GPa) is observed reasonably a high value compared to
the bulk Pt.

5 Conclusions

We have realized the effectiveness of the typical three-point


bending test of ultrathin Pt wires having the nominal diame-
ter of 625 nm. The testing scheme also provides the option of
video recording of the deformation patterns of the wires. The
local plastic deformation in the wire was successfully in-
duced with the closely-coupled force probes. Young’s mod-
ulus of the ultrathin Pt wires was determined from the exper-
imental load-displacement relationship. Moreover, the yield
stress and hardening modulus of the wires were determined
by fitting the load-displacement relationships obtained by
Fig. 6 (a) E vs. a/ l. (b) σY vs. a/ l. (c) E  vs. a/ l. The available the finite-element analyses with experimental ones. The ex-
values for bulk Pt are shown in the figures amined Pt wires showed higher yield stress as compared
with bulk Pt and work hardening effect due to their crys-
higher than the FEA estimation. Figure 5(c) shows the dis- talline structures.
tributions of equivalent plastic strain of these loading states
Acknowledgements The authors thank Mr. H. Takeda and Mr. T.
A and B. The distribution for state A indicates that the full
Muramatsu for their help in arrangement of the experimental setup.
cross-section except a narrow part at the center of the wire This work was supported by Grant-in-Aid for Scientific Research (S)
suffers plastic strain. From the figure it is also clear that the 18106003 and by Grant-in-Aid for Young Scientists (A) 21686012.
plastic strain at the loading point increases with the increase
in probe displacement.
Figures 6(a) to (c) display the determined values of E, σY References
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