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inducing a large pulse-ISHE (p-ISHE) response that may be measurable even for materials with very weak SOC. In addition, benefiting
from the versatility of organic semiconductor (OSEC) synthesis,
their SOC can be enhanced by integrating intrachain heavy metal
atoms (such as Pt, Ir, and so on)29,30 , in contrast to the passive
intrinsic systematic variation of SOC in transition metals13,14 . Therefore, by chemically adjusting the heavy metal concentrations in
the polymer chains, the SOC strength in OSECs can be systemically tuned30 and quantitatively investigated by means of the ISHE
response generated from pulsed-FMR (p-FMR).
Here we present the experimental realization of p-FMR for generating and detecting spin currents in OSEC compounds with tunable
SOC through the p-ISHE response. Using this technique we develop
methods to effectively eliminate various spurious effects, such as
AMR, the AHE and resonant MW heating, that interfere with
the p-ISHE current. To highlight the usefulness of these technical
advances, we report a systematic study of the p-ISHE response
in a variety of OSEC materials with tunable SOC, ranging from
-conjugated polymers (PCP) having strong SOC that contain intrachain Pt atoms with various concentrations, to PCP that have
very weak SOC and are fully organic, to C60 films. We unravel the
important role of SOC in spin-current charge-current conversion
within these materials, and quantitatively determine the value of the
spin-diffusion length and spin Hall angle in each compound, exploring potential candidate materials for organic spin orbitronics3137 .
Department of Physics & Astronomy, University of Utah, Salt Lake City, Utah 84112, USA. These authors contributed equally to this work.
*e-mail: boehme@physics.utah.edu; val@physics.utah.edu
NATURE MATERIALS | ADVANCE ONLINE PUBLICATION | www.nature.com/naturematerials
Device B
plane
Cu
JC
EISHE
IISHE
VISHE
+0.5 mV
+0.1 mV
0.3 mV
0.7 mV
1.1 mV
1.5 mV
6
4
2
60
120
B ()
Vp-ISHE (mV)
100
105
110
115
120
125
130
135
180
135
110
180
80
45
0
40 20
20
0.0
Vcw-ISHE at 200 mW 10
0.5
1.0
Vp-ISHE
1.5 at 1,000 W
2.0
50
1.0
0.5
0.0
25
0
25
BBres (mT)
50
1.0
0.5
0.0
0.5
1.0
10
0 1 2 3 4 5 6 7 8
Acquisition time (s)
0.5
2
4
6
8
Acquisition time (s)
Vp-ISHE (a.u.)
B (mT)
JS
Vp-ISHE in NiFe/Pt
1.0
B1
0.5
1.5
0.5
0.0
50 nm
NiFe
Polymer
d
MW pulse sequence
FMR (a.u.)
1.5
1.0
SiO
NiF 2
e
C
60
Cu
Cu
trodes
ec
Copper el
Polymer
Vp-ISHE (normalized)
NiFe ferromagnet
Vp-ISHE (mV)
V/VMAX
ARTICLES
NiFe/Pt
NiFe only
5
0
5
BBres (mT)
10
40
BBres (mT)
60
120
180
B ()
Figure 1 | Detection of pulsed spin current through the p-ISHE response. a, Schematic illustration (not to scale) of the NiFe/OSEC/Cu device on a glass
template held by a sample rod with a built-in contact system for thin-film electrical connections23 . The inset shows a transmission electron microscope
image for the cross-section of an organic-based p-ISHE device fabricated as sketched in the main panel. Different layers can be distinguished as labelled.
B, B1 and M denote, respectively, the static external magnetic field, the magnetic component of the pulsed MW field, and the dynamic magnetization in the
NiFe film, which precesses around B. JS , S, JC , EISHE , VISHE and IISHE denote, respectively, the flow of the pulsed spin current, the spin polarization vector, the
generated electric current, the generated electric field, the detected p-ISHE voltage and the detected p-ISHE current. b,c, Time (t) and field (B) responses
of the p-ISHE voltage (Vp-ISHE ) measured for the prototype NiFe (15 nm)/Pt (10 nm)/Cu (30 nm) device under 1 kW microwave excitation. The blue solid
line in b shows the one-pulse MW excitation. The red solid line indicates the moving-average ISHE voltage response. The colour plot in c shows a
resonance at B = Bres = 120 mT. The two spurious regions outside the MW pulse originate from MW switching artefacts and non-resonant inductive
coupling. d, Comparison of Vp-ISHE (at 1 kW) and the maximum cw-ISHE (at 200 mW) response on the same NiFe/Pt/Cu device. The inset shows the MW
power dependence response of Vp-ISHE ; it increases linearly with MW power ( B21 ) in range used in this work (see Supplementary Discussion 2). eh, Field
(B) and angular (B ) dependencies of FMR absorption and p-ISHE response, respectively, in the NiFe/Pt/Cu device. e, Comparison of the NiFe FMR
response before (red) and after (black) the deposition of Pt. f, Resonance field as a function of B , as obtained from FMR in the NiFe film. g, Normalized
Vp-ISHE (B, B ) response, where Bres is normalized. h, Normalized Vp-ISHE amplitude and polarity versus B .
Pt
P(n-Bu)3
Ph
IC
Cu
Pt
P(n-Bu)3
P(n-Bu)3 N
Pt
P(n-Bu)3
FL
Ph
300
100
0
100
200
180
300
0.0
1.5
2.0
2.5
3.0
Energy (eV)
B ()
Pt-1
200
0.0
0.5
0
90 45 0 45 90
3.5
4.0
1
20
IS
FL
Pt-Q
IF
Cu
P(n-Bu)3
Pt-3
0.5
1.0
NiFe
OSC
dN
FL
0.0
Bres (T)
Ph
FMR (a.u.)
Pt-1
0.5
1.0
P(n-Bu)3
1.0
40
20
20
NiFe only
NiFe/Pt-1
10
0
BBres (mT)
1,000 W
500 W
250 W
125 W
1.0
0.8
0.6
p-ISHE
normalized
ARTICLES
10
20
0
500 1,000
0
MW power (W)
0.4
0.2
0.0
40
BBres (mT)
60
30
0
30
BBres (mT)
60
Figure 2 | Electroluminescence spectra of the Pt-polymer series studied here, and observation of the p-ISHE response in Pt-1 polymer. a, Normalized
electroluminescence spectra for Pt-1 (black), Pt-3 (red) and Pt-Q (blue) polymers, respectively. The SOC strengths can be estimated from the
electro-Ph/FL intensity ratios30 . The insets show the building blocks of the studied Pt-polymers. The spacer in Pt-1 has a single phenyl ring, whereas that
of Pt-3 has three phenyl rings. b, Schematic illustration of the p-ISHE-IS current response in OSEC-based devices. IC , IF and IS are, respectively, the electric
current source generated by the ISHE in the organic layer, the AHE in the NiFe thin film (suppressed by capacitor geometry) and the current response
detected by the preamplifier; dN and l are the material thickness and length of device, respectively. c, FMR spectra of the Cu/Pt-1 polymer/NiFe/SiO2 /Cu
device measured by MW transmission without (black) and with (red) the spin-coated Pt-1 polymer. The inset shows the FMR resonance field, Bres versus
the external field angle, B . d, Typical p-ISHE(B) response (in terms of current, IS ) in the Pt-1 polymer device (ISHE/AHE ratio 9). The black squares and
red circles in d are data with the in-plane magnetic field B (at 0 ) and B (at 180 ), respectively. e, p-ISHE(B) response versus the MW power, as denoted.
The inset shows the obtained linear IS versus MW power dependence.
ARTICLES
Table 1 | Summary of the p-ISHE parameters for the investigated OSEC materials obtained from the experiments.
Materials
Pt
Pt-1
Pt-3
Pt-Q
PEDOT
DOO-PPV
C60
SOC (Ph/FL)
N/A
27
12
0.75
N/A
N/A
N/A
Vp-ISHE (V)
1,615
76
52
26
17
15
209
p-ISHE-IS (nA)
SH (nm)
2,892
246
231
145
69
54
668
(nm)
0.3 ,
SH
3.410
1.5
1.5 0.5
5 1 , 3
10 2
40 10 , 2719
25 10 , 1646,
5 2 , 1250,
The relative SOC for the three Pt-polymers was obtained from the intensity ratio of the electro-Ph/FL in OLED devices. Vp-ISHE and p-ISHE-IS are the ISHE voltage and current, respectively, between the
Cu electrodes measured at Bres using a MW power of 1 kW. SH is the lambda-theta product obtained from the fit to the ISHE response versus the OSEC thickness using equations (1)(3) (or
Supplementary Equations 68). is the spin-diffusion length extracted from equation (2) (or Supplementary Equation 6) (marked by ), independent values from GMR response in OSVs at low
temperature (marked by ), or literature reports. SH (in radians) is the spin Hall angle calculated from independent spin-diffusion length estimations (see Supplementary Table 2).
180
0
500
150
1,000
MW power (W)
ISHE/AHE: 3
150
FMR (a.u.)
60
20
30
180
0
1,000
500
MW power (W)
60
10
0
10
BBres (mT)
40
20
20
d
n
S
O
ISHE/AHE: 7
0
1
50
100
30
150
60
60
10
0
10
BBres (mT)
20
30
C8H17
ISHE/AHE: 4
1
0
1
20 10 0 10
BBres (mT)
PEDOT:PSS
30
180
1
20
C8H17
30
60
40
20
180
300
30
p-ISHE-Is (nA)
C14H29
0
FMR (a.u.)
30
60
30
600
10
0
10
BBres (mT)
20
10
40
20
60
30
180
0
500
1,000
MW power (W)
ISHE/AHE: 33
300
PBTTT
10
600
20
20
1
20
p-ISHE normalized
p-ISHE-Is (nA)
f
0
FMR (a.u.)
0
BBres (mT)
C14H29
60
DOO-PPV
20
BBres (mT)
C8H17
O
FMR (a.u.)
S
O
FMR (a.u.)
p-ISHE-Is (nA)
50
180
p-ISHE-Is (nA)
40
C8H17
60
20
BBres (mT)
150
100
Pt-Q
0
BBres (mT)
ISHE/AHE: 6
1
20
300
Pt-3
30
150
1
20 10
0
10
BBres (mT)
300
p-ISHE normalized
FMR (a.u.)
p-ISHE-Is (nA)
150
300
p-ISHE-Is (nA)
300
p-ISHE normalized
ARTICLES
1
20
10
0
10
BBres (mT)
40
BBres (mT)
20
20
C60
0
20
40
60
BBres (mT)
Figure 3 | p-ISHE(B) response in various OSEC materials with tunable spinorbit coupling. af, p-ISHE(B) current response in a variety of NiFe/OSEC/Cu
devices as denoted, measured under a 1 kW pulsed MW excitation with a 500 Hz repetition rate. The OSEC materials are four pristine -conjugated
polymers, PCPs (a, b, d, and e), one heavily doped PCP (c), and a fullerene (C60 ; f). Their respective molecular structures and ISHE/AHE ratios are shown in
the appropriate panels. All devices are capped with a SiO2 /Cu capacitor layer to suppress the AHE(B) response component. The open black squares and
red circles represent an in-plane field B (at 0 ) and B (at 180 ), respectively. When Bres is reversed from B = 0 to B = 180 , all signals reverse polarity,
as expected for the ISHE. For the NiFe/Pt-3 and NiFe/Pt-Q bilayers, the proper IS values for the ISHE (that is, after separating the ISHE and AHE
components) are 230 nA and 150 nA, respectively. When the Pt-containing polymer is replaced by a fully OSEC polymer (that is, PEDOT:PSS or
DOO-PPV), IS is significantly reduced (69 nA for PEDOT:PSS; 54 nA for DOO-PPV). The respective insets show the NiFe FMR(B) responses measured by
MW absorption in devices, with (red) and without (black) the OSEC overlayer (for details on the broadening of FMR linewidth due to the spin pumping, see
Supplementary Discussion 7) and, in a,b and f, the obtained p-ISHE response versus MW power (see also Supplementary Fig. 14). The red lines through the
data points show a linear fit. The connecting line in f is a guide for the eye.
ARTICLES
a
NiFe/Pt
0.8
Pt = 1.5 0.3 nm
800
150
NiFe/Pt-1
100
50
0.4
Thickness (nm)
10
600
NiFe/C60
400
C60 = 5 2 nm
200
0
2
p-ISHE-Is (nA)
1.2
0.0
1,000
200
p-ISHE-Is (nA)
p-ISHE (mV)
1.6
250
20
40
60
80
100
Thickness (nm)
30
60
90
120
150
Thickness (nm)
Figure 4 | p-ISHE(B) responses versus the OSEC thickness. ac, Thickness dependence of the p-ISHE (IS ) responses (open squares) in NiFe/Pt/Cu,
NiFe/Pt-1/Cu and NiFe/C60 /Cu, respectively. Red solid lines are fits to the p-ISHE data using equation (1) (for Pt) and Supplementary Equation (6)
(for Pt-1 and C60 ). The respective spin-diffusion length extracted from the fit of each OSEC device is denoted. The error bars are determined from the noise
level in the time/field-dependent p-ISHE(B) response, which varies with the individual device under operational conditions (see Methods and
Supplementary Fig. 1).
Outlook
The pulsed, high MW power detection allows experimental access
to the ISHE dynamics with an approximately 5 ns time resolution,
suggesting that the p-ISHE response may have potential for fast
spin-orbitronics-based logic applications. It also enables the use
of traditional ferromagnets (for example, NiFe) instead of the
technically more demanding magnetic insulators (such as yttrium
iron garnet)13,14,40 , thus opening many research opportunities for
both the organic and inorganic spintronics communities. The ability
to pump large pure spin currents into most classes of OSEC offers
a robust methodology for investigating spin-transport properties,
and a simple method to probe the strength of SOC in OSEC-based
devices. Our work also indicates the possibility of tunable SOC in
OSECseither passively, through chemical synthesis, or actively,
using an electric fieldpaving the way for the future studies of spin
orbitronics in plastic materials.
Methods
Methods and any associated references are available in the online
version of the paper.
Received 6 January 2015; accepted 3 March 2016;
published online 18 April 2016
References
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Acknowledgements
We acknowledge support by the National Science Foundation (DMR-1404634) for sample
preparation, execution of the experiments and data processing of the ISHE experiments.
We also acknowledge the NSF-Material Science & Engineering Center (DMR-1121252)
for supporting Pt-polymer synthesis, execution of the OSV experiments and development
of the ISHE device structures, as well as support for the device preparation facilities.
Author contributions
D.S., K.J.v.S., C.B. and Z.V.V. conceived this study and the experiments. D.S. fabricated the
devices. K.J.v.S., D.S. and H.M. implemented the p-ISHE set-up. K.J.v.S., H.M. and M.K.
measured the p-ISHE response; D.S., M.K. and C.Z. measured the device conductivity
and capacitance. C.Z. and D.S. measured the Pt-polymer electroluminescence spectra.
M.G. measured the frequency dependence of the FMR spectra. D.S. carried out the
circuit modelling for the p-ISHE current. C.B. and Z.V.V. were responsible for the project
planning, group management, and final writing of the manuscript . All authors discussed
the results, and worked on data analysis and manuscript preparation.
Additional information
Supplementary information is available in the online version of the paper. Reprints and
permissions information is available online at www.nature.com/reprints.
Correspondence and requests for materials should be addressed to C.B. or Z.V.V.
ARTICLES
Methods
Device preparation for the p-ISHE measurements. Al thin-film electrodes
(150 nm) on glass templates (3 50 mm) were fabricated by sputtering and using
conventional optical lithography23,24 . Two Cu contacts with a gap of 50 m
(extended from an Al bottom electrode) were grown by e-beam evaporation
through a shadow mask in a glove-box-integrated vacuum deposition chamber
(Angstrom Engineering), dedicated to metal deposition, having a base pressure of
3 108 torr. Cu is chosen as the electrode material because it has negligible SOC,
and thus does not interfere with the ISHE from the spin current diffusion through
the OSEC film into the underlying electrode20 . The templates were subsequently
transferred into a second glove box that is dedicated to OSEC spin coating through
an antechamber under a nitrogen atmosphere (0.1 ppm).
The Pt-1, Pt-3, Pt-Q and DOO-PPV PCPs were synthesized in house using
literature methods30 . The PEDOT:PSS polymer (Clevios, P VP AI 4083) was
purchased from Heraeus, and the PBTTT-C14 polymer was purchased from
Luminescence Technology Corp (Lumtec) and used without further purification.
The polymer/chloroform solutions were spin-coated onto the templates at various
spinning speeds (from 1,000 to 8,000 r.p.m.) to obtain different OSEC film
thicknesses, followed by a post-annealing procedure (100 C for 30 min) in the
glove box. The C60 powder was purchased from American Dye Source, and C60
films were thermally evaporated onto the template at a rate of 0.5 to 1.0 s1 . The
OSEC-coated templates were transferred in a nitrogen atmosphere back to the first
glove box, with the vacuum deposition chamber.
Ni80 Fe20 ferromagnetic layers (15 nm thickness) were grown by e-beam
evaporation through a shadow mask on the spin-coated polymer thin films.
Without breaking the vacuum, the fabricated structures were transferred with
another shadow mask back to the deposition chamber for e-beam evaporation of a
SiO2 (150 to 750 nm) dielectric layer and a top Cu thin film (30 nm). All thin-film
thicknesses were calibrated using a profilometer. The active device area was
0.7 mm 1.0 mm .
p-ISHE measurement set-up. The p-ISHE measurements were carried out at room
temperature in a Bruker ElexSys E580 X-band (9.7 GHz) pulsed EPR
spectrometer equipped with a dielectric resonator (Bruker FlexLine ER 4118
X-MD5). Both cw and pulsed MWs were applied to the p-ISHE templates under a
rough vacuum. The purpose of the all-thin-film device design is to ensure that all
conducting components are thinner than the MW skin depth at 9.7 GHz, leaving
the device mostly unperturbed by the intense E-fields within the cavity. Figure 1a
illustrates a p-ISHE device on a glass template that was designed specifically to fit
in the MW resonator. The position of the template during operation is such that its
contact pads are well outside the resonator volume whereas the actual sample
structure is located at the opposing far end in the centre of the resonator. The MW
pulse duration time was either 2 s or 5 s (chosen depending on the rise time of
the current amplifier being used) at a repetition rate of 500 Hz. The device
geometry is chosen such that it places the sample at a position within the
cylindrical MW cavity where the B1 field is both maximal and homogeneous,
whereas the E1 field is minimal. The maximum pulsed MW power was 1 kW,
resulting in an amplitude B1 = 1.1 mT at the sample location.
The p-ISHE responses were detected by means of the induced electromotive
force, VISHE , using a Femto DHPCA 100 for metals, and a Stanford Research SRS
570 current preamplifier for OSEC material (that is, IS , see Supplementary
Discussion 7), with a bandwidth setting of 100 Hz1 MHz. The current-amplifier
output was connected to the input of a Bruker SpecJet transient recorder
(250 MS s1 , 8-bit digitizer) that is built into the ElexSys spectrometer. The
sensitivity of the current preamplifier was chosen to be 103 A V1 (Femto
DHPCA-100) or 20 A V1 (SRS 570). The p-ISHE(B) response measurements and
time dynamics required averaging over 10,240 shots. The error bar is determined
from the maximum noise level in the time/field-dependent p-ISHE(B) response
from each device (for example, Supplementary Fig. 1), which depends randomly on
the power fluctuation in each MW pulse (maximum: 10%) and the device stability
under the pulsed MW operational conditions. For the cw-ISHE measurement we
used a cw MW source with a power of 200 mW applied to the same resonator and
VISHE (as a derivative spectrum) was measured by magnetic field modulation and
lock-in amplification. The VISHE (B) spectrum is converted to a voltage amplitude
by numerical integration. The parallel capacitance and resistance in the devices
were measured using an Agilent E4980A precision LCR meter. The out-of-plane
and in-plane conductivities for various materials were measured by a Keithley 4200
at room temperature.
Spin Hall angle calculation. The observed p-ISHE responses enable us to calculate
the spin Hall angles (SH ) for various OSEC materials. Here we quantify the values
of SH based on a phenomenological model21 and equivalent circuit model of our
set-up (see Supplementary Fig. 11). The p-ISHE response is measured during each
MW pulse excitation (5 s duration) at a repetition rate of 500 Hz. Consequently,
the generated p-ISHE response contains a wide bandwidth of a.c. signals (from
100 Hz to 1 MHz, see Supplementary Discussion 7). The capacitance of each
OSEC film, CN , also needs to be considered in the circuit model (Supplementary
Fig. 11). By taking into account the device structure, detection electronics, and
the a.c. response of each electronic component, a simplified expression may
be written:
#
"
(IC + IF )RF
(2)
IS (pISHE) = Re SUM
SUM
RS + RF + (2RSUM
)
N /1 + i( j CN (j) RN (j) )
where RF and RSUM
are the series resistances of the NiFe film and
S
current-preamplifier impedance, respectively. j , CN (j) = (N (j) w(l/2))/dN and
RN (j) = dN /(N (j) W (l/2)) are, respectively, the jth frequency component
(established by the finite Fourier transform), parallel capacitance and resistance of
the organic layer at j (see Supplementary Discussion 7 for the derivation). The
variables N (j) and N (j) are the dielectric constant and conductivity of the OSEC
material at j . RSUM
and (j CN (j) RN (j) )SUM are the respective sum of parallel
N
resistance and sum of the CN RN product terms averaged over the entire frequency
range of the measurement apparatus (Supplementary Figs 12 and 13). The
parameter w is the width of NiFe layer and l is the length of NiFe thin film. The
currents IC and IF are the generated ISHE responses at the NiFe/OSEC interface
and the AHE response from the NiFe thin film, respectively. The latter response is
greatly suppressed by the MW shunt capacitor incorporated into our devices
(Fig. 2), but not completely eliminated. The spin-pumping-related IC through the
OSEC layer can be expressed as21 :
IC = lSH
2e
}
N tanh
dN
2N
j0S
(3)
where SH and N are the respective spin Hall angle and spin-diffusion length in the
OSEC, and j0S is the spin current in the OSEC perpendicular to the NiFe/OSEC
interface and along l (ref. 21). By measuring the IC dependence on the OSEC
thickness, dN at fixed l and j0S , we can obtain N from a normalized version of
equation (3) (see Fig. 4 and Supplementary Fig. 15). The spin current j0S is obtained
from the attenuation of the FMR response (that is, FMR(B ) resonant field and
spectral width dependencies, see Supplementary Fig. 18). The lambda-theta
product ( SH ) can be accurately calculated by substituting the above parameters
into equations (2) and (3)21 .