IEEE TRANSACTIONS ON APPLIED SUPERCONDUCTIVITY, VOL. 32, NO.

4, JUNE 2022 2100404

Investigation of the Superconducting Ti/PdAu

Bilayer Films for Transition Edge Sensors
Xiaolong Xu, Mauro Rajteri , Jinjin Li , Shuo Zhang, Eugenio Monticone , Jian Chen, Carlo Pepe ,
Huifang Gao, Wei Li, Xu Li, Qi Li, Ying Gao, Zheng Liu, and Xueshen Wang

Abstract—High quality superconducting films are crucial for the material is limited. In our previous work, Tc of a 100 nm Ti film
development of transition edge sensors (TESs) with high energy was 550 mK [8], while other research groups reported that for
resolution ability. Controlling the superconducting transition tem- their Ti thin films, the Tc was from 360 mK to 500 mK [9]–[11].
perature (Tc ) and the transition width (ΔTc ) of the films from
the superconducting to normal metal state is important for the A common method to tune the Tc in a wider range is exploiting
performance of TESs. We present a new kind of superconducting the proximity effect which occurs at the interface between a
Ti/PdAu bilayer film. The influence of Ti/PdAu thickness ratio on superconducting and a normal metal film [12]. Several kinds
Tc through the proximity effect is investigated. The Tc can be tuned of bilayer films have been used in TESs, such as Mo/Cu [13],
from 175 mK to 336 mK by setting the PdAu thickness to 60 nm Mo/Au [14], Ti/Au [15], Ti/Al [16], Ir/Au [17] and so on. For
and varying the thickness of Ti from 50 nm to 70 nm. The minimum
ΔTc is ∼1 mK. The element distribution at the interface between UV-Vis-NIR TESs the Tc typically ranges between ∼100 mK
the Ti and PdAu layers has been analyzed by a high-resolution and 500 mK [9], [11], [14], [16].
transmission electron microscopy (HRTEM), energy-dispersive In this paper, we show some results on a new superconducting
spectrometer (EDS) and X-ray diffraction (XRD). Roughness, elec- Ti/PdAu bilayer film for TESs. PdAu is an alloy easily made in
trical resistivity, and cryogenic properties are also shown. The different ratios [18], and remains in the normal state even when
superconducting Ti/PdAu bilayer film shows a great promise as
a new material for TESs. the temperature is at millikelvin level [19]. Pd has a narrower lat-
tice spacing than Au, which can block the diffusion of Au atoms
Index Terms—Proximity effect, superconductivity, Ti/PdAu, to the Ti layer via the pinning effect [20]. We expect that the
transition-edge sensor.
Ti/PdAu bilayer film will show a better long-term stability than
Ti/Au. Moreover, as the resistivity of PdAu is much higher than
I. INTRODUCTION Au, Ti/PdAu bilayer will show a larger resistance than Ti/Au,
RANSITION Edge sensors (TESs) have been widely used which allows sensors with smaller rise time and higher saturation
T as energy detectors for microwave [1], NIR-visible-UV
light [2], X-ray [3] and gamma-ray [4]. The key sensor unit is
energy possibility[21]. The Tc is tuned by the thickness ratio of
Ti and PdAu layers. The nanoscale morphology and structure of
often a superconducting thin film, such as Ti [5], W [6] and Hf the interface between the two layers, and the electrical properties
[7]. However, the tunable range of the transition temperature are characterized.
(Tc ) by the thickness for a superconducting film based on single
II. EXPERIMENTAL DETAILS
Manuscript received September 28, 2021; revised December 8, 2021 and
February 5, 2022; accepted February 15, 2022. Date of publication February 24, A. Deposition of Ti/PdAu Thin Films
2022; date of current version May 16, 2022. This work was supported in part
by Young Scientists Fund of the National Natural Science Foundation of China The superconducting Ti/PdAu bilayer films are deposited on
under Grants 61901432 and 61701470, in part by the Science and Technology a silicon substrate in a magnetron sputtering system with a base
project of State Administration for Market Regulation, China, under Grants
2020MK153 and 2019MK112, and in part by the Fundamental Research Projects
pressure of ∼10−6 Pa. A Ti target (99.995 at. %) and a PdAu
in Basic Scientific Research at NIM under Grant AKYZD1903. (Corresponding target with a mass ratio of 35 (Pd, 99.99 at. %): 65 (Au, 99.95 at.
author: Jinjin Li.) %) are used as sources. The substrate is kept at 20°C during the
Xiaolong Xu, Jinjin Li, Jian Chen, Huifang Gao, Wei Li, Xu Li, Qi Li,
Ying Gao, Zheng Liu, and Xueshen Wang are with the National Institute of
deposition process using a water-cooling system and rotated at 5
Metrology (NIM), Beijing 100029, China (e-mail: [email protected]; rpm to improve the uniformity of the film. The sputter pressure
[email protected]; [email protected]; [email protected]; [email protected]. is 0.1 Pa and the sputtering power is 200 W for both Ti and
cn; [email protected]; [email protected]; [email protected]; lzheng@
nim.ac.cn; [email protected]).
PdAu targets. The PdAu film is deposited immediately after the
Mauro Rajteri and Eugenio Monticone are with the Istituto Nazionale di deposition of the Ti film to avoid the contamination of Ti film.
Ricerca Metrologica (INRiM), 10135 Torino, Italy (e-mail: [email protected]; The thickness of the PdAu (dPdAu ) film is kept to 60 nm and the
[email protected]).
Shuo Zhang is with Center for Transformative Science, ShanghaiTech Uni-
dTi is changed from 50 nm to 70 nm.
versity, Shanghai 201210, China (e-mail: [email protected]).
Carlo Pepe is with Politecnico di Torino, 10129 Torino, Italy (e-mail:
[email protected]). B. Characterization of Ti/PdAu Thin Films
Color versions of one or more figures in this article are available at
https://doi.org/10.1109/TASC.2022.3153233. Focused ion beam milling is used to expose the cross section
Digital Object Identifier 10.1109/TASC.2022.3153233 of the bilayer film with a dual beam SEM/FIB system. In order to
1051-8223 © 2022 IEEE. Personal use is permitted, but republication/redistribution requires IEEE permission.
See https://www.ieee.org/publications/rights/index.html for more information.

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2100404 IEEE TRANSACTIONS ON APPLIED SUPERCONDUCTIVITY, VOL. 32, NO. 4, JUNE 2022

TABLE I
PROPERTY SUMMARY EVALUATED IN THIS ARTICLE

Fig. 1(b) shows the crystalline structure distribution at the

interface between the Ti and PdAu layers. The upper gray area
corresponds to the cubic Ti (110) plane with a lattice spacing
of 2.34 Å, and the bottom deep dark area shows the cubic Pd
(111) plane with a lattice spacing of 2.25 Å and the cubic
Au (111) plane with a lattice spacing of 2.35 Å. The lattice
spacing of Ti (110) plane and Au (111) planes are very close,
which may be responsible for the instability of Ti/Au TESs.
The similar crystalline structure will induce the diffusion of
Au and Ti atoms. Pd atoms at the interface will decrease the
atom diffusion process by separating the Au and Ti atoms and
blocking the Au atom via the pinning effect [20]. The interface
between the superconducting Ti layer and the normal metal
Fig. 1. (a) Element distribution at the cross-section of the Ti (55nm)/PdAu
(60nm) bilayer film on a silicon substrate, with protective Pt films coated.
PdAu layer plays an important role in the modulation of the
(b) Crystalline structure distribution at the interface. Tc due to the Usadel theory [22]. The interval time between
the deposition of PdAu and Ti is critical because Ti is easily
oxidated. The interface quality affects the critical temperature
protect the bilayer structure, two layers of Pt are prepared by an and transition sharpness [23]. The thin Ti oxidation layer will
electron beam and an ion beam deposition process, respectively. affect the proximity effect at the interface between the PdAu
Then the cross-section is characterized by a high-resolution and Ti layers making the critical temperature unpredictable. So,
transmission electron microscope (HRTEM) and energy disper- based on our experimental results, the interval time should be
sive X-ray spectroscopy (EDS) to obtain element information <10 s. It worth to notice that the area at intermediate layer in
in each layer. X-ray diffraction (XRD) pattern of the films Fig. 1(b) (marked with dashed oval) is Au phase with lattice
are recorded on a Panalytical X’Pert PRO MRD diffractometer distortion, probably due to the interface, stress, and Ti doping
using Cu λKα radiation (λ = 1.541874 Å) with the incidence during deposition with such a short interval time.
angle fixed at 0.5°. The 2θ range is from 10° to 90° with a The Rq of the films with 60 nm of PdAu and different thick-
scanning step of 0.05°. nesses of Ti films (NIM-1 to NIM-4) are shown in Table I. As
The surface roughness Rq (root mean square roughness) of shown, all the bilayer films show a similar roughness <1 nm,
thin films is measured using a Veeco Dimension Icon system. which is equivalent or better than peer report of other kinds of
The data are acquired by scanning 2 µm × 2 µm area with 256 superconducting films for TES [13], [24]. The smooth surface
lines of resolution. The resistivity is mapped at room temper- indicates the sputter factors are set at the suitable values. The Rq
ature with a CDE Resmap 178 system based on the van der is mainly due to the PdAu layer as shown in Fig. 1(a) considering
Pauw method. Cryogenic performance of the films such as the the smaller fluctuation in the surface of the Ti layer.
Tc and ΔTc is measured in a HPD adiabatic demagnetization
refrigerator (ADR) with an excitation current of 316 nA. B. Structure and Phase
Fig. 2 shows the X-ray diffraction (XRD) pattern of a typical
III. RESULTS AND DISCUSSION Ti/PdAu film. Two intense preferential peaks of PdAu alloy
(Palladium, JCPDS card # 46-1043 and Gold, JCPDS card
A. Morphology of the Ti/PdAu Films
# 04-0784) are clearly present at 2θ = 39.52° and 66.82°,
Fig. 1 shows the TEM image of the cross-section of a Ti which correspond to the PdAu alloy crystal plane (111) and
(55 nm) /PdAu (60 nm) bilayer film. Fig. 1(a) shows the clear (220). There are two weak signals at 2θ = 45.73° and 80.26°
multi-layer Pt/PdAu/Ti/Si interface structure as marked with which correspond to the PdAu alloy (200) and (311) planes,
different colors. The Pt protection layers are deposited before respectively. Ti (211) planes (Titanium, JCPDS card # 44-1288)
the FIB milling process. There is no oxidized Ti layer between shows a shoulder peak at 2θ = 69.48°, and another Ti (110) plane
the PdAu/Ti layers. The Ti films is uniform, Ti-PdAu interface should appear at 2θ = 38.48°, but it is unfortunately submerged
appears much smoother than the PdAu-Pt interface. in the high-intensity signal of PdAu (111) plane. But there is

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XU et al.: INVESTIGATION OF THE SUPERCONDUCTING Ti/PdAu BILAYER FILMS FOR TRANSITION EDGE SENSORS 2100404

Fig. 4. The Tc of the Ti/PdAu bilayer thin films.

Fig. 2. XRD pattern of a typical Ti/PdAu bilayer thin film.

D. Cryogenic Property
The Tc and ΔTc of the measured films are shown in Fig. 4. The
PdAu film has suppressed the Tc of the Ti films via the proximity
effect. The Tc of PdAu/Ti bilayer decreases with the dTi . The
Tc of NIM-1, with the largest dTi /dPdAu ratio, is 335.6 mK,
showing a weakest proximity effect among 4 samples; inversely,
the Tc of NIM-4 is 175.3 mK with more intense proximity effect.
The ΔTc ranges from 0.9 mK to 4.7 mK. The theoretical energy
resolution (ΔE) and effective response time (τ eff ) of a TES, is
given by the following equations [25]:
 
4kTc2 C n/2
ΔE = 2.35 (1)
α
τth
Fig. 3. Thickness of Ti/PdAu bilayer thin film vs. effective resistivity. τef f ∝ (2)
1 + αn
∂ log R
α= (3)
clear evidence that Ti (110) plane exists as shown in Fig. 1(b). ∂ log T
Considering that PdAu alloy has a heavy density and can easily where k is the Boltzmann constant, Tc is the transition temper-
scatter the X-ray, the weak XRD pattern signal of the Ti film is ature, C is the heat capacity of TES, α is the thermal sensitivity
predictable. The XRD is used to obtain macro-scale elementary of superconducting thin film, n is an exponent factor of thermal
information of the sample. conductance, τ th is thermal time constant, respectively.
With narrow ΔTc and higher value of resistance, the transition
zone has a sharp and linear edge, which represent higher thermal
C. Electrical Property sensitivity α and current sensitivity. With these properties our
The resistivity of the films is strongly correlated with the TES has the potential to obtain improved ΔE and smaller τ eff .
thickness ratio dTi /dPdAu as shown in Fig. 3 and Table I. The
dPdAu is fixed as 60 nm and the dTi is changed from 70 nm to IV. CONCLUSION
50 nm, named as NIM-1 to NIM-4 The effective resistivity ρeff
In this paper we have presented a new kind of Ti/PdAu
of the bilayer film is defined as R × (dPdAu + dTi ), where R is
superconducting bilayer films suitable for the development of
the sheet resistance. The bilayer film could be considered as an
TESs. The Tc of the films could be tuned between 336-175 mK
integrated structure, and the ρeff could exclude the thickness
as the dTi /dPdAu decreases. The resistivity keeps as large as Ti
effect of the single film. The resistivities of pure PdAu and
film, in the meanwhile the Tc and ΔTc are lowered, which will
Ti films are 297 nΩm and 681 nΩm at room temperature,
be beneficial to improve the energy resolution of single photon
respectively. As shown in Fig. 3, the ρeff increases with the ratio
detection.
dTi /dPdAu . NIM-1 shows the highest ρeff as 403 nΩm, and
NIM-4 shows the lowest one as 373 nΩm. The ρeff increases
ACKNOWLEDGMENT
towards to that of a pure Ti film as the dTi increases. The Ti/PdAu
bilayer film could keep relative high resistivity as a single film The author would like to thank Mrs Q. Zhong at NIM for
of Ti. helpful discussion.

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2100404 IEEE TRANSACTIONS ON APPLIED SUPERCONDUCTIVITY, VOL. 32, NO. 4, JUNE 2022

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