Terahertz HgTe Nanocrystals: Beyond Confinement

Article abstract of DOI:10.1021/jacs.8b02039

We report the synthesis of nanocrystals with an optical feature in the THz range. To do so, we develop a new synthetic procedure for the growth of HgTe, HgSe, and HgS nanocrystals, with strong size tunability from 5 to 200 nm. This is used to tune the abs

Full text of DOI:10.1021/jacs.8b02039

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TeraHertz HgTe nanocrystals: beyond confinement
Nicolas Goubet, Amardeep Jagtap, Clément Livache, Bertille Martinez, Hervé
Portalès, Xiang Zhen Xu, Ricardo Lobo, Benoit Dubertret, and Emmanuel Lhuillier
J. Am. Chem. Soc., Just Accepted Manuscript • DOI: 10.1021/jacs.8b02039 • Publication Date (Web): 04 Apr 2018
Downloaded from http://pubs.acs.org on April 4, 2018
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TeraHertz HgTe nanocrystals: beyond confinement
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Nicolas Goubet , Amardeep Jagtap , Clément Livache , Bertille Martinez , Hervé Portalès ,
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1*
Xiang Zhen Xu , Ricardo P.S.M. Lobo , Benoit Dubertret , Emmanuel Lhuillier
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Sorbonne Université, CNRS, Institut des NanoSciences de Paris, INSP, Fꢀ75005 Paris, France
2
LPEM, ESPCI Paris, PSL University, CNRS, Fꢀ75005 Paris, France
3
Sorbonne Université, CNRS, LPEM, Fꢀ75005 Paris, France
4
Sorbonne Universités, UPMC Univ Paris 06, CNRS, UMR 8233, MONARIS, 4 Place Jussieu, 75005 Paris, France
Supporting Information Placeholder
Among HgX, HgTe is the compound that leads to the best perꢀ
formances, with the lowest dark current and the fastest time reꢀ
sponse. However, the current state of the art synthesis for midꢀ
ABSTRACT: We report the synthesis of nanocrystals with
optical feature in the THz range. To do so, we develop a new
synthetic procedure for the growth of HgTe, HgSe and HgS nanoꢀ
crystals, with strong size tunability from 5 nm to 200 nm. This is
used to tune the absorption of the nanocrystal all over the infrared
range up to the teraHertz (from 2 µm to 65 µm for absorption
peak and even 200 µm for cutꢀoff wavelength). The interest for
this procedure is not limited to large size since for small objects
we demonstrate low aggregation, good shape control (i.e. spheriꢀ
cal object) while using nonꢀexpansive and simple mercury
halogenide precursors. By integrating these nanocrystals into an
electrolyteꢀgated transistor, we evidence a change of carrier densiꢀ
ty from pꢀdoped to nꢀdoped as the confinement is vanishing.
25
IR HgTe CQD relies on Keuleyan et al. synthesis and keep sufferꢀ
ing from several limitations, which are discussed in more details
26,27
in the supporting information.
In particular the material grows
with an anisotropic shape (tetrapod or tetrahedron, see figure S1ꢀ
S4) which tends to selfꢀassemble into pairs (see figure S4) and
leads to a loss of colloidal stability even for moderate size CQD.
This is extremely detrimental to the design of pinhole free layer
for vertical geometry device. Moreover, the final objects are
strongly faceted and present the least reactive facet, which is
limiting for growth of heterostructures. This perspective is even
more challenging due to the high reactivity of mercury with chalꢀ
cogenides. Consequently, nucleation and growth steps are difficult
to be timeꢀseparated and low temperature growth is used in curꢀ
rent synthesis (60ꢀ120°C), making the obtained material incomꢀ
patible with usual high temperature (200ꢀ300°C) growth process
Colloidal quantum dots (CQD) have garnered significant scienꢀ
tific and technological interests because of their tunable optical
features from ultraviolet (UV) to infrared (IR). While their photoꢀ
luminescence appears as the first mass market application, CQD
are actually as interesting for the design of low cost optoelectronic
devices that combine the ease of processing of solutionꢀ
processable material with the robustness of inorganic systems.
This is especially true in the IR range where current technologies
remain pricy. CQD offer an interesting platform, however reachꢀ
ing mid (λ>3 µm) and far infrared wavelength is challenging on a
8
,28
of wide band gap colloidal material.
HgTe has not yet reached the maturity of CdSe. 2D HgTe plateꢀ
lets have recently been proposed by Izquierdo et al. but they
remain limited to the nearꢀIR range. Shen et al have also proꢀ
In term of shape control
29
30
posed the use of a more reactive precursor such as bisꢀ
(trimethylsilyl)telluride (TMSTe) as a way to improve sphericity
and aggregation. However, TMSTe is expensive and has a very
limited stability, which prevents such synthesis to be viable at
least at the industrial scale. Last, the current range of size spans
from 3 to 20 nm, which makes that the obtained material is still
strongly confined since HgTe presents a large exciton Bohr radius
1
–3
material perspective.
Only few materials can address absorption tunability up to the
4
5,6
terahertz range: graphene , doped semiconductors (Si, InSb) and
31
of 40 nm. This prevents current material to address wavelengths
7
topological insulators such as Bi Se . However, the strong field
27,32
2
3
above 12 µm
and also limits the emergence of topologically
localization of terahertz plasmon in a subwavelength volume
makes that materials need to be designed in gratings. The wet
chemical synthesis can be a potential alternative and easy way to
produce terahertz materials. To reach this goal, the current synꢀ
thetic procedures need to be pushed toward CQDꢀbased terahertz
protected states which are expected for poorly confined obꢀ
33,34
jects.
In this paper, we report a new and simple synthetic procedure for
the growth of HgTe CQD. We demonstrate size control from 5
nm to above 200 nm, which allows for the first time to cover the
whole infrared range from 2 µm up to the THz range (65 µm)
with a single material. In particular, we focus on long waveꢀ
lengths (10ꢀ100 µm range), which are nonꢀaddressable based on
previously reported synthesis. We also integrate these materials
into electrolyteꢀgated transistors and demonstrate that HgTe CQD
switch from pꢀtype for the smallest size to nꢀtype for the largest
CQD.
8
,9
10–12
technology. Mercury chalcogenides (HgX: HgS, HgSe
and
13
HgTe ) have reached the highest maturity to address this part of
the electromagnetic spectrum because they combine midꢀIR tunaꢀ
ble optical features with photoconduction. Lots of effort have
been made for the integration of HgX CQD, including the design
1
4,15
16
17
of photoconductive
, photovoltaic, phototransistor, devices ,
18–20
21,22
plasmon assisted photodetection,
even hybrid with graphene
multicolor detection
. A recent review on the field is
and
2
3,24
25
given in ref
.
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To achieve a higher degree of control on HgTe CQD synthesis,
we investigate for less reactive precursors. Our approach is based
While the role of reaction time is rather trivial with an increase of
the final size with time, the role of halide is more complex. We
observe that chloride leads to larger objects compare to the other
halides (>Br>I), see Figure 2. This trend is confirmed by followꢀ
ing the absorption of the solution at 415 nm, which is the signaꢀ
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on the simultaneous injection of HgX (with X=Cl, Br or I) and
2
Te complexed with trioctylphosphine (TOP) in a hot solution of
oleylamine. It is worth noting that the procedure can be extended
to the growth of HgSe and HgS (see figure S9 and S10), while
using NaBH4 reduced Se and elemental sulfur in oleylamine,
respectively.
32
ture of the amount of crystalline HgTe, see figure S5. Even at
low temperature (120 °C), the reaction is almost complete after 3
min in the case of HgCl , while it is still unfinished after 3 h while
2
using HgI . As shown in Figure 2a, d and e, iodine precursor leads
2
to more faceted objects. This may be attributed to the soft base
character of iodine that allow a better bonding and poisoning
39
surface made of soft acid mercury.
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As recently proposed by Shen et al, it is possible to tune the
magnitude of the long wavelength peak of the absorption spectra
while tuning the reaction stoichiometry. For moderate size CQD
(12ꢀ40 nm), only the interband contribution is observed in the
case of stoichiometric reaction (Hg:Te=1:1), while the long waveꢀ
length feature is obtained in Hg rich condition, see figure S8. Hg
rich material tends to be nꢀtype doped, which favor the observaꢀ
tion of the intraband/plasmonic feature as observed for HgS and
40
HgSe which are intrinsically nꢀdoped.
Figure 1. (a). absorption spectra of HgTe CQD with various sizes.
(b) absorption spectra of HgTe CQD with various sizes, presentꢀ
ing a plasmonic feature in the LWIR, VLWIR or THz range. (c)
Cut off wavelength of the interband transition (for material withꢀ
out plasmonic feature) and plasmonic peak wavelength (for doped
material) as a function of the CQD size (diameter for spherical
object). SWIR corresponds to ShortꢀWavelength Infrared range
(1.5 to 3 µm), MWIR to MidꢀWavelength Infrared range (3 to 8
µm), LWIR to LongꢀWavelength Infrared range (8 to 12 µm), and
VLWIR to Very LongꢀWavelength Infrared range (12 to 30 µm).
Inset: full width at half maximum (FWHM) of intraband peak as
function CQD size.
The size of the CQD is driven by three key parameters, which are
temperature, the reaction time and the chosen mercury halide
precursor. By tuning the reaction temperature from 120 °C up to
340 °C, the mean size of the CQD can be tuned from 5 nm up to
2
00 nm, see Figure 1c, 2 and Figure S5. Thus, it is possible to
obtain absorption all over the infrared range from 2 µm up to 65
µm, see Figure 1. This approach presents the key advantages to
both be able to synthesize small CQD sizes with sharp excitonic
transition, but is also well suited to obtain large CQD, which are
able to address long wavelength (>12 µm). Figure 1b shows how
the LongꢀWavelength Infrared range (LWIR, 8ꢀ12 µm range),
Very LongꢀWavelength Infrared range (VLWIR, 12ꢀ20 µm range)
and THz (λ>30 µm) can be finely addressed using the developed
protocol. The optical features have been pushed to an energy
Figure 2 (a), (b) and (c) are Transmission Electron Microscopy
(TEM) images of HgTe CQD synthetized at 180°C with HgI2,
HgBr and HgCl as Hg precursor, respectively. (d) and (e) are
2
2
TEM images of HgTe CQD synthetized using HgI as precursor at
2
2
50°C and 300°C, respectively. (f) and (g) are low and high resoꢀ
lution images of spherical HgTe CQD with limited aggregation.
h) is an Scanning Electron Microscopy (SEM) image of HgTe
(
CQD synthetized at 300°C using HgCl and (i) the corresponding
2
Xꢀray diffractogram.
1
0
typically twice smaller than the previous record.
In the case of large CQD, the spectrum is made of two compoꢀ
nents: an interband absorption at high energy and an intraꢀ
band/plasmonic peak at low energy, see Figure 1a and b. The
exact nature of the long wavelength feature actually depends on
Transmission electron microscopy (TEM) images (Figure 2)
clearly show a limited aggregation. Moreover, it is possible at low
temperature to obtain almost nearly spherical objects, see Figure
2 f and g. As shown in Figure 2 d, e and h, the size dispersion is
large for large objects. However, this is not critical since the
plasmon linewidth of CQD is driven by the doping level rather
8
particle size and doping level. The energy of this transition can
be made low enough, so that the peak overlaps with the absorpꢀ
ꢀ
1
tion resulting from the LO phonon line (at 123 cm ). The Raman
spectrum in figure S11 confirms the phonon character of this line.
Another striking behavior is the exceptional narrowness of the
8
than the confinement. The crystalline nature of the obtained
material is well revealed by high resolution TEM (Figure 2 g) as
well as by X–ray diffraction (Figure 2i). The diffraction pattern is
consistent with the zincꢀblende structure of HgTe.
ꢀ1
intraband/plasmonic peak (< 200 cm ) compared to what it can be
35
36–38
for doped nanocrystals of Si or oxides
>1000 cm ).
(with a FWHM
ꢀ
1
To better highlight the role of doping on the optical properties, we
integrate the film of HgTe CQD into electrolyteꢀgated transistor
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(
see Figure 3a for a scheme of the device). Such gating method
ASSOCIATED CONTENT
Supporting Information
1
2
3
4
5
6
7
8
9
is convenient because it combines low bias operation thanks to the
large gate capacitance with air operability. As the nanoparticle
size is increased, the material switches from pꢀtype (conduction
under hole injection) (Figure 3b) to ambipolar (Figure 3c) and
finally to nꢀtype only (conduction under electron injection) for the
largest sizes (Figure 3d). This change of behavior is further quanꢀ
tized by the increase of the ratio of electron mobility over hole
mobility while the band gap is reduced, see Figure 3e.
The Supporting Information is available free of charge on the
ACS Publications website.
Additional information includes experimental details on HgTe,
HgSe and HgS nanocrystal synthesis, TEM pictures of HgTe
CQD shape evolution with time and selfꢀassembly in dimer, reacꢀ
tivity of different HgX precursors, absorption spectra with differꢀ
ent stoichiometry of HgTe CQD, size distribution, experimental
details on electron microscopies, UVꢀVis, FTIR and Raman specꢀ
troscopies (PDF)
This emergence of nꢀtype conduction is similar to what has been
observed for HgS and HgSe nanocrystals. Due to the combinaꢀ
tion of narrow band gap and high work function in HgX CQD, the
material can be reduced by the environment. This reduction
however occurs for much larger size (ie lower confinement) beꢀ
cause of the lower work function of HgTe material compared with
HgS and HgSe. This is interesting on an applied point of view
because it preserves the gate effect even for large particles, while
for other chalcogenides gate control is lost due to their too metalꢀ
lic character. This means that even for the largest particle the
number of carrier per particle remains in the range of what can be
tuned by electrolyte gating (0ꢀ6 electrons typically). As a result,
the long wavelength feature observed in the absorption spectra is
probably not fully plasmonic and preserves an intraband characꢀ
ter.
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AUTHOR INFORMATION
Corresponding Author
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* el@insp.upmc.fr
43
Notes
The authors declare no competing financial interests.
ACKNOWLEDGMENT
EL acknowledges the financial support of the European Research
Council (ERC) starting grant (blackQD – n°756225). We
acknowledge the use of cleanꢀroom facilities from the “Centrale
de Proximité ParisꢀCentre”. We thank Agence Nationale de la
Recherche for funding through grant Nanodose and H2DH. This
work has been supported by the Region IleꢀdeꢀFrance in the
framework of DIM NanoꢀK. This work was supported by French
state funds managed by the ANR within the Investissements
d'Avenir programme under reference ANRꢀ11ꢀIDEXꢀ0004ꢀ02,
and more specifically within the framework of the Cluster of
Excellence MATISSE. This work is also supported by the NextIR
grant funded by Nexdot.
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