We demonstrate that structural and spectroscopic information can be obtained on exfoliated nanocrystals as thin as 6 nm. This can be achieved by using a combination of micro X-ray fluorescence (μXRF), micro X-ray absorption near-edge spectroscopy (μXANES), and X-ray microdiffraction (μXRD) techniques. Highly focused, tunable X-ray beams available at synchrotron sources enable one to use these non-invasive characterization tools to study exfoliated samples on a variety of substrates. As an example, we focused on exfoliated nanocrystals of the high temperature superconductor Bi2Sr2CaCu2O8+δ. μXRF is used to locate the sample of desired thickness; μXANES and μXRD are used to obtain electronic and structural information, respectively. We find that the “4.7b” structural modulation, characteristic of the bulk crystals, is drastically suppressed for exfoliated crystals thinner than 60 nm.

1.
K. S.
Novoselov
,
D.
Jiang
,
F.
Schedin
,
T. J.
Booth
,
V. V.
Khotkevich
,
S. V.
Morozov
, and
A. K.
Geim
,
Proc. Natl. Acad. Sci. U.S.A.
102
,
10451
(
2005
).
2.
J. T.
Ye
,
S.
Inoue
,
K.
Kobayashi
,
Y.
Kasahara
,
H. T.
Yuan
,
H.
Shimotani
, and
Y.
Iwasa
,
Nat. Mater.
9
,
125
(
2010
).
3.
R. V.
Gorbachev
,
I.
Riaz
,
R.
Nair
,
L.
Jalil
,
R.
Britnell
,
B. D.
Belle
,
E. W.
Hill
,
K. S.
Novoselov
,
K.
Watanabe
,
T.
Taniguchi
,
A. K.
Geim
 et al,
Small
7
,
465
(
2011
).
4.
S.
Zhao
,
C.
Beekman
,
L.
Sandilands
,
J.
Bashucky
,
D.
Kwok
,
N.
Lee
,
A.
Laforge
,
S.
Cheong
, and
K.
Burch
,
Appl. Phys. Lett.
98
,
141911
(
2011
).
5.
K. M. F.
Shahil
,
M. Z.
Hossain
,
D.
Teweldebrhan
, and
A. A.
Balandin
,
Appl. Phys. Lett.
96
,
153103
(
2010
).
6.
D.
Teweldebrhan
,
V.
Goyal
, and
A. A.
Balandin
,
Nano Lett.
10
,
1209
(
2010
).
7.
T.
Ohta
,
A.
Bostwick
,
T.
Seyller
,
K.
Horn
, and
E.
Rotenberg
,
Science
313
,
951
(
2006
).
8.
A.
Splendiani
,
L.
Sun
,
Y.
Zhang
,
T.
Li
,
J.
Kim
,
C.-Y.
Chim
,
G.
Galli
, and
F.
Wang
,
Nano Lett.
10
,
1271
(
2010
).
9.
C.
Lee
,
H.
Yan
,
L. E.
Brus
,
T. F.
Heinz
,
J.
Hone
, and
S.
Ryu
,
ACS Nano
4
,
2695
(
2010
).
10.
L.
Ren
,
X.
Qi
,
Y.
Liu
,
G.
Hao
,
Z.
Huang
,
X.
Zou
,
L.
Yang
,
J.
Li
, and
J.
Zhong
,
J. Mater. Chem.
22
,
4921
(
2012
).
11.
G. E.
Ice
,
J. D.
Budai
, and
J. W. L.
Pang
,
Science
334
,
1234
(
2011
).
12.
I.
McNulty
,
B.
Lai
,
J.
Maser
,
D. J.
Paterson
,
P.
Evans
,
S. M.
Heald
,
G. E.
Ice
,
E. D.
Isaacs
,
M. L.
Rivers
, and
S. R.
Sutton
,
Synchrotron Radiat. News
16
,
34
(
2003
).
13.
J. L.
Jordan-Sweet
,
IBM J. Res. Dev.
44
,
457
(
2000
).
14.
See supplementary material at http://dx.doi.org/10.1063/1.4768234 for additional information on the structural study of Bi2Sr2CaCu2O8+δ nanocrystals and preliminary data on Bi2Se3 exfoliated nanocrystals.
15.
R.
Feng
,
A.
Gerson
,
G.
Ice
,
R.
Reininger
,
B.
Yates
, and
S.
McIntyre
,
AIP Conf. Proc.
879
,
872
(
2007
).
16.
A. P.
Hammersley
,
S. O.
Svensson
,
A.
Thompson
,
H.
Graafsma
,
Å.
Kvick
, and
J. P.
Moy
,
Rev. Sci. Instrum.
66
,
2729
(
1995
).
17.
N. L.
Saini
,
A.
Lanzara
,
A.
Bianconi
, and
H.
Oyanagi
,
Phys. Rev. B
58
,
11768
(
1998
).
18.
M.
Holt
,
Z.
Wu
,
H.
Hong
,
P.
Zschack
,
P.
Jemian
,
J.
Tischler
,
H.
Chen
, and
T.-C.
Chiang
,
Phys. Rev. Lett.
83
,
3317
(
1999
).
19.
V.
Petricek
,
Y.
Gao
,
P.
Lee
, and
P.
Coppens
,
Phys. Rev. B
42
,
387
(
1990
).
20.
X. B.
Kan
and
S. C.
Moss
,
Acta Crystallogr., Sect. B: Struct. Sci.
48
,
122
(
1992
).
21.
Y.
Le Page
,
W. R.
McKinnon
,
J.-M.
Tarascon
, and
P.
Barboux
,
Phys. Rev. B
40
,
6810
(
1989
).
22.
H.
Eisaki
,
N.
Kaneko
,
D. L.
Feng
,
A.
Damascelli
,
P. K.
Mang
,
K. M.
Shen
,
Z.-X.
Shen
, and
M.
Greven
,
Phys. Rev. B
69
,
064512
(
2004
).
23.
N.
Fukushima
,
H.
Niu
,
S.
Nakamura
,
S.
Takeno
,
M.
Hayashi
, and
K.
Ando
,
Physica C
159
,
777
(
1989
).
24.
J. P.
Castellan
,
B. D.
Gaulin
,
H. A.
Dabkowska
,
A.
Nabialek
,
G.
Gu
,
X.
Liu
, and
Z.
Islam
,
Phys. Rev. B
73
,
174505
(
2006
).
25.
M.
Izquierdo
,
S.
Megtert
,
J. P.
Albouy
,
J.
Avila
,
M. A.
Valbuena
,
G.
Gu
,
J. S.
Abell
,
G.
Yang
,
M. C.
Asensio
, and
R.
Comes
,
Phys. Rev. B
74
,
054512
(
2006
).

Supplementary Material

You do not currently have access to this content.