Fabrication of titanium tips via electrochemical etching is commonly hindered by the formation of a tough oxide layer. A new one-step approach based on dc etching in a non-aqueous electrolyte is presented. The electrochemical tip etching was carried out at 20 V in a benign etchant of 1M NaCl in ethylene glycol. Tip radii below 100 nm are demonstrated using current cut-off control and approaching 150 nm without cut-off control. The simplicity and efficiency of the approach eliminates pre and post electropolishing steps due to the electropolishing capability of a NaCl-ethylene glycol based electrolyte.
REFERENCES
1.
M. J.
Donachie
Jr., Titanium: A Technical Guide
, 2nd ed. (ASM International
, Materials Park
, 2000
), p. 11
.2.
W. H.
Colner
, M.
Feinleib
, and J. N.
Reding
, J. Electrochem. Soc.
100
, 485
(1953
).3.
M.
Yata
, M.
Ozaki
, S.
Sakata
, T.
Yamada
, A.
Kohno
, and M.
Aono
, Jpn. J. Appl. Phys.
28
, L885
(1989
).4.
W. S.
Williams
, Int J. Refract. Met. Hard Mater.
17
, 21
(1999
).5.
E. M.
Kelliher
and T. L.
Rose
, IEEE Trans. Biomed. Eng.
BME-31
, 532
(1984
).6.
I. V.
Borzenets
, I.
Yoon
, M. W.
Prior
, B. R.
Donald
, R. D.
Mooney
, and G.
Finkelstein
, J. Appl. Phys.
111
, 074703
(2012
).7.
C. C.
Neacsu
, S.
Berweger
, and M. B.
Raschke
, Nanobiotechnology
3
, 172
(2007
).8.
M.
Kulakov
, I.
Luzinov
, and K. G.
Kornev
, Langmuir
25
, 4462
(2009
).9.
K.
Fushimi
and H.
Habazaki
, Electrochim. Acta
53
, 3371
(2008
).10.
P. A.
Hodgson
, Y.
Wang
, A.
Awez Mohammad
, and P.
Kruse
, Rev. Sci. Instrum.
84
, 026109
(2013
).11.
J. P.
Ibe
, P. P.
Bey
Jr., S. L.
Brandow
, R. A.
Brizzola
, N. A.
Burnham
, D. P.
DiLella
, K. P.
Lee
, C. R. K.
Marrian
, and R. J.
Colton
, J. Vac. Sci. Technol. A
8
, 3570
(1990
).12.
K. S.
Raja
, T.
Gandhi
, and M.
Misra
, Electrochem. Commun.
9
, 1069
(2007
).13.
R. B.
De Lima
, V.
Paganin
, T.
Iwasita
, and W.
Vielstich
, Electrochem. Acta
49
, 85
(2003
).14.
K.
Fushimi
, K.
Kond
, and H.
Konno
, Electrochim. Acta
55
, 258
(2009
).15.
K.
Tajima
, M.
Hironaka
, K.
Chen
, Y.
Nagamatsu
, H.
Kakigawa
, and Y.
Kozono
, Dent. Mater. J.
27
, 258
(2008
).16.
Q. A.
Nguyen
, Y. V.
Bhargava
, and T. M.
Devine
, Electrochem. Commun.
10
, 471
(2008
).17.
Y.
Zhou
, L.
Shu'ni
, Q.
Zhai
, and M.
Hu
, J. Chem. Eng. Data
55
, 1289
(2010
).18.
N. M.
Cullinane
and S. J.
Chard
, Nature (London)
164
, 710
(1949
).19.
D.
Wang
, R.
Yu
, N.
Kumada
, and N.
Kinomura
, Chem. Mater.
11
, 2008
(1999
).20.
C. O.
Bostwick
, U.S. patent 2643262 (28 April 1950
).21.
A. P.
Abbott
, G.
Capper
, K. J.
McKenzie
, and K. S.
Ryder
, Electrochem. Acta
51
, 4420
(2006
).22.
J. S.
Zhu
, B. M.
Kim
, J. L.
Schworn
, K. C.
Green
, and P.
Guilmette
, U.S. patent 6835300 (13 Sept 2004
).23.
See supplementary material at http://dx.doi.org/10.1063/1.4865759 for tip quality metrics and etching statistics as well as EDX data.
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