Professional Documents
Culture Documents
discussions, stats, and author profiles for this publication at: https://www.researchgate.net/publication/259629436
CITATIONS READS
4 90
5 authors, including:
Chao Lin
University of Oxford
3 PUBLICATIONS 11 CITATIONS
SEE PROFILE
Some of the authors of this publication are also working on these related projects:
All content following this page was uploaded by Lionel C Gontard on 11 September 2014.
Article
Abstract
There is great interest in developing novel position-sensitive direct detectors for transmis-
sion electron microscopy (TEM) that do not rely in the conversion of electrons into
photons. Direct imaging improves contrast and efficiency and allows the operation of the
microscope at lower energies and at lower doses without loss in resolution, which is espe-
cially important for studying soft materials and biological samples. We investigate the
feasibility of employing a silicon strip detector as an imaging detector for TEM. This
device, routinely used in high-energy particle physics, can detect small variations in elec-
tric current associated with the impact of a single charged particle. The main advantages
of using this type of sensor for direct imaging in TEM are its intrinsic radiation hardness
and large detection area. Here, we detail design, simulation, fabrication and tests in a
TEM of the front-end electronics developed using low-cost discrete components and
discuss the limitations and applications of this technology for TEM.
Key words: electron microscopy, TEM, direct electron detectors, silicon strip detectors, front-end electronics,
charge sensitive amplifier
© The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved.
For permissions, please e-mail: journals.permissions@oup.com 119
120 Microscopy, 2014, Vol. 63, No. 2
combination with back-thinning can overcome this problem Y-coordinate. The overall structure is equivalent to a distrib-
and provide a much improved detector quantum efficiency uted array of diodes. When the appropriate voltage is
(DQE) and modulation transfer function. And if the applied, these diodes are placed under reverse bias condi-
detector is operated in counting mode, then the dynamic tions, each producing a large depletion zone and acting
range can also be extended [4–11]. together similar to an array of capacitors of value Cb. When
For beam-sensitive samples like biological samples, the an electron impacts on the sensor, it loses energy and thus
use of lower electron energies and electron doses is a must to generates mobile charge carriers in the depletion region.
reduce beam damage in transmission electron microscopy The electron loses its energy gradually along its trajectory,
(TEM) [5]. If electrons can be detected directly without which can span hundreds of micrometres (see Fig. 1b), gen-
using scintillators/coupling, then the efficiency of the erating in turn a cloud of electron–hole (e–h) pairs, until the
camera system will increase. This means that if noise is kept particle is completely absorbed or exits the sensor. The bias
low, lower electron doses on the TEM sample can be used voltage applied to the sensor induces an electric field across
and still have a suitable signal-to-noise ratio (SNR) at the the depletion region, in addition to the built in voltage,
image. Moreover, lower electron beam energies can be used forcing electrons and holes to drift towards opposite sides of
without degrading resolution, effectively reducing the point the sensor until they are collected at the respective electro-
spread function at the sensor because the penetration depth des. These mobile charge carriers induce an electric current
of the incoming electron is lower [12,13]. that can be amplified, thus allowing the detection of the
Fig. 1. (a) Schematic diagram of a doublesided SSD (DSSD) with orthogonal p- and n-doped strip diodes
at opposite sides of the device. With the reverse bias applied, strip diodes have a deep depletion zone
and act similar to capacitors Cb. As a 200 keV electron impacts on the sensor, it generates e–h pairs
Fig. 2. (a) Block diagram of system architecture for a position-sensitive counting detector using a DSSD. Each strip is
connected to one front-end circuit like the one shown in Fig. 3. The strips at each side of the detector are connected to
respective X and Y modules that encode position of triggered strip to a binary word. (b) A coincidence detection module filters
simultaneous triggers on the X and Y channels, and signals interrupt request (IRQ) high when a particle is detected. IRQ
output signals to an external communication module (e.g. a streamer) that the two-dimensional position of a detected
electron is available for readout.
When the required number of strips is low, the number of strips is high, the common strategy is the inte-
front-end circuit can be implemented using discrete elec- gration of the readout circuitry within an application-
tronics with temporal window resolutions down to 10 ns specific integrated circuit (ASIC) in CMOS technology
[29], and/or field-programmable gate arrays (FPGAs). [31–38].
For example, a low-cost FPGA Spartan from Xilinx has Figure 2a illustrates the overall architecture of an asyn-
been used with a DSSD detector of 128 channels moni- chronous circuit for a position-sensitive counting detector
tored at a speed of 30 kHz [30]. When the required using a DSSD, where the main components are:
122 Microscopy, 2014, Vol. 63, No. 2
The dimensions (width and length) of the metal contacts where ν is the speed of the electrons. If electrons are
are the same as the strips; therefore, the resistance of the accelerated at E = 200 kV, their speed is v ¼ 0:695 c, c being
metal electrodes is Rs ¼ ρwtl, ρ being the resistivity and t the speed of light. Substitution in Eq. (4) gives ne = 30 electrons
the thickness of the metal contact of the strip. For sputtered m−1 nA−1, and hence, the average distance between two con-
aluminium, ρ ≈ 4 µΩ cm and t = 1 µm, which gives for this secutive electrons is Δz ≅ 3:3 cm. This means that electrons
sensor Rs ¼ 2 Ω. in a TEM for a current of 1 nA will impact on the sensor
one at a time and the average arrival time between successive
electrons will be Δtmin ¼ Δz=v ¼ 3:3 × 102 =2:085
Free charge generated by the impact of one ×108 ¼ 1:44 × 1010 s ≅ 16 ns.
electron In practice, the frequency of electron impacts will depend
We can now calculate the amount of charge generated by on the total sensing area, illumination conditions, beam
the impact of one single electron in the SSD sensor. The current, geometry of the sensor and the type of signal being
charge induced in a semiconductor is a function of the measured (coherent scattering, Rutherford scattering, inelastic
incident particle energy and the detector material, and is scattering etc.). For example, a typical current density in TEM
given by bright-field mode may be 0.1 nA/cm2, which gives 160 ns
between electron events per square centimetre of sensing area.
Ee The active sensing area of one strip of the DSSD sensor used in
Qd ¼ ð3Þ
Just after the coupling capacitor, the first stage of the duration of the pulse. However, for the case of this applica-
circuit is the preamplifier, designed to integrate the electric tion, the pulses must be processed at high speed in order to
charge injected from the sensor and to amplify the voltage discriminate locations of the electron events. If the pulses in
built on Cd . This is the most critical block because it deter- the electronic system are processed too slowly, or if they are
mines the overall sensitivity of the system. The preamplifier too wide, they will overlap (pile-up) and it will not be pos-
consists on an operational amplifier configured as a charge- sible to determine the X and Y coordinates of each impact.
sensitive amplifier (CSA), as shown in Fig. 3b. The CSA The simplest band pass filter consists of resistors and
employs a negative feedback network with capacitance Cf capacitors forming a differentiator (CR) followed by an
and resistance Rf. For the CSA to act as a current integrator, integrator (RC). The band pass filter can be obtained from a
the values of Rf and Cf of the CSA must be chosen in such a combination of the intrinsic low-pass characteristic of the
way that the time constant Tf ¼ Rf Cf is high. At the same CSA amplifier and the use of passive first-order differentia-
time, the total input capacitance must be low to minimize tors (see Fig. 5a) to a satisfactorily time constant of
noise, and therefore, Cf must be small. However, this value is Ts ¼ 1 k Ω 100 pF ¼ 100 ns. The shaper also amplifies
set in accordance with the sensor capacitance, and therefore the signal 8.6 times in each operational amplifier of the
must be sufficiently large to minimize cross-coupling between AD812AR integrated circuit and outputs an amplitude level
strips. On the other hand, a high value of Rf is required to that can be used as input for the analogue-to-digital (A/D)
minimize thermal noise. As shown in Fig. 3b, the feedback converter. This A/D converter consists of a fast comparator
total noise at the input of the CSA, expressed as the equiva- and noise contributions are equal, which corresponds to the
lent charge for an SNR equal to1, i.e. the equivalent noise minimum of curve (c). For the geometry and electrical
charge (ENC), is given by: characteristics of the sensor that we are using, the DSSD
used here adds 1.070 e− to the ENC, a value that is typical
4kT ð4kTRs þ e2na ÞC2 of this type of sensors. When the noise of the preamplifier is
Q2n ≅ 2qe Id þ þ i2na Ts þ ð6Þ
Rb Ts included, ENC reaches around 3300 e − for an optimum
shaping time (minimum noise) of 40 ns.
where Ts is the shaping time. The first term includes the dif- But this optimum time does not take into account
ferent current noise sources i2n , and the second term includes the collection time of charge carriers, which is a function of
the voltage noise sources e2n [28]. Equation (6) shows that bias voltage. If the sensor operates at full depletion, the col-
noise can be reduced by minimizing the spectral density of lection time of electron and holes can be estimated as
input noise of the preamplifier e2na and i2na and by reducing
the input capacitance C (e.g. decreasing Cf , Cd , capacitance z z z d
of the connectors). This can be achieved by reducing the tc ≈ ¼ ¼ ð7Þ
v μE μVb
diode bias, reducing Rs , increasing RB , lowering the tem-
perature T or optimizing Ts that determines the bandwidth,
where z is the average distance that an electron will go
and therefore the maximum speed of the circuit and the
Fig. 4. Graphical user interface of software developed to model a range of design parameters as a function of the sensor
specifications.
126 Microscopy, 2014, Vol. 63, No. 2
and capacitive matching between sensor and electronics can doses are used. In this case and because the strips extend all
result in cross-coupling between neighbouring strips that the length of the sensor, readout electronics has to operate
would degrade the collection efficiency of the electrodes and at very high speed in order to cope with ghost counts.
charge redistribution, resulting in peaks with much lower Nevertheless, DSSDs could be advantageous in terms of
amplitudes. In fact, Fig. 7c shows that when the electron design flexibility, ease of fabrication and cost of the sensor
dose changes, the baseline of the output signal shifts for applications requiring low spatial resolution (≤1K × 1K)
≅ 150mV, which indicates that the design of coupling and using ASICs for the electronic readout.
between sensor and electronics was imperfect. Moreover, Nowadays, there is great interest in segmented detectors
peaks with amplitude up to 1.9 V were sporadically for scanning TEM (STEM) with potential application in
observed. techniques like differential phase contrast, strain analysis by
Figure 7b also shows the presence of a sine wave oscil- nano beam electron diffraction or annular bright-field
lation of the baseline with a frequency of ∼1 MHz and (ABF) [46–48]. STEM detectors available in the market use
VRMS ¼ 50 mV. Shaping time of the electronic circuit a single-crystal yttrium aluminum perovskite or yttrium alu-
determines at which frequency the amplifier gain peaks minum garnet scintillator and a solid quartz light pipe
and it is given by f ≈ 1=2πTs . The circuit has a shaping extending from the scintillator (inside the vacuum) to the
time Ts;experimental ¼150 ns (Fig. 7b), meaning that the entrance of a photomultiplier and achieve >90% DQE [49].
noise gain will be maximum at 1.06 MHz, and which is in SSD technology could be used instead with high DQE with
8. Moldovan G, Li X, Wilshaw P, Kirkland A I (2008) Thin silicon 24. Atwood W B (1994) Gamma Large Area Silicon Telescope
strip devices for direct electron detection in transmission electron (GLAST) applying silicon strip detector technology to the detec-
microscopy. Nucl. Instrum. Meth. A 591: 134–137. tion of gamma rays in space. Nucl. Instrum. Meth. A 342:
9. Macmullan G, Faruqi A R, Henderson R, Guerrini H, 302–307.
Turchetta R, Jacobs A, Van Hoften G (2009) Experimental 25. Lutz G (1997) Semiconductor Radiation Detectors. (Springer,
observation of the improvement in MTF from backthinning a Berlin).
CMOS direct electron detector. Ultramicroscopy 109: 26. Catacchini E, Ciampolini L, Civinini C, D’Alessandro R,
1144–1147. Focardi E, Lenzi M, Meschini M, Parrini G, Pieri M (1998)
10. Moldovan G, Jeffery B, Nomerotski A, Kirkland A (2009) Direct Design, characterization and beam test performance of different
electron detection for TEM with column parallel CCD. Nucl. silicon microstrip detector geometries. Nucl. Instrum. Meth. A
Instrum. Meth. A 604: 108–110. 419: 544–548.
11. Moldovan G, Jeffery B, Nomerotski A, Kirkland A (2009) 27. Bellazzini R, Angelini F, Bagagli R, Baldini L, Brez A,
Imaging modes for direct detection in TEM with column parallel Ceccanti M, Cohen Tanugi J, Kuss M, Latronico L, Massai M M,
CCD. Nucl. Instrum. Meth. A 607: 13–16. Minuti M, Omodei N, Spandre G, Vigiani L, Zetti F (2003) The
12. Faruqi A R, Subramaniam S (2000) CCD detectors in high- silicon-strip tracker of the Gamma ray Large Area Space Tele-
resolution biological electron microscopy. Q. Rev. Biophys. 33: scope. Nucl. Instrum. Meth. A 512: 136–142.
1–27. 28. Spieler H (2005) Semiconductor Detector Systems. (Oxford
13. Jin L, Milazzo A -C, Kleinfelder S, Li S, Leblanc P, Duttweiler F, Science Publications, Oxford).
Bouwer J C, Peltier S T, Ellisman M S, Xuong N H (2008) Appli- 29. Branning D, Bhandari A, Beck M (2010) Low-cost coincidence-
40. De Graef M (2003) Introduction to Conventional Transmission 46. Shibata N, Findlay S D, Kohno Y, Sawada H, Kondo Y,
Electron Microscopy. (Cambridge University Press, Cambridge). Ikuhara Y (2012) Differential phase-contrast microscopy at
41. Brandt S, Grupen C, Roschangar R, Schofer B (1977) A high reso- atomic resolution. Nat. Phys. 8: 611–615.
lution low cost charge sensitive amplifier. Nucl. Instrum. Meth. 47. Müller K, Ryll H, Ordavo I, Ihle S, Strüder L, Volz K, Zweck J,
145: 593–600. Soltau H, Rosenauer A (2012) Scanning transmission electron
42. OPA 657 “1.6 GHz, Low-Noise, FET-Input Operational microscopy strain measurement from millisecond frames of a
Amplifier”, www.ti.com. direct electron charge coupled device. Appl. Phys. Lett. 101:
43. Farr W D, Smith G C (1983) Emitter followers and source fol- 212110.
lowers as low noise pre-amplifiers for gas proportional detectors. 48. Ishikawa R, Okunishi E, Sawada H, Kondo Y, Hosokawa F,
Nucl. Instrum. Meth. A 206: 159–167. Abe E (2011) Direct imaging of hydrogen-atom columns in a
44. Levit L B, Farr W D, Vincelli M L (1985) The phenomenology of crystal by annular bright-field electron microscopy. Nat. Mater
low noise charge sensitive amplifiers. Nucl. Instrum. Meth. A 10: 278–281.
235: 355–361. 49. Kirkland E J, Thomas M G (1996) A high efficiency
45. Beltrán D, Perlas J A (2002) A fast low noise charge preamplifier annular dark field detector for STEM. Ultramicroscopy 62:
for position sensitive detectors. Rev. Sci. Instrum. 73: 3075. 79–88.