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Received 20 April 2004; received in revised form 17 August 2004; accepted 18 August 2004
Available online 25 September 2004
Abstract
A novel electrical sensor platform containing a porous silicon (PSi) layer on a crystalline silicon substrate has been developed in which the
electrical contacts are made exclusively on the backside of the substrate allowing complete exposure of the surface to the sensing molecules.
The PSi layers were 20 m thick with an average pore diameter of 1 m. Real-time measurements of capacitance (C) and conductance (G)
were performed and the response produced by the addition of different organic solvents was evaluated. The observed response is attributed to
the combined effect of a change in dielectric constant inside the porous matrix and a modification in the depletion layer width in the crystalline
silicon structure. A space charge region modulation model was used to explain the effect induced by molecules of different dipole moments,
dielectric constants, polarizabilities and water solubilities.
© 2004 Elsevier B.V. All rights reserved.
Keywords: Macroporous silicon; Electrical sensors; Organic solvent detection; Chemical sensor
0925-4005/$ – see front matter © 2004 Elsevier B.V. All rights reserved.
doi:10.1016/j.snb.2004.08.016
348 M. Archer et al. / Sensors and Actuators B 106 (2005) 347–357
Fig. 2. (a) Schematic cross sectional view of the porous silicon sensor. The electrical contacts are placed on the back part of the layer (c-Si) by aluminum
evaporation or colloidal silver paint 700 m apart. (b) Pictures of the front and backsides of the device.
Fig. 3. (a) Phase angle (Θ) and (b) impedance (Z) as a function of frequency. The measurements were done in a dry sample (no infiltration of the porous layer)
with a dc bias of 0 V and an ac signal of 90 mV.
and then determined the optimal frequency based on the 2.3. Measurements with organic solvents
measured values of impedance (Z) and phase angle (Θ).
The results are shown in Fig. 3. At low frequencies the To evaluate the response of our sensor to organic solvents,
device behaves as a resistor and, as the frequency increases, we exposed the device to molecules with different dipole mo-
the phase angle shifts towards a capacitive behavior and ments, polarizabilities and dielectric constants. The solvents
the impedance is reduced. We selected a frequency of were separated in two groups, polar and non-polar molecules.
100 kHz to reduce the effect of parasitic capacitances and Water was analyzed independently. The characteristics of the
of interface states at the contact site [24]. The measure- solvents used are shown in Table 1 [25] Four characteristics
ments under these experimental conditions correspond were selected to understand the response:
to a parallel C–G circuit. All the experiments were per-
• Dielectric constant: related to the electric field distribution
formed at room temperature (22 ◦ C) under a controlled
inside the porous layer.
humidity ambient (40–50% relative humidity). A schematic
• Dipole moment: related to the local fields on the surface of
representation of the measurement setup is shown in
the porous layer.
Fig. 4.
• Polarizability: related to the orientation of the molecule
with respect to the porous layer surface.
• Bond character: related to water solubility (polar
molecules are more soluble in water than non polar
molecules).
Prior to the addition the sensor was allowed to stabilize
for at least 20 min under the temperature and humidity con-
ditions indicated in Section 2.2. Individual experiments were
performed on different layers by adding 10 l of solvent. We
have investigated the sensitivity of the sensor to volumes in
the range of 2–10 l and our results suggest that the volume
Fig. 4. Schematic of the measurement setup. An inductance–capacitance–
resistance (LCR) meter controlled by LabViewTM is used to measure the real-
of the solvent is not related to the magnitude but rather to
time changes of capacitance (C) and conductance (G). The measurements the duration of the response (time during which the layer
are performed under a low humidity ambient. remains wet). A more detailed characterization of the volu-
350 M. Archer et al. / Sensors and Actuators B 106 (2005) 347–357
Table 1
Values of dielectric constant (ε), dipole moment (µ) and electronic polarizability (α) of the organic solvents tested [25]
Solvent dc dielectric constant Dipole moment (D) Electronic polarizability (×1024 cm3 ) Bond character
Acetonitrile 37.5 3.45 4.4 Polar
Acetone 20.7 2.85 6.33 Polar
Ethanol 24.5 1.69 5.41 Polar
Chloroform 4.81 1.15 9.5 Polar
Benzene 2.27 0 10.32 Non-polar
Toluene 2.83 0.43 12.26 Non-polar
Water 80 1.82 1.45 Polar
metric sensitivity of the device would require the handling of layer that can modulate the field in the c-Si channel by two
subnanoliter volumes. Within this range the response could mechanisms: (1) change in the space charge region by charge
be significantly influenced by the solvent’s vapor pressure and redistribution and (2) change in the width of the conductive
its surface tension, which in turn would affect the infiltration channel.
of the solvent into the porous layer. In our experiments, the In the SCRM model, adsorbed molecules change the space
response of the capacitance (C) and the conductance (G) was charge region or depletion layer of the crystalline silicon rods
measured as the percentage change of the signal with respect and even affect the crystalline silicon substrate. In lightly
to the reference value. doped Si small changes in the surface charge produce a large
change in the space charge region width. Since the oxide that
covers the surface is thin the effect of electrical charges on
3. Model the oxide surface can influence the underlying silicon. These
two characteristics constitute the principle of detection and
3.1. Space charge region modulation (SCRM) model transduction of our PSi sensor. We note that they have recently
been exploited for the development of other devices such as
In order to understand our results and to compare them cantilever field effect sensors [26].
with those in the literature we have developed a space charge When the surface of the porous layer is exposed to a liquid,
region modulation (SCRM) model. We will first describe our electrostatic equilibrium at the solid/liquid interface must be
sensor as a field effect device and derive an equivalent elec- established. This produces an electric field that results in an
trical circuit. The principles of detection and the assumptions electrical double layer formed by the space charge region
made in the analysis will then be discussed. Finally, the cor- (in the semiconductor) and the Gouy layer (equivalent to the
relation of the electrical response with the electrical charac- space charge region in the electrolyte). Adsorbed ions be-
teristics of the molecules will be presented in Section 4. tween these two layers form the Helmholtz region, which to-
In a field effect transistor (FET) current flows through a gether with the semiconductor space charge region, accounts
channel when a voltage is applied between the source and for most of the potential drop (Galvani potential) across the
drain terminals. The conductance in the channel, which is double layer. While the Helmholtz region is primarily sensi-
directly proportional to its dimensions and the number of tive to the adsorption/desorption of ions and the electrolyte
carriers can be modulated by changing either of these two composition, the role of the semiconductor space charge re-
variables. This modulation is done by applying an electric gion is to compensate charge until equilibrium is reached
field through a metal gate terminal which can be placed at the [21]. The response of our device is produced by the charge
same plane between the source and drain (e.g., MESFET) or compensation in the c-Si along with changes in the dielec-
parallel to them (e.g., JFET). When FETs are used as electro- tric constant of the porous layer. The change in the space
chemical transducers the metal gate is substituted by an elec- charge region will depend on the sign of the charge “felt”
trolyte or a synthetic selective membrane and modulation of by the c-Si rod and its magnitude, which is also influenced
the conductance in the channel results from the change in po- by the orientation of the molecule with respect to the sur-
tential at the semiconductor surface when chemical species face. If the effect is that of a positive charge then the width
are present. In our device the gate electrode is substituted by of the space charge region increases, the opposite being true
the porous layer and the channel is the c-Si substrate. Al- for negative charges. Water soluble molecules tend to as-
though the experiments are carried out under a controlled sociate closer to the surface therefore inducing a stronger
humidity ambient, the presence on the porous layer surface effect.
of at least a monolayer of water is unavoidable. This initial
condition of the porous layer surface renders it with a larger 3.2. Simulations and equivalent circuit
hydrophilic character, which influences its adsorption prop-
erties. When a molecule is infiltrated in the porous layer its In order to evaluate the field distribution in our device
interaction with the surface will change the field distribution we performed a simulation of the electric field using com-
in the c-Si rods. The porous layer then becomes a charged mercially available software (Ansoft, Maxwell 2-D). Fig. 5
M. Archer et al. / Sensors and Actuators B 106 (2005) 347–357 351
Fig. 5. Simulation of the electric field distribution in the cross section of a c-Si substrate with two parallel electrodes. An ac voltage of 1 V peak to peak at
100 kHz excitation frequency and a dc voltage of 0 V were used as experimental parameters.
shows the calculated electric field distribution for 15 cm alized conditions (all silanols protonated) the same approach
p-type Si with two parallel contacts placed on the back. The has been used in other sensor devices [26] with satisfactory
applied ac voltage is 1 V peak to peak at 100 kHz excita- results. Fig. 6 shows the calculated dc electric field distribu-
tion frequency and the dc voltage is 0 V. The field intensity tion under these conditions. A modification in the charge at
is larger near the contacts and gradually decreases towards the top silicon surface induces a strong variation in the field
the top c-Si surface. This field distribution is very similar to distribution (1 order of magnitude) with respect to the undis-
the one reported by Ramos et al. [27] for dielectrophoresis turbed condition (results not shown) and therefore a change
applications with a similar electrode geometry. The current in the measured electrical properties.
density distribution is also such that its magnitude is larger at The results of the simulations and the following assump-
the interface with the electrodes close to the gap, and grad- tions were used in the model:
ually reduces towards the surface of the c-Si substrate. The • The interface states at the metal–semiconductor junction
simulation shows that the electric field can reach the top of do not affect the response. A junction capacitance is present
the c-Si where the PSi layer is located. As mentioned before at each electrical contact and its value remains constant at
the response of our device is based on changes in the porous the given excitation frequency [24].
layer induced by the presence of molecules. This effect was • The porous layer is modeled as a composite material made
simulated by considering a uniform sheet of charge on the of alternating pores (or void space) and crystalline silicon
top surface in the presence of a dc voltage of 1 V and an ac rods with bulk silicon properties.
voltage of 0 V between the electrodes. As an example a line of • The electric field (E) and the current density (J) reach the
charge of 34 nC was used for this simulation. We calculated porous layer.
this value from the number of silanol (Si OH) groups per • The infiltration of the porous layer with materials of dif-
unit area on chemically oxidized silica surfaces as reported ferent physical properties produces a change in the width
in the literature [28]. The calculations were made considering of the depletion region of the c-Si rods and a change in
a density of ∼3 × 1012 silanols/cm2 [21,28] distributed over dielectric constant of the void space.
a line of charge of 7 mm length and 1 mm width with each • The PSi layer can be considered as a charged layer in con-
silanol group contributing to one elemental charge (1.6 × tact with the c-Si substrate. Changes in the charge distribu-
10−19 C). Although this is just an approximation under ide- tion within the porous layer extend into the c-Si substrate.
Fig. 6. Simulation of the electrostatic field distribution in the cross section of the c-Si substrate with a uniform line of charge of 34 nC on the top surface. A dc
voltage of 1 V and an ac voltage of 0 V were used as the experimental parameters.
352 M. Archer et al. / Sensors and Actuators B 106 (2005) 347–357
Fig. 7 shows a schematic representation of a section of the 4.1. Response to polar molecules
PSi device composed of pores, c-Si rods and a c-Si substrate.
In the porous layer the pores and the rods are modeled as Fig. 9 shows the real-time evolution of the normalized ca-
impedances composed of a parallel capacitor–resistor (RC) pacitance (C) and conductance (G) of the sensor after expo-
element. Zpore (Cpore || Rpore ) accounts for the pores and Zrod sure to 10 l of chloroform, acetone, ethanol, and acetonitrile
(Crod || Rrod ) for the c-Si rods. The c-Si substrate is rep- at room temperature. The device’s response is different for
resented by Zsubs (Gsubs ) and two junction impedances at each solvent and suggests that they can be identified by at
the contacts sites Zjunc (Cjunct ). The equivalent impedance is least three parameters: magnitude, sign, and duration of the
given by: response (related to the evaporation rate of the solvent). The
reversibility of the response with ethanol and acetone is con-
[(Zsubs )(Zpore + Zrod )] sistent with the reported literature [12,29] for luminescent
Zeq = + 2Zjunct (1)
Zsubs + Zpore + Zrod PSi. In Table 2, we present for each solvent the maximum
Fig. 9. Real-time capacitance (C) and conductance (G) measurements of individual porous silicon sensors upon exposure to (a) chloroform, (b) acetone, (c)
ethanol, and (d) acetonitrile. In each case 10 l of the solvent was added at a time indicated by the black arrow.
change in capacitance (% C) and conductance (% G) with below 2.5, molecules exhibit only electronic polarizability
respect to reference. A negative (positive) value corresponds and, above this value, a certain degree or orientation polar-
to a reduction (increase) below (above) the reference value. ization (for example water). The polarizability plays a role in
Fig. 10 shows that the results of Table 2 are correlated with the response since it defines the orientation of the molecule
the dielectric constant. with respect to the electric field and the surface and therefore
According to the SCRM model infiltration of the pores its effect in the space charge region.
with a different material changes Cpore . We need to explain In order to explain the effects in both the pores and the
why chloroform, ethanol and acetone produce a negative shift rods, we will first consider the simplified model presented
with respect to reference. If the only variable involved in the in Fig. 8. The porous silicon capacitance (CPSi ) consists of a
response was Cpore then as the solvent penetrates the pores a series arrangement of Cpore and Crod , therefore:
reduction in the capacitance would never be observed. This
suggests that a mechanism other than pore filling needs to Crod Cpore
CPSi = (2)
be considered and that the other physical properties (water Cpore + Crod
solubility and dipole moment) of the molecules affect Crod ,
specifically via the electrical double layer as described ear-
lier. The four polar solvents evaluated in this part of the study
possess different degrees of water solubility and a dielectric
constant larger than three. The water solubility influences
the adsorption on the surface and the value of the dielectric
constant the type of polarizability. For a dielectric constant
Table 2
Maximum percentage changes in capacitance (% C) and conductance
(% G) with respect to the reference value for the polar molecules tested
Solvent (% C) (% G)
Chloroform −44 −46
Acetone −13 −21
Ethanol −7 −10
Acetonitrile 53 37
Fig. 10. Measured change in capacitance (% C) and conductance (% G)
A negative sign indicates a reduction of the variable below the reference with respect to the reference value as a function of the dielectric constant for
value. chloroform, acetone, ethanol and acetonitrile.
354 M. Archer et al. / Sensors and Actuators B 106 (2005) 347–357
If Crod Cpore then CPSi ≈ Crod and, since Crod decreases troducing states that act as a charged layer at the surface.
as a result of the increase in Wd , then the change will be The effect of chloroform on oxidized PSi is not documented
negative (− CPSi ). If Crod Cpore then CPSi ≈ Cpore and but in hydrogen-terminated silicon (no oxide) other chlori-
the change will be positive (+ CPSi ). Chloroform, acetone nated hydrocarbons produce a reversible effect in its lumi-
and ethanol produce a decrease in capacitance. Out of these nescence [30]. The difference in reversibility suggests that an
three molecules chloroform is the less water soluble with the irreversible modification of the oxidized surface takes place.
lowest dipole moment, which suggests that it is interacting Similar considerations apply for acetonitrile, which has not
weakly with the surface and that the orientation of the dipole been studied on oxidized surfaces but can be chemically ad-
array is inducing an effect “felt” as a large positive charge sorbed on clean silicon surfaces [31]. The relevance of the
that depletes the c-Si rod making Crod Cpore . As the water oxide properties on the sensitivity of PSi has been widely in-
solubility increases along with the dipole moment and the vestigated by Sailor and coworkers [13]. It is also interesting
dielectric constant, the positive charge-like effect is reduced to notice that acetonitrile and chloroform have the highest
making Crod ≈ Cpore . Acetonitrile, which has a larger dipole ionization potential of the four solvents tested (12.194 and
moment, larger dielectric constant and a high water solubility, 11.37 eV, respectively). The energy of chemisorption is the
induces a positive shift by making Crod Cpore . The mod- difference between the work function of the semiconductor
ulation of the space charge region width in the c-Si rods is and the ionization energy of the molecule [32]. If chemisorp-
similar to what has been reported for silicon nanowires [29] tion is taking place then changes in the surface charge influ-
and is strongly dependent on the surface charge. ence the response of the device. When the samples initially
Fig. 11 presents a simple simulation of the model variables exposed to acetonitrile were subsequently exposed to ethanol,
over time for molecules acting as a positive and a negative no response was observed which confirms that exposure to
charge on the surface. Both the time scale and the values acetonitrile produced a permanent surface modification. This
shown are arbitrary values for illustrative purposes only. In was further confirmed when the sensors were reexposed to the
these simulations we have further assumed that the equivalent solvent for several times allowing the recovery of the baseline
capacitance (Ceq ) is given by the porous silicon capacitance between additions. For ethanol and acetone, in which the re-
(CPSi ) in series with a fixed junction capacitance (Cjunct ) at sponse was reversible, the variation of the maximum change
each contact and that the equivalent conductance (Geq ) is in capacitance (% C) and conductance (% G) was no more
given by the substrate conductance (Gsubs ). The conductance than ±1% with a maximum shift in the baseline of 5% over
is considered to be directly proportional to the number of a 20 min timeline. For acetonitrile and chloroform, the re-
carriers in the c-Si substrate (NA ) as well as the width of the sponse is not reversible therefore the same sensor could not
channel (a). Starting with a dry device (air in the pores) three be tested but the reproducibility of the response in different
stages in the response are identified: exposure (addition of sensors was good (±5%).
the solvent), stabilization (complete infiltration of the pores)
and evaporation (drying of the pores). According to these 4.2. Influence of the channel width (a) in the response
simulations the effect of acetonitrile is that of a negatively
charged molecule, which produces the response in Fig. 11b It was mentioned before that the value of Gsubs depended
while chloroform, ethanol and acetone act as a positive charge on the change in the space charge region width (Wd ) by
(Fig. 11a). changing the majority carrier distribution underneath and
As it can be seen in Fig. 9, neither chloroform nor ace- the width of the conduction channel (a). Neither of these
tonitrile return to the reference value after the solvent has two variables can be probed directly or their independent
evaporated, even after flushing the chamber with nitrogen. contribution extracted from the experimental value of
This suggests that a chemical reaction has taken place, in- conductance. Nevertheless the channel width can be also
Fig. 11. Effect of the modification in the model parameters Cpore , Crod , and CPSi in the equivalent capacitance (Ceq ) and conductance (Geq ) when molecules
acting as a positive charge (a) and a negative charge (b) interact with the surface. The exposure phase corresponds to the initial contact with the organic solvent
that infiltrates into the layer. The stabilization period corresponds to the complete infiltration of the layer. As the solvent evaporates the signal returns to the
reference value.
M. Archer et al. / Sensors and Actuators B 106 (2005) 347–357 355
Fig. 12. Real-time capacitance (C) and conductance (G) measurements of the porous silicon sensor upon exposure to water. (a) The first part of the response
with a coupled behavior in capacitance (C) and conductance (G) is observed over the first minutes of the response. (b) Over a large period of time the two
responses are different.
356 M. Archer et al. / Sensors and Actuators B 106 (2005) 347–357
Fig. 13. Real-time capacitance (C) and conductance (G) measurements of porous silicon sensors upon exposure to (a) benzene and (b) toluene. In each case
10 l of the solvent was added as indicated by the black arrow.
results will be explained based on the predictions of the ductance. To explain our results, we proposed a space charge
SCRM model. The hydrophobicity (low water solubility) of region modulation (SCRM) model that considers the effect
toluene and benzene and their low dielectric constant ex- of changes in the dielectric constant of the porous silicon
plain the small change in capacitance and conductance, and matrix along with the interaction of different molecules with
the sign of the maximum change (indicative of a positive the surface. The simulations performed consider the simul-
charge). Assuming that these molecules interact weakly with taneous change in dielectric constant and charge distribution
the surface, do not produce permanent chemical modifica- induced by molecules with different properties and the results
tions (reversibility of the response) and do not have a perma- obtained are in accordance with our experimental results.
nent dipole moment the only parameter left to influence the In this paper, we demonstrated the use of our device as
response is the electronic polarizability (α). The propagation a chemical sensor capable of producing a different response
of the field inside the structures is orienting the molecules upon exposure to water, ethanol, acetone, chloroform, ace-
perpendicular to the pore wall surface and the lack of orien- tonitrile, benzene and toluene. The sensitivity to charged
tation polarizability eliminates any counteracting effect. The molecules can however extend the use of these devices to
orientation of the dipole array is “felt” as a positive charge. biological applications. We have also demonstrated the use
According to the SCRM model, this effect and the weak inter- of our sensor for selective and reproducible detection of DNA
action of the molecule with the surface produce a very small hybridization in real-time [36].
increase in the space charge region width (Wd ) therefore de-
creasing slightly Crod , which impacts on the charge redistri-
bution at the substrate (Gsubs ). A small change in Cpore is also Acknowledgements
expected due to the low dielectric constant. These results sug-
gest that the interaction of the molecule with the surface and This work was supported in part by a grant from the In-
the orientation of the dipole play a crucial role in the response fotonics Center of Excellence and the sponsors of the Center
of the device. Reversibility of toluene and benzene has also for Future Health. M.A. was the recipient of a dermatology
been reported in as anodized luminescent PSi [12,30]. training grant.
5. Conclusions
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Berger, R. Arens-Fischer, H. Munder, Investigation of different ox-
idation processes for porous silicon studied by spectroscopic ellip-
sometry, Thin Solid Films 276 (1996) 36–39. Professor Philippe Fauchet has 20 years of experience in semiconductor
[24] M. El Yacoubi, R. Evrand, N.D. Nguyen, N. Schmeits, Electri- optoelectronics, ultrafast phenomena and lasers, nanoscience and nan-
cal conduction by interface states in semiconductor heterojunctions, otechnology with silicon, biosensors, electroluminescent materials and
Semicond. Sci. Technol. 15 (2002) 341–348. devices, and optical diagnostics. His research on porous Si and nanoscale
[25] Chemical Rubber Company Handbook of Chemistry and Physics, Si, and applications to LEDs and displays, biosensors, and nanoscale Si
80th ed., Cleveland, OH, 2000. electronic devices, has led to dozens of plenary, invited and contributed
[26] J. Fritz, E.B. Cooper, S. Gaudet, P.K. Sorger, S.R. Manalis, Elec- publications, and numerous invited conference presentations and seminars
tronic detection of DNA by its intrinsic molecular charge, Proc. Natl. in North America, Japan and Europe. He chaired dozens of symposia and
Acad. Sci. U.S.A. 99 (2002) 14142–14146. conferences devoted to various topics in his fields of interest He has also
[27] A. Ramos, H. Morgan, N.G. Green, A. Castellanos, Ac electroki- given many tutorials and short courses. Dr. Fauchet received an IBM
netics: a review of forces in micoroelectrode structures, J. Phys. D: Faculty Development Award in 1985, an NSF Presidential Young Inves-
Appl. Phys. 31 (1998) 2338–2353. tigator Award in 1987, an Alfred P. Sloan Research Fellowship in 1988,
[28] Y. Dong, S.V. Pappu, Z. Xu, Detection of local density distribution the Princeton University Alfred Rheinstein Class of 1911 Faculty Award
of isolated silanol groups on planar silica surfaces using nonlinear in 1888, and the 1990–1993 Prix Guibal & Devillez for his work on
optical molecular probes, Anal. Chem. 70 (1998) 4730–4735. porous silicon. Dr. Fauchet is the author nearly 300 publications, and has
[29] Y. Cui, Q. Wei, H. Park, C.M. Lieber, Nanowire nanosensors for edited five books. He is a Fellow of the Optical Society of America, the
highly sensitive and selective detection of biological and chemical American Physical Society, and the Institute of Electrical and Electronic
species, Science 293 (2001) 1289–1292. Engineering, and a member of the Materials Research Society.