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Sensitivity of an optical sensor that operates at

angular or wavelength interrogation mode


L.C. Oliveira , T.A.T. de Sousa , F.C.C. Loureiro , E.U.K. Melcher , A.M.N. Lima and H. Neff
Dept.

of Electrical Engineering, UFCG, Campina Grande - PB, Brazil


Email: {leiva.oliveira,amnlima}@ee.ufcg.edu.br
Programa de P
os-Graduaca o em Engenharia Eletrica, PPgEE, UFCG, Brazil
Dept. of Computer Science, UFCG, Campina Grande - PB, Brazil
Northeast Center for Strategic Technologies, Recife - PE, Brazil

AbstractThis paper presents a sensitivity study for a surface


plasmon resonance (SPR) sensor system based on a polymer
prism chip capable of operating both at angular and wavelength
interrogation modes. This investigation aims at optimizing the
manufacturing procedure for maximizing the the sensitivity and
the detectivity of the sensor system. Given a selected operating
point the sensor detectivity has been calculated allowing the direct
comparison of achievable performance at both interrogation
modes.

I. I NTRODUCTION
The surface plasmon resonance (SPR) is a quite important technology for detecting, identifying and quantifying
biomolecular interactions [1]. The biosensors based on the
SPR technology combine high optical resolution with the
specificity of biological processes [2]. Such combination
makes SPR biosensing a relatively versatile label free detection
tool which can be employed in a broad range of applications
like pharmaceutical industry [3], beverage industry [4] and
serological diagnosis in biomedical industry [5]. The SPR
biochip design, from now on denoted as prism biochip, proposed in [6] and tested in [7] has numerous advantages like
reduced size, relatively low manufacturing cost (around 1US$)
and thus can be considered a promising alternative for implementing a bio-sensing measurement equipment. However, to
complete the picture one needs to perform a comprehensive
investigation regarding the sensitivity of the prism biochip
which constitutes the main objective of the present paper.
Sensitivity studies for SPR biosensors operating at wavelength
interrogation [8] and angular interrogation [9] have already
been done. The use of a unified theoretical model has also
been proposed for accessing the resolution of SPR sensors
[10]. However, there are design aspects of the prism biochip
which preclude the direct usage of these results, specifically
when sensitivity is exploited for optimizing the biochip design.
The sensitivity of the prism biochip for a given operating point
allows one to evaluate how the properties of the materials
employed in the prism biochip manufacturing process affect
the sensing performance [11][13]. The detectivity at a given
operating point allows for a fair and direct comparison between
the operation in wavelength and angular interrogation modes
which can lead to design changes for improving the prism
biochip performance.

II. T HEORETICAL ASPECTS


The general form of the resonance condition for a three
layer structure condition reads as
r
2
2 3
2
1 sin () .
(1)
=

2 + 3

This equation expresses the matching condition kx = ksp


when the incident light vector (kx ) and plasmon wave vector
(ksp ) are equal. The dielectric function of metal is denoted
by 2 whereas 1 and 3 represent the dielectric function
of the polymer prism chip (biochip) and the bio-recognition
layer (assumed to be semi-infinite), respectively. The incidence
angle of the light beam that hits the multilayer arrangement is
while denotes its wavelength. In the angular interrogation
mode (AIM) the wavelength of incident light is fixed; the angle
of incidence is varied and thus the coupling conditions. By
using the matching condition, may be find that
s
2
3 (1 sin (R ))
2
n3 =
(1 sin (R )) ,
(2)
2

 r
2
n3
(3)
R = arcsin
n1 2 + n23
which represents the refractive index of bio-recognition layer
and R represent the resonance angle when the reflectance is
minimum.
However, the third layer of the tree layer structure usually
cannot be considered as semi-infinite and thus the surface plasmon is also affected by the environmental medium and thus
one must consider a four layer structure. Figure 1 illustrates
the multilayer structure of an SPR biosensor. The four layers
of such structure are namely (1) the polymer prism chip, (2)
the metal layer, (3) the bio-recognition layer and (4) a semiinfinite environmental medium, usually water. The four-layer
system can be reduced to a three-layer system by replacing
the sensor element and the environmental medium by a semiinfinite effective medium with a refractive index neff . Thus,
one may consider that neff n4 represents the change in the
refractive index observed by the SPR sensing element [14].
On the other hand in the wavelength interrogation mode
(WIM) the angle of incidence is kept constant and the coupling
condition depends and varies with the wavelength. One cannot

III. M ANUFACTURING DECISIONS


The manufacturing of the prism biochip embodies all the
relevant choices for the providing the SPR effect excitation.
The procedure is divided into two stages (see Fig. 2), first
one aiming at the prism geometry fabrication, i.e., the choice
for the substrate optical of the multilayer structure (Fig. 1)
and second one dealing with the metal deposition on the
prism surface, i.e., the choice for the thin metallic layer. The
sensitivity study allows one to make the best decision at each
step of the manufacturing procedure.
A. Geometry
Fig. 1. Biosensor multi-layer structure [15]. Dielectric constants, wave vectors
and layer thicknesses are indicated.

determine an analytical expression for refractive index in


WIM directly from the resonance condition equation since
explicitly appears at both side and thus will be cancelled
out. However, since both the dielectric functions of gold, 2 ,
and of the polymer substrate, 1 , vary with the incident light
wavelength one may study the sensitivity by determining how
the changes in neff are sensitive to . Thus, by using the
analytical formulation proposed in [7] one may express the
complex dielectric function of the bio-layer as given in (5)
and consequently the respectives the refractive index will be
given by
r
n3 =

p
3R (R )2
3R (R )2 + 3I (R )2 +
2

(4)

in which 3R and 3I denote the real and imaginary parts of


3 , respectively and R represent the wavelength when the
reflectance is minimum.
3
3R

3I

= 3R + j3I
2R 1 sin2 () + 2R + 22I
= 
2
2
2R 1 sin ()
+ 22I
2I 21

sin ()
= 
2
2
2R 1 sin ()
+ 22I

Fig. 2. Manufacturing methodology for prism biochip.

(5)

Design requirements provide guidelines for prism geometry


(width, height, thickness). A cross sectional view of the prism
biochip is shown in Fig. 3. Due to the trapezoidal shape of
prism, the light source and the image sensor must be placed
as indicated in Fig. 3. The distance travelled by the light after
being reflected at the left side mirror until it reaches middle
point of the top surface determines the physical dimensions of
the prism biochip and the incidence angle at the metallic layer.
The temperature effect on the prism geometry is detailed in
[7].
B. Substrate
The Sellmeier dispersion relation [15] describes the variation of the refractive index (RI) of a selected glass material as
function of wavelength, i.e.:
s

 
 

B1 2
B2 2
B3 2
+
+
n1 () = 1 +
2 C1
2 C2
2 C3
(6)
where Bi , Ci , i = 1, 2, 3 depend on the type of glass, recalling
that 1 = n21 . It is worth to remind that n1 also depend on
temperature according to [16]
n1 (, T )
T
P (T )

n21 (, T0 ) 1
P (T ) , with
(7)
2n1 (, T0 )
E0 + 2E1 T
,
= D0 + 2D1 T + 3D2 T 2 2
2T K

where T0 is a reference temperature (room temperature), T is


the difference between T and T0 and the values Di , i = 0, 1, 2,
Ej , j = 0, 1 and T K depend on the type of glass or polymer.
The material chosen for the first prism manufacturing was a
cyclo-olefin copolymers (COC) having the trade name TOPAS
5013 [16]. One approximation of the Selmmeier formulation

Fig. 3. Biochip geometry [6]. Ideal ray tracing with incident angle of =
68 deg. Details of the experimental set-ups for a) WIM and b) AIM.

E. Thin film

TABLE I
VALUES OF THE PARAMETERS FOR n1 (, T ) AND 1 ()
B1
1.039
D0 106
1.81
b0
1.805

B2
0.231
D1 108
1.20
b1
-0.001

B3
1.010
D2 1011
-2.30
b2 106
1.921

C1
0.006
E0 107
4.95
b3 109
-1.320

The dielectric function of the metallic layer can be described

C2
C3
0.020
103.560
E1 1010
T K
7.71
0.149
b4
3.2671013

for TOPAS polymer consider the use of fourth order polynomials to represent the dependence of the dispertion relation
with the wavelength (see Fig. 7(a)), where the coefficients have
been determined numerical interpolation of experimental data
sets. [7]
1 () = b4 4 + b3 3 + b2 2 + b1 + b0

2 () = 2R () + j2I ()

C. Fabrication
The manufacturer recommends the use of injection molding
for fabricating pieces with TOPAS. Such process introduces
residual stresses which increases the birefringence of the
prism, thus degrading the biosensor performance. To minimize this effect, the prisms are polished and annealed after
fabrication. Annealing process induces changes in the optical
properties of the prism (n1 ) and can be used to influence the
refractive index. In practice, the following equation expresses
how the RI changes after this process:
(9)

with hx representing the annealing rate (K/h) and md is the


annealing dependence coefficient.
D. Light source
Fig. 4 show how the absorbance of TOPAS 5013 varies with
the wavelength. From this plot we select the feasible range for
the ligth source as indicated in the figure.

Fig. 4. Polymer absorbance dispersion at different wavelengths. Graph


obtained with the spectrophotometer FENTO 800 XI

(10)

where 2R and 2I can be determined based on Drudes model,


i.e.,
c 2
2 () = 1 2
,
p (c + j)
in which p = 1.6826 107 , c = 8.9342 106 (Gold)
or p = 1.4541 107 , c = 1.7614 105 (Silver) [8],
the major metallic materials used in SPR applications. In this
paper, we also consider the use of fourth order polynomials
to represent the dependence of the dielectric function of Gold
with the wavelength as given by [7]

(8)

The numeric values of the parameters used in n1 (, T ) and


1 () are given in Table I

nT1 x = nT1 0 + md log (hx )

by

2R () = a4r 4 + a3r 3 + a2r 2 + a1r + a0r

(11)

2I () = a4i 4 + a3i 3 + a2i 2 + a1i + a0i

(12)

and

where the coefficients have been determined numerical interpolation of experimental data sets and the results are practically identical thus facilitating differentiation in relation to
wavelength (see Fig. 7(b)). The temperature also influence in
the scattering mechanisms between particles in a metal treated
by Drude model, these being then temperature-dependent [17].
F. Deposition technique
The sputtering technique was used for deposition of gold. Is
worth mentioning that details such as the continuity, thickness
[18] and roughness [19] of the metal layer directly affects
quality of sensor response.
G. Operating point
In the design of the prism biochip it is assumed that the
incidence angle of the light is 68 deg (Fig. 3). In this case the
resonance condition occurs at R = 670 nm when just pure
water flows over the metallic layer thus it yields neff = 1.332
at ambient temperature; this condition will, from now on,
be considered as the reference case for system response to
calibration, or Operating Point (OP). It is important to point
out that the substrate layer is a TOPAS polymer and the
metallic layer is a thin gold film with 50 nm of thickness.
Fig. 5 shows how the effective refractive index varies
with the wavelength for different types of metal layers.
When one replaces gold by silver the wavelength changes to
R = 600 nm for TOPAS and R = 730 nm for BK7 (for
neff = 1.332, i.e., pure water) and thus a redesign of the prism
biochip must be carried to change 1 to 66 deg to get the same
OP specifications.
For the angular interrogation, the OP is selected such that
the resonance condition for = 670 nm occurs at R = 68 deg
for TOPAS and gold arrangement. According to Fig. 6 when
one replaces gold by silver R changes to 66 deg. When BK7
is used instead of TOPAS R changes to 69.5 deg and to 67 deg
for gold and silver, respectively.

The sensitivity study presented in the following section has


been conducted for this reference condition, i.e., for the OP
shown in Figs. 5 and 6.

Fig. 5. Effective refractive index neff for the prism biochip employing TOPAS
and two types of metallic layers of 50 nm (Gold and Silver). For the Gold
case the results obtained indicate an equity between BK7 and TOPAS. For
Silver the wavelength should be 600 nm for TOPAS and 730 nm for BK7 to
proving the same refractive index for water, i.e, neff = 1.332.

2R
2I
1
. By using
|=R ,
|=R , |=R and
neff
neff
the expressions for 2 and 1 (not shown here) one may
determine how the different design options would affect neff .
The dielectric constants of glasses (TOPAS used in the
prism manufacturing) and metal (two formulations for GOLD)
are shown in Fig. 7a and 7b, respectively; at the OP indicated,
1 = 2.28 (n1 = 1.51) and 2 = 15.2 + j1.01. As
one can see in Fig. 7c the sensitivity for the wavelength
interrogation mode increases with the wavelength, whose value
was Sn3R (OP ) = 6, 373 nm/RIU (Refractive Index Units).
To the same OP, prism biochip may exhibits more sensitivity
replace TOPAS by BK7.
1) Detectivity: The detectivity at the chosen OP is calculated as D = Sn3R / hv i, where the sensor noise feature
hv i at R can be expressed as the square root of the total
wavelength differential, composed of two terms, one related
to the fluctuations of dielectric function of the metal and
substrate, and ones of the analyte effective refractive index,
as given by
s
2 
2
neff 1
neff 2
+
neff . (15)
hv i =
2
1
2
|=R

The optimal value for hv i is 0.1 nm, limitation arising


from the spectrometer. At the optimal condition detectivity
is D (OP ) = 6.367 104 RIU1 (See Fig. 7d)
B. Angular Interrogation

Fig. 6. neff in AIM for the same materials employing in WIM. For the same
refractive index of water, i.e, neff = 1.332, the incident angle for Gold is
68 deg and must also 66 deg for Silver layer using TOPAS polymer.

IV. S ENSITIVITY STUDY


In this section we define mathematically the sensitivity and
detectivity for both interrogation modes.
A. Wavelength Interrogation
Adopting the neff notation, as explained before, the sensitivity of the prism biochip can be obtained by calculating

1
neff
R
Sn3 =
|=R ,
(13)

Derivative (eq. 3) with respect to n3 one may obtain an


analytical expression for the sensitivity SnR3 in the AIM , i.e.:

2R 2R
R
p
Sn3 =
.
(16)
(2R + n23 ) 2R (n23 1 ) 23 1
Fig. 8(a) shows the profile of SnR3 at different wavelengths
whose it value was SnR3 (OP ) = 120.7 deg/RIU. As was
observed in WIM, the sensitivity also increases when the prism
is manufactured with the BK7 polymer. However, in this case
the sensitivity decreases when the wavelength increases.
1) Detectivity: The detectivity at the OP is calculated as
D = SnR3 / hv i where sensor noise hv i at R is given by
square root of the total angle differential as
s
2

2

2
R
R
R
hv i =
21 +
22 +
n2eff ,
1
2
neff
where

where R is the wavelength at the resonance condition when


the reflectance reaches its minimum. To calculate S one must
recall the chain rule and thus
neff
neff 2
neff 1
=
+
(14)

2
1

and

where the first term represents how the metal layer properties
affect the sensitivity and second one shows that the polymeric
material chosen for manufacturing the prism also affects the
sensitivity. By using such polynomial representations, the
metal dielectric function dependence one needs to compute

For the AIM the technical achievable instrumental resolution


is 3.3 105 deg and thus D (OP ) = 6.381 104 RIU1
(see Fig. 8(b)).

R
1
= q
2
2

1 2
1 +n2eff

n3eff
r
1 n2eff +2 n2eff
2
(1 + n2eff )
1 2 +n
( 2 3eff )1

neff 2
R
= p
.
1
1 1 2 + (1 2 ) n2eff

(a)

(a)

(b)
(b)
Fig. 8. Sensitivity and detectivity of the prism biochip with angular interrogation: a) Sensitivity and b) Detectivity.

WIM we found that hv i = 0.35 nm and Sn3R = 2161 nm/RIU


yielding D = 6.174 103 RIU1 .
C ONCLUSIONS
(c)

(d)
Fig. 7. Optical properties, sensitivity and detectivity of the prism biochip:
a) Dielectric function of the metal layer, b) Glass dispersion, c) Sensitivity
in WIM and d) Detectivity maximum refractive index value. The OP label
indicate the selected operating point.

C. Experimental results
All experimental procedures have been conducted at
25 C since sensitivity and detectivity are both temperaturedependent [16]. Changes in refractive index has been provoked
to verify the sensitivity of the manufactured biochips; the
obtained results are given in Table II. Three different concentrations of PBS (Phosphate Buffered Saline) solutions (50%,
77% and 100%), have been employed in the experimental tests
as shown in Fig. 9(a), 9(b) (AIM) and 10(a), 10(b) (WIM).
For the AIM case we found that hv i = 3.5 105 deg and
SnR3 = 126 deg/RIU yielding D = 6.280104 RIU1 . For the

The materials chosen for manufacturing the prism biochip


proposed in [6] (Gold+TOPAS) proved to be appropriate. The
theoretical results show that the detectivity for AIM and WIM
differs about 14 RIU1 . It is worth to point out that BK7
is also a viable replacement for TOPAS without any change
in the prism geometry, being less expensive. The sensitivity
and detectivity predicted with theoretical model for the AIM
agreed quite well with the experimental findings. However,
due to manufacturing problems (low adhesion of thin metallic
layer to the substrate) with the prism biochip the agreement
of the theoretical and the experimental results was not quite
good as its was for AIM; the same prism biochip was used in
both modes and the first experiments have been done for the
AIM.
TABLE II
R , R , nEFF OBSERVED IN THE EXPERIMENTAL TESTS FOR BOTH
INTERROGATION MODES (WIM AND AIM).

PBS
100%
77%
50%
PBS
100%
77%
50%

AIM
R (deg)
0.17
0.14
0.10
WIM
R (nm)
3.89
2.33
1.55

neff (RIU )
1.27x103
1.03x103
7.91x104
neff (RIU )
1.80x103
1.12x103
7.52x104

(a)

(a)

(b)

(b)

Fig. 9. a) neff and b) R changes in AIM for three different PBS solutions.

Fig. 10. a) neff and b) R changes in WIM for three different PBS solutions.

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The authors would like to thank PPgEE, CAPES, CNPq and


CETENE for the financial support and research grants.
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