Results in Physics 15 (2019) 102772

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Results in Physics
journal homepage: www.elsevier.com/locate/rinp

Development of scattering based glucose sensor using hydrothermally T

synthesized cuprous oxide nanoparticles
⁎
Swati Singha, Utkarsh Kumarb, B.C. Yadavc, , Kuldeep Kumarb, Ravi Kant Tripathib,
Kaman Singhc
a
Nano Optoelectronics, University Institute of Engineering and Technology, Babasaheb Bhimrao Ambedkar University, India
b
Nanomaterials and Sensors Research Laboratory, Department of Physics, Babasaheb Bhimrao Ambedkar University, Lucknow 226025, U.P., India
c
Department of Chemistry, Babasaheb Bhimrao Ambedkar University, Lucknow 226025, U.P., India

A R T I C LE I N FO A B S T R A C T

Keywords: The aim of the present paper is to develop an optical glucose sensor employing the scattering effect of light. The
Light scattering cuprous oxide nanoparticles were prepared by a hydrothermal route. The surface morphology, elemental dis-
Glucose sensor tribution and the average crystallite size of the synthesized nanoparticles have been analyzed by using SEM, EDX
Bandgap and XRD techniques respectively. The SEM images show the spherical structure of cuprous oxide nanoparticle
Functionality
and the highest peak of the cuprous and oxygen in the EDX illustrates the formation of cuprous oxide nano-
particles. The XRD confirms that the Cu2O was successfully synthesized by hydrothermal route with its crystallite
size 12.33 nm. The optical characterization of the film was carried out by UV–VIS spectroscopy and optical band
gap was found as 3.98 eV. The optical glucose sensing behavior of the sensor was investigated by the perpen-
dicular arrangement of laser and detector employing the solution of glucose and cuprous oxide as a scattering
medium. The maximum sensitivity of the sensor was recorded as 7.19 nW/mole and the % of sensor response as
898.

Introduction
Diabetes is the disease which causes the change in glucose con-
centration in the body. For the immunity system, glucose plays an
important role if there is any type of disturbance equilibrium glucose
due to our unmanaged lifestyle it creates lots of problems.
Nanotechnology takes a very important role in the diagnosis of many
diseases. It's a new potential technology which gives reproducible re-
sults. Glucose is a type of important clinical diagnosis sensor and it
belongs to the monosaccharide group and also called dextrose. It is a
simple sugar but provides energy and circulates into the blood. It is
highly soluble in water and forms paste. Glucose is reducing sugar; it
contains free aldehyde and ketone functional groups. If the concentra-
tion of glucose increases or decreases in a body it causes the diabetic
problem. To detect the glucose concentration in blood or any sample
various methods are used. Diabetes is a chronic disease that causes
when the pancreas does not produce insulin properly. There are three
types diabetics Type 1 and Type 2 and Gestational diabetes. In Type 1
deficient insulin production and in Type 2 excess production of insulin,
most people are suffering from type 2 diabetes, in third type diabetes
that's called Gestational diabetes. This is the state where blood glucose
level is above normal but still below that type 2 of diabetes. In females
during the pregnancy chance of gestational diabetes is increased due to
some complications. It also diagnosed through prenatal screening ra-
ther than reported symptoms [1,2]. According to the report of the
World Health Organization, the number of population suffering from
diabetes has risen from 108 million in 1980 to 422 million in 2014. This
rate is increasing day by day and in 2015, it was estimated that 1.6
million death caused by diabetes. The WHO report has confirmed that
diabetes is the seventh leading cause of death in the world [3]. So there
is requirement to develop such type of devices which measure the
concentration of glucose for clinical purpose and it should be cost ef-
fective, easy to handle & fast access. There is an optical sensor which
measures the concentration of glucose in the given sample. This sensor
based on the scattering of light using cuprous oxide nanoparticle.
Cuprous oxide is derived from copper oxide. It is a transition metal
oxide and has many properties e.g. it shows a color indication, exists at
various oxidation state and also act as a good semiconductor material.
Cuprous oxide belongs to the p-type semiconductor. To prepare cuprous
oxide; requirement of the inert atmosphere is required because it shows
rapid phase change [4]. There are various methods used for the
synthesis of cuprous oxide to achieve the unique surface morphologies

⁎
Corresponding author.
E-mail address: balchandra_yadav@rediffmail.com (B.C. Yadav).

https://doi.org/10.1016/j.rinp.2019.102772
Received 2 March 2019; Received in revised form 22 October 2019; Accepted 22 October 2019
Available online 25 October 2019
2211-3797/ © 2019 Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/BY-NC-ND/4.0/).
S. Singh, et al.
relevant to the various field of applications. Cu/Cu2O has gained lots of
interest due to its optoelectronic, electrical and sensing properties
[5–9]. As in general nowadays some carbon nanomaterials like gra-
phene and carbon nanotubes have been used in optoelectronic and
sensing devices [10–15] however the cost of these materials are very
high. Therefore, for the cost effectiveness point of view and low-tem-
perature synthesis technique, cuprous oxides are more favorable for the
fabrication of such devices. It is a well-known p-type semiconductor
with an energy band gap of 2.17 eV. There are several methods for the
synthesis of such material as reactive sputtering, molecular beam epi-
taxy, chemical and thermal oxidation, electroplating, hydrothermal,
sol-gel, laser ablation, chemical reduction, polyol synthesis etc. There is
variation in the size and shape of the cuprous oxide per variety of the
method of synthesis [16–30].
Synthesis of cuprous oxide using the hydrothermal route
The hydrothermal method has been used for the synthesis of sphe-
rical cuprous oxide nanoparticle. In this method, the crystal synthesis or
crystal growth takes place under high pressure and high-temperature
environment. The autoclave plays an important role in the synthesis of
nanoparticle and the growth takes place inside the autoclave at a
maintained temperature. For the synthesis of Cu2O nanoparticles,
CuSO49·5H2O (2 M) was dissolved in 30 ml of deionized water and
stirred for 2 h. During stirring starch (7.0 g) was dissolved in 30 ml of
deionized water and added dropwise in the given solution. After dis-
solving starch solution (0.25 M) of ascorbic acid prepared in 50 ml
water and added in the precursor. Ascorbic acid acts as a reducing agent
and the color of the solution gets changed from blue to pale green. Then
the solution of NaOH (1.5 M) was dissolved in 30 ml deionized water
add drop by drop in the prepared solution, the color of solution con-
verted into dark yellow. This sample was placed in the autoclave at
80 °C for 2 h, the orangey color was appeared. The prepared sample was
kept at room temperature for one day. The solution was filtered and
washed with deionized water for removing impurity. Further, this
material was dried at 60 °C in the furnace at 2 h and finally, the black
colored material was obtained. The obtained material was ground and
preserved for characterization and its potential applications.
Characterization
The surface morphology of prepared cuprous oxide was analyzed
using SEM (JEOL, JESM- 6490LV) & by the detection of back scattered
electrons, it gave the information about composition of the material. UV
visible spectroscopy of liquid sample was carried out using UV/Vis
spectrophotometer (Evolution 201). Fourier Infrared Spectroscopy
(Nicole 6700) of pellet sample gave information about the presence of
the functional groups. The particle size of the diluted sample gave the
size of the particle by zeta nanosizer (Nano-ZS90). X-Ray diffraction of
powder sample was undergone and crystal size was calculated using
Scherer’s formula.
Scanning electron microscopy and EDX analysis
The surface morphology of the sensing element in the form of
powder was investigated by SEM (JEOL, JESM-6490LV). Fig. 1(a) & (b)
shows the SEM images of sensing nanomaterial prepared by hydro-
thermal route. Fig. 1(a) exhibits that the nanoparticles of Cu2O are
agglomerated with each other and left some spaces as pores. The sur-
face structure of that nanomaterial is fundamental for optical glucose
sensing. Most of the particles in Fig. 1(b) are spherical in shape leaving
some spaces as pores. The hydrothermal synthesis process reduces the
residual stress on the surface of the material. At room temperature, the
particles are randomly oriented with a variation of size. But when we
placed material inside the autoclave at high temperature and pressure,
the crystals were grown and the nanoparticles get ordered in specific
2
Results in Physics 15 (2019) 102772
manner. Fig. 2 shows the EDX pattern of the sample which reveals the
elemental composition of the nanomaterial. This sample contains the
composition of copper and oxygen and the amount of copper is more in
comparison to oxygen as shown in the spectrum.
X-Ray diffraction analysis
It gives the information about the crystal structure and size of cu-
prous oxide nanoparticle. The peaks of Fig. 3 were observed at different
value of 2θ. The peaks were observed at 2θ values 48.92˚, 50.47˚, 75.46˚
correspond to (1 1 1), (2 0 0), (2 2 0) & it shows the plane of metallic Cu.
These peaks have quite match with standard JCPDS card no −04–0836,
besides these peaks more diffraction peaks are formed at 2 θ value
29.75˚, 36.43˚, 42.26˚, 61.43˚, 73.74˚, 77.52˚ correspond to (1 1 0),
(1 1 1), (2 0 0), (2 2 0), (3 1 1), (2 2 2). These peaks confirmed fcc crystal
lattice of cuprous oxide match with standard JCPDS card no- 78–2067.
The XRD pattern reveals that prepared nanoparticles were the mixture
of copper (Cu) & cuprous oxide (Cu2O). The average crystal size (D) of
this Cu2O was estimated using Debye-Scherer formula [31]:
D = 0.9λ β cos θ (1)
where, λ is the wavelength of X-ray beam, β is the full width at half
maxima and θ is the diffraction angle. The minimum crystallite size of
cuprous oxide nanoparticle was estimated as 8 nm and average crystal
size was 12.33 nm. The formation of fcc crystal structure of cuprous
oxide with lattice constant a = 4.24 Å.
Ultraviolet–visible spectroscopic analysis
The optical absorption spectrum of the synthesized sample of cu-
prous oxide is shown in Fig. 4. The observed results show the material
response in the ultraviolet region. The absorption spectrum (Fig. 4)
shows an absorption peak at 340 nm. The band gap of material was
calculated by the formula:
Eg = hν − (αhν )2 (2)
Using the formula, the optical band gap was estimated as 3.9 eV.
Particle size analyzer analysis
The average particle size distribution of the synthesized nano-
particle is shown in Fig. 5. The principle of particle size is based on
dynamic light scattering (DLS) due to the Brownian motion of the
particle. In this method, dynamic light scattered from the dilute solu-
tion and observed that there is two type of particle found in the solu-
tion. 20% particle belongs to the range of 10 to 25 nm and 80% particle
belongs to the range of 30 to 200 nm. Most of the particles belong to the
higher size because of having agglomeration nature of Cu nano-
particles.
Fourier transforms infra-red spectral analysis
Fig. 6 illustrates the FTIR spectrum of synthesized cuprous oxide
nanoparticles. FTIR peaks give the information about the chemical
properties of cuprous oxide. The absorbed radiation creates vibration &
rotational energy in the molecules of cuprous oxide. FTIR only responds
when there is presence of dipole moment in the given molecule. In the
unit cell of cuprous oxide the oxygen tetrahedral coordinated by four
copper atom and the copper is linearly bounded by two oxygen atom
(Chang and et. al). The band in the given Fig. 6 from 3410.5 cm−1 to
1663.2 cm−1 shows the maximum stretching and indicates the presence
of hydroxyl ion (-OH). The sharp peak at 625.1 cm−1 confirms the
formation of cuprous oxide nanoparticles. The synthesized nanoma-
terial is further used for the detection of glucose in the representative
sample. Here a simple, eco-friendly and the cost-effective sensor is
S. Singh, et al. Results in Physics 15 (2019) 102772

Fig. 1. SEM micrographs of spherical cuprous oxide nanoparticles.

Fig. 2. EDX analysis of cuprous oxide nanoparticle.

Fig. 4. Absorption versus wavelength graph of cuprous oxide and in-situ plot
Fig. 3. XRD pattern of synthesized cuprous oxide nanoparticles. shows the Tauc plot with an optical band gap as 3.9 eV.

designed.

Working set-up

In this sensor, we use a simple set up for monitoring the glucose

concentration even the amount of glucose at a very low level. The
whole experiment was performed in the darkroom. This sensor is based
on the light scattered by the prepared particles of cuprous oxide. Fig. 7
shows the working setup of the glucose sensor. The glucose sensing
setup consist the He-Ne laser, Glass cuvette, photodetector (model
Fig. 5. Particle size analysis of cuprous oxide nanoparticles showing that 10%
specification- Newport model, 818-SL), optical power meter (model
particle belongs to the 10 to 25 nm and the rest of 40% particle in 30 to 200 nm
specification- Newport OPM-1916 R) with the proper optical arrange- range.
ment as shown in Fig. 7(a).

3
S. Singh, et al. Results in Physics 15 (2019) 102772

Table 1
The variation in output power with glucose concentration at different angle.
I. 30°

n (refractive Amount of glucose (molar Power Is

Ii
index) concentration) (nW)

1.3322 Distilled water 6.12 0.6676 × 10-19

1.3325 1M 3.11 0.6687 × 10-19
1.3327 2M 2.12 0.6694 × 10-19
1.3335 3M 1.73 0.6724 × 10-19

II. 45°

n (refractive Amount of glucose (molar Power Is

Ii
index) concentration) (nW)

1.3322 Distilled water 10.15 1.3351 × 10-19

1.3325 1M 5.92 1.3373 × 10-19
1.3327 2M 3.12 1.3387 × 10-19
1.3335 3M 1.91 1.3447 × 10-19

Fig. 6. FTIR spectrum of Cu2O nanoparticles synthesized by hydrothermal III. 60°

route.
n (refractive Amount of glucose (molar Power Is
Ii
index) concentration) (nW)
Glucose sensing characteristics
1.3322 Distilled water 15.24 2.0026 × 10-19
The cuprous oxide based optical sensor has been developed for the 1.3325 1M 7.85 2.0059 × 10-19
1.3327 2M 4.55 2.0080 × 10-19
detection of glucose level. The variations in output power w.r.t. glucose 1.3335 3M 2.03 2.0170 × 10-19
level have been recorded through the detector. The sensitivity of the
sensor has been defined as the ratio of change in output power (ΔIo ) to IV. 75°
the change in glucose concentration (ΔC ) [32]. i.e.
n (refractive Amount of glucose (molar Power Is
Ii
ΔIo index) concentration) (nW)
S= nW/mole
ΔC (3)
1.3322 Distilled water 18.75 2.4913 × 10-19
Sensor Response of a sensing material is defined as 1.3325 1M 9.47 2.4954 × 10-19
1.3327 2M 6.12 2.4981 × 10-19
SR = (OPi − OPf )/OPf (4) 1.3335 3M 2.11 2.5092 × 10-19

where, OPi is the initial output power and OPf is the final output power. V. 90°
For the given monochromatic light, the Stratton formula for the
n (refractive Amount of glucose (molar Power Is
ratio of scattered incident light intensity Is to the incident light Ii , at a Ii
index) concentration) (nW)
distance r from a particle of spherical shape is given by [33].
16π 4a6 (n2 − 1)2 1.3322 Distilled water 23.56 2.6704 × 10-19
Is sin ψ ∗ sin Ψ 1.3325 1M 11.13 2.6748 × 10-19
(n2 + 2)2
= 1.3327 2M 8.45 2.6776 × 10-19
Ii r 2 λ4 (5)
1.3335 3M 2.26 2.6896 × 10-19
Where n is the refractive index of the medium, λ is the wavelength
of incident light, a is the radius of spherical particle and ψ is the angle purchased from Merck limited was dissolved in double distilled water.
measured from the scattering direction to the direction of incident light. By varying the amount of glucose powder, various solutions of different
concentrations were prepared. pH of the prepared samples were mea-
Preparation of glucose sample sured by pH meter. The pH values of samples were found between 7.0
and 7.5.
Glucose powder (Dextrose anhydrous GR 61787605001046)

Fig. 7. (a) Working setup of the glucose sensor (b) Lab model of the glucose sensor.

4
S. Singh, et al.
Fig. 8. (a) Variation in the output power vs. concentration of glucose (mol/L) at different scattering angles (b) Is/Ii vs. concentration of glucose (mol/L) at different
scattering angles.
Fig. 9. Schematic of the possible mechanism of the non-enzymatic glucose
sensing on the surface of Cu/Cu2O nanoparticle.
Result and discussion
In the present case, cuprous oxide nanoparticle is spherical in shape
and therefore on substituting all the values in Eq. (5), the variation in
output power with glucose concentration at a different angle is given in
Table 1 (I–V).
In the present case, all the observations were carried out in the dark
room at room temperature with humidity 40% and the pH of glucose
sample was maintained between 7.35 and 7.45 which is also the pH of
human blood. Fig. 8(a) shows that as the glucose concentration in-
creases the output optical power of the sensor decreases and after some
time it stabilizes. Fig. 8(b) illustrates that as the glucose concentration
increases, the output intensity first increases and later it stabilizes. The
glucose sensor is a type of opto-electronic sensor which works on the
principle of scattering of light. A cost-effective set-up is used in this
experiment. The results are obtained between the output intensity
Fig. 10. (a) Variation of sensitivity (b) % Sensor response of optical sensor with the variation of scattering angle.
5
Results in Physics 15 (2019) 102772
versus concentration of glucose (mole/L) with fixed amount of cuprous
oxide. The output intensity increases with increase in the concentration
of glucose.
Sensing mechanism
The variation of scattered intensity w.r.t. glucose is based on the
oxidation of glucose on the surface of cuprous oxide nanoparticle.
When the cuprous oxide was dissolved in the double distilled water
then the surface is oxidized to catalytically active Cu (III) radical. The
glucose absorbs onto the radial surface and oxidized to glucono-δ -lac-
tone by the Cu (III) radical species as shown in Fig. 9. The oxidized
species absorbs the laser light so less scattered light was observed on
the detector as shown in Fig. 8(a).
Fig. 10(a, b) shows the variation of sensitivity and sensor response
of the sensor with the variations of the scattering angle and maximum
sensitivity was found at 90° of the scattering angle.
It is also useful for the detection of low concentration glucose. The
observed results are very useful for diabetic patient as a measuring tool
for glucose in the blood sample. There is no toxic effect of this sensor.
Its operation is simple.
Conclusion
Nanostructured spherical cuprous oxide nanoparticles have been
successfully synthesized using the hydrothermal route and employed as
a tool for detecting the glucose levels in the human blood. The XRD
pattern revealed that the synthesized nanoparticle have minimum
crystallite size as 8 nm and average crystallite size as 12.33 nm. The
S. Singh, et al.
observed IR peaks between 500 and 1500 cm−1 confirm the char-
acteristic peak of cuprous oxide. The maximum sensitivity of the sensor
at scattering angle 90° is 7.19 and the % of sensor response is 898. Thus,
optical glucose sensor developed is a cheap, robust and eco-friendly
which may be further fabricated for its industrial application.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influ-
ence the work reported in this paper.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://
doi.org/10.1016/j.rinp.2019.102772.
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