Chinese Journal of Physics 60 (2019) 510–521

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Chinese Journal of Physics

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Growth, structure, thermal, electrical and optical properties of

T
potassium aluminum sulfate dodecahydrate (potash alum) single
crystal
⁎
A.M. Abdulwahaba, , Yusra Abdullah Ahmed Al-magdashia, Abdo Meftaha,
Dyab A. Al-Eryanib, A.A. Qaidc
a
Physics Department, Faculty of Applied Science, Thamar University, Dhamar 87246, Yemen
b
Department of Chemistry, Faculty of Science, King Abdulaziz University, P.O. Box 80203, Jeddah 21589, Saudi Arabia
c
Chemistry Department, Faculty of Applied Science, Thamar University, Dhamar 87246, Yemen

A R T IC LE I N F O ABS TRA CT

Keywords: Single crystal of potassium aluminum sulfate dodecahydrate (potash alum) was grown by the
Potash alum slow evaporation technique of supersaturated aqueous solution at room temperature. The ob-
Electrical conductivity tained crystal was characterized by using powder X-ray diffraction, DSC, TGA, electrical con-
Optical band gap energy ductivity, optical transmittance and optical reflectance measurements. Structural and thermal
Normal dispersion
analyses were performed on potash alum crystal. The electrical conductivity of potash alum as
Dielectric constant
electrolyte sample was 1.894 × 10−6 S/cm. The optical transition and optical band gap energy of
potash alum crystal were studied for the first time. Direct and indirect optical band gap energies
were 5.75 and 4.50 eV respectively. Extinction coefficient, refractive index, real and imaginary
dielectric constants and optical conductivity were calculated for potash alum crystal at a range of
photon energies between 1.4 and 6.2 eV. Normal dispersion parameters of potash alum crystal
were calculated for the first time.

1. Introduction

Potassium aluminum sulfate dodecahydrate (potash alum), which has the chemical formula KAl(SO4)2·12H2O, belongs to a large
family of isotopic compounds called alums. The general formula of alums family is M1+ M3+ (XO4)2·12H2O where M1+ is a
monovalent cation (NH4, K, Rb, Cs, Na) and M3+ is a trivalent cation (Al, Ga, In, Cr, Fe), X = S, Se. The crystal structures of alums
have the cubic system, Pa3 space group and four formula units in the unit cell. These structures are divided into three types α, β and γ
because the atomic arrangements are different [1]. Potash alum, KAl(SO4)2·12H2O, belongs to the type of α-alums and its lattice
constant a = 12.157 Å [2].
The water molecules are eliminated from KAl(SO4)2·12H2O when heating it to 510 K (237 °C) and the heated sample becomes
crystalline KAl(SO4)2 [3]. Kishimura et al. [4] found a phase transition from a crystalline to an amorphous phase of KAl(SO4)2·12H2O
when heating it at 180 °C for 2 h. They found also that the anhydrous potash alum, KAl(SO4)2, can be obtained by heating KAl
(SO4)2·12H2O powder at 500 °C for 2 h. They reported in another work [5] that the structural phase transition from crystalline to
amorphous phase of KAl(SO4)2·12H2O began at around 75 °C and this phase remained to approximately 180 °C. Then, the anhydrous
KAl(SO4)2 appeared at 180 °C and above. Crystallization of potash alum and the effects of some conditions on the growth rate of this

⁎
Corresponding author.
E-mail address: abduhabdulwahab@yahoo.com (A.M. Abdulwahab).

https://doi.org/10.1016/j.cjph.2019.05.034
Received 5 February 2019; Received in revised form 23 April 2019; Accepted 13 May 2019
Available online 05 June 2019
0577-9073/ © 2019 The Physical Society of the Republic of China (Taiwan). Published by Elsevier B.V. All rights reserved.
A.M. Abdulwahab, et al. Chinese Journal of Physics 60 (2019) 510–521

crystal were the subjects of many publications [6–10].

Potash alum has been used in many applications like food additive, antiperspirants, cleansing products and skin care products.
Furthermore, it has been used in Raman laser converters [11] and potential applications in optical limiting and switching [12,13].
Hemalatha et al. [14] reported that Potassium aluminium sulphate dodecahydrate crystal belongs to cubic system with the space
group Pa3, lattice constant a = 12.24 Å and Z = 4. They, also, reported that the conductivity of this crystal at 308 K is
3.154 × 10−10 S/cm. Gu and Li [15] found that potassium alum crystals are colored electrolytically below 100 °C and under various
voltages using a pointed cathode and a flat anode.
Recently, some papers used potash alum in new medical applications. Ali [16] studied the antimicrobial effects of alum and
coalescence between alum and antibiotics to killing microorganisms. In this study, it was found that potash alum salt inhibits growth
of the bacteria, its antibacterial effect increases with its concentration and it has excellent antimicrobial inhibitory effects on mi-
croorganisms especially commixed with antibiotics. Uzkul and Alkan [17] dyed the silk fabric by using green walnut shell extract
which has an antimicrobial effect and they used potash alum as mordant. Wang and Lu [18] used potash alum to fabricate oral ulcer
powder and they studied it by temperature-dependent X-ray diffraction technique.
To the best of our knowledge, the studies on potash alum crystal are little in terms of some important physical properties like
electrical and optical properties. In addition, some important constants and parameters of this crystal did not calculated yet. In this
work, single crystal of potash alum will be grown and then its structure, thermal, electrical and optical properties will be studied.
Also, some constants and parameters of potash alum crystal will be calculated for the first time.

2. Experimental procedures

2.1. Crystal growth

Potassium aluminum sulfate dodecahydrate (potash alum), KAl(SO4)2·12H2O, compound was dissolved in double distilled water
at a 500 ml beaker to prepare the starting aqueous solution for crystal growth. The aqueous solution is kept in an undisturbed place
for evaporation. The solution was allowed to evaporate slowly the excess amount of water (to be supersaturated) at room tem-
perature. The good quality of seed crystals have been produced due to spontaneous nucleation within 7 days. The obtained seeds
were photographed and are displayed in Fig. 1(a). Clear and pure seed was chosen for the growth of potash alum single crystal by
using the slow evaporation of the supersaturated aqueous solution at room temperature. The seed was suspended in the super-
saturated solution by using a nylon thread in order to allow the crystal to grow from all sites. Single crystal with dimensions of
1.1 × 1.0 × 0.7 cm3 was grown in a period of 30 days. The photograph of the harvested single crystal of potash alum is displayed in
Fig. 1(b) which shows that the crystal is colorless, transparent, has good quality with regular shape and has well-defined edges.

2.2. Powder X-ray diffraction measurement

Powder X-ray diffraction (XRD) was measured for a sample which was powdered well from the obtained single crystal of potash
alum. The measurement was performed by using XD–2 X-ray diffractometer with CuKα1 radiation of λ = 0.154056 nm. The mea-
surement was performed at room temperature. It was operated with target voltage and current of 40 kV and 30 mA respectively.

2.3. Thermal measurements

The differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) were measured for potash alum by using the
analyzer (NETZSCH STA 449F3-Jupiter) at a heating rate of 10 K/min. Powder sample of mass 9.2 mg was used for DSC and TGA
scans between room temperature (23 °C) and 210 °C while the atmosphere was the nitrogen gas. Both DSC and TGA were recorded
simultaneously. The output of DSC was in mW/mg.

Fig. 1. Photographs of the obtained seeds (a) and single crystal (b) of potash alum.

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Fig. 2. The X-ray powder diffraction scan of potash alum crystal.

2.4. Electrical conductivity measurement

The electrical conductivity measurement was achieved for potash alum sample by using (conductivity meter and 3540 pH). The
used sample for this measurement was cut from the grown single crystal and then it was dissolved in double distilled water to obtain
sample as an electrolyte.

2.5. Optical measurements

The optical transmittance (T) and reflectance (R) were measured for potash alum crystal with unpolarized monochromatic light
using UV–Visible spectrophotometer (Varian, Cary 50). The measurements were performed at room temperature in the wavelength
range 200–900 nm (photon energies between 1.4 and 6.2 eV) and the surrounding medium was the air. The used sample for optical
measurements was cut from the grown single crystal as a rectangular plate with thickness 2 mm. The prepared plate was clear and
free from noticeable defects. It was polished by using a wet piece of soft cloth in order to be very smooth and transparent. The sample
was fixed to a suitable holder by special glue.

3. Results and discussion

3.1. Crystal structure

Fig. 2 shows the X-ray powder diffraction scan of the obtained crystal. The peaks of diffraction match very well the reported
values of the peaks for potash alum crystal in the PDF file No. 07-0017. TREOR [19] computer program was used to treat the powder
X-ray diffraction (XRD) output data in order to find the crystal structure and to calculate the lattice parameters of the grown crystal.
The structure results obtained from the treatment are listed in Table 1 where a is the lattice constant, V is the unit cell volume, Z is the
number of lattice points in unit cell, F30 and F20 are F-factors for the first 30 and 20 lines respectively.

Table 1
Crystal structure results that obtained in this work from TREOR program for potash alum crystal.
System Space group a(Å) V(Å3) Z F30 F20

Cubic Pa3 12.15 1793.6 4 52 74

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Fig. 3. DSC and TGA thermograms for potash alum crystal.

The values in Table 1 have very good agreement with the literature [1,2] and therefore it can be deduced that the grown crystal in
this work is potash alum KAl(SO4)2·12H2O.

3.2. Thermal analysis

DSC and TGA curves of the grown crystal are portrayed in Fig. 3 as functions of temperature. Two endothermic peaks can be seen
clearly in DSC curve. One from these two peaks is associated with loss in mass and the other is not as it is observed in TGA curve. The
first peak, which is independent of mass loss and reaches its maximum intensity at 102 °C, can be attributed to a structural phase
transition. The second peak, which is associated with mass loss and reaches its maximum intensity at 159 °C, can be attributed to a
decomposition or dehydration process. The structural phase transition starts at about 80 °C and it finishes at about 137 °C which is the
point of starting the dehydration process. This process finishes at about 190 °C. The structural phase transition, between 80 °C and
137 °C, transforms the crystalline phase of potash alum, KAl(SO4)2·12H2O, to the amorphous phase. Then, KAl(SO4)2·12H2O loses
some of its water molecules between 137 °C and 190 °C (dehydration process). TGA curve shows that the loss in mass reaches to 34%
at 190 °C which means that there are nine water molecules evolved from the crystal and the anhydrous KAl(SO4)2 started to appear.
These results have very good agreement with the literature [3–5]. This agreement, also, confirms that the grown crystal in this work
is potash alum KAl(SO4)2·12H2O.

3.3. Electrical conductivity

The value of DC electrical conductivity (σDC) of the electrolytes can be calculated by using the following equation [20]:
l
σDC =
ARb (1)

where l is the thickness, A is the area of the electrolyte sample and Rb is the bulk resistance of the electrolyte sample. The obtained
value of σDC for potash alum electrolyte is 1.894 × 10−6 S/cm. It is called the ionic conductivity of the material because the used
sample for conductivity measurement is an electrolyte sample.

3.4. Optical properties

3.4.1. Optical band gap energy

The measured transmittance (T) and reflectance (R) of potash alum single crystal are sketched in Fig. 4 against wavelength (λ) at a
range of 200–900 nm. R values are between 0 and 0.12 while T values are between 0.15 and 0.50. T values do not exceed 0.50
because the used sample for optical measurements has high thickness (2 mm). Both T and R decrease rapidly with decreasing λ at the
range of wavelengths lower than ∼ 300 nm. At the range of wavelengths higher than ∼ 300 nm, T decreases while R increases with
decreasing λ.
The absorption coefficient (α) can be estimated from the measured T and R by using the following formula [21]:

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Fig. 4. Transmittance (T) and Reflectance (R) against wavelength (λ) for potash alum crystal.

1 ⎡ (1 − R)2 ⎤
α= Ln
d ⎢ ⎣ T ⎥
⎦ (2)
where d is the sample thickness. The absorption coefficient (α) is exhibited in Fig. 5 as a function of photon energy (E). A continuous
increase of α with increasing E can be seen at all measured range of photon energies (1.4–6.2 eV), and the increment becomes more
rapidly at the values of E near the optical band gap energy of the material (more than ∼ 4 eV).
To calculate the optical band gap energy (Eg) of potash alum crystal, we can use the following relation [22]:
(αE )r = A (E − Eg ) (3)
where A is an energy-independent constant, E is the incident photon energy and r is a number which characterizes the optical

Fig. 5. Absorption coefficient (α) as a function of photon energy (E) for potash alum crystal.

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Fig. 6. (αE)2 versus photon energy (E) for potash alum crystal.

transition process in the material. The number r equals to 2 for direct allowed transition, 1/2 for indirect allowed transition, 2/3 for
direct forbidden transition and 1/3 for indirect forbidden transition.
To the best of our knowledge, no experimental data are available in the literature for the type of optical transition or the value of
optical band gap energy of potash alum crystal. Therefore, the optical data in this work were tested to find the dominant type of
optical transition in potash alum crystal according to Eq. (3) and to obtain its optical band gap energy. Figs. 6 and 7 show respectively
the plots of (αE)2 and (αE) 1/2 versus photon energy (E). It is noticed from these two figures that both (αE)2 and (αE) 1/2 give straight
lines at higher photon energies and therefore potash alum crystal has two optical allowed transitions (direct and indirect). The
straight line of each plot in Figs. 6 and 7 is extended on E axis to obtain the values of direct (Egd) and indirect (Egi) optical band gap
energies. It is clear that Egd = 5.75 eV and Egi = 4.50 eV. These values of Egd and Egi are calculated for potash alum crystal in the
present work for the first time.

1/2
Fig. 7. (αE) versus photon energy (E) for potash alum crystal.

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Fig. 8. Extinction coefficient (K) versus photon energy (E) for potash alum crystal.

3.4.2. Optical constants

The extinction coefficient (K) and refractive index (n) are called optical constants. They can be calculated from the absorption
coefficient (α) and reflectance (R) by using the following two equations [23]:
αλ
K=
4π (4)

(n − 1)2+ K2
R=
(n + 1)2 + K 2 (5)
The obtained K and n for potash alum single crystal are plotted versus photon energy (E) in Figs. 8 and 9 respectively. It is evident
that K ≅ 10−5n at all measured range of photon energies (K values are between 0.9 × 10−5 and 1.8 × 10−5 while n values are

Fig. 9. Refractive index (n) versus photon energy (E) for potash alum crystal.

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between 1 and 2.1). The values of K are very small comparing with n because potash alum crystal is transparent, colorless (Fig. 1) and
it has low reflectance and high transmittance (Fig. 4). Furthermore, this relation between K and n is one from the characteristics of
insulators.

3.4.3. Normal dispersion

Dependence of the material refractive index (n) on the incident photon energy (E) is called dispersion. The normal dispersion is
the type of dispersion when n increases with increasing E. This type occurs at photon energies region below the fundamental ab-
sorption edge of the material. The reverse type is called anomalous dispersion and it occurs at photon energies region above the
fundamental absorption edge of the material [24].
It is noticed from Fig. 9 that the refractive index (n) increases with increasing photon energy (E) at the lower values of E (below
Eg). This behavior indicates the presence of normal dispersion for potash alum crystal at this range of photon energies. At the higher
values of E (above Eg), the refractive index decreases rapidly with increasing photon energy. This behavior is related to the effect of
fundamental absorption edge and anomalous dispersion [24] of the material at this range of photon energies.
The relation between refractive index (n) and incident photon energy (E) at region of photon energies below the optical band gap
energy (normal dispersion region) can be expressed by Wemple and DiDomenico equation [25]:
E0 Ed
εr = n2 = 1 +
E02 − E 2 (6)
where εr is the real part of the complex dielectric constant, E0 is the single oscillator energy and Ed is the dispersion energy. We can
change Eq. (6) to the following form:

E 1 ⎞ 2
(n2 − 1)−1 = ⎛ 0 ⎞ − ⎛
⎜ ⎟ ⎜E ⎟

⎝ Ed ⎠ ⎝ E0 Ed ⎠ (7)
−1
Fig. 10 shows the plotting of (n −1) as a function of E for potash alum crystal at a range of E between 7 and 8 eV (at normal
2 2 2 2

dispersion region). The relation was fitted to the best straight line according to Eq. (7) by using Origin program. An excellent straight
line was obtained as it is clear in Fig. 10. The parameters E0 and Ed were calculated from the slope (1/E0Ed) and intersection (E0/Ed) of
the straight line and the obtained values are listed in Table 2.
The oscillator strength (f) of potash alum crystal was calculated from E0 and Ed by using the following relation [25]:
f = E0 × Ed (8)
and the obtained value is inserted to Table 2.
Putting E = 0 in Eq. (6) leads to the following relation:
Ed
ε (0) = n2 (0) = 1 +
E0 (9)
where n(0) is the static refractive index (the refractive index at zero photon energy) of the material and ε(0) is the static dielectric

Fig. 10. (n2−1)−1 versus E2 fitted to the best straight line at a range of E2 between 7 and 8 eV2 for potash alum crystal.

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Table 2
Normal dispersion parameters for potash alum crystal.
Equation E0 (eV) Ed (eV) f (eV) 2
n(0) ε(0) a1 (eV)−2 M−1 M−3 (eV)−2

Wemple and DiDomenico 6.26 15.56 97.41 1.87 3.49 – 2.4878 0.0636
Cauchy–Sellmaier – – – 1.84 3.38 0.024 – –

constant (dielectric constant at zero photon energy). For potash alum crystal, the values of n(0) and ε(0) were calculated from E0 and
Ed by using Eq. (9) and they are listed in Table 2.
The optical spectrum moments (M−1 and M−3) can be calculated also from E0 and Ed by using the following two equations [25]:
M−1
E02 =
M−3 (10)

M −31
Ed2 =
M−3 (11)

The obtained values of M−1 and M−3 for potash alum crystal are listed in Table 2.
Dependence of n on E at normal dispersion region can be expressed, also, by another equation. It is the approximated
Cauchy–Sellmaier equation expanded in even powers of photon energy (E). The first approximation of this equation gives the fol-
lowing expression [26]:

n = n (0) + a1 E 2 (12)
2 2
where a1 is constant represents the dispersion dn/d(E) of the material. Fig. 11 displays the plotting of n against E for potash alum
crystal at a range of E2 between 7 and 8 eV2 (at normal dispersion region). The relation was fitted to the best straight line according to
Eq. (12) by using Origin program. It is clear from Fig. 11 that the fitting gives an excellent straight line. The parameters n(0) and a1
were obtained respectively from the intersection and slope of the straight line and their values are listed in Table 2. ε(0) was
calculated by squaring n(0) according to Eq. (9) and the obtained value is inserted to Table 2. It is clear from Table 2 that the values of
n(0) and ε(0) obtained from Cauchy–Sellmaier equation are very close to those obtained from Wemple and DiDomenico equation.
This indicates the high accuracy of the optical data in this work for potash alum crystal.
To the best of our knowledge, normal dispersion of potash alum crystal was not studied yet and its parameters (E0, Ed, f, n(0), ε(0),
a1, M-1 and M-3) were not calculated yet. This means that the present work studies normal dispersion of potash alum crystal and
calculates its parameters for the first time.

3.4.4. Dielectric constant

The complex dielectric constant (ε) and its real (εr) and imaginary (εi) parts can be obtained from the refractive index (n) and
extinction coefficient (K) by using the following relations [27]:

Fig. 11. Refractive index (n) versus E2 fitted to the best straight line at a range of E2 between 7 and 8 eV2 for potash alum crystal.

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Fig. 12. Real dielectric constant (εr) as a function of photon energy (E) for potash alum crystal.

ε = (n + iK )2 = εr + iεi (13)

εr = n2 − K 2 (14)

εi = 2nK (15)

For potash alum crystal, εr and εi are displayed as functions of photon energy (E) in Figs. 12 and 13 respectively. In general, one
can see that εi ≅ 10−5εr (εi values are between 3 × 10−5 and 6.7 × 10−5 while εr values are between 1 and 4.2) at all measured range
of photon energies (1.4–6.2 eV). These values of εr and εi indicate that potash alum is insulator material.

3.4.5. Optical conductivity

The optical conductivity (σopt.) is related to the absorption coefficient (α) and the refractive index (n) by the following equation
[28]:

Fig. 13. Imaginary dielectric constant (εi) as a function of photon energy (E) for potash alum crystal.

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Fig. 14. Optical conductivity (σopt.) against photon energy (E) for potash alum crystal.

αnc
σopt. =
4π (16)
where c is the velocity of light in vacuum. For potash alum crystal, the plot of the obtained optical conductivity (σopt.) against photon
energy (E) is depicted in Fig. 14. It is clear that the values of σopt. are between 1.1 × 1010 and 2.7 × 1010 Ω−1 m−1 at all measured
range of photon energies (1.4–6.2 eV). The optical conductivity depends directly on the absorption coefficient and is found to in-
crease sharply for higher energy values due to large absorption coefficient for these values. On the other hand, the optical con-
ductivity (σopt.) values are very high when comparing with those of electrical conductivity (σDC) for insulator material as potash alum.
This because σ, in general, increases with increasing the operating frequency (f) which it is very small (0 Hz) for σDC and very high for
σopt. (∼1014 Hz).

4. Conclusions

The structural, thermal, electrical and optical properties of potassium aluminum sulfate dodecahydrate (potash alum) single
crystal were studied. The structural analysis confirmed that potash alum crystal has the cubic system, its space group is Pa3 and the
lattice constant a = 12.15 Å. DSC curve exhibited two clear peaks at 102 °C and 159 °C. The first peak represents a structural phase
transition and the second peak represents a dehydration process. DC electrical conductivity (σDC) of potash alum electrolyte is
1.894 × 10−6 S/cm. Potash alum crystal has allowed direct and indirect optical transitions with direct and indirect optical band gap
energies of 5.75 and 4.50 eV respectively. The extinction coefficient values are between 0.9 × 10−5 and 1.8 × 10−5 while the
refractive index values are between 1 and 2.1 at a range of photon energies between 1.4 and 6.2 eV. At the same range of photon
energies, the values of imaginary dielectric constant are between 3 × 10−5 and 6.7 × 10−5 while the values of real dielectric
constant are between 1 and 4.2. The optical conductivity increases with increasing the absorption coefficient and its values are
between 1.1 × 1010 and 2.7 × 1010 Ω−1 m−1 at all measured range of photon energies (1.4–6.2 eV).

Declarations of interest

None.

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