APT 1694 No.

of Pages 8, Model 5G
30 August 2017

Advanced Powder Technology xxx (2017) xxx–xxx

1

Contents lists available at ScienceDirect

Advanced Powder Technology

j o u r n a l h o m e p a g e : w w w . e l s ev i e r . c o m / l o c a t e / a p t

2 Original Research Paper

4
Effect of reduced graphene oxide (rGO) on structural, optical, and
6
7
5 dielectric properties of Mg(OH)2/rGO nanocomposites
⇑
8 Richa Bhargava, Shakeel Khan
9 Department of Applied Physics, Z.H. College of Engineering and Technology, Aligarh Muslim University, Aligarh 202002, India

11
10
12 article info abstract
1 4

2 6
15 Article history: In this paper, we report the synthesis of Mg(OH)2 NPs and Mg(OH)2–rGO nanocomposites (NCs) by micro-wave assisted co- 27
16 Received 6 May 2017 precipitation method. The crystal phase, structural morphology and functional groups of the as-synthesized samples were 28
analyzed by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR). 29
17 Received in revised form 16 August 2017
Raman spectroscopy was used to study the defects in the samples. Raman spectroscopy and the SEM results validate the 30
18 Accepted 21 August 2017
growth of Mg(OH)2 NPs on the rGO nanosheets. The chemical composition of the prepared samples was analyzed by EDAX. 31
19 Available online xxxx Optical properties of the as-synthesized samples were studied by UV–visible spectroscopy and the energy band gap was cal- 32
culated by Tauc relation which shows a decrease in band gap with an increase in the amount of Graphene Oxide (GO) in the 33
NCs. The dielectric properties were studied as a function of frequency over a range of 50 Hz to 5 MHz at room temperature.
20 Keywords: 34
The value of dielectric constant decreases with an increase in fre-quency, this could be due to the existence of a polarization
21 XRD 35
process at the border of the rGO sheets and Mg (OH) 2 NPs. The value of dielectric loss shows a decreasing trend with an
22 Reduced graphene oxide 36
increase in frequency whereas the larger value of AC conductivity in Mg(OH)2–rGO NCs as compared to Mg(OH)2 NPs 37
23 Mg(OH)2
2
24 Nanocomposites approves the restoration of sp network in the graphene sheets. 38
25 39
40
2017 Published by Elsevier B.V. on behalf of The Society of Powder Technology Japan. All rights reserved. 41
42
43

44

45
46 1. Introduction Oxide (rGO). In the reduction of GO to rGO, the attached functional groups 65
are removed to recover graphene sheet by changing its edge structure and by 66
2 chemical modification of its interior or edges. By the reduction of GO its 67
47 Graphene is a two-dimensional flat monolayer of sp hybridized
48 carbon bonded in a hexagonal honey comb lattice with a minute optical, magnetic and electrical properties can be tailored [10]. 68
49 overlap between valance band (VB) and conduction band (CB), 69
50 which has attracted widespread attention since its discovery in Recently, nanostructures of magnesium hydroxide (Mg(OH) 2) have been 70
51 2004 [1]. Graphene is considered as an emerging material for the 71
widely studied. Mg(OH)2 is a large-band-gap insulating metal oxide with
52 synthesis of graphene based composites because of its unique 72
band gap 5–6 eV [11]. It is of great interest of research from both theoretical
53 nanostructure and interesting properties which includes high 73
and experimental point of view since decades. Magnesium hydroxide holds
54 specific surface area, thermal conductivity, carrier mobility, unu- exceptional properties such as low weight, nontoxicity, high specific stiffness, 74
55 sual band structure and mechanical strength [2]. Due to these noncorro-sive, thermally stable, and electromagnetic shielding property [12]. 75
56 extraordinary properties, graphene has a wide range of application These properties are beneficial for various devices in the fields of electronics, 76
57 in optoelectronic, supercapacitors, sensors, nanocomposites, nano- automotive applications, aerospace, solid-state elec-tronics, photovoltaic 77
58 electronics, batteries, energy harvesting, water purification, photo- devices and biomedicine [13,14]. Various methods for synthesis of 78
59 catalysis, etc. [3].The reduction of Graphene Oxide (GO) can be magnesium hydroxide nanoparticles have been reported such as precipitation 79
60 done by many methods such as chemical reduction by hydrazine method, hydrothermal route, ultrasonic synthesis, laser ablation, microwave- 80
61 hydrate and sodium bromide [4], laser irradiation [5], microwave assisted synthesis, sol-gel process, electrochemical deposition etc. [15–19]. 81
62 irradiation [6], photo-reduction [7], hydrothermal reduction [8] Over the past few years, great efforts have been made to study dielectric 82
63 and thermal reduction [9]. Generally, the graphene product materials which are capable of storing energy. These materials are important 83
64 acquired by the above methods is known as the reduced Graphene for making electrical devices such as capacitors, electronic switches, 84
resonators, etc. The material which has high 85
⇑ Corresponding author. 86
E-mail address: skhan.ap@amu.ac.in (S. Khan). 87

http://dx.doi.org/10.1016/j.apt.2017.08.008
0921-8831/ 2017 Published by Elsevier B.V. on behalf of The Society of Powder Technology Japan. All rights reserved.
Please cite this article in press as: R. Bhargava, S. Khan, Effect of reduced graphene oxide (rGO) on structural, optical, and dielectric properties of Mg(OH) 2/ rGO nanocomposites,
Advanced Powder Technology (2017), http://dx.doi.org/10.1016/j.apt.2017.08.008
 APT 1694 No. of Pages 8, Model 5G
30 August 2017
2 R. Bhargava, S. Khan / Advanced Powder Technology xxx (2017) xxx–xxx

88 dielectric constant (e0) and low dielectric loss (tan d) are appropri- 2.3. Preparation of Mg(OH)2-rGO NCs 145
89 ately used to design efficient and miniaturized devices [20]. There-
90 fore, the synthesis of such materials is of great interest in today’s 0.1 g of GO was added in 100 mL distilled water in a beaker and sonicated 146
91 research. Graphene based metal oxide composites show outstand- for 1 h. Then 3 g of Mg(NO 3)2 6H2O was added and the mixture was stirred 147
92 ing dielectric properties and have potential applications in field of for 1 h. 0.5 mL of hydrazine hydrate was added to the mixture. Then, 10 mL 148
93 electronic, optoelectronics and electro-mechanical systems such as NaOH aqueous solution (1 M) was dripped into the solution. GO solution was 149
94 supercapacitors, dielectric actuators, rechargeable batteries and heated in microwave oven for 30 s in two cycles, the color of the solution 150
95 energy storage devices. Various graphene-based metal oxide such changes from brown to black which confirms the reduction of GO to rGO. 151
96 as TiO2, SnO2, ZnO, Fe2O3, Cu2O, Ni(OH)2 and WO3 composites have Then the solution was washed several times with distilled water and ethanol. 152
The resultant product was dried at 60 LC for 24 h. This was names as
97 been synthesized to achieve good dielectric properties [21–26]. 153
98 The metal oxides grown above graphene have a high dielectric con- Mg(OH)2-rGO1.Another concentration of GO (0.2 g) was taken and the same 154
99 stant and low dielectric loss along with the enhanced interfacial procedure was followed to synthesize Mg(OH) 2-rGO2. For comparison 155
100 interaction between the graphene layers and metal oxide nanos- Mg(OH)2 NPs were prepared by the same process without the addition of GO 156
101 tructures. These metal oxides grown on graphene play a vital role and hydrazine hydrate. 157
102 in altering the various properties of the composite. 158
103 By considering the intrinsic properties of Mg(OH)2 and Mg 159
104 (OH)2-rGO NCs; Mg(OH)2-rGO NCs are expected to exhibit better
105 results than pure Mg(OH)2. Herein, a microwave assisted co-
106 precipitation method for the preparation of Mg(OH)2-rGO NCs is 2.4. Characterizations 160
107 reported, in which the formation of Mg(OH)2 NPs and the reduc-
108 tion of GO occurs simultaneously and resulted in formation of The crystalline structure of GO, Mg(OH)2 NPs, Mg(OH)2-rGO NCs was 161
109 Mg(OH)2 NPs on the surface of rGO. The morphologies and investigated by powder X-ray diffraction (XRD) using a Bruker D8-Advance 162
110 microstructures of the as-prepared Mg(OH)2-rGO NCs were charac- X-ray diffractometer with Cu Ka radiation (k = 1.5418 Å) operated at a 163
111 terized. Optical and dielectric properties of Mg(OH)2 NPs and Mg voltage of 30 kV and current of 15 mA in 2h range from 5L to 80L. The 164
112 (OH)2-rGO NCs are also discussed. The polarization of the elec- morphological and compo-sitional analysis of the prepared samples was done 165
113 tronic charge of Mg(OH)2 NPs grown above the rGO sheets is by Scanning electron microscope SEM (JSM 6510LV, JAPAN) and energy 166
114 expected to modify in comparison to that of the pure Mg(OH)2 disper-sive X-ray spectroscopy EDAX attached with the SEM equipment. The 167
115 NPs because of the presence of localized electrons on the graphene functional group analysis was done by Fourier Transform Infra-red 168
116 surface. As a result, the dielectric properties are modified at the Spectroscopy FTIR (Perkin Elmer spectrophotometer). Raman spectroscopy 169
was carried out on the STR 500 Confocal Microraman spectrometer
117 interface. Thus, in the current report, the effect of Mg(OH)2 NPs 170
118 and rGO interface on dielectric properties such as dielectric con- (excitation wavelength: 532 nm). The UV–Visible spectra of Mg(OH) 2 NPs, 171
119 stant, dielectric loss, and AC conductivity of Mg(OH)2-rGO NCs Mg(OH)2-rGO1 and Mg(OH)2-rGO2 NCs were performed in the range of 172
120 have also been considered. The assynthesised NCs can widely be 200–700 nm by UV–Visible spec-trophotometer (Perkin Elmer, Lambda 35). 173
121 applied to manufacture charge storage capacitors in future. Frequency dependence of dielectric spectroscopy measurements were carried 174
out in the frequency range of 50 Hz to 5 MHz using LCR meter (HIOKI, 175
JAPAN). For these measurements, the samples were pelletized and were 176
coated with silver paste on the both sides to obtain geometry of parallel plate 177
122 2. Experimental capacitor. 178
179
123 2.1. Materials and reagents 180

124 Graphite powder (purity 99.999%) and hydrazine hydrate (N2

125 H4 H2O) were obtained from Alfa Aaser, hydrochloric acid (HCl, 3. Results and discussion 181
126 36–38.0 wt%), hydrogen peroxide (H2O2, 30 wt%), sulfuric acid (H2-
127 SO4,98 wt%), potassium permanganate (KMnO4), magnesium 3.1. X-ray diffraction analysis 182
128 nitrate (Mg(NO3)2 6H2O), sodium hydroxide (NaOH) and ethanol
129 were purchased from Central Drug House (CDH), India. All chemi- The X-ray diffraction pattern of the GO, Mg(OH) 2 NPs, Mg(OH)2-rGO1 183
130 cals were of analytical grade and used directly without further and Mg(OH)2-rGO2 NCs are shown in Fig. 1. The XRD pat-terns shows that 184
131 purification. Deionized (DI) water with a resistivity of 18.1 M X all samples consist of single crystalline phase and no impurity phases were 185
132 cm was used for all experiments. present in the samples. The diffrac-tion peak (0 0 1) of GO is positioned at 2h 186
= 9.96L. 187
All the diffraction peaks of Mg(OH)2 NPs, Mg(OH)2-rGO1 and 188
Mg(OH)2-rGO2 NCs can be indexed to the (0 0 1), (1 0 0), (1 0 1), (1 0 2), (1 189
133 2.2. Synthesis of GO 190
1 0), (1 1 1),(1 0 3) and (2 0 1) planes of hexagonal phase of Mg(OH) 2,
whereas the strongest peak in the XRD pattern can be attributed to the (1 0 1). 191
134 GO was synthesized by modified Hummers method [27]. In this The intensities and positions of the diffraction peaks are in good agreement 192
135 process, 2 g of graphite powder was added into 100 mL Conc.
with the standard XRD data for the hexagonal phase of Mg(OH) 2 (JPPDS no. 193
136 H2SO4 in a 500 mL beaker and the mixture was stirred in ice bath 44-1482). The peaks were indexed by Powder-X Software. The slight shifting 194
137 for 2 h. 8 g KMnO4 was added gradually and the mixture was 195
in the diffraction pattern and an increase in lattice parameter of Mg (OH) 2-
138 heated to 35 LC and stirred for 3 h. Then 160 mL distilled water 196
139 was slowly added to the mixture and external heating was intro- rGO1 and Mg(OH)2-rGO2 NCs is due to the interaction between the oxygen
197
140 duced to retain the reaction temperature at 98 LC for 20 min. groups in rGO and Mg(OH)2 [28]. The reflec-tions of Mg(OH) 2 NPs were
198
141 Finally, the reaction was terminated by the addition of 10 mL of detected on both Mg(OH)2-rGO1 and Mg(OH)2-rGO2 NCs, showing that 199
142 30% H2O2 solution. The resultant product was washed with 1% Mg(OH)2 particles attached onto rGO were highly crystalline [29]. No peaks 200
143 HCl aqueous solution and with distilled water until the pH of GO at 9.96L (0 0 1) can be observed, which demonstrates the significant 201
144 becomes 7. The resultant product was dried at 60 LC for 24 h. reduction of
202

Please cite this article in press as: R. Bhargava, S. Khan, Effect of reduced graphene oxide (rGO) on structural, optical, and dielectric properties of Mg(OH) 2/ rGO nanocomposites,
Advanced Powder Technology (2017), http://dx.doi.org/10.1016/j.apt.2017.08.008
 APT 1694 No. of Pages 8, Model 5G
30 August 2017
R. Bhargava, S. Khan / Advanced Powder Technology xxx (2017) xxx–xxx 3

Fig. 1. XRD patterns of GO, Mg(OH)2, Mg(OH)2-rGO1 and Mg(OH)2-rGO2 nanocomposites.

203 GO and a small peak around 24.4L appears which shows the pres-
204 ence of rGO [30].
205 The crystallite size for Mg(OH)2 NPs, Mg(OH)2-rGO1 and Mg
206 (OH)2-rGO2 NCs were calculated by using Debye–Scherrer formula
207 [31]:
208
D ¼ 0:9k ð1Þ
210 bcosh
211 The crystallite size and the lattice parameter (a = b, c) are listed
212 in Table 1 for the most intense peak (1 0 1) which reveals that the
213 crystallite sizes increases with the increases in lattice parameter as
214 the amount GO increases in the Mg(OH)2-rGO NCs.
215 The lattice strain (e) of the as synthesised sample can be evalu-
216 ated by the expression [32]:
217
219
e¼ b ð2Þ
4 tan h
220 where b corresponds to the full width at half maxima (FWHM) and
Fig. 2. SEM images (a) GO, (b) Mg(OH) 2-rGO1 and (c) Mg(OH)2-rGO2 nanocom-posites
221 h corresponds the Braggs angle. The calculated value of the lattice
(reveals the decoration of Mg(OH)2 NPs on rGO sheet).
222 strain for the peak (0 0 1) for the composites is listed in Table 1
223 which shows that the lattice strain decrease as the particle size
224 increases [33]. Fig. 2(b) and (c) presents typical SEM images of Mg(OH) 2-rGO1 and 233
Mg(OH)2-rGO2 NCs respectively. The images show that both the 234
225 3.2. SEM and EDAX analysis nanocomposites have similar morphologies exhibiting irregu-lar hexagonal 235
shape of Mg(OH)2 NPs which are attached heteroge-neously on the rGO 236
226 The Scanning Electron Microscopy (SEM) was used to analyse 237
sheets. Due to the larger amount of Mg(OH) 2 on the rGO sheets, aggregation
227 the morphologies of GO and Mg(OH)2-rGO NC. The SEM image of 238
could be found in both the nanocomposites.
228 GO is shown in Fig. 2(a), with a layered structure of GO nanosheets 239
229 which has highly wrinkled surface textures. The folded regions of In order to confirm the chemical composition of GO and Mg (OH) 2-rGO1 240
230 the nanosheets are found to be thin and severely wrinkled, which 241
and Mg(OH)2-rGO2 NCs EDAX spectroscopy investiga-tion was carried out.
231 gives rise to the large specific surface area and make it easier to The Fig. 3(a) shows the EDAX spectra of GO, 242
232 composite with Mg(OH)2 NPs.

Table 1
Variation of crystallite size, lattice parameters, lattice strain and band gap of samples.

Samples Lattice parameter Crystallite size (nm) Lattice strain (e) Eg (eV)
a = b (Å) c (Å)

Mg(OH)2 3.1442 4.770 4.93 0.1134 5.41

Mg(OH)2-rGO1 3.1446 4.775 6.65 0.0854 5.03
Mg(OH)2-rGO2 3.1448 4.778 8.69 0.0500 4.73

Please cite this article in press as: R. Bhargava, S. Khan, Effect of reduced graphene oxide (rGO) on structural, optical, and dielectric properties of Mg(OH) 2/ rGO nanocomposites,
Advanced Powder Technology (2017), http://dx.doi.org/10.1016/j.apt.2017.08.008
 APT 1694 No. of Pages 8, Model 5G
30 August 2017
4 R. Bhargava, S. Khan / Advanced Powder Technology xxx (2017) xxx–xxx

Fig. 3. EDAX spectra of (a) GO, and (b) Mg(OH) 2-rGO1 and (c) Mg(OH)2-rGO2 nanocomposites.

243 which confirms the presence of two peaks of C and O atoms. Fig. 3 (O-H) with is due to absorption of water vapour in the air. The broad band in 256
1
244 (b) and (c) show the EDAX spectra of Mg(OH)2-rGO1 and Mg(OH)2- the range of 3100–3500 cm is assigned to the appearance of the stretching of 257
245 rGO2 NCs, which confirm the presence of three peaks of C, O and OAH [34]. The small absorption peak at 2100 cm
1
arises due to CO. The 258
246 Mg atoms in the nanocomposite. The EDAX results are in good 1 1 1 259
absorption peaks at 1440 cm , 1600 cm and 1217 cm can be assigned to
247 agreement with the expected chemical composition and it is clear the stretching vibration of C@C and CAO of rGO respectively which cannot 260
248 that the Mg(OH)2 NPs were successfully synthesized on the surface -1 261
be reduced by N2H4. The peak at 1097 cm is due to the absorption of CO2
249 of the GO. -1 262
from air. The strong absorption band at 467 cm can be assigned to the 263
vibrations of the MgAO [35]. After the reduction of GO by Hydrazine
250 3.3. FTIR and Raman analysis hydrate, peaks for the oxygen functional groups (at 3470, 1660, 1440, 1217
264
1 265
and 1097 cm ) decrease or even disappear, showing that a majority of the
251 The functional groups of GO, Mg(OH)2 NPs, Mg(OH)2-rGO1 and 266
oxy-genic groups in GO are eliminated.
252 Mg(OH)2-rGO2 NCs were investigated by FTIR spectroscopy in the 267
1 268
253 wave number range of 4000–400 cm and the results are shown
254
1
in Fig. 4. The sharp peak around 3700 cm on Mg(OH)2 NPs and The Raman spectra further confirms the rGO in the NCs as shown in Fig. 269
255 Mg(OH)2-rGO1 and Mg(OH)2-rGO2 NCs is of the hydroxyl group 5. The Mg(OH)2-rGO1 and Mg(OH)2-rGO2 NCs is 270

Fig. 4. FTIR spectra of GO, Mg(OH)2, Mg(OH)2-rGO1 and Mg(OH)2-rGO2

nanocomposites. Fig. 5. Raman spectra of GO, Mg(OH)2-rGO1 and Mg(OH)2-rGO2 nanocomposites.

Please cite this article in press as: R. Bhargava, S. Khan, Effect of reduced graphene oxide (rGO) on structural, optical, and dielectric properties of Mg(OH) 2/ rGO nanocomposites,
Advanced Powder Technology (2017), http://dx.doi.org/10.1016/j.apt.2017.08.008
 APT 1694 No. of Pages 8, Model 5G
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R. Bhargava, S. Khan / Advanced Powder Technology xxx (2017) xxx–xxx 5

-1 -1
271 dominated by two strong peaks at 1344 cm and 1588 cm corre-
272 sponding to the D and G modes respectively. The in-plane bond-
2
273 stretching of the pairs of C sp atom corresponds to the G band
274 and the reduction extent is usually determined by the D band
275 [36]. The minor increase in the ID/IG ratio recommends a decrease
2
276 in the size of the sp domains upon reduction of GO into rGO, i.e.,
277 the rGO has a small size and a huge number of edges, and these
278 edges act as defects and increase the D band [37].Compared with
279 GO, a high ID/IG ratio is found for both Mg(OH)2-rGO1 and Mg
280 (OH)2-rGO2 NCs, e.g., Mg(OH)2-rGO1 (0.91), and Mg(OH)2-rGO2
281 (0.98) vs. GO (0.84), indicating the presence of rGO with a high
282 amount of disordered structure in the NCs. Thus Raman spec-
283 troscopy completely supports the facts observed through XRD,
284 FTIR, SEM analysis.

285 3.4. UV–Visible spectroscopy

286 The absorption peak at 236 nm obtained from UV–Visible

287 absorption spectra for GO shown in inset of Fig. 6(a) corresponds
⁄
288 to p–p transitions of aromatic CAC bonds. UV–Vis absorption
289 spectra of Mg(OH)2 NPs and Mg(OH)2-rGO NCs are shown in
290 Fig. 6. The pure Mg(OH)2 shows a sharp absorption at 229 nm.
291 The peak of Mg(OH)2 at 229 nm shows a red shift 246 nm and
292 261.5 nm in Mg(OH)2-rGO1 and Mg(OH)2-rGO2 NCs respectively.
293 The Mg(OH)2-rGO NCs holds a strong and wide range of absorption
294 in the visible region which may be due the restoration of p elec-
295 tronic conjugation within the graphene sheets. Compared to pure
296 Mg(OH)2 NPs, the absorption intensity of Mg(OH)2-rGO NCs is
297 increased. In addition, it is clear that there is an enhancement in
298 absorption with the carbon content in the Mg(OH)2-rGO NCs.
299 Due to the introduction of graphene there is an increase in surface
300 electric charge of Mg(OH)2 NPs in the NCs, which may alter the
301 exciton formation upon irradiation [38].
302 The band gap of these samples can be evaluated from the
303 absorption spectra. The Tauc relation [39] was used to calculate
304 the optical band gap for pure Mg(OH)2 NPs and Mg(OH)2-rGO NCs
305
307 aht ¼ Aðht Eg Þ n ð3Þ

308 where a is the absorption coefficient, ht is the energy of inci-

309 dent photon in eV, A is a constant and Eg is the band gap measured
310 in eV. The value of n is taken to be 1/2 for indirect band gap and 2
311 for direct band gap materials. The linear extrapolation of the Tauc
2
312 plot [(aht) vs ht] intercepts on a certain point on the x axis as
313 shown in Fig. 6(b). The value of intercept with the x axis gives
314 the value of the optical band gap (Eg). The value of optical band
Fig. 6. (a) UV–Vis absorption spectra of GO (inset), Mg(OH) 2, Mg(OH)2-rGO1 and Mg(OH)2-
315 gap listed in Table 1 were calculated for Mg(OH)2 NPs, Mg(OH)2- 2
rGO2 nanocomposites. (b) ( aht) vs ht plots of Mg(OH) 2, Mg(OH)2-rGO1 and Mg(OH)2-rGO2
316 rGO1 and Mg(OH)2-rGO2 NCs. The decrease in the band gap of nanocomposites.
317 Mg(OH)2-rGO NCs may be attributed to the interaction of the
318 rGO sheets and the Mg(OH)2 NPs grown over it. It is in good agree-
319 ment with the results reported in the earlier study [13]. Hence, the
circular pellet. The frequency dependence of real part of dielectric constant 334
320 light absorption and emission properties of Mg(OH)2 NPs may be
(e΄) of Mg(OH)2 NPs and Mg(OH)2-rGO NCs calculate in frequency range 335
321 modified by decorating it over the rGO sheet, which may be useful
50 Hz to 5 MHz is shown in Fig. 7. 336
322 to find its applications in various fields of science and technology.
The dielectric response of the Mg(OH) 2 NPs and Mg(OH)2-rGO NCs has 337
strong frequency dependence, the higher dielectric values at lower 338
323 3.5. Dielectric analysis
frequencies are related with the interfacial polarizations at the conductor- 339
insulator interface. This can be clarified on the basis of Koop’s theory [41], 340
324 The dielectric constant (e0) describes the energy stored inside which is created on the Maxwell– Weigner model [42]. In this model, a 341
325 the sample in the applied electric field. The value of dielectric con- dielectric medium is sup-posed to be made of well conducting grains 342
326 stant (e0) of Mg(OH)2 NPs and Mg(OH)2-rGO NCs were calculated (conductor) which are disconnected by poorly conducting (insulator) grain 343
327 using the following relation [40]:
bound-aries. Under the influence of external electric field, the charge car-riers
328 344
Ct can effortlessly drift the grains but are gathered at the grain boundaries which 345
e0
ð4Þ
330 ¼ produce large polarization and high dielectric constant. The occurrence of the 346
e0A polarization process in Mg(OH) 2 NPs, and Mg(OH)2-rGO NCs can be due to 347
331 where C is the parallel plate capacitance of the specimen in the existence of a huge 348
332 Farad (F), t is the thickness of the pellet in meters, e0 is the permit- 349
12 1
333 tivity of free space (8.854 10 F m ) and A is the area of the

Please cite this article in press as: R. Bhargava, S. Khan, Effect of reduced graphene oxide (rGO) on structural, optical, and dielectric properties of Mg(OH) 2/ rGO nanocomposites,
Advanced Powder Technology (2017), http://dx.doi.org/10.1016/j.apt.2017.08.008
 APT 1694 No. of Pages 8, Model 5G
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Fig. 7. Variation of dielectric constant with frequency for Mg(OH) 2, Mg(OH)2-rGO1 and
Mg(OH)2-rGO2 nanocomposites.

350 number of trap states at the grain boundaries of the synthesized

351 samples. These trap states are produced due to the presence of
352 vacancies or defects such as, oxygen vacancies, micro porosities, Fig. 8. Variation of dielectric loss with frequency for Mg(OH) 2, Mg(OH)2-rGO1 and Mg(OH)2-
353 dangling bonds [32]. The small conductivity of grain boundary con- rGO2 nanocomposites.
354 tributes to the high value of dielectric constant at low frequency.
355 The higher value of dielectric constant can be described on the
356 basis of interfacial charge polarization due to inhomogeneous rent. Thus restricting the electron transfer by hindering the tun-nelling 395
357 dielectric arrangement and the decrease in dielectric constant at between adjacent rGO through oxygen functional group which results in low 396
358 higher frequencies can be explained by the polarization relaxation dielectric loss [47]. Thus the increase in dielectric loss at higher rGO 397
359 phenomenon. The dipoles do not have enough time to follow rapid concentrations might also be due to the leakage current, since rGO provides a 398
360 field variations due to which the dielectric value decreases at greater number of con-ductive pathways. 399
361 higher frequencies [43]. The dielectric constant in Mg(OH)2-rGO 400
362 NCs grows as compare to Mg(OH)2 NPs as the defects increases The ac conductivity of Mg(OH)2 NPs and Mg(OH)2-rGO NCs has been 401
363 when the majority of the oxygenic groups in GO are eliminated calculated from dielectric data as a function of frequency in the range 50 Hz 402
364 which in turns enhances the interfacial polarization. Wang et al. to 5 MHz as shown in Fig. 9. The ac conductivity of a dielectric material is a 403
365 have synthesised RGO/Mn3O4 nanocomposites by hydrothermal summation of two terms [48]: 404
366 method, which shows much improved dielectric properties due 405
rac ¼ r0ðTÞ þ rðx; TÞ ð5Þ 407
367 to increment in the interfacial polarization and the unique conduc-
368 tivity of RGO [44]. The first term in the above equation gives the frequency indepen-dent or dc 408
369 The dielectric loss or tangent loss (tand) gives the energy dissi- conductivity which is associated to drifting of charge car-riers and the second 409
370 pated in the dielectric material. term gives the frequency dependent or ac conductivity which is associated to 410
371 Fig. 8 shows the dependence of dielectric loss (tand) for the Mg the dielectric relaxation caused 411
372 (OH)2 NPs and Mg(OH)2-rGO NCs as function of the frequency. The
373 dielectric loss in the case of Mg(OH)2 NPs and Mg(OH)2-rGO NCs is
374 found to decrease with increasing frequency. The high frequency
375 process is related with dipolar relaxation, whereas at lower fre-
376 quency, the contributions of interfacial polarization and conductiv-
377 ity are related [45]. The variation of tand at lower frequency is
378 higher in case of Mg(OH)2-rGO NCs than that of Mg(OH)2 NPs. This
379 shows that more energy is being utilized to induce polarization
380 and dipoles in Mg(OH)2-rGO NCs at lower frequency compared to
381 Mg(OH)2 NPs. This shows that at higher frequency, the induced
382 polarization and dipoles do not follow the applied field, resulting
383 in a decrease in dielectric loss at higher frequency. The enhance-
384 ment in interfacial polarization may be due to the accumulation
385 of charge at the interface of Mg(OH)2 NPs and the rGO sheet. Wang
386 et al. reported the synthesis of porous rGO/Fe2O3 composites by
387 hydrothermal method, which exhibit extraordinarily improved
388 dielectric properties and EM wave absorbing performance [46]
389 due to the presence of rGO which contains a lots of electric polar-
390 ization and dipolar polarization.
391 Generally rGO can be imagined as the sheets of graphene deco-
392 rated with oxygen functional groups on the basal planes and at the
393 edges. So, oxygenated functional groups on the rGO could act as an Fig. 9. Variation of AC conductivity with frequency for Mg(OH) 2, Mg(OH)2-rGO1 and
394 insulating layer or intrinsic barriers that bound the leakage cur- Mg(OH)2-rGO2 nanocomposites.

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412 by the localized electric charge carriers which is governed by the the rGO sheet through oxygenated functional groups attached to the rGO 477
413 power law [49] sheet. These results suggest that synthesized NCs are promising materials for 478
414
416
rðxÞ ¼ Cx s ð6Þ practical applications in energy storage devices. 479
480

417 where C is a constant and has units of conductivity, x is the

418 angular frequency of the ac signal (x = 2pf) in Hz and s is temper- Acknowledgments 481
419 ature dependent factor having a value less than 1 at room temper-
420 ature. The ac conductivity is calculated by the following equation Authors are grateful to the University Grants Commission, New Delhi for 482
421 [50]: financial support in the form of UGC-Non Net Fellowship. We are also 483
422
424
rac ¼ e0e0xtand ð7Þ thankful to Material Research Centre, MNIT, Jaipur for characterizing 484
samples through Raman spectroscopy. 485
425 In Mg(OH)2 NPs, and Mg(OH)2-rGO NCs, the value of ac conduc-
426 tivity is exponentially increased with increase in frequency. The
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