Fabrication and Characterizations of Silica Nanoparticles Carbon

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Fabrication and Characterizations of Silica Nanoparticles Carbon Nanofiber Composite Basma I. Waisi, Sama al-jubouri, and Jeffrey R. McCutcheon Ind. Eng. Chem. Res., Just Accepted Manuscript • DOI: 10.1021/acs.iecr.8b05825 • Publication Date (Web): 27 Jan 2019 Downloaded from http://pubs.acs.org on January 28, 2019

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Industrial & Engineering Chemistry Research

1

Fabrication and Characterizations of Silica Nanoparticles

2

Carbon Nanofiber Composite

3

Basma I. Waisi a,b*, Sama M. Al-Jubouri a, Jeffrey R. McCutcheon b

4 5 6

*Corresponding Author E-mail: [email protected]

7 8

a

9

Baghdad, Baghdad, Iraq

Department of Chemical Engineering, College of Engineering, University of

10

b

11

Science and Engineering, University of Connecticut, Storrs, USA

12

Abstract

13

Department of Chemical and Biomolecular Engineering, Center for Environmental

Silica nanoparticles/carbon

nanofiber

composites

were

fabricated

via

14

electrospinning of the polymeric solution (polyacrylonitrile polymer in N,N-

15

dimethylformamide solvent) containing different amounts of silica nanoparticles,

16

followed by carbonization in an inert gas. The properties of surface morphology,

17

surface area, surface chemistry, and mechanical strength were characterized using

18

Fourier transform scanning electron microscopy (SEM), N2 Physisorption Analyzer,

19

infrared

20

SiO2 nanoparticles with average size about 200 nm showed interesting dispersion

21

along the carbon nanofiber surface.

22

nanoparticles affects the structure and properties of the carbonized nanofibers

spectroscopy

(FTIR),

and

dynamic

mechanical

analyzer

(DMA).

The results indicated that adding silica

ACS Paragon Plus Environment

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composites. Here, the capability to use silica nanoparticles was demonstrated to create

24

high surface area carbonized nanofiber with improved mechanical strength for easier

25

handling in the applications requiring good mechanical properties materials such as

26

water treatment processes. The specific surface area of the PAN/silica carbon

27

nanofibers composite reached 280 m2/g which is higher than the surface area of pure

28

carbon PAN nanofibers which was 19 m2/g .

29 30

Keywords: Carbon nanofiber; Nonwoven; Silica nanoparticles; Electrospinning;

31

Surface area; Flexibility.

32

1 Introduction

33

Generally, Engineered nanomaterials structures (including nanofibers and

34

nanoparticles) have been attracting attention due to the advantages of their small size

35

and unique properties such as the relatively high surface area that can potentially

36

improve catalytic processes, chemical reactivity, strength; and interfacial driven

37

phenomena including wetting and adhesion 1. carbon nanofiber (in different forms and

38

compositions) have been widely used in various potential applications including fuel

39

cells 2, unconventional energy sources 3, hydrogen storage

40

their unique structures and functionalities.

4

and batteries

5

due to

41

Various precursors can be used to prepare carbon fibers such as,

42

polyacrylonitrile polymer (PAN) which is a common precursor for about 90 % of

43

manufactured carbon fibers due to its high melting point and high carbon yield.


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Moreover, the molecular structure of PAN can be relatively easily embedded with

45

nanoscale components such as nanoparticles, nanotubes, nanowires, or catalysts to

46

fabricate CNFs composite 6,7.

47

The most commonly used approach to fabricate carbon nanofibers (CNFs) is

48

an electrospinning method that comprises spinning of polymeric precursor fibers

49

followed by thermal treatment 7. Electrospinning method to fabricate the nonwoven

50

polymeric fibers has the merits of simple handling and low-cost. Moreover,

51

electrospinning method has emerged as a powerful and highly versatile technique

52

which uses an electrically forced fluid jet to fabricate micro- and nano-scale fibers

53

from process polymeric solutions or melts using an electrically forced fluid jet 6,8.

54

The thermal treatment steps include stabilization and carbonization.

55

Stabilization is carried out by controlled heating of the precursor fibers in an oxidizing

56

atmosphere at temperatures ranging of 180 - 300 °C. During this step, a sudden and

57

rapid evolution of heat occurs along with various chemical reactions such as

58

cyclization, dehydrogenation, aromatization, oxidation, and crosslinking. Stabilization

59

results in slight mechanical of the weakening of the carbon backbone. While

60

carbonization is carried out in an inert atmosphere at temperatures ranging of 300 -

61

1000 °C 9. Carbonization is the most important step during which, fundamental

62

changes occur to both chemical composition and physical properties. Therefore,

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carbonization can be considered as the heart of the CNFs fabrication process. The

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mechanical properties of CNF’s decrease significantly during this step 10



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Various nanoparticles could be used to functionalize CNFs. These

66

nanoparticles are incorporated into the precursor to fabricate CNFs composite and

67

create strong interactions between the nanoparticles and the fiber matrix. To impart

68

functionalities to CNFs, a variety of nanoparticles could be used; these are

69

incorporated into the precursor to fabricate CNFs composite strong interactions

70

between the nanoparticles and the fiber matrix. Many investigations explored the use

71

of composite nanofibers in different applications such as electrical devices, electrode

72

materials for batteries, proton exchange membrane, supercapacitors and sensors 1,11–13.

73

Combining the advantages of metal nanoparticles and polymer nanoﬁbers can

74

result in composites with unique mechanical, electrical, chemical and optical

75

properties 14. Various types of inorganic nanoparticles were used to fabricate CNFs

76

composites such as palladium (Pd) nanoparticles were used to produce a composite

77

with high electrocatalytic activity and stability towards methanol oxidation 15. Silver

78

(Ag) nanoparticles were used to fabricate high activity catalyst

79

nanoparticles (SiO2) were used for porous carbon nanofibers material preparation

80

required for rechargeable lithium-ion batteries by carbonizing PAN/SiO2 composite

81

precursor followed by silica etching using HF acid

17

16

. Also, silica

.

82

However, examining the trade of mechanical properties and surface area using

83

high surface area nanoparticles on CNFs composites has not been studied so far.

84

Mesoporous silica materials with controlled particle size, morphology, and porosity,

85

and high specific surface area reaches to (850 m2/g) along with their chemical

86

stability, have made highly attractive silica matrices for a wide range of


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nanotechnological applications such as adsorption, catalysis, sensing, and separation.

88

18

. In the present study, PAN-based CNFs containing various concentrations of

89 90

silica

nanoparticles

(PAN/SiNF

CNFs

Composites)

91

electrospinning subsequent by heat treatments. This study focused on the influence of

92

the concentration of SiNP on the microstructure and properties of the CNFs. The

93

morphologies and microstructures of the CNFs were studied in details using scanning

94

electron microscopy (SEM), the N2 Physisorption Analyzer, and dynamic mechanical

95

analyzer (DMA). SiNPs in CNFs were also characterized using infrared (FTIR)

96

spectroscopy to understand the structural changes occurring during the heat

97

treatments. The capability of using silica nanoparticles to create high surface area

98

carbonized nanofiber compared to pure carbon nanofibers was demonstrated. In

99

addition, the fabricated PAN/silica CNFs composite have excellent flexibility for

100

easier handling for some applications such as water treatment.

101

2 Materials and methods

102

2.1 Preparation of polymer precursors

were

fabricated

via

103

Polyacrylonitrile (PAN) from Scientific Polymer Products Inc. (MW avg.

104

150,000 g/mol) and Dimethylformamide (DMF) from Acros Organics were used to

105

prepare 14 wt. % PAN in DMF solution by continuous stirring at 60 °C for 2 h as the

106

base polymer solution. High surface area silica nanoparticles (SiNP) were purchased

107

from Sigma Aldrich (SiNP, particle size 200 nm).



108

To prepare composite precursors, firstly a solution of SiNP with DMF solvent

109

was mixed at 60 °C for 2 h, then PAN was added to the previous solution. Different

110

PAN:SiNP loadings of 12:1, 5:1 and 2:1 (corresponding to 1.2, 2.8 and 7.0 wt.%

111

SiNP) were prepared. The resulting solutions were mixed thoroughly at 60 °C for 2 h

112

then sonicated at 60 °C for 1 h using ultrasonic bath to produce a homogeneous

113

polymer/nanoparticles solution. Spinning of a homogeneous solution will help to produce

114

nanofibers with well-distributed nanoparticles within all the fabricated nanofiber

115

composite.

116

2.2. Electrospinning precursors composite

117

A high pressure syringe pump (KD Scientific) was used to dispense the

118

charged solution at a constant rate of 1 ml/hr onto a grounded collector drum rotating

119

at 70 rpm.

120

The applied voltage was 24, 23, 22, and 20 kV (for 0, 1.2, 2.8 and 7.0 wt. % SiNP,

121

respectively) and the tip to collector distance was 18 cm. The precursor mats were all

122

spun at room temperature under a relative humidity of 10–20% to produce strongest

123

PAN precursor mats 19.

124

2.3 Fabrication of CNFs composite

125

When electrospinning finished, the precursor mats were stabilized in air at 280

126

°C for 1 h in a muffle furnace (Carbolite) through a ramp rate of 1 °C/min. Then, the

127

sample was allowed to cool overnight before carbonization to produce stronger

128

nonwovens 10. The samples were then carbonized in a tubular furnace (Lindberg Blue


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129

M, Thermo Scientific) in an inert nitrogen atmosphere with a 3 °C/min ramp rate at

130

600 o C for 2 h as these conditions produce strongest carbonized PAN nanofibers

131

During the thermal treatment steps, the white color of electrospun composite samples

132

changed to brown (after stabilization), then to black (after carbonization) due to

133

occurring of various reactions.

134

2.4 Membrane characterization

135

2.4.1 Fiber Morphology and Size

20

.

136

The PAN and composite CNFs nonwoven samples were sputter coated with

137

platinum and imaged using an FE-SEM (FEI Quanta). These images allow studying of

138

the SiNP distribution within the carbonized nanofibers and analyzing the possible

139

changes occurred in fiber structure/morphology.

140

2.4.2 Surface Chemistry (FTIR)

141

The surface chemistry of the PAN and composite nonwoven carbonized

142

samples were analyzed using a Nicolet iS10 FT-IR (Thermo Scientific). Infrared

143

spectra were recorded in the wave number range of 700–4000 cm-1 with a resolution

144

of ±4 cm-1 and 16 scans per sample. The attenuated total reflection mode with a

145

diamond crystal was used to scan the samples.

146

2.4.3 Mechanical Properties

147

The tensile strength and elasticity of the samples are the parameters which

148

were used to assess the mechanical strength of the PAN and composite nanofiber



149

carbonized samples. A Dynamic Mechanical Analyzer (DMA) from TA instruments

150

was used for this analysis. A sample size of 3 cm, 6 mm was used for the tests which

151

were performed at 25 °C and ambient humidity. All results presented were the average

152

of three individual tests.

153

2.4.4 Specific Surface Area

154

The specific surface area was measured using N2 Physisorption Analyzer

155

(Micromeritics Instrument Corporation). The samples were first degassed at 300 °C

156

for 2 h and then analyzed for nitrogen sorption at 77 K. The adsorption isotherms

157

were used to calculate the specific surface area by applying the BET model. All

158

results presented were the average of three individual tests.

159

3 Results and Discussion

160

3.1. The CNF's composites morphology

161

The SEM images presented in Figure 1 are for the 14 wt.% PAN:SiNP

162

composite fibers prepared from polymer precursor with different SiNP weight percent

163

(1.2, 2.8, and 7 wt. %). Further increasing in weight percent of SiNP is not

164

recommended with these conditions to avoid the spinning difficulties due to the

165

significant increasing in the viscosity of the precursor solution prepared. When the

166

silica concentration loaded was relatively low (1.2 and 2.8 wt. %) (Figure 1 b and c),

167

they do not show a tendency for agglomeration. The PAN:SiNP CNFs composites

168

showed smooth fibrous morphologies; except for a few large SiNP agglomerates

169

dispersed in the carbon fiber matrix. Further increase in the SiNP content led to


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170

difficult SiNP dispersion in the polymer solution as a result of increasing the

171

solution's viscosity which produced lots of agglomerations during the spinning

172

process as shown in (Figure 1 d).

173

To assure that the silica nanoparticles have been distributed throughout the

174

composite carbonized network and combined within the nanofibers, EDX analysis has

175

been performed in Figure (2) for the different prepared composites carbonized

176

nanofibers. The obtained results indicated the existence of SiNP peak in the different

177

samples. The Silica peak is observed to be increased with increasing the silica

178

nanoparticles percentage. The weight percentages of the various elements in the

179

fabricated samples were concluded in Table (1).

180 181

(a) 0.0 wt.%

(b) 1.2 wt.%

(c) 2.8 wt.%

(d) 7.0 wt.%

182 183 184 185

Figure (1) The SEM images of 14 wt.% PAN/DMF and PAN:SiNP CNFs composites (a) 0.0 wt.% (b) 1.2 wt.% (c) 2.8 wt.% (d) 7.0 wt.% .



186 187 188

Figure (2) EDX analysis of 14 wt.% PAN/DMF and PAN:SiNP CNFs composites (a) 0.0 wt.% (b) 1.2 wt.% (c) 2.8 wt.% (d) 7.0 wt.% .

189 190

Table (1) the percentage of the concentration of each element in the various fabricated samples

Element 0.0 wt.% SiNP 1.2 wt.% SiNP 2.8 wt.% SiNP 7.0 wt.% SiNP 76.33 68.70 56.43 53.46 C K, wt.% 19.45 16.92 11.45 9.93 N K, wt.% 4.22 6.84 14.61 12.21 O K, wt.% 0 7.55 17.51 24.39 SiK, wt.% 191

3.2.

The CNF's composites surface area

192

Using the high surface silica nanoparticles extensively affected the CNF's surface

193

area as shown in Figure 3. Using only 1.2 wt. % of SiNP increased the surface area of

194

14 wt.% PAN CNF from 19 to 60 m2/g. Increasing the SiNP loading percentage to 7.0

195

wt. % resulted in tangible increasing in the CNFs surface area (reached to 280 m2/g).

196

Increasing the specific surface area of the fabricated composite carbonized

197

nanofibers can be explained by the effect of the embedded percentage of SiNP on the


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198

pore size distribution (Figure 4 a) and the adsorption isotherm curves (Figure 4 b) of

199

the fabricated composite materials. The pore size of the composite carbonized

200

nanofibers increased with increasing the silica nanoparticles percentage. The isotherm

201

of CNFs (0 wt.% PAN:SiNP) showed very little pores in its structure. Embedding

202

silica nanoparticles resulted in increase the quantity adsorbed as the relative pressure

203

over the system (P/Po) was increased due to presence of the micropores in the

204

fabricated composites (PAN:SiNP). Increasing the silica nanoparticles percentage

205

making more micropores in the composites.

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Figure (3) The effect of SiNP on CNF's composites surface area (Average of three individual samples)

209



210 211 212

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(a)

(b)

Figure (4) The effect of SiNP on nitrogen physisorption analysis of CNF's composites. (a) Pore size distribution (b) Isothermal curves.

213 214

3.3 The CNF's composites mechanical strength

215

The results presented in Figure (5) shows an obvious effect of embedding silica

216

nanoparticles within the CNFs composite on the mechanical strength. Increasing the

217

SiNP percentage loading (1.2, 2.8, and 7 wt. %) decreased both of the stress (0.4, 0.2,

218

and 0.1MPa) and Young's modulus (30, 10, and 4 MPa) respectively. Although

219

decreasing the tensile strength of the CNFs composites with increasing the SiNP

220

amount, they became less brittle because of decreasing of the Young's modulus. Low

221

Young's modulus materials means high flexibility which is an acceptable property for

222

some applications that need flexible materials.

223 224 225 226

(a)

(b)

Figure (5) Mechanical properties of 14 wt.% PAN:SiNP CNF's composites (Average of three individual samples): (a) Tensile strength and (b) Young’s modulus.


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227


3.4.

The CNF's composites FTIR

228

FTIR spectra were conducted to the CNFs composite mats to analyze the

229

surface chemistry, composition of PAN/SiNP CNFs composite and the possible

230

interactions between PAN and SiNP. Figure (6) shows a comparison between the

231

FTIR of pure PAN-based and of PAN/SiNP CNFs composite nonwoven samples

232

(various SiNP loading).

233

The characteristic peaks in pure PAN-based CNFs mats are generally

234

associated with the aliphatic CH groups at 1270 and 1350 cm-1. The peak observed at

235

1590 cm-1 was for a mixture of C꞊N, C꞊C, and N-H groups which resulted during the

236

heat treatment step of the CNF fabrication

237

attributed to the NH2 bending vibration and the C-O-C asymmetric stretching

238

vibration of the epoxy group

239

hydrolysis of nitrile groups 24.

22,23

10,21

. The peaks at 1562 and 1296 cm−1 are

. The peak appeared at 1627 m-1 is ascribed to the

240

The PAN/SiNP CNFs composite mats with different SiNP contents showed

241

similar peaks to those of pure PAN-based CNFs mats. Those peaks showed a gradual

242

broadening and strengthening with increasing of SiNP content in the composite

243

matrix. These new peaks observed confirm the good attachment of SiNP within the

244

carbonized nanofibers and a favorable interaction occurring between PAN and SiNP.

245

The dominant peaks at 798 and 960 cm−1 are attributed to silica nanoparticles owing

246

to Si-O-Si symmetric stretching and Si-OH stretching. The peak revealed at 1638

247

cm−1 was assigned to the OH bending of physisorbed water molecules 22.



248 249 250

2.8 wt.% (d) 7.0 wt.%

251

Conclusions

252

Carbon nanofiber could be prepared with improved properties when it is embedded

253

with silica nanoparticles. The pure 14 wt.% PAN CNFs prepared are brittle materials

254

with a low specific surface area (19 m2/g). However, these properties were improved

255

when silica nanoparticles with a high surface area have been added to the polymer

256

solution. PAN/silica nanofibers composite was prepared with different loading amount

257

of silica nanoparticles using the electrospinning method. The CNFs composite mats

258

resulted have a high surface area (reaches to 280 m2/g) and high flexibility which

259

allows easy handling for various applications.

260

Acknowledgments

Figure (6) FTIR analysis of 14 wt. % PAN:SiNP CNF's composites (a) 0.0 wt.% (b) 1.2 wt.% (c)


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The authors would like to acknowledge the Higher Committee for Education Development (HCED) in Iraq for financially supporting Basma Waisi (Grant Number is 1000324) to conduct this work in the Connecticut University labs. The authors also acknowledge the University of Connecticut Center for Clean Energy Engineering for the use of the nitrogen adsorption analyser.

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