ISSN : 0970 - 020X, ONLINE ISSN : 2231-5039
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Impervious Nature of Al2O3-PANI Composite Against Corrosion on Mild Steel in Strong Acidic Environment

P. Kamatchi Selvaraj,  S. Sivakumar and S. Selvaraj

P.G and Research Dept. of Chemistry, Govt. Arts College for Men (AUT), Nandanam, Chennai – 35, India.

Corresponding Author E-mail: porbal96@gmail.com

DOI : http://dx.doi.org/10.13005/ojc/3404017

Article Publishing History
Article Received on : 19-06-2018
Article Accepted on : 11-07-2018
Article Published : 14 Aug 2018
Article Metrics
ABSTRACT:

Solubility problem of composite in aqueous medium is resolved on  adding Al2O3 during the oxidative polymerization of aniline using ammonium peroxydisulphate as an oxidant and sodium salt of dodecyl bezenesulphonic acid  as surfactant and dopant at  273 K temperature.  The yielded water soluble Al2O3-PANI composite is confirmed by comparing the FTIR, XRD and SEM recorded spectra with previously reported one.  Gravimetric method exposes that the prepared composite is having confrontation  against corrosion. Only a slight change in efficiency on continuous exposure up to eight hours is observed.  OCP data are transformed in to potential graph to exposes the invincibility of the composite against corrosion.  Measurement of  potentiodynamic polarization and EIS studies also confirms the defiance against corrosion.

KEYWORDS:

Al2O3-PANI; EIS; Mild Steel; OCP; Potentiodynamic Polarization

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Selvaraj P. K, Sivakumar S, Selvaraj S. Impervious Nature of Al2O3-PANI Composite Against Corrosion on Mild Steel in Strong Acidic Environment. Orient J Chem 2018;34(4).


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Selvaraj P. K, Sivakumar S, Selvaraj S. Impervious Nature of Al2O3-PANI Composite Against Corrosion on Mild Steel in Strong Acidic Environment. Orient J Chem 2018;34(4). Available from: http://www.orientjchem.org/?p=48375


Introduction

Metalworking industries suffers mishap due to chemical or electrochemical attack on metal. Metal corrosion is a resolute threat to national economy and industry design.1,2 It is miserable that corrosion can’t be completely eradicated, as it is a natural process. Corrosion activities may be slow downed by other dynamic and/or substitute mechanisms.  The undeniable methods include cathodic protection,3,4 protective coating5 and addition of inhibitors.Most of the protective coating layers lost their identity on prolonged exposure to corrosive environment .7-9 Corrosion resistive performance of epoxy coatings were improved on insertion of TiOnanomaterials.10,11 It is a well known fact that corrosion of aluminum utensils is prevented due to the formation of protective Al2O3 layer on the surface of aluminum. Utility of Al2O3 have been found in  the activities of catalyst,12 retardant for fire,13 absorbent14 and filler.15  Stability against chemical action, good  conducting property, idiosyncratic doping behavior of polyaniline and other applications of it in energy storage and sensors attracted significantly to employ it as inhibiting material.16-18 The structural morphology, thermal property and  conductivity of PANI varied on insertion of TiO2 and Al2O3.19,20 Reinforced dielectric properties have been noticed for Al2O3-PANI compositie.20,21 Usage of solid Al2O3-PANI showed high value for dielectric property and impedance with very high  Z values.22 All above observations stimulated to synthesis water soluble composite (Al2O3-PANI) and to evolve its capacity to diminish corrosion of carbon steel in strong acidic  environment.

Materials and Instrumentation

Materials

AR grade  monomer (aniline) was procured from Merck Ltd.  After adding a pinch of zinc dust, it was purified by distillation to employ for polymerization. Phosphoric acid, Al2O3, ammonium peroxydisulphate (APS) and sodium salt (DBSA) chemicals with AR grade purchased from Merck Ltd. were used without purification.

Instrumentation

The infrared spectrum, in the frequency range of 4000-450 cm-1, was recorded by  Perkin-Elmer 337 spectrometer.  The XRD and SEM spectra were registered in Rigaku Maniflex diffractometer (Japan) and JSM-6390 Scanning Electron Microscope respectively.  Potentiodynamic polarization studies and impedance measurements were documented in ECLAB 10.37 model.  To observe the  OCP values, CHI electrochemical analyzer instrument 1200B model was adopted.

Experimental

Synthesis  of Al2O3 -Polyaniline Composite

Al2O3-PANI composite was synthesized by modified in-situ chemical oxidative polymerization method.23-25 Aniline (18.6g) was added to 1M solution of Phosphoric acid (200ml) and stirred for half-an-hour. Solution prepared by dispersing required amount of Al2O3 in100 ml of 0.1M DBSA using 42 kHz oscillation frequency for 45 minutes in a sonicator  was mixed with aniline solution. The  mixture was kept under constant stirring for two hours  at  273 K  along with addition of 200 ml of 1M APS solution in drops.  Complete polymerization  was achieved by stirring the above mixture  for another  three hours. The  product (dark green in color) obtained was filtered, washed with deionized water, acetone, and dried in hot air oven at 55°C for 24 hours.

Results and Discussion

Characterization of  Al2O3-PANI Composite

FTIR Analysis

The peak appears at 613 cm-1 in the FTIR spectrum of Al2O3 [Fig.1(a)] was assigned to Al-O stretching vibration and the peak arises around 3460 cm-1 was ascribed to O-H vibration mode.26,27  The bands appear in the FTIR spectrum of PANI [Fig. 1(b)] around 1562 cm-1 and 1447 cm-1 are due to stretching vibration of quinoid and benzenoid  rings.  The bands emerge about 1230 cm-1 and 1033 cm-1 are ascribed to C-N stretching vacillation.28,29 The N-H stretching of secondary amine fetch up near 3400 cm-1.

Figure 1: FTIR spectra of (a) Al2O3 (b) PANI (c) Al2O3- PANI.

Figure 1: FTIR spectra of (a) Al2O3 (b) PANI (c) Al2O3- PANI.



Click here to View figure

 

The FTIR spectrum of Al2O3-PANI composite [Fig. 1(c)] consist of the peaks due to Al2O3 and PANI with small blue or red shift.  The O-H stretching of Al2O3     appears at 3490 cm-1.  The C=C stretching mode of quinoid rings occur around 1550 cm-1 and 1490 cm-1.  The Al-O stretching emerge at 508 cm-1.  Above results implies that the PANI has been coated over the surface of Al2O3.22,30,31

XRD Analysis of PANI and Al2O3-PANI Composite

The XRD of Al2O3-PANI composite (Fig. 2b) contains various peaks assigned  to alumina.32,33  The broad peak of PANI34 (Fig. 2a) centered between 2θ= 20°C-30°C is  reappeared in the XRD of composite.  This reveals the interaction of PANI with Al2O3.31

Figure 2a: XRD spectra of  PANI.

Figure 2a: XRD spectra of  PANI.



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Figure 2b: XRD spectra of  Al2O3-PANI composite.

Figure 2b: XRD spectra of  Al2O3-PANI composite.



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SEM Analysis of Al2O3 and Al2O3– PANI Composite

The SEM of metal oxide (Fig. 3a) gazes  like a cluster with diameter ranging from 150 nm to 270 nm.  The composite SEM (Fig. 3b) display flake  structure having diameter ranging from 427 nm to 452 nm.  This compeers to the previous work.30,31

Figure 3: SEM spectra of (a) Al2O3 and  (b) Al2O3-PANI composite.

Figure 3: SEM spectra of (a) Al2O3 and  (b) Al2O3-PANI composite.



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Preparation of Electrode Materials

Specimens fraternized with C: 0.21%, Si: 0.035%, Mn: 0.25%, P: 0.082% and 99.28% of Iron was trimmed into pieces measuring 4 cm x 2 cm x 0.2 cm and were scoured with disparate abrasive sheets  starting from 600 grit to 1200 grit.  The polished specimens were effaced by double distilled water, acetone and dried in a desiccators.  Above freshly polished coupons were utilized in weight loss measurements.

Preparation of Electrolytic Solutions

The belligerent solutions of one molar and two molar sulphuric acid were prepared by diluting analytical quality sulphuric acid.  Required amount (125-500ppm) of composite was added to the belligerent solution to obtain  test solutions.

Evaluation of Inhibition Property

Assessment of Corrosion by Weight loss Measurement

Weight loss determination is the preliminary technique to measure corrosion.  Freshly polished mild steel coupons were fully immersed in 250 ml of belligerent solutions and test solutions for eight hours continuously under room condition.  The coupons were taken out at two hours time intervals, washed with bristle brush under tap water and then cleaned by distilled water, ethyl alcohol and acetone.  After drying at room temperature, they were reweighed to assess the inhibition efficiency (IE %) and surface coverage (θ)35. The assessed values of IE and (θ) are provided in Table 1 and 2.

Table 1: IE and θ values assessed from the weight loss measurement  in 1M belligerent and test solutions.

Conc. of Composite (ppm)

2-hours

4-hours

6-hours

8-hours

Weight loss (g)

 I.E (%)

(θ)

Weight loss (g)

I.E (%)

(θ)

Weight loss (g)

 I.E (%)

(θ)

Weight loss (g)

I.E (%)

(θ)

Blank

0.1351

0.2275

0.2982

0.3666

125

0.0299

78

0.778

0.0534

76

0.765

0.0806

72

0.724

0.1080

70

0.705

250

0.0272

80

0.798

0.0484

79

0.787

0.0615

79

0.793

0.0965

73

0.736

375

0.0180

87

0.866

0.0332

85

0.854

0.0551

81

0.815

0.0930

75

0.746

500

0.0158

88

0.883

0.0301

87

0.867

0.0510

82

0.825

0.0715

80

0.804

 

Table 2: IE and θ values assessed from the weight loss measurement  in 2M belligerent and test solutions.

Conc. of Composite (ppm)

2-hours

4-hours

6-hours

8-hours

Weight loss (g)

 I.E (%)

(θ)

Weight loss (g)

I.E (%)

(θ)

Weight loss (g)

 I.E (%)

(θ)

Weight loss (g)

I.E (%)

(θ)

Blank

0.2412

0.4172

0.5507

0.7046

125

0.0748

69

0.689

0.1388

67

0.667

0.1901

65

0.654

0.2609

63

0.629

250

0.0680

72

0.718

0.1261

70

0.697

0.1850

67

0.678

0.2404

65

0.652

375

0.0631

74

0.738

0.1142

72

0.724

0.1668

70

0.698

0.2226

68

0.684

500

0.0522

78

0.783

0.1010

76

0.757

0.1402

74

0.745

0.2016

71

0.714

 

Attentive examination of the data’s existing in the Tables 1 and 2 discloses the substantial conservative nature of Al2O3-PANI composite against corrosion.  Minimal changes in efficacy observed even after eight hours committed that the prepared water soluble composite have good resistivity versus  corrosion.

Open Circuit Potential

The OCP values up to 120 minutes were recorded  using CHI Electrochemical analyzer 1200B model.  A cell comprise  of  working electrode made from mild steel having 1 cm2 area, saturated calomel electrode as reference electrode and platinum electrode as counter electrode was employed to measures the OCP statistics. The perceived information are  given  in Fig.  4 and 5.

Figure 4: OCP plot for mild steel in 1 M H2SO4

Figure 4: OCP plot for mild steel in 1 M H2SO4



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Figure 5: OCP plot for mild steel in 2 M H2SO4

Figure 5: OCP plot for mild steel in 2 M H2SO4



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Shift of OCP points to positive potential value on addition of Al2O3-PANI composite implies the resistive character.36,28

Electrochemical Measurements

Potentiodynamic polarization and EIS studies were detected in EC-LAB analyzer model 10.37 instrument assembled  with three electrode compartment cell.  Specimen, having 1cm2 area and the remaining area covered with araldite epoxy resin, cut  from ASTM 415 mild steel was used as working electrode. Calomel electrode and Platinum electrode were used as reference electrode and  counter electrode respectively.  On maintaining the potential between -200 to +200 m V with scan rate of 0.5m V s-1, the potentiodynamic polarization studies were documented.  Impedance measurements were executed with 10 mV AC sine wave amplitude in the frequency range of 100 kHz – 10 mHz.

Potentiodynamic Polarization Measurements

The parameters such as Icorr, Ecorr, bc and ba and surface coverage (θ) area measured from the Tafel plots given in Fig. 6 and 7 are bestowed in the Table 3 and 4 respectively.  Reported formula37  was used to calculate the resistivity of Al2O3-PANI composite.

Figure 6: Tafel plots of  mild steel in 1M belligerent and test solutions. Figure 6: Tafel plots of  mild steel in 1M belligerent and test solutions.


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Table  3: Corrosion resistive parameters for Mild Steel in 1M belligerent and test solution.

Conc. of  Composite (ppm)

-ECorr

(mV vs. SCE)

ba

(mV dec-1)

bc

(mV dec-1)

Icorr

(µA cm-2)

Inhibition Efficiency (%)

Surface coverage   (θ)

Blank

455

61

63

1960

100

484

36

40

1269

35

0.3525

200

483

33

37

997

49

0.4913

300

508

33

45

636

67

0.6755

400

496

21

23

616

69

0.6857

500

488

18

20

564

71

0.7122

Figure 7: Tafel plots  of  mild steel in 2M belligerent and test solutions.

Figure 7: Tafel plots  of  mild steel in 2M belligerent and test solutions.



Click here to View figure

 

Table 4: Corrosion resistive parameters for Mild Steel in 2M belligerent and test solution.

Conc. of Composite   (ppm)

-ECorr

(mV vs. SCE)

ba                (mV dec-1)

bc                   (mV dec-1)

Icorr

(µA cm-2)

Inhibition efficiency  (%)

Surface coverage   (θ)

Blank

439

44

57

2537

100

470

24

29

1733

32

0.3169

200

455

48

66

1510

40

0.4048

300

472

20

23

1399

45

0.4485

400

477

20

22

937

63

0.6306

500

480

20

21

904

64

0.6463

 

Increase in corrosion current is noticed with increase in the concentration of acid. The protection accomplishment of the composite is reflected in the steady fall in noticed Icorr value. Changes in efficiency on increasing the concentration of composite undeniably prove the resistivity of the composite. Inconsiderable changes  observed in the Ecorr, ba and bc value presented in table 3 & 4 on varying the concentration of Al2O3-PANI disclose it as mixed type inhibitor.38

Electrochemical Impedance Measurements

Impedance parameters (Rct, Cdl) were calculated using the following equivalent circuit.

Scheme 1

Scheme 1



Click here to View scheme

 

Semicircle manifestation of Nyquist plots indicate the protection against corrosion and also reflects single charge transfer process.39 The decrease in flow of corrosion current reflected in the increase in diameter of capacitive loop.  On increasing the  concentration of composite, the diameter of the Nyquist plots increases in the Figures 8 and 9. This reveals that the composite gets adsorbed on the metal surface and prevents the flow of corrosion current and thereby acts as a better inhibitor in low pH environment.   Previously reported formula37 is used to measure the inhibition efficiency.

Figure 8: Cole-Cole plots for mild steel in 1M belligerent and test solution.

Figure 8: Cole-Cole plots for mild steel in 1M belligerent and test solution.



Click here to View figure

 

Table  5: Impedance parameters for Mild Steel in 1M belligerent and test solution.

Conc. of

Composite (ppm)

Rs (Ω)

Cdl (µ F cm-2)

Rct (Ω cm2)

Inhibition efficiency (%)

Surface

Coverage(θ)

Blank

1.076

643

0.5018

100

1.070

712

0.7583

34

0.3417

200

1.278

565

0.8841

38

0.4324

300

1.256

608

0.8961

44

0.4400

400

1.153

500

0.9932

50

0.5032

500

1.154

552

1.372

63

0.6350

 

Figure 9: Cole-Cole plots for mild steel in 2M belligerent and test solution.

Figure 9: Cole-Cole plots for mild steel in 2M belligerent and test solution.

 



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Table 6: Impedance parameters for mild steel in  2M belligerent and test solution.

Conc. of

Composite (ppm)

Rs (Ω)

Cdl (µ F cm-2)

Rct (Ω cm2)

Inhibition efficiency (%)

Surface

Coverage(θ)

Blank

0.6460

1196

0.3773

100

0.5787

772

0.5945

36

0.3656

200

0.6177

985

0.6168

40

0.3982

300

0.7320

722

0.7212

48

0.4768

400

0.6505

414

1.0076

62

0.6247

500

0.5549

594

1.0080

63

0.6269

 

The increase in Rct values have been assigned to the formation of  protective layer at the metal/electrolyte interface.40 Decrease in Cdl values have been allotted to the increase in thickness of  electrical double layer.41  Reflection of similar behavior in the present observation persist the inhibitive  nature of composite.

Conclusion

Water soluble PANI coated aluminum oxide composite prepared exhibit  good protection efficiency up to 88%  in 1M acidic solution for two hours and is stable  up to eight hours with little changes in efficiency (80%) on weight loss measurement. Increasing trend of corrosion resistivity upon increasing the concentration of composite is noticed in OCP measurements  and electrochemical studies.  All observations exposes that synthesized water soluble composite can equipped for industrial maintenance process.

Acknowledgement

The authors acknowledge the support from Dr.B.V., Dean for Research, SRM group of institutions,  Dr. C. Jayaprabha, Associate Professor of Chemistry, University college of Engineering (Anna University) Dindigul-624622 and the Management of Rajalakshmi Engineering college, Chennai-600 105 for the electrochemical analysis of samples on free of cost. This research did not receive any specific grant from funding agencies in the public, commercial or not for profit sectors.

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