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IRJET- Experimental Investigation on Properties of DGEBA based Epoxy Resin
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HARDNESS, FRACTURE TOUGHNESS AND STRENGTH OF CERAMICS
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IRJET- Experimental Investigation on Properties of DGEBA based Epoxy Resin
1.
International Research Journal
of Engineering and Technology (IRJET) e-ISSN: 2395-0056 Volume: 06 Issue: 03 | Mar 2019 www.irjet.net p-ISSN: 2395-0072 © 2019, IRJET | Impact Factor value: 7.211 | ISO 9001:2008 Certified Journal | Page 394 Experimental Investigation on Properties of DGEBA Based Epoxy Resin Mr. Khan Muzaffar Khan1, Prof. Rameshwar V. Chavan2 1M.Tech (Mechanical Engineering) Deogiri Institute of Engineering & Management Studies Aurangabad, Maharashtra, India. 2Assistant professor, Department of Mechanical Engineering, Deogiri Institute of Engineering & Management Studies Aurangabad, Maharashtra, India. -----------------------------------------------------------------------***-------------------------------------------------------------------- Abstract - The Mechanical, Chemical, Thermalpropertiesof Diglycidyl ether of bisphenol-A (DGEBA) based epoxy resin material with varying content of SiO2 are studied in order to find out best composition. The ultimate aim is to modify the epoxy resin to improve mechanical and thermal properties. Tensile test and fracture toughnessKICofanalyteasperASTM E399 of SEN-B specimen performed on Instron 5980 universal testing system. Thermogravimetric Analysis (TGA) is performed on TGA 5500 by TA Instruments. Differential Scanning Calorimetry Analysis is done on DSC 4000 system by PerkinElmer. Key Words: Diglycidyl ether of bisphenol-A (DGEBA), SiO2, SEN-B, Tensile Test, Fracture test, Thermogravimetric Analysis (TGA), Differential Scanning Calorimetry Analysis. 1. INTRODUCTION There has been a denotation of epoxy resin to the engineering field from decades. It has played a vital role in terms of their material properties that is chemical,adhesive, thermal and electrical. It has been widely used in fibre reinforcement inside the composite materials and adhesive. Many approaches have been done in order to increase the characteristics, performance of epoxy resin which includes adding of nano composites, some rubber additives/agents, thermoplastic stuffings, inorganic fillers and upgrading its chemical composition are in common practice. [1] In the last decade it has been proved that improvement in mechanical and thermal characteristics of unadulterated polymer composition can be achieved by reinforcing composites in a very minute percentage of strong stuff/fillers. These modifications can be achieved by traditional processing techniques which resultsinnegligible harmful effects on processability, aesthetics, thickness, capacity of structure. These compounds are considered for multiple uses which include electronics, automotive, packaging, marine and aviation industries etc. [2-3] According to the results it has been observed flourishing combination with epoxy resin. Based on the results nano- scale fillers has been considered as filler material to manufacture high outcome composite material with upgraded properties [4-7]. As compare to microscale fillers, nano-clays have larger aspect ratio, plate morphology combined with less cost and low content requirement which make them a perfect filler reinforcement upgraded in structural properties have significant interest in nano composite material in numerous applications [8,9]. The integration of element is crucial in nano composites to produce a nano material with upgraded properties [10-12]. To obtain the best results from nano particles a homogeneous mixing is required the various mixing techniques of nano composites fabrication discussed in reference [13-14]. Epoxy resin have numerous applications in the field of electrical insulation, it has property to withstand high voltage system. Due to their low cost, light weight, ability to be moulded in any shape and electrical insulationofpolymer matrix, there is a need to develop numerous types ofresin to overcome generating requirement of high-performance thermoset material. In the above-mentioned field various applications are circuit board, bushing board and structural component [18,19]. The required result is composite with good mechanical integrity and high insulation properties [20,21]. In this study special attention is given to Mechanical, Chemical, thermal properties of epoxy resin in order to develop a material with best properties. 2. MATERIALS The material used for preparation of analyte specimen are commercially available Diglycidyl ether of Bisphenol-A (DGEBA) based epoxy resin Epofine -5900 purchased from Changzou Chemical factory, Jiangsu province, China. Pathilic Anthydride (commercial name-HY905) and Dimethyl benzylamine (commercial name-DY061)asaccelerator,both materials are purchased from Huntsman Advanced material (material)Pvt.Ltd. Silica powder 300 meshispurchasedfrom a local vendor from Aurangabad. 3. PREPARATION To remove the moisture content in SiO2 powder and preheating the DGEBA epoxy resin Epofine 5900 and silica powder are placed in a furnace for period of 2hrs at constant temperature of 150 OC. After preheating materials are taken in ratio as follows,
2.
International Research Journal
of Engineering and Technology (IRJET) e-ISSN: 2395-0056 Volume: 06 Issue: 03 | Mar 2019 www.irjet.net p-ISSN: 2395-0072 © 2019, IRJET | Impact Factor value: 7.211 | ISO 9001:2008 Certified Journal | Page 395 Resin : Hardener : Accelerator = 1 : 1 : 0.004 The quantity of SiO2 is varied to make four different type of materials as 0 wt.%, 30 wt.%, 63 wt.%, 70 wt.%. As per above mentioned composition materials are mixed in a mixing chamber at 130 OC and 600 Mbar vacuum pressure for a time period of 50 min after that mixture is poured in a preheated mold of required specimen. 4. Experimental 4.1 Tensile strength The tensile test is performed using Instron 5980 Universal Testing System, a machine with flexibility to test tensile, compression, shear, peel, cyclic and bend test for metals composites and advanced plastics as per ASTM standard. According to ASTM D638 standard the specimen size is selected. ASTM D638 specifies method for testing the tensile strength of epoxy resin material for calculating their mechanical properties and outline accuracy requirement for test frames accessories used. The specimens for ASTM D638 are dumbbell shaped with either a 25 mm or 50 mm gauge length, a 50 mm gauge length is recommended. As per ASTM D638, specimen type 1 is selected whose dimension are as follows. (Refer the figure-1) Full length (l3) = 165 mm Parallel length (l2) = 57 mm Gauge length (l1) = 50 mm Parallel section width (strong) = 13 mm Thickness (h) = 3.4 mm Grip section width (strong) = 19 mm Distance between grips = 115 mm The test is performed on four specimens at crosshead speed of 1 mm/min with increasing weight percentage of SiO2 in each specimen. Fig -1: Dumbbell shaped specimen 4.2 Fracture toughness Fracture toughness is an indication of the amount of stress required to propagate a preexisting flaw. Flaws may appear ascracks, voids,metallurgicalinclusions,welddefects,design discontinuities,orsomecombinationthereof.alsodenotedby KIC [22,23]. Fracture toughness is measured of a three-point single edge notch bend (SEN-B) specimen as shown in figure-2 with the help of Instron 5980 universal testing system as per ASTM E399 standard KIC determined by ASTM E399 standard method characterizes the resistance of a material to fracture in a neutral environment in the presence of a sharp crack under essentially linear-elastic stress and severe tensile constraint, such that The state of stress near the crack front approaches plane strain. The crack-tip plastic zone is small compared to the crack size, specimen thickness, and ligament ahead of the crack. A V-notchat center of specimen is created.Tomakeacrackof depth 3.2±0.2 mm, a razor blade is pressed at the bottom most point of the notch. The sample is of 10 mm thickness and the fracture toughness KIC is calculated by following equation. KIC = (F S) / (B W^ (3/2)) f(x) Where, F = load required to start propagation of pre-crack B = thickness of sample S = distance between support reactions W = width of the sample A = total depth of notch/crack f(x) = shape factor f(x) depend on specimen design and loading and it is a dimensionless quantity. Where, X=A/W Fig -2: SENB specimen 4.3 Thermogravimetric Analysis (TGA) Thermogravimetric analysis (TGA) is a method of thermal analysisinwhichchangesinphysicalandchemicalproperties of materials are measured as a function of increasing temperature (with constant heating rate) or as a function of time(with constant temperatureand/orconstantmassloss). In simple words the propertiesofanalytesarestudiedasthey change with temperature [24-26]. If some property, which changes at some particular temperature range is known then the type of reaction that is taking place can be found out.
3.
International Research Journal
of Engineering and Technology (IRJET) e-ISSN: 2395-0056 Volume: 06 Issue: 03 | Mar 2019 www.irjet.net p-ISSN: 2395-0072 © 2019, IRJET | Impact Factor value: 7.211 | ISO 9001:2008 Certified Journal | Page 396 In this experimental technique the mass of an analyte is monitored as a function of its temperatureortimeandforthe result two types of curve can be obtained, one is mass wt.% versus temperature and if the temperature is available in terms of OC/min the mass versus time curve can also be potted. The TGA 5500 from TA Instruments Inc. is used to carry out Thermogravimetric analysis which possess ambient to 1200 OC temperaturerangeandlinearcontrolledheatingrateof0.1 to 500 OC/min. A sample of 1 kg mass is placed in the machine in the presence of air as environment.Thetemperatureisincreased from room temperature to 1000 OC at a rate of 10 OC/min. The plot of masschange in percentageversustemperatureor time (known as TGA curve) is typical result of TGA analysis. 4.4 Differential Scanning Calorimetry (DSC) Differential Scanning Calorimetry, or DSC, is a thermal analysis technique that looks at how a material’s heat capacity (Cp) is changed by temperature. A sample of known mass is heated or cooled and the changes in its heat capacity are tracked as changes in the heat flow. This allows the detection of transitionssuchasmelts,glasstransitions,phase changes, and curing. Since we work here with polymeric material, the glass transition is important to understanding the material [27-30ss]. At first the sample is prepared with the composition of 63 wt.% of SiO2 only because thiscompositionisfoundbestinall other tests of mechanical properties. The sample size is selected as 10 mg. To neutralize any antecedent effect of temperature sample is preheated to 200 OC at a constant heating rate of 25 OC/min subsequently it is quenched to -25 OC. Differential ScanningCalorimeter(DSC4000System,100- 240V/50-60Hz by PerkinElmer) isusedtomeasureheatflow from -25 OC to 225 OC at 25 OC/min. 5. RESULTS AND DISCUSSION 5.1 Tensile strength Chart -1: Effect of SiO2 on tensile stress-strain curve Four specimens of DGEBA were prepared with different percentage of SiO2 according to ASTMD638standardandthe test is performed. The values obtained from the test were plotted on stress strain curve. The tensile properties were tabulated as shown in table-1s. In all of the four cases after the maximum stressvalueisreachedthespecimenstookvery subordinateamount of timeto fail. Though no apparentyield point can be decided from the results the curve deviate from straight line to some extent prior to reaching the maximum stress. Based on the table-1 and chart-1 it can be said that as we go on increasing the SiO2 percentage in DGEBA its strength increases. Out of all the compositions the one with 2 wt.% of SiO2 is by far the best with 18.32% gain in strength. If the percentage is further increased it does not show that much improvement, But the modulus increases almost steadily with weight percentage of SiO2. Table -1: Tensile properties of SiO2 modified epoxy Materials Strength (MPa) Gain in strength (%) Modulus (GPa) Gain in Modulus (%) Neat epoxy 59.43±2.32 - 2.73±0.12 - 30 wt.% SiO2 65.34±0.43 09.94 2.85±0.32 4.39 63 wt.% SiO2 70.09±2.52 17.93 3.12±0.18 14.28 70 wt.% SiO2 64.43±3.08 08.41 3.42±0.22 25.27 5.2 Fracture toughness The four sample which are tested for fracture toughness contains unadulterated, 30 wt.%, 63 wt.% and 70 wt.% SiO2 nanoparticles and the calculated KIC values for those materials are delineated in the graph. The unadulterated DGEBA sample have the lowest fracture toughness value out of all the four samples and the third sample which contains 63 wt.% of SiO2 nanoparticles have the highest KIC value that is 17.82. It is observed thataswego on increasing the weight percentage the beyond that the KIC value start to reduce. Since lower density of crosslinksleadstoincreaseinductility of material it can be a cause for increment in critical stress intensity factor (KIC) in other sample, but it is not the sole effect of density of cross link there may be other factors such as the microstructure of the epoxy changes with addition of SiO2 and becomes more heterogeneous in nature this may automatically leads to lower density of cross links or it may have separate effect in the form of increasing toughness.
4.
International Research Journal
of Engineering and Technology (IRJET) e-ISSN: 2395-0056 Volume: 06 Issue: 03 | Mar 2019 www.irjet.net p-ISSN: 2395-0072 © 2019, IRJET | Impact Factor value: 7.211 | ISO 9001:2008 Certified Journal | Page 397 Chart -2: Fracture toughness (KIC) values off samples 5.3 Thermogravimetric Analysis (TGA) The chart-3 shows the mass change in percentage versus temperature TGA curve. From the graph the nature of curve can be considered as multistage decomposition curve. This curve reveals the multistage decomposition processes as a result of various reactions but the stages are not clearly defined in the curve due to fast heating rate or no intermediates. The general causes of weight loss may be desorption, drying, dehydration, desolvation, sublimition, vaporization, and solid-state reaction in some cases, but in our specimen dehydration or drying is not possiblebecausethesilicanano- particles as well as the epoxy resin wereheatedto150OCand kept there for 2hrs to eliminate moisture so there is no moisture present in the analyte. The major causes of weight loss might be sublimation and vaporization and desorption may have contributed to some extent. Four samples of different composition percentage of SiO2 in the epoxy resin were placed in machine and Thermogravimetric analysis is performed. The machine automatically produces the curves for respective sample as shown in chart-3. First, we defined temperature for start of decomposition as 5% reduction in mass. The start of decomposition for the analyte samples that is for 0 wt.% (unadulterated), 30 wt.%,63 wt.% and 70 wt.% is at 221 OC, 246OC, 265OC, 254 OC respectively. Chart -3: TGA curves 5.4 Differential Scanning Calorimetry (DSC) The inflection point temperature from the chart-4 gives the glass transition temperatureof Diglycidyl ether of bisphenol A (DGEBA). The glass transition (Tg) has been called the “melting ofamorphousmaterial”andasunscientificasthatis, it's an adequate description. In non-crystalline and semi- crystalline polymer of any type – synthetic high polymers such as polypropyleneandpolystyrene,naturalpolymerslike rubber, or biological polymers such as proteins – the glass transition is the best indicator of material properties. As the glass transition changes due to either different degrees of polymerization or modification by additives, the physical properties of the material change. Similarly, material properties also change dramatically above the Tg. The hard and solid nature of sample turns to soft and mobile like jelly. The value of Tg for DGEBA sample is 56.23OC. Chart -4: DSC curves 6. CONCLUSIONS Mechanical, chemical and thermal properties were experimentally investigated onDiglycidyletherofbisphenol- A based SiO2 modified epoxy resin composite as per the experimental results following conclusions were reached. 1. Highest gain in strength of 17.93% is obtained from 63 wt.% of SiO2 and for the same gain in modulus is 14.28%. 2. Highest fracture toughness of 7.82 among all the materials obtained from 63 wt.% of SiO2. 3. Starting temperature of decomposition of sample with 63 wt.% of SiO2 is 265 OC which differ by 44 OC from unadulterated sample. 4. TGA result shows that DGEBA was fully degraded above 600 OC in both air and nitrogen atmosphere and transition temperature Tg=56.23 OC. The analysis of samples revealed thatwhen63wt.%ofSiO2 is mixed with the composition mentioned in material gives modified properties.
5.
International Research Journal
of Engineering and Technology (IRJET) e-ISSN: 2395-0056 Volume: 06 Issue: 03 | Mar 2019 www.irjet.net p-ISSN: 2395-0072 © 2019, IRJET | Impact Factor value: 7.211 | ISO 9001:2008 Certified Journal | Page 398 REFERENCES [1] Y.P. Zheng, Y. Zheng, R.C. Ning, Mater. Lett. 57 (2003) 2940–2944. [2] M. Hussain, Y. Oku, A. Nakahira, K. Niihara, Mater. Lett. 26 (1996) 177–184. [3] N. Chisholm, H. Mahfuz, V. Rangari, A. Ashfaq, S. Jeelani, Compos. Struct. 6 (2005) 115–124. [4] R.J. Day, P.A. Lovell, A.A. Wazzan, Compos. Sci. Technol. 61 (2001) 41–56. [5] R. Bagheri, R.A. Pearson, Polymer 41 (2001) 269–276. [6] T. Kawaguchi, R.A. Pearson, Polymer 44 (2003) 4239– 4247. [7] H. Mahfuz, A. Adnan, V.K. Rangari, S. Jeelani, B.Z. Jang, Compos. A: Appl. Sci. Manufact. 35 (2004) 519–527. [8] V.M.F. Evora, A. Shukla, Mater. Sci. Eng. A361 (2003) 358–366. [9] Y. Iwahori, S. Ishiwata, T. Sumizawa, T. Ishikawa, Compos. A 36 (2005) 1430–1439. [10] J.H. Koo, Polymer Nanocomposites: Processing, Characterization, and Applications, McGraw-Hill, New York (2006). [11] K.I. Winey and R.A. Vaia, MRS Bull., 32, 314 (2007). [12] E. Tuncer, G. Polizos, I. Sauers, D.R. James, A.R. Ellis, and K.L. More, CEIDP 2009 Annual Report, ser. Conference on Electrical Insulation and Dielectric Phenomena.IEEE Dielectrics and Electrical Insulation Society, IEEE Publications, Piscataway New Jersey, 527 (2009). [13] D.R. James, I. Sauers, M.O. Pace, and A.R. Ellis, CEIDP 2002 Annual Report, ser. Conference on Electrical Insulation and Dielectric Phenomena. IEEE Dielectrics and Electrical Insulation Society, IEEE Publications, Piscataway New Jersey, 542 (2002). [14] L.A. Dissado, V. Griseri, W. Peasgood, E.S. Cooper, K. Fukunaga, and J.C. Fothergill, IEEE Trans. Dielectr. Electr. Insul., 13, 903 (2006). [15] E. Tuncer, I. Sauers, D.R. James, and A.R. Ellis, IEEE Trans. Appl. Superconductivity, 19, 2359 (2009). [16] C.A. Harper, High Performance Printed Circuit Boards, McGraw-Hill Professional, New York (2000). [17] M.W. Jawitz, Printed Circuit Board Materials Handbook, McGraw-Hill Professional, New York (1997). [18] R.W. Coppard, J. Bowman, L.A. Dissado, S.M. Rowland, and R.T. Rakowski, J. Phys. D Appl. Phys., 23, 1554 (1990). [19] I. Sauers, D.R. James, A.R. Ellis, and M.O. Pace, IEEE Trans. Dielectr. Electr. Insul., 9, 922 (2002). [20] A. Allaoui, S. Bai, H.M. Cheng, and J.B. Bai, Compos. Sci. Technol., 62, 1993 (2002). [21] T. Imai, F. Sawa, T. Nakano, T. Ozaki, T. Shimizu, M. Kozako, and T. Tanaka, IEEE Trans. Dielectr. Electr. Insul., 13, 319 (2006). [22] X.L. Xie, Y.W. Mai, and X.P. Zhou, Mater. Sci. Eng. RRep., 49, 89 (2005). [23] K. Bula, T. Jesionowski, A. Krysztafkiewicz, and J. Janik, Colloid Polym. Sci., 85, 1267 (2007). [24] H.M. Ma, J.J. Zeng, M.L. Realff, S. Kumar, and D.A. Schiraldi, Compos. Sci. Technol., 63, 1617 (2003). [25] S.G. Prolongo, M. Buron, M.R. Gude, R. Chaos-Moran, M. Campo, and A. Urena, Compos. Sci. Technol., 68, 2722 (2008). [26] H. Wang, C.C. Zeng, M. Elkovitch, L.J. Lee, and K.W. Koelling, Polym. Eng. Sci., 41, 2036 (2001). [27] E. Tuncer, I. Sauers, D.R. James, A.R. Ellis, M.P. Paranthaman, A. Goyal, and K.L. More, Nanotechnology, 18, 325704 (2007). [28] G. Polizos, E. Tuncer, I. Sauers, and K.L. More,Appl.Phys. Lett., 96, 152903 (2010). [29] H.J. Lee, S.J. Oh, J.Y. Choi, J.W. Kim, J. Han, L.S. Tan, and J.B. Baek, Chem. Mater., 17, 5057 (2005). [30] H.L. Zeng, C. Gao, Y.P. Wang, P.C.P. Watts, H. Kong, X.W. Cui, and D.Y. Yan, Polymer, 47, 113 (2006).
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