CLAY/EPOXY COMPOSITES

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1 149 Paper presented at the International Conference on Diagnosis and Prediction in Mechanical Engineering Systems (DIPRE 09) October 2009, Galati, Romania CLAY/EPOXY COMPOSITES Adrian CÎRCIUMARU, Iulian-Gabriel BÎRSAN, Vasile BRIA, Ion POSTOLACHE Dunărea de Jos University, Galati, ROMANIA ABSTRACT Fillers are generally used to decrease the costs of a composite material but they are changing also some of composite s properties due to their physical properties, their dimensions and their shapes. Filled polymer could be used as matrix for reinforced composites in order to improve the material response to external changes. In this manner it is possible to design multi-functional materials which might be obtained using cheap components and simple forming techniques. This is a comparative study of two particulate composites Clay/Epoxy and Zn/Epoxy. KEYWORDS: Clay, Zn powder, epoxy, thermal properties, mechanical properties. 1. INTRODUCTION Filler is an inert substance (organic and inorganic with low to high weights) that is added to plastics to reduce costs. It is usually low in cost and may also improve processing and physical and mechanical properties, particularly hardness, thermal insulation, stiffness, and impact strength. The particles are usually small, in contrast to those of reinforcements [1]. Almost all fillers do not exist as the discrete individual particles of their primary structure. They form aggregates, secondary structures, which can agglomerate into tertiary structures in the material to be filled. An aggregate is a collection of primary particles that are chemically bonded together. The surface area of an aggregate is less than the sum of surface areas of all primary particles in that aggregate. In general, aggregates are extremely difficult to be broken down into individual primary particles by physical methods such as mechanical mixing. The union of aggregates, although weakly associated through non-bonded physical interactions, leads to a cluster. Filler materials often exist as agglomerates in their natural state. The total surface area of a cluster is similar to the sum of individual surface areas of aggregates in that cluster. The mixing and dispersion of fillers in a material involves primarily the incorporation and distribution of filler pellets or powders, and breakdown into agglomerates, and then into aggregate structures [2]. Polymer matrix nano-composites are a fairly new class of engineered materials which offer for a broad range of properties, an interesting and even radical alternative to more conventional filled polymers, yet at much lower filler loadings. They can be defined as polymer matrix systems in which the dispersed inorganic reinforcing phase has at least one of its dimensions in the nanometer range, which is quite close to the scale of elementary phenomena at the molecular level. The resulting unique combination of large interfacial area and small inter-particle distance strongly influences nano-composite behavior [3]. Epoxies are one of the most versatile classes of polymers with diverse applications such as metal can coatings, automotive primer, printed circuit boards, semiconductor encapsulants, adhesives, and aerospace composites. Most cured epoxy resins provide

2 150 THE ANNALS OF UNIVERSITY DUNĂREA DE JOS OF GALAŢI amorphous thermosetting with excellent mechanical strength and toughness; outstanding chemical, moisture, and corrosion resistance; good thermal, adhesive, and electrical properties; no volatiles emission and low shrinkage upon cure; and dimensional stability-a unique combination of properties generally not found in any other plastic material. These superior performance characteristics, coupled with outstanding formulating versatility and reasonable costs, have gained epoxy resins wide acceptance as materials of choice for a multitude of bonding, structural, and protective coatings applications [4]. Commercial epoxy resins contain aliphatic, cycloaliphatic, or aromatic backbones and are available in a wide range of molecular weights from several hundreds to tens of thousands. The most widely used epoxies are the glycidyl ether derivatives of bisphenol A (>75% of resin sales volume). The capability of the highly strained epoxy ring to react with a wide variety of curing agents under diverse conditions and temperatures imparts additional versatility to the epoxies. The major industrial utility of epoxy resins is in thermosetting applications. Treatment with curing agents gives insoluble and intractable thermosetting polymers. In order to facilitate processing and to modify cured resin properties, other constituents may be included in the compositions: fillers, accelerators, and tougheners. 2. MATERIALS For this study the EPIPHEN RE4020 DE4020 epoxy system was used as matrix and Zn powder and Clay powder as fillers. The named epoxy system consists of two liquid components A (bisphenol A - RE) and B (modified aliphatic amines DE). The A component was used to disperse the Zn (<53 µm) powder, respectively the Clay powder and then the required amount of B component was added. Three values of weight ratio (Zn/Epoxy or Clay/Epoxy) were set 1:2, 1:1 and 3:2 in order to investigate the filler s influence over the mechanical (bending parameters), tribological (wear resistance) and thermal properties (coefficient of thermal expansion and specific heat) of particulate composites. The samples were formed by direct molding in normal conditions (atmospheric pressure and laboratory temperature). For each concentration there were formed samples on various thermal conditions (I, II, III, IV, V) to point out the influence of thermal cures over the investigated properties. I-type, natural samples with normal temperature polymerization (2 weeks); after natural polymerization for the II-type samples, materials were kept for 8 hours at 60ºC; for the III-type 2 more hours at 90ºC last two stages represent the recommended thermal treatment; the IV-type samples were obtained after 1 hour at 120ºC (post cure recommended by the producer); the last type V suffered another 1 hour at 150ºC. From bulk formed materials samples for each analysis were extracted. 3. MEASUREMENTS AND RESULTS The thermal analysis was carried out using a differential scanning calorimeter DSC1 from Mettler Toledo and evaluations for specific heat were done using the Stare software also from Mettler Toledo. Using the same DSC method the specific heat was evaluated for Zn powder (fig. 1), Clay powder (fig. 2) 2 and for pure epoxy (fig. 3), the obtained values are kj/(kg K) for Zn, kj/(kg K) for Clay powder and kj/(kg K) for pure epoxy (without thermal treatment). With these values the composite specific heat was evaluated using mixture rule (for weight ratios) the results are shown in figure 4. Fig. 1. DSC curves for Zinc powder; heat flow (up), Fig. 2. DSC curves for Clay powder; heat flow (up), Fig. 3. DSC curves for Epoxy resin; heat flow (up),

3 151 The thermal behavior of the three components was made using the same heating ratio (15ºC/min) and starting from the same initial temperature of 30ºC, as in the case of particulate composites, because some of components features have to be found in the composites behavior. For example the peak which appears at Epoxy heating (representing a phase transition) has to appear also in the case of filled epoxy and at the same temperature of 60ºC. In the case of Clay powder it has to be said that it is a cosmetic powder and it was used without any thermal treatment. In the upper part of figure 2 it can be observed a large peak around 105ºC which may represent the elimination of crystallization water. The Zn powder behavior is a pure metallic one with a low increasing of specific heat with temperature. explanation for the Clay/Epoxy composites specific heat could be that in natural state the Clay powder contains organic substances which are involved in chemical reactions when the powder is dissipated in A component and then when the B component is added. Also it has to be taken into account the fact that in order to measure the specific heat of the powders small amounts of each one were pressed into the DSC pans changing the natural behavior. c [kj/kgk] Specific Heat (c) - Zinc/Epoxy Zinc Epoxy 1:2 1:1 3: Fig. 6. Specific heat of Zinc/Epoxy composites. c [kj/kgk] Fig. 4. Specific heat of composites (theoretical) Specific Heat (c) - Clay/Epoxy Clay Epoxy 1:2 1:1 3:2 Fig. 5. Specific heat of Clay/Epoxy composites. The measured specific heat of two types of particulate composites is presented in figures 5 and 6. Both for Clay/Epoxy and Zinc/Epoxy composites the measured values are lower than theoretically evaluated ones but in the case of Zinc/Epoxy they are in the interval between components values while in the case of Clay/Epoxy they are below the two values. An Regarding the thermal treatment of filled materials, it seems that it does not have a strong influence over the specific heat. Fact is that in the case of Zinc/Epoxy III-type materials show a relatively lower value which means instability while in the case of Clay/Epoxy the instability is displaced toward higher temperatures treatments. Also it has to be noticed that mixture rule works for filled polymers while in the case of 3:2 ratio of presented materials, the situation is opposite. For the formed particulate composites, the coefficient of thermal expansion was evaluated using a thermo-mechanical analyzer TMA-SDTA 840 also from Mettler Toledo. The results are presented in figures 7 and 8. For all the samples the coefficient evaluation was done for the temperature interval between 80ºC and 160ºC, all the samples were heated from 30ºC to 210ºC with a heating ratio of 10ºC/min. In the case of Zinc/Epoxy the 3:2 ratio leads to more dimensionally unstable composite. All the Clay/Epoxy materials look as being more dimensionally stable than the epoxy system. The 3:2 Clay/Epoxy material acts as a ceramic one especially after the high temperature treatments and also shows the highest dimensional stability. This material but with an improved electrical conductivity could be used as external layers of a stratified composite if its thermal conductivity is not too high. So, it has to be studied the behavior of such materials when another filler is used together with the clay. Using fillers to improve thermal and electrical properties of polymers, other properties are affected

4 152 THE ANNALS OF UNIVERSITY DUNĂREA DE JOS OF GALAŢI because of granular structure of composite. The mechanical properties (bending behavior) will be influenced by the absence of bonds between polymer crystallites (due to the Zn or Clay particles presence) also the wear properties will be affected. Coefficient of Thermal Expansion (CTE) - Clay/Epoxy 2.20E E-04 Epoxy 1:2 1:1 3:2 Measurements were performed for both types of properties using a Multi-Specimen Test System UMT from CETR adapted according to [5, 6] (for wear) and a M350-5AT testing machine from Testometric, results being presented in figures 9 and 10. The two higher concentrations of Zinc are lowering the wear resistance. It seems that from the bending and wear point of view only the 1:2 ratio is valuable. For the two higher Clay ratios, the wear resistance is increased by the thermal treatment. CTE [mm/k] 1.80E E E E E E+10 Wear Resistance (WR) Epoxy C/E 1:2 C/E 1:1 C/E 3:2 Z/E 1:2 Z/E 1:1 Z/E 3:2 1.00E-04 Fig. 7. Coefficient of thermal expansion; Clay/Epoxy.. WR [Nm/m*3] 1.50E E E+09 Coefficient of Thermal Expansion (CTE) - Zinc/Epoxy Epoxy 1:2 1:1 3:2 0.00E+00 CTE [mm/k] 3.50E E E E E E-04 Fig. 8. Coefficient of thermal expansion; Zinc/Epoxy. BS [MPa] Bending Strength at Break (BS) Epoxy C/E 1:2 C/E 1:1 C/E 3:2 Z/E 1:2 Z/E 1:1 Z/E 3:2 1.20E E E E E E E+00 Fig. 9. Bending strength at break. Fig. 10. Wear resistance of particulate composites. 4. CONCLUSIONS It is possible to use clay as filler for epoxy based composites, but the weight ratios purposed in this study are too high so the study has to be carried out for Zinc or Clay concentrations under 50%. A large characterisation of particulate composites had been performed in order to answer the question regarding the benefits of using such material as external layers of a reinforced epoxy based composite. The results encourage the start of a new study regarding the use of two or more fillers in the same time. The multi-component composites could represent the cheapest solution when controllable properties are required. In order to establish the right amount of filler, it is necessary not only to analyse the electromagnetic and mechanical properties but also the thermal properties. A structural microscopically analysis is also required in order to identify the quality of interfaces. In the case of a n-components composite there are n-1 interfaces, each one of them having its own contribution at composites properties. Using a single filler, it is possible to improve one or two properties, electrical and thermal conductivity for instance, and mean time to induce a decrease of other properties such as bending strength, shock resistance etc. That is way we consider that the layered pseudo-laminates could be a solution. Using polymer layers with relatively high electrical conductivity as external layers of laminate and

5 153 magnetic particles filled polymer as core layers. An electric circuit might be, at the same time, the composite reinforcement, leading to lighter structures and, based on carbon fiber s properties will transmit information about material s integrity. Exhaustive analysis has to be performed in order to investigate the thermal conductivity and fire resistance and ways to improve them such as polymeric composites to replace metals in various applications. The aim of improving the electrical conductivity seems to be reachable using fillers with high electrical conductivity together with Clay to fill the polymer for the external layers of a fabric reinforced composite. Using various fiber fabrics as reinforcements could solve the problems regarding dimensional stability (both carbon and aramide fiber show negative values of CTE), wear resistance (using aramide whiskers to supplementary fill the external polymer layers), mechanical properties (by realizing appropriated architectures and geometrical arrangements of reinforcement sheets). ACKNOWLEDGMENT This work was carried out with the support of Project 6583 SIMBAD, code POSDRU/6/1.5/5/15. REFERENCES 1. Rosato D.V., Rosato M.G., Rosato D.V., 2000, Concise Encyclopedia of Plastics, Kluwer Academic Publishers. 2. Tsou A.H., Waddell W.H., 2004, Fillers, in Mark, H.F. (ed), Encyclopedia of Polymer Science and Technology, John Wiley & Sons, Inc., vol. 10, pp Lefebvre J.-M., 2004, Nanocomposites, Polymer-Clay, in Mark H.F. (ed), Encyclopedia of Polymer Science and Technology, John Wiley & Sons, Inc., vol. 3, pp Pham H.Q., Marks M.J., 2004, Epoxy resins, in Mark H.F. (ed), Encyclopedia of Polymer Science and Technology, John Wiley & Sons, Inc., vol. 9, pp El-Tayeb N.S.M., 2009, Two-body abrasive behaviour of untreated SC and R-G fibers polyester composites, Wear, vol. 266, pp Mimaroglu A., Sen U., Unal H., 2008, Abrasive Wear Volume Maps for PA6 and PA6 Composites Under Dry Working Condition, Appl. Compos. Mater., vol. 15, pp

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