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Heat-Resistant Composite Materials Based on Polyimide Matrix ORIENTAL JOURNAL OF CHEMISTRY ISSN: 0970-020 X CODEN: OJCHEG An International Open Free Access, Peer Reviewed Research Journal 2016, Vol. 32, No. (6): Pg. 3155-3164 www.orientjchem.org Heat-Resistant Composite Materials Based on Polyimide Matrix VITALY SERGEYEVICH IVANOV, ALYONA IGOREVNA WOZNIAK and ANTON SERGEYEVICH YEGOROV* Federal State Unitary Enterprise «State Scientific Research Institute of Chemical Reagents and High Purity Chemical Substances» (FSUE «IREA») *Corresponding author E-mail: [email protected] http://dx.doi.org/10.13005/ojc/320638 (Received: October 05, 2016; Accepted: November 25, 2016) Abstract Heat-resistant composite materials with a polyimide-based binder were obtained in this paper. Composites were prepared with different content of single-wall carbon nanotubes (SWCNT) and nanostructured silicon carbide, and polyimides coated carbon fibers woven into the cloth. Composite materials showed high values of thermostability and resistance to thermo-oxidative degradation, as well as good mechanical properties. Keywords: Heat-resistant composite materials, Carbon fiber, Silicon carbide, Polyimide matrix, Carbon nanotube. IntroDUCTION as filaments, ropes, rovings, ribbons (PCM with continuous filaments, reinforced plastics). Such Due to the increasing demand for structural fillers as carbide fibers, carbon nanotubes (CNTs), materials, the most widely used in current technology fullerenes and other nano-objects have a normal rate (primarily aerospace), new chemical structures of growth in technologies. Polymer nanocomposites having a certain range of physical properties that represent a new class of materials have are constantly developing. The extensive use of unique barrier properties, electrical conductivity, composite materials (CM), especially polymeric thermal conductivity, high strength, heat resistance, composite materials (PCM), has resulted in the thermostability and low flammability1-9. enormous progress in polymer chemistry and physics. Currently the most popular fillers among Polyimides (PI) represent one of the most PCM are continuous filaments and textile forms important polymers, commercially available for 3156 IVANOV et al., Orient. J. Chem., Vol. 32(6), 3155-3164 (2016) a variety of applications, such as aerospace and toughness, crack resistance, solidity, practically electronics industry, in which structural materials are the whole range of technological and operational often exposed to extreme conditions of mechanical, properties of PCM. electrical, radiation, and other stresses. Despite the outstanding performance parameters of PI, these The authors23, 24 have chosen as a model polymers have disadvantages. Among others, one of two well-studied polyimides -LaRC CP2 and APB/ the most important disadvantage is the low bending ODPA, obtained by polymerization in situ. Filling and breaking strength and frangibility, caused by the these PIs with nanotubes in the range from 0.1 presence of group-linkers in diamine or dianhydride to 1.0% by volume, significantly increased the fragments in the polyimide chain structure, the mechanical properties of polymers. Thus, when using introduction of which is necessary to reduce the the PI, CNT matrix of 1%, PCM modulus of elasticity glass-transition temperature (Tg) and thus improve based on LaRC CP2 is increased by 65% and 43% the processability of the polymer product10-13. for APB / ODPA25. Currently PIs are used as matrices to However, when preparing PCM based on PI create reinforced composites based on light carbon as a matrix and nano-objects as a filler, we often have fibers as a replacement for metal parts in the to face with such a problem as the inhomogeneity aerospace industry and airframe parts, due to their of the filler dispersion in the matrix, which leads to outstanding thermal and mechanical resistance. PIs deterioration of the mechanical properties of the are used in the cable industry in the preparation of PCM. To circumvent difficulties associated with electrical-insulating varnishes and enamels having inhomogeneity of dispersion, we often resort to high thermostability and elasticity, good dielectric chemical inoculation of filler molecules to the end properties for coating wires and products14. fragments of polymer chain or the side chain26. On the basis of the received data, it is possible notice One of the ways to increase the mechanical that when the content of the modified CNTs in PCM parameters of PIs, is the introduction of such fillers as amounts only 0.5% by weight, the tensile strength nanotubes, fullerenes and fibers into the polymeric (s) increased nearly by 1.8 times, and a modulus of structure that act as a “molecular lubricant” and elasticity (E) – by 1.2 times. It is worth noting that allow the polymer chains move more freely relative further filling of polyimide matrix with the filler results to each other, which in turn, leads to improvement in a reduction of mechanical characteristics of the of the shear moduli, relative deformations , strength PCM samples. So, while filling of 5 wt.%, s, and characteristics and other physical and mechanical elongation (Dl) becomes lower than initial values for properties15. Adding only 0.1% of weight of the filler, the unfilled PI, and E becomes only slightly greater in certain cases, increases the mechanical strength than unfilled sample. These facts can be explained considerably. by the aggregation of CNT between each other due to Van der Waals interactions that make a significant Using the light elements (like carbon, silicon contribution when increasing the concentration of or boron) is the most promising for the production CNTs in a polymer matrix. of materials with high mechanical properties as the theoretical strength of the material depends The purpose of this paper is to obtain heat- on the radius of the atom, forming a chemical resistant composites based polyimides with different bond. Thermostability of PCM when filling with content of single-wall carbon nanotubes (SWCNT) high-strength and stable objects (carbide fibers, and nanostructured silicon carbide, as well as nanotubes, fullerenes)16-19 will be determined mainly polyimides coated carbon fiber woven into the fabric. by the choice of the polymer matrix, the less heat- As used polyimide matrices are insoluble in organic stable component of PCM. Mechanical properties solvents, and their softening temperature exceeds of PCM are largely determined by the properties of 300°C, it is advisable to use the method of in-situ the filler. However, the properties of PCM depend polymerization. The thermostability in argon and in on the ratio of matrices and fillers’ properties that air and mechanical properties were measured for the determine the interaction of components, fracture composite obtained. Tensile stress and elongation IVANOV et al., Orient. J. Chem., Vol. 32(6), 3155-3164 (2016) 3157 at break were measured for composites with CNTs a reflux condenser, a tube for injection of inert gas and SiC. Flexural strength and modulus of elasticity was filled with 40 ml of N-methylpyrrolidone and 22.9 were measured for composites with HC. mmol of diamine. Then, with stirring and cooling in argon flow, maintaining the temperature at 15°C Experimental part it was added 22.9 mmol dianhydride portionwise. Process for obtaining composite polymeric When adding all of the dianhydride, the cooling was materials with continuous filaments is divided into two stopped and it was stirred at room temperature for 24 stages: obtaining the half-finished product (saturated hours. Upon completion of mixing the carbon cloth with pre-preg resin) of a given configuration UT-900- PM was impregnated with the resultant and molding it to achieve high strength and polyamic acid and left under pressure for 8 hours. toughness2. Flowed out binder was removed with a spatula. The resulting pre-preg was spread on a ceramic tile Materials and Reagents and placed in a vacuum oven. The pre-preg was Pyromellitic anhydride (PMDA), 3,3', 4,4'- dried in a vacuum oven at 80°C for 6 hours, then at benzophenonetetracarboxylic acid dianhydride 150°C, 200°C, 250°C and 300°C for 1 hour at each (BPDA) and 3,3', 4,4' - diphenyl oxide tetracarboxylic temperature and then at 350°C for 15 minutes. acid dianhydride (DPDA) were previously obtained by the authors27. Mass fraction of basic substance Preparation of composite materials PI-SiC is not less than 95%. 4,4 ‘- oxydianiline (ODA) and A three-necked 250 ml flask equipped N-methyl pyrrolidone were purchased from Vekton, with an ultrasonic disperser, a reflux condenser, a 4 - aminophenylsulfone (PS) was purchased from tube for injection of inert gas was filled with 55 ml of Acros Organics. Single-walled carbon nanotubes N-methylpyrrolidone, nanostructured SiC and 45.8 (SWCNTs) were purchased from OCSiAl. Multiwall mmol of diamine. The reaction mass was sonicated at carbon nanotubes (MWCNTs) were purchased from a frequency of 20 kHz for 20 minutes while cooling in NanoTechCenter. Carbon fiber (CF), woven into the an ice bath. Then it was stirred using a conventional cloth of the brand UT-900-PM was purchased from mechanical stirrer. When stirring portionwise it was Argon. Nanostructured silicon carbide is purchased added 45.8 mmol of dianhydride, and then stirred for from InChem-Synthesis. 24 hours at room temperature. The resulting mixture was cast onto a ceramic tile to obtain films using an Preparation of composite materials PI-SWCNT applicator and then it was placed in a vacuum oven. A three-necked 250 ml flask equipped The film was dried in a vacuum oven at 80°C for with an ultrasonic disperser, a reflux condenser, a 6 hours, then at 150°C, 200°C, 250°C and 300°C tube for injection of inert gas was filled with 90 ml for 1 hour at each temperature and then at 350°C of N-methylpyrrolidone, CNTs and 71.9 mmol 4,4'- for 15 minutes. oxydianiline. The reaction mass was sonicated at a frequency of 20 kHz for 15 minutes while cooling in The film of composite material is obtained an ice bath. Then it was stirred using a conventional with a color ranging from light brown to black mechanical stirrer.
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