Co-reporter:Shameel Farhan, Rumin Wang, Kezhi Li
Journal of the European Ceramic Society 2017 Volume 37(Issue 2) pp:499-508
Publication Date(Web):February 2017
DOI:10.1016/j.jeurceramsoc.2016.09.008
•A two-step process for making preform and SiC/Si3N4/SiC ceramics.•One-step pyrolysis and siliconization treatment at 1600 °C/4 h.•SiC/Si3N4 preform containing in situ grown Si3N4 whiskers.•Isotropic physical and thermal properties contrary to bio-mimetic ceramics.•Densification using chemical vapor infiltration for higher densities.A two-step process has been developed for silicon carbide (SiC) coated polyurethane mimetic SiC preform containing silicon nitride (Si3N4) whiskers. SiC/Si3N4 preforms were prepared by pyrolysis/siliconization treatment at 1600 °C, of powder compacts containing rigid polyurethane, novolac and Si, forming a porous body with in situ grown Si3N4 whiskers. The properties were controlled by varying Si/C mole ratios such as 1–2.5. After densification using a chemical vapour infiltration, the resulting SiC/Si3N4/SiC composites showed excellent oxidation resistance, thermal conductivity of 4.32–6.62 Wm−1 K−1, ablation rate of 2.38 × 10−3 − 3.24 × 10−3 g cm−2 s and a flexural strength 43.12–55.33 MPa for a final density of 1.39–1.62 gcm−3. The presence of a Si3N4 phase reduced the thermal expansion mismatch resulting in relatively small cracks and well-bonded layers even after ablation testing. This innovative two-step processing can provide opportunities for expanded design for using SiC/Si3N4/SiC composites being lightweight, inexpensive, homogeneous and isotropic for various high temperature applications.
Co-reporter:Shameel Farhan, Rumin Wang, Dandan Zhang
Journal of Analytical and Applied Pyrolysis 2017 Volume 125(Volume 125) pp:
Publication Date(Web):1 May 2017
DOI:10.1016/j.jaap.2017.03.008
•A novel approach to use shirt polyvinyl acetyl fibers as sacrificial template.•Pyrolysis at 1000 °C to create channel like pores in resulting carbon foam.•Use of different cross-linking initiators to control excessive void formation.•Dicumyl peroxide proved to be superior in controlling pore-size distribution.Carbon foams with channel like pores have been prepared by pyrolysis of a thermosetting resin system; bismaleimide (BMI) modified allyl novolac (BAN) as carbon precursor and polyvinyl acetyl fibers (PVAF) as an organic sacrificial template. For improving the cross-linking density and glass transition temperature, dicumyl peroxide (DCP) was chosen as a curing initiator and compared the results with that of the most commonly used Hexamethylenetetramine (HTMA). After pyrolysis at 1000 °C, the resulting PVAF/HTMA/BAN carbon foam developed excessive voids with linear lengths and widths up to 3 and 0.25 mm respectively. Excessive bubbling of discrete self-curable BMI resin molecular chains surrounded by phenolic hydroxyl groups created such excessive voids and gaps. The PVAF/DCP/BAN carbon foam exhibited no such voids and the shape of the pores replicated the shape of PVAF template. Channel like pores were orientated at random with a non-cylindrical, flat, or kidney bean shape cross section with a maximum dimension of 25–50 μm. Moreover, general characteristics were studied including density, porosity, open cell, pore-size distribution, thermal conductivity and flexural strength. Results have showed that the PVAF/DCP/BAN carbon foam possessed improved properties including density, thermal conductivity and flexural strength of 0.53 g cm−3, 0.87 W m−1 K−1 and 19.12 MPa respectively.
Co-reporter:Shameel Farhan;Dandan Zhang;Kezhi Li
CrystEngComm (1999-Present) 2017 vol. 19(Issue 36) pp:5432-5441
Publication Date(Web):2017/09/18
DOI:10.1039/C7CE01121K
Si3N4 saw-tooth nanoribbons (SNSNs) have been synthesized via a novel approach involving a by-product pyrolysis–nitridation process during carbon foam manufacturing at 1450 °C. The SNSNs formed are ribbon shaped, 80–750 nm wide, 70–80 nm thick and several micrometres in length. The process simply involved thermal pyrolysis of a powdered mixture containing carbon foam precursors and silicon powder under flowing high-purity nitrogen. Pyrolysis gases rich in silicon, silicon oxide and active nitrogen vapours promoted the subsequent synthesis of the SNSNs over the outer surface of the carbon foams via a vapour–solid mechanism. The crystal structure, morphology, chemical composition, growth mechanism and photoluminescence (PL) properties have been studied. The infrared adsorption of SNSNs exhibited two absorption bands with all the peaks related to the Si–N bonds of the α-Si3N4 crystalline structure. X-ray photoelectron spectroscopy measurements further confirmed the chemical composition, with minor impurities such as oxygen and carbon. A single nanoribbon has the same width-to-thickness ratio, suggesting a stable morphology resulting from the reduction of the overall surface energy. Intense PL was observed centred at 2.03, 2.48, 2.62, and 3.01 eV, which resulted from the recombination between the intrinsic conduction band edges and silicon dangling bonds with deep-level or trap-level states.
Co-reporter:Shameel Farhan, Rumin Wang, Kezhi Li
Journal of Alloys and Compounds 2016 Volume 682() pp:695-705
Publication Date(Web):15 October 2016
DOI:10.1016/j.jallcom.2016.04.319
•A new carbonization activated pack cementation process for coating.•One-step simultaneous carbonization and coating.•Excessive in situ growth of nanowires.•No cracking/debonding after thermal shocks due to matched CTEs.In order to improve the oxidation resistance of carbon foam, a silicon carbide (SiC) coating was prepared using carbonization-activated pack cementation method. Carbon foam was firstly carbonized partially at 500 °C and then fully carbonized at 1600 °C with pack powder containing activated carbon, silicon powder, and iron chloride. The as-obtained coating was characterized using scanning and transmission electron microscopies, X-ray diffraction, thermogravimetric analysis, oxidation thermal shock and coefficient of thermal expansion. The results showed that the coating was mainly composed of randomly distributed SiC nanowires extended inside the surface pores forming pinning effect. The growth mechanism involved dissolution of SiO and CO (vapors) in the Fi-Si melt (liquid) and precipitation of one-dimensional SiC nanowires (solid). In non-isothermal oxidation, the coated carbon foam showed a mass loss of only 1.97%. The thermal shock results indicated that due to matching of thermal expansion coefficients, no cracks occurred on the surface after 15 cycles under temperature drop of 1475 °C. Consequently, we expect that this new high temperature coating method, and the subsequent microstructure that it creates, can be widely applied to improve the thermal shock and oxidation resistance of carbon foam.
Co-reporter:Hao Jiang;Shameel Farhan;Dan Zhang ;Shuirong Zheng
Polymer International 2016 Volume 65( Issue 4) pp:430-438
Publication Date(Web):
DOI:10.1002/pi.5073
Abstract
A thermosetting resin system, based on tetraglycidyl-4,4′-diaminodiphenylmethane, has been developed via copolymerization with 4,4′-diaminodiphenylsulfone in the presence of a newly synthesized liquid crystalline epoxy (LCE). The curing behavior of LCE-containing resin system was evaluated using curing kinetics method and Fourier transform infrared spectroscopy. The effect of LCE on the thermal and mechanical properties of modified epoxy systems was studied. Thermogravimetric analysis indicated that the modified resin systems displayed a high T0.05 and char yield at lower concentrations of LCE (≤5 wt%), suggesting an improved thermal stability. As determined using dynamic mechanical analysis and differential scanning calorimetry, the glass transition value increased by 9.7% compared to that of the neat resin when the LCE content was 5 wt%. Meanwhile, the addition of 5 wt% of LCE maximized the toughness with a 175% increase in impact strength. The analysis of fracture surfaces revealed a possible effect of LCE as a toughener and showed no phase separation in the modified resin system, which was also confirmed by dynamic mechanical analysis. © 2016 Society of Chemical Industry
Co-reporter:Hao Jiang;Shameel Farhan;Shuirong Zheng
Polymer Composites 2016 Volume 37( Issue 7) pp:2260-2271
Publication Date(Web):
DOI:10.1002/pc.23404
A thermosetting resin system, bismaleimide (BMI) modified allyl novolac (BAN), was developed via reactive blending of formaldehyde and catalyst drop wise to improve the extent of reaction between BMI and phenol-carbenium ions. For improving the curing behavior and mechanical properties, dicumyl peroxide (DCP) was selected as a novel curing initiator to compare with hexamethylenetetramine (HTMA) which is the most common curing initiator used in the manufacture of phenolic resins. BAN was characterized by 1H nuclear magnetic resonance and Fourier transfer infrared spectroscopy. Curing behavior with initiators was analyzed by differential scanning calorimetry and glass transition temperature of the cured resins was examined by dynamic mechanical analysis. For evaluating efficiency of the modified system, composite samples using polyvinyl acetyl fiber were molded and tested for flexural properties before and after ageing at 150°C for 1,000 h. The morphology of composite samples was examined by scanning electron microscope, and the effects of the incorporated initiators on the mechanical and thermal properties of composite were investigated. The results indicated that the initiators reduced the curing temperature effectively and improved the curing process. DCP proved to be more effective in crosslinking and heat resistance than HTMA. Meanwhile, the molded composite with DCP showed higher mechanical properties before and after ageing when compared with HTMA curing initiator. Therefore, DCP/BAN resin system with good heat resistance, higher mechanical properties, and better process ability can be applied as matrix resin for the manufacturing of advanced fiber reinforced composites. POLYM. COMPOS., 37:2260–2271, 2016. © 2015 Society of Plastics Engineers
Co-reporter:Shameel Farhan;Kezhi Li
Journal of Materials Science 2016 Volume 51( Issue 17) pp:7991-8004
Publication Date(Web):2016 September
DOI:10.1007/s10853-016-0068-4
Carbon foam filled with silver particles was fabricated by a powder molding process using polyurethane as pore former, novolac resin as binder, coal-tar pitch as densification additive, and silver foils as a filler. High-temperature treatment at 1200 °C, transformed the silver into spherical particles covered with in situ grown Ag nanowires. Their microstructure, electromagnetic interference (EMI) shielding effectiveness (SE), and shielding mechanism was investigated. It was found that the micron-sized silver foils converted into particles during heat treatment and strongly bonded in carbon matrix. The addition of silver significantly enhanced both conductivity and SE. Carbon foam containing 1.5 wt% silver exhibited very impressive total SE and dielectric loss tangent owing to the more conductive network of silver particles providing fast electron-transport channels. A maximum specific EMI SE value of 58.21 dB g−1 cm3 at 12 GHz was achieved in the carbon foam at 1.5 wt% Ag loading. The dominant mechanism was absorption with only 6–10 % reflectance, resulting from the multiple reflections at interfaces inside the foam. Due to controlled attachment of silver particles and in situ reactions, this novel substrate has unique opportunities for future surface tailoring required in various commercial and aerospace fields.
Co-reporter:Shameel Farhan, Rumin Wang, Kezhi Li
Ceramics International 2015 Volume 41(Issue 8) pp:9763-9769
Publication Date(Web):September 2015
DOI:10.1016/j.ceramint.2015.04.048
Three-dimensional carbon/carbon (C/C) composites with an apparent density higher than 1.84 g/cm3 were fabricated using multiple carbon fiber tows oriented in four directions and densified using a combined process. This consists of a pre-densification step using a thermal-gradient chemical vapor infiltration process followed by pitch impregnation/carbonization cycles carried out under high pressure. The samples were machined along X-, Y- and Z-axis of the preform architecture denoting the weakest to the strongest direction in the composite respectively. The Y-directional sample showed the highest thermal diffusivity and the lowest CTE values. The directional ablative behavior was studied using plasma arc testing on a Huels type arc-heater. The Z-directional sample showed the lowest ablation and erosion rates while the other two showed a discrepancy in the linear and calculated erosion rates. To further investigate it, the samples after the test were analyzed in the heat-affected zone for a reduced density. Based on empirical correlation, a new term called “corrected linear ablation rate” has been formulated which also helped in the calculation of surface roughness after the ablation testing. Compressive tests were performed before and after plasma testing. After plasma testing, the compressive strength and modulus were almost the same except for the X-directional sample whose modulus reduced to 50%. The X-directional sample, being the weakest direction, showed a double shear type failure, while the other two failed with end crushing, resulting from the different fiber architecture.
Co-reporter:Hao Jiang;Shameel Farhan ;Shuirong Zheng
Polymer International 2015 Volume 64( Issue 12) pp:1794-1800
Publication Date(Web):
DOI:10.1002/pi.4982
Abstract
A new hyperbranched polymer (HBP) with a flexible aromatic skeleton and terminal epoxy groups was synthesized to improve the toughness of diglycidyl ether of bisphenol A. The HBP was characterized using nuclear magnetic resonance, Fourier transfer infrared spectroscopy and gel permeation chromatography. The effect of HBP on the thermomechanical and mechanical properties of modified epoxy systems was studied. For evaluating the efficiency of the modified epoxy systems, composite samples using glass fiber cloth were molded and tested. Using dynamic mechanical analysis, a slight reduction in glass transition temperature (Tg) with increasing HBP content was observed. Analysis of fracture surfaces revealed a possible effect of HBP as a toughener and showed no phase separation in the modified resin systems. The results showed that the addition of 15 phr HBP maximized the toughness of the modified resin systems with 215 and 40% increases in impact and flexural strengths, respectively. Tg and heat resistance of cured modified resin systems decreased slightly with an increase in HBP content and, at 15 phr HBP, only a 2.6% decrease in thermomechanical properties was observed. Meanwhile, a molded composite with HBP showed improved mechanical properties and retention rate at 150 °C as compared to that made with neat resin. © 2015 Society of Chemical Industry
Co-reporter:Hao Jiang;Shameel Farhan ;Shuirong Zheng
Journal of Applied Polymer Science 2015 Volume 132( Issue 15) pp:
Publication Date(Web):
DOI:10.1002/app.41829
ABSTRACT
For reducing the cure temperature and improving the thermal stability and mechanical properties, a thermosetting resin system composed of novolak and bismaleimide (BMI) was developed by reactive blending and using dicumyl peroxide (DCP) as a novel curing agent. Novolak was allylated and reacted with BMI to produce bismaleimide allylated novolak (BAN), and the effect of DCP on flexural, impact and heat distortion temperature of cured resin were investigated. On the basis of improved mechanical and thermal properties at 0.5% DCP contents, the curing behavior of DCP/BAN resin system was evaluated by DSC analysis. Ene, Diels-Alder, homo-polymerization and alternating copolymerization which occurred in DCP/BAN resin system were further verified using FTIR at sequential cure conditions from 140 to 200°C. Kissinger and Ozawa-Flynn-wall methods were used to optimize the process and curing reactions of DCP/BAN resin system. The results showed that the addition of 0.5% DCP in BAN reduced the curing temperature and time of the modified resin. For evaluating process ability of the modified system, composite samples using polyvinyl acetyl fiber were molded and tested for flexural properties. The resulting samples showed better flexural properties when compared with the composite made with neat BAN. The modified 0.5% DCP/BAN resin system with good mechanical properties and manufacturability can be used for making bulk molding compounds and fiber reinforced composites required in various commercial and aerospace applications. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015, 132, 41829.
Co-reporter:Shameel Farhan, Ru-Min Wang, Hao Jiang, Noaman Ul-Haq
Journal of Analytical and Applied Pyrolysis 2014 110() pp: 229-234
Publication Date(Web):
DOI:10.1016/j.jaap.2014.09.003
Co-reporter:Tao Ai;Wenying Zhou
Polymer Composites 2007 Volume 28(Issue 3) pp:412-416
Publication Date(Web):10 MAY 2007
DOI:10.1002/pc.20313
This research applied the methodology of metalation and grafting alkoxysilane to modify the surface of Kevlar-29 fiber. The surface properties of the modified Kevlar fiber were characterized by scanning electron microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, atomic force microscopy, and Brunauer-Emmett-Teller isothermal adsorption analysis. The relationship between surface characteristics of Kevlar fiber and its interfacial adhesion of Kevlar fiber-reinforced epoxy resin composites was also discussed. Compared with the untreated fiber, the surface of the modified Kevlar fiber was much rougher, its oxygen content increased by about 12%, the surface area enlarged about 10 times, and the wetting behavior improved. Due to the modification of the fiber, the adhesion between the fiber and the resin matrix was markedly improved and the Interlaminar Shear Strength of its epoxy composites increased by about 57%. POLYM. COMPOS. 28:412–416, 2007. © 2007 Society of Plastics Engineers.