Fabrication of CNT-SiC/SiC composites by electrophoretic deposition

Due to the outstanding mechanical and thermal properties of carbon nanotubes (CNTs), they are considered suitable reinforcement for structural materials. In this study, for the first time, electrophoretic deposition (EPD) was used to deposit (multi-walled) CNTs onto SiC fibres (SiC_f) to form an effective CNT interphase layer for SiC_f/SiC composites. This deposition was followed by electrophoretic infiltration of the CNT-coated SiC fibre mats with SiC powder to fabricate a new CNT-SiC-fibre-reinforced SiC-matrix (SiC_f/SiC) composite for fusion applications. In these EPD experiments, a commercial aqueous suspension of negatively charged CNTs and an optimized aqueous suspension of negatively charged SiC particles were used. The CNT-coatings on the SiC fibres were firm and homogenous, and uniformly distributed nanotubes were observed on the fibre surfaces. In a following step of EPD, a thick SiC layer was formed on the fibre mat when the CNT-coated SiC fibres were in contact with the positive electrode of the EPD cell; however, spaces between the fibres were not fully filled with SiC. Conversely, when CNT-coated SiC fibres were isolated from the electrode, the SiC particles were able to gradually fill the fibre mat resulting in relatively high infiltration, which leads to dense composites.     

Multi-walled carbon nanotube/polyimide composite film fabricated through electrophoretic deposition

Multi-walled carbon nanotube (MWCNT)/polyimide composite films were fabricated through electrophoretic deposition (EPD) of MWCNT-polyamic acid colloidal suspension which was derived from carboxylated-MWCNTs and poly(pyromellitic dianhydride-co-4,4′-oxydianiline) (PMDA-ODA). Under electric field, both negatively charged MWCNTs and PMDA-ODA colloid particles migrate onto a positively charged anode simultaneously, and are converted to a coherent MWCNT/polyimide composite film in the ensuing imidization reaction. Uniform dispersion of MWCNTs in the composite film was observed using transmission electron microscopy. The thickness of the prepared composite film can be tuned by varying processing conditions such as deposition time and anode conductivity. The electrical conductivity of the composite film increased with increasing the concentration of MWCNTs in EPD suspension. The mechanical reinforcement of polyimide using MWCNTs was evaluated by tensile testing and nanoindentation testing.     

Elektrophoretische Abscheidung zur Herstellung von faserverstärkten Keramik‐ und Glasmatrix‐Verbundwerkstoffen — Eine Übersicht

In this paper, we review the application of the electrophoretic deposition (EPD) technique in the fabrication of fibre reinforced composites, with particular emphasis on composites with glass and ceramic matrices containing metallic or ceramic fibre fabric reinforcement. The review covers research published in the last 10 years. EPD has been used to infiltrate preforms with tight fibre weave architectures using different nano‐sized ceramic particles, including silica and boehmite sols, as well as dual‐component sols of mullite composition. The principles of the EPD technique are briefly explained and various factors affecting the EPD behaviour of ceramic sols and their optimisation to obtain high infiltration of the fibre preforms are considered. Overall, the analysis of the published data and our own results demonstrate that EPD, being simple and inexpensive, provides an attractive alternative for ceramic infiltration and coating of fiber fabrics, even if they exhibit tight fibre weave architectures.     

Multi-functional multi-walled carbon nanotube-jute fibres and composites

Jute fibres and corresponding epoxy based composites with sensing abilities could be realized by depositing multi-walled carbon nanotubes (MWCNTs) on the surfaces of jute fibres or fabrics using simple and scalable dip coating. The formation of electrically semiconducting MWCNT networks on jute fibre surfaces was confirmed, which in turn caused the formation of jute/epoxy interphases with highly concentrated MWCNTs. The sensing behaviour of the MWCNT coated jute fibres and jute/epoxy composites for temperature, relative humidity and stress/strain was further established in detail, which were strongly influenced by the intrinsic physical and chemical features of the fibres. In addition, a significant improvement in dielectric properties of the MWCNT-jute/epoxy composites was observed compared to neat jute/epoxy composites. Based on this approach, the electrically insulating natural fibres along with semiconducting MWCNTs on surface will stimulate and realize a broad range of multi-functional applications.     

Electrophoretic deposition of ceramic coatings on ceramic composite substrates

Abstract

The applicability of electrophoretic deposition (EPD) for the fabrication of single layer and multilayer ceramic coatings on dense ceramic composite materials has been examined. Al₂O₃/Y-tetragonal zirconia polycrystal (TZP) functionally graded composites of tubular shape were successfully coated with a two layer coating comprising porous alumina and dense reaction bonded mullite layers. The dual layer coating structure was designed to eliminate the numerous cracks caused by volume shrinkage during sintering of the individual EPD formed layers. In another example, mullite fibre reinforced mullite matrix composites were coated with a thin layer of nanosized silica particles using EPD. The aim was to achieve a compressive residual stress field in the silica layer on cooling from sintering temperature, in order to increase composite fracture strength and toughness. The EPD technique proved to be a reliable method for rapid preparation of single layer and multilayer ceramic coatings with reproducible thickness and microstructure on ceramic composite substrates.     

Synthesis of glass fiber‐multiwall carbon nanotube hybrid structures for high‐performance conductive composites

The conductive polyamide 66 (PA66)/carbon nanotube (CNT) composites reinforced with glass fiber‐multiwall CNT (GF‐MWCNT) hybrids were prepared by melt mixing. Electrostactic adsorption was utilized for the deposition of MWCNTs on the surfaces of glass fibers (GFs) to construct hybrid reinforcement with high‐electrical conductivity. The fabricated PA66/CNT composites reinforced with GF‐MWCNT hybrids showed enhanced electrical conductivity and mechanical properties as compared to those of PA66/CNT or PA66/GF/CNT composites. A significant reduction in percolation threshold was found for PA66/GF‐MWCNT/CNT composite (only 0.70 vol%). The morphological investigation demonstrated that MWCNT coating on the surfaces of the GFs improved load transfer between the GFs and the matrix. The presence of MWCNTs in the matrix‐rich interfacial regions enhanced the tensile modulus of the composite by about 10% than that of PA66/GF/CNT composite at the same CNT loading, which shows a promising route to build up high‐performance conductive composites. POLYM. COMPOS. 34:1313–1320, 2013. © 2013 Society of Plastics Engineers     

Fabrication technologies for oxide–oxide ceramic matrix composites based on electrophoretic deposition

Electrophoretic deposition (EPD) was used to fabricate alumina matrix composites with high volume fraction of woven fibre mat (Nextel™ 720) reinforcement in a multilayer structure. Colloidal suspensions of Al₂O₃ nanoparticles in ethanol medium with addition of 4-hydrobezoic acid were used for EPD. Two different techniques were developed for fabrication of Al₂O₃ matrix/Nextel™ 720 fibre composites. The first method is a combination of standard EPD of single fibre mats with a subsequent lamination procedure to fabricate the multilayered composite. The second method involves the simultaneous infiltration of several (three or more) Nextel™ 720 fibre mats by EPD in a tailor-made cell. The composites exhibit a homogeneous matrix microstructure, characterised by a very high particle packing density and relatively low porosity after sintering at 1300 °C. The EPD cell allows production of relatively large bodies (10 cm diameter). By combination of the multilayer EPD infiltration and lamination processes developed here, thick ceramic matrix composite components (>10 mm thickness) can be fabricated, which opens the possibility of greater industrial application of the materials.     

Fabrication and performance of mini SiC/SiC composites with an electrophoresis-deposited BN fiber/matrix interphase

The feasibility of fabricating a BN matrix/fiber interphase of SiC/SiC composites via electrophoresis deposition (EPD) was investigated based on the simplicity and non-destructiveness of the process and the excellent interfacial modification effects of BN. The BN suspension and SiC fiber surface properties were both adjusted to generate suitable conditions for the EPD process of the BN interphase. Next, the deposition dynamics and mechanism were studied under different deposition voltages and time, and the relationship between the deposition morphology of the BN interphase and mechanical properties of the fabricated mini SiC/SiC composites were also discussed. After oxidation at high temperature (600–1000 ℃), the mechanical properties of the mini SiC/SiC composites were studied to verify the oxidation resistance effect of the EPD-deposited BN interphase, whose oxidation resistance mechanism was briefly analyzed as well.     

Experimental evidence of the interface/interphase formation between powder coating and composite material

The present study focuses on the physicochemical characterization of the interface between an epoxy/polyester-based powder coating and an epoxy/thermoplastic-based composite material. An in-mold process has been used for the powder coating deposition on carbon/glass fibers reinforced composite substrates, and different methods have been performed to characterize the interface. We evidence here the strong dependence of the structural, chemical and thermal behaviors of the interface on the cure time/temperature conditions at which the powder coating was crosslinked. At a low crosslinking rate of coating (∼48%), experimental results reveal the development of a large heterogeneous organic/organic interphase between coating and substrate. However, thin interphases have been detected when the crosslinking rate goes beyond 69%. Besides, a phase segregation of thermoplastic additive within the composite matrix was identified in the formation of this interphase. Energy-dispersive X-ray spectroscopy (EDS) as well as FTIR/Raman experiments enabled us to put in evidence the diffusion process of the thermoplastic additive toward the coating. From thermal analysis, glass transition temperature Tg for both components was observed, which confirm the proposed mechanism. This study highlights the importance of the thermal processes on the complex competition between the interdiffusion between two epoxy matrix and the existence of thermoplastic toughening agent at the interface of powder coating and composite material.     

Processing and characterisation of 2-D woven metal fibre-reinforced multilayer silica matrix composites using electrophoretic deposition and pressure filtration

A novel, cost-effective and rapid processing route including electrophoretic deposition (EPD) and pressure filtration (PF) has been developed for the fabrication of 2-D woven metallic fibre mat reinforced multilayer silica matrix composites. Commercially available silica sol containing ultrafine ceramic particles (15 nm) was used as the matrix whilst 2-D woven metal stainless steel 316L fibre mat was used as the metal reinforcement to produce a composite having 2-D isotropic properties. The colloidal silica sol was modified with boria and boehmite in order to produce a silica matrix which could be sintered at 900°C (the maximum use temperature for the particular fibre architecture employed), and with densification taking place before crystallisation. An in-situ electrophoretic deposition (EPD) cell capable of measuring the weight gain in real time during deposition was designed. This technique enabled the woven fibre inter/intra tow regions to be infiltrated with the ultrafine silica particles in a very short time (2 min). Green bodies made from electrophoretically deposited fibre mats were further consolidated using pressure filtration. The EPD parameters were optimised in terms of time, voltage and deposition thickness as well as deposit formation rate. Microstructural observation indicated that the composites produced were dense and of high microstructural homogeneity.     

Formation of thin boron nitride coating on multiwall carbon nanotube surfaces

Thin boron nitride films were deposited onto outer surfaces of multiwall carbon nanotubes (MWCNTs) by dip coating, which involves infiltration by boric acid solutions and subsequent nitridation of the boron oxide in ammonia flow at 1050 °C. The overall composition of the samples was determined by electron energy loss (EELS) and X-ray photoelectron spectroscopy (XPS), the surface composition and chemical structure of the BN coatings by XPS, the morphology of the BN/MWCNT composites by scanning and transmission electron microscopy (SEM, TEM), and the resistance against oxidation at elevated temperatures by thermal analysis (TGA). It was proved that single and multilayer BN coverage were achieved at the applied experimental conditions, and the coated samples showed significantly increased oxidation resistance compared to the uncoated MWCNTs.     

Effect of intermediate heat treatment on mechanical properties of SiCf/SiC composites with BN interphase prepared by ICVI

SiC_f/SiC composites with BN interface were prepared through isothermal-isobaric chemical vapour infiltration process. Room temperature mechanical properties such as tensile, flexural, inter-laminar shear strength and fracture toughness (K_IC) were studied for the composites. The tensile strength of the SiC_f/SiC composites with stabilised BN interface was almost 3.5 times higher than that of SiC_f/SiC composites with un-stabilised BN interphase. The fracture toughness is similarly enhanced to 23 MPa m^1/2 by stabilisation treatment. Fibre push-through test results showed that the interfacial bond strength between fibre and matrix for the composite with un-stabilised BN interface was too strong (>48 MPa) and it has been modified to a weaker bond (10 MPa) due to intermediate heat treatment. In the case of composite in which BN interface was subjected to thermal treatment soon after the interface coating, the interfacial bond strength between fibre and matrix was relatively stronger (29 MPa) and facilitated limited fibre pull-out.     

1D/2D carbon nanotube/graphene nanosheet composite anodes fabricated using electrophoretic assembly

This study examines the direct assembly of hybrid graphene nanosheets (GNSs) and multiwalled carbon nanotubes (MWCNTs) onto Ni current collectors in the presence of an electric field. The dissociation of Ni nitrate salt, which provides ions to charge the GNSs and MWCNTs positively, facilitates the homogeneous dispersion of each powder and assists in electrophoretic deposition. Direct assembly by this electrophoretic deposition results in the effective packing of GNS/MWCNT composites without any appreciable agglomeration, which is desirable for achieving high electrochemical performance of the composite electrodes in Li-ion batteries. Hence, GNS/MWCNT composite electrodes exhibit higher specific capacity compared to electrodes made of pure GNSs or MWCNTs owing to better realization of electrolyte permeability and Li-ion transfer.     

Formation of Ti3SiC2 interphase coating on SiCf/SiC composite by electrophoretic deposition

To improve the oxidation resistance of SiC composites at high temperature, the feasibility of using Ti₃SiC₂ coated via electrophoretic deposition (EPD) as a SiC fiber reinforced SiC composite interphase material was studied. Through fiber pullout, Ti₃SiC₂, due to its lamellar structure, has the possibility of improving the fracture toughness of SiC_f/SiC composites. In this study, Ti₃SiC₂ coating was produced by EPD on SiC fiber; using Ti₃SiC₂‐coated SiC fabric, SiC_f/SiC composite was fabricated by hot pressing. Platelet Ti₃SiC₂ powder pulverized into nanoparticles through high‐energy wet ball milling was uniformly coated on the SiC fiber in a direction in which the basal plane of the particles was parallel to the fiber. In a 3‐point bending test of the SiC_f/SiC composite using Ti₃SiC₂‐coated SiC fabric, the SiC_f/SiC composite exhibited brittle fracture behavior, but an abrupt slope change in the strength‐displacement curve was observed during loading due to the Ti₃SiC₂ interphase. On the fracture surface, delamination between each layer of SiC fabric was observed.     

Fabrication of SiC/diamond composite coatings by electrophoretic deposition and chemical vapor deposition

In this research, SiC/diamond composite coatings were fabricated by a novel procedure that consisted of the electrophoretic deposition (EPD) of diamond particles onto graphite substrates followed by chemical vapor deposition (CVD) of SiC. Various concentrations of MgCl₂ were employed to increase the deposition rate and uniformity of the deposits during the EPD process by giving a positive charge to diamond particles. The CVD of SiC was found to have a tightly connected diamond‐graphite interface and spherical texture. With higher weight fraction of diamond particles deposits, the wear of steel ball increased, while the wear of SiC coating decreased.     

Conductive, Polypyrrole Coating on Mullite/Alumina Fibers for Electrophoretic Deposition of Oxide Matrices

Mullite/alumina fibers (Nextel™ 720) have been rendered conductive for electrophoretic deposition (EPD) by coating with polypyrrole (Ppy) from an aqueous solution of pyrrole (Py). The polymer coating was characterized by thermogravimetric (TG) analysis, scanning electron microscopy (SEM), and conductivity measurements. The Ppy coating thickness is ∼0.1 μm and the fiber resistance 1–2 (kΩ/cm)/fiber tow. A maximum conductivity of ∼48 S/cm was achieved from a 0.005 M pyrrole solution. A Nextel 720/Al₂O₃ composite was synthesized using Ppy-coated fibers as the cathode in an EPD cell. The green and sintered microstructures of the resultant composites are reported.     

Development and characterisation of high-density oxide fibre-reinforced oxide ceramic matrix composites with improved mechanical properties

A low cost and reliable ceramic matrix composite fabrication route has been developed. It involves the coating of 2D woven ceramic fibres (Nextel? 720) with oxide nano-size ceramic particles by electrophoretic deposition (EPD) followed by impregnation of the coated fibres with ceramic matrix and warm pressing at 180 °C to produce the “green” component ready for pressureless sintering. The effects of two different weak interface materials, NdPO₄ and ZrO₂, on the thermomechanical properties of the composites are also examined. Damage mechanisms, such as debonding, fibre fracture, delamination and matrix cracking within the composite plates subjected to tensile loading are analysed using acoustic emission technique and correlated with microstructure. It is shown that the composites with NdPO₄ interface, 10% porosity and 40 vol.% fibre loading have superior themomechanical properties in terms of strength and damage-tolerant behaviour in multilayer plate form. The improved sinterability and microstructure stability at moderate temperatures ensure both the fibre integrity and load transfer efficiency resulting in high strength damage-tolerant composites. The final components produced are considered to be suitable for use as shroud seals and insulating plates for combustor chambers in aircraft engines.     

High dispersion and electrochemical capacitive performance of NiO on benzenesulfonic functionalized carbon nanotubes

This work describes an effective method to synthesize structurally uniform composite of nickel oxide/benzenesulfonic functionalized multiwalled carbon nanotubes composite (NiO/f-MWCNTs) using benzenesulfonic MWCNTs as the substrate. Benzenesulfonic group here is bifunctional both for solubilizing MWCNTs into aqueous solution and for tethering Ni²⁺ precursor onto MWCNTs surfaces to facilitate the follow-up chemical deposition of NiO by supplying surface binding and anchoring groups. The composite has a uniform surface dispersion and large coverage of NiO onto f-MWCNTs, which is characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscope, cyclic voltammetry and galvanostatic charge/discharge measurements. The NiO/f-MWCNTs composite improved the utilization of electrochemical capacitive materials and delivered capacity of 384 F/g at the constant current of 0.20 A/g due to f-MWCNTs as substrate.     

Study of interphase in glass fiber–reinforced poly(butylene terephthalate) composites

It is well known that application of a coupling agent to a glass fiber surface will improve fiber/matrix adhesion in composites. However, on commercial glass fibers the coupling agent forms only a small fraction of the coating, the larger part being a mixture of processing aids whose contribution to composite properties is not well defined. The interfacial region of the composite will therefore be affected by the coating composition but also by the chemical reactions involved in the vicinity of the fiber and inside the surrounding matrix. The main feature of this study consists in dividing the interface region into two separate regions: the fiber/sizing interphase and the sizing/matrix interphase. A wide range of techniques was used, including mechanical and thermomechanical tests, infrared spectroscopy, gel permeation chromatography, carboxyl end group titrations, extraction rate measurements, and viscosity analysis. Experiments were performed on poly(butylene terephthalate) composites and results indicate that the adhesion improvement is due to the presence of a short chain coupling agent and of a polyfunctional additive, which may react both with the coupling agent and the matrix. According to the nature of this additive, it may be possible to soften the interphase and then to increase the composite impact strength.     

Electrophoretic deposition of carbon nanotubes onto carbon-fiber fabric for production of carbon/epoxy composites with improved mechanical properties

Carbon nanotubes (CNTs) have been deposited onto carbon-fiber fabric using electrophoretic deposition (EPD) prior to the infusion of epoxy resin for the production of carbon/epoxy composites. The carbon-fiber fabric employed for EPD was used in the as-received condition, in which the proprietary epoxy sizing-agent was present. CNTs were functionalized prior to EPD using ozone treatment for oxidation, followed by chemical reaction with polyethyleneimine. The CNT oxidation used a novel recirculating system which enabled ozonolysis to be conducted on large-volume solutions of CNTs in the presence of high-powered sonication, facilitating preparation of stable dispersions suitable for EPD. Significant increases in the shear strength and fracture toughness of the carbon/epoxy composites with the CNT treatment have been measured relative to composites without the CNT treatment. Analysis of fracture surfaces revealed interlaminar regions with high levels of CNTs and evidence of good adhesion between the carbon nanotubes and sized carbon-fiber, which is believed to have contributed to the measured improvement in mechanical properties.