Optimization of the chemical vapor deposition process for fabrication of carbon nanotube/Al composite powders

In order to optimize the chemical vapor deposition process for fabrication of carbon nanotube/Al composite powders, the effect of different reaction conditions (such as reaction temperature, reaction time, and reaction gas ratio) on the morphological and structural development of the powder and dispersion of CNTs in Al powder was investigated using transmission electron microscope. The results showed that low temperatures (500-550 °C) give rise to herringbone-type carbon nanofibers and high temperatures (600-630 °C) lead to multi-walled CNTs. Long reaction times broaden the CNT size distribution and increase the CNT yield. Appropriate nitrogen flow is preferred for CNT growth, but high and low nitrogen flow result in carbon nanospheres and CNTs with coarse surfaces, respectively. Above results show that appropriate parameters are effective in dispersing the nanotubes in the Al powder which simultaneously protects the nanotubes from damage.     

Elevated temperature tensile properties and thermal expansion of CNT/2009Al composites

1.5 vol.% and 4.5 vol.% carbon nanotubes reinforced 2009Al (CNT/2009Al) composites with homogeneously dispersed CNTs and refined matrix grains, were fabricated using powder metallurgy (PM) followed by 4-pass friction stir processing (FSP). Tensile properties of the composites between 293 and 573 K and the coefficient of thermal expansion (CTE) from 293 to 473 K were tested. It was indicated that load transfer mechanism still takes effect at temperatures elevated up to 573 K, thus the yield strength of the 1.5 vol.% CNT/2009Al composite at 423–573 K, was enhanced compared with the 2009Al matrix. However, for the 4.5 vol.% CNT/2009Al composite, the yield strength at 573 K was even lower than that for the matrix, due to the quicker softening of ultrafine-grained matrix. Compared with the 2009Al matrix, the CTEs of the composites were greatly reduced for the zero thermal expansion and high modulus of the CNTs and could be well predicted by the Schapery’s model.     

Effect of carbon nanotube (CNT) content on the mechanical properties of CNT-reinforced aluminium composites

The interest in carbon nanotubes (CNTs) as reinforcements for aluminium (Al) has been growing considerably. Efforts have been largely focused on investigating their contribution to the enhancement of the mechanical performance of the composites. The uniform dispersion of CNTs in the Al matrix has been identified as being critical to the pursuit of enhanced properties. Ball milling as a mechanical dispersion technique has proved its potential. In this work, we use ball milling to disperse up to 5 wt.% CNT in an Al matrix. The effect of CNT content on the mechanical properties of the composites was investigated. Cold compaction and hot extrusion were used to consolidate the ball-milled Al–CNT mixtures. Enhancements of up to 50% in tensile strength and 23% in stiffness compared to pure aluminium were observed. Some carbide formation was observed in the composite containing 5 wt.% CNT. In spite of the observed overall reinforcing effect, the large aspect ratio CNTs used in the present study were difficult to disperse at CNT wt.% greater than 2, and thus the expected improvements in mechanical properties with increase in CNT weight content were not fully realized.     

Fabrication and effective thermal conductivity of multi-walled carbon nanotubes reinforced Cu matrix composites for heat sink applications

A novel particles-compositing method was used for the first time to disperse different contents of multi-walled carbon nanotubes (CNTs) in micron sized copper powders, which were subsequently consolidated into CNT/Cu composites by spark plasma sintering (SPS). Microstructural observations showed that the homogeneous distribution of CNTs and dense composites could be obtained for 0–10 vol.% CNT contents. The CNT clusters were appeared in the powder mixture with 15 vol.% CNTs, which resulted in an insufficient densification of the composites. The effective thermal conductivity of the composites was analyzed both theoretically and experimentally. The addition of CNTs showed no enhancement in overall thermal conductivity of the composites due to the interface thermal resistance associated with the low phase contrast of CNT to copper and the random tube orientation. Besides, the composite containing 15 vol.% CNTs led to a rather low thermal conductivity due possiblely to the combined effect of unfavorable factors induced by the presence of CNT clusters, i.e. large porosity, lower effective conductivity of CNT clusters themselves and reduction of SPS cleaning effect. The CNT/Cu composites may be a promising thermal management material for heat sink applications.     

Mechanical characterization of copper coated carbon nanotubes reinforced aluminum matrix composites

In this investigation, carbon nanotube (CNT) reinforced aluminum composites were prepared by the molecular-level mixing process using copper coated CNTs. The mixing of CNTs was accomplished by ultrasonic mixing and ball milling. Electroless Cu-coated CNTs were used to enhance the interfacial bonding between CNTs and aluminum. Scanning electron microscope analysis revealed the homogenous dispersion of Cu-coated CNTs in the composite samples compared with the uncoated CNTs. The samples were pressureless sintered under vacuum followed by hot rolling to promote the uniform microstructure and dispersion of CNTs. In 1.0 wt.% uncoated and Cu-coated CNT/Al composites, compared to pure Al, the microhardness increased by 44% and 103%, respectively. As compared to the pure Al, for 1.0 wt.% uncoated CNT/Al composite, increase in yield strength and ultimate tensile strength was estimated about 58% and 62%, respectively. However, in case of 1.0 wt.% Cu-coated CNT/Al composite, yield strength and ultimate tensile strength were increased significantly about 121% and 107%, respectively.     

Morphology and thermal conductivity of polyacrylate composites containing aluminum/multi-walled carbon nanotubes

Polyacrylate composites with various fillers such as multi-walled carbon nanotube (CNT), aluminum flake (Al-flake), aluminum powders and Al–CNT were prepared by a ball milling. The thermal decomposition temperature increased by as much as 64 °C for polyacrylate/Al-flake 70 wt% composite compared to polyacrylate. The thermal conductivity of polyacrylate/Al–CNT composites increased from 0.50 to 1.67 W/m K as the Al–CNT content increases from 50 to 80 wt%. The thermal conductivity of the composite sheet increases with the sheet thickness. At the given filler concentration (90 wt%), the composite filled with aluminum powder of 13 μm has a higher thermal conductivity than the one filled 3 μm powder, and the composite filled with mixture of two powders showed a synergistic effect on the thermal conductivity. The morphology indicates that the dispersion of CNT in the polyacrylate/Al-flake + CNT composite is not perfect, and agglomeration of CNTs was observed.     

球磨工艺对原位合成碳纳米管增强铝基复合材料微观组织和力学性能的影响

将原位化学气相沉积法合成的碳纳米管(CNTs)与铝的复合粉末进行球磨混合,进而粉末冶金制备CNTs/Al复合材料,研究球磨工艺对复合材料的微观组织和力学性能的影响。结果表明:球磨过程中不添加过程控制剂所得到的复合材料力学性能优异;随着球磨时间的增加,CNTs逐步分散嵌入铝基体内部,复合材料的组织也变得更加致密均匀。CNTs/Al复合材料的硬度和抗拉强度均随球磨时间的延长持续增加,但是伸长率先增后减。经90min球磨的CNTs/Al复合材料展现了强韧兼备的特点,其硬度和抗拉强度较原始纯铝提高了1.4倍和1.7倍,并且具有17.9%的高伸长率。     

Enhancing tensile and compressive strength of magnesium using ball milled Al+CNT reinforcement

In this work, Mg/Al–CNT nano-composites were fabricated using powder metallurgy route involving microwave assisted rapid sintering and hot extrusion. Ball milled Al–CNT particles comprising different contents of CNTs coated with fixed amount of Al were used for strengthening. Microstructural characterization of these Mg/Al–CNT nano-composites reveal reasonably uniform distribution of Al–CNT particles up to CNT content of 0.30% by weight, significant grain refinement and the presence of minimal porosity compared to monolithic Mg. Importantly, for the nominally identical processing conditions, the textures of as-extruded nano-composite specimens is significantly influenced by the presence of Al–CNT particles. Nano-composite configurations exhibit different tensile and compressive response as a function of CNT content. Among the different Mg/Al–CNT formulations synthesized, the Mg/Al–CNT configuration with Al–CNT particles composition of 1.00% Al and 0.30% CNT by weight (Mg/1.00Al–0.30CNT) exhibit higher tensile yield strength (0.2% YS), ultimate tensile strength (UTS) and failure strain (FS) (up to +72%, +48%, +9%, respectively) compared to monolithic Mg.     

Nanoscale structure and local mechanical properties of fiber-reinforced composites containing MWCNT-grafted hybrid glass fibers

Carbon nanotubes (CNTs) were grown from the surface of glass fibers by chemical vapor deposition, and these hybrid fibers were individually dispersed in an epoxy matrix to investigate the local composite structure and properties near the fiber surface. High-resolution transmission electron microscopy revealed the influence of infiltration and curing of a liquid epoxy precursor on the morphology of the CNT “forest” region, or region of high CNT density near the fiber surface. Subsequent image analysis highlighted the importance of spatially dependent volume fractions of CNTs in the matrix as a function of distance from the fiber surface, and nanoindentation was used to probe local mechanical properties in the CNT forest region, showing strong correlations between local stiffness and volume fraction. This work represents the first in situ measurements of local mechanical properties of the nano-structured matrix region in hybrid fiber-reinforced composites, providing a means of quantifying the reinforcement provided by the grafted nanofillers.     

Reinforcing brittle and ductile epoxy matrices using carbon nanotubes masterbatch

In this study, the mechanical and thermal properties of epoxy composites using two different forms of carbon nanotubes (powder and masterbatch) were investigated. Composites were prepared by loading the surface-modified CNT powder and/or CNT masterbatch into either ductile or brittle epoxy matrices. The results show that 3 wt.% CNT masterbatch enhances Young’s modulus by 20%, tensile strength by 30%, flexural strength by 15%, and 21.1 °C increment in the glass transition temperature (by 34%) of ductile epoxy matrix. From scanning electron microscopy images, it was observed that the CNT masterbatch was uniformly distributed indicating the pre-dispersed CNTs in the masterbatch allow an easier path for preparation of CNT-epoxy composites with reduced agglomeration of CNTs. These results demonstrate a good CNT dispersion and ductility of epoxy matrix play a key role to achieve high performance CNT-epoxy composites.     

Structural characterization of a mechanically milled carbon nanotube/aluminum mixture

The structural evolution of carbon nanotubes (CNTs) during mechanical milling was investigated using SEM, TEM, XRD, XPS and Raman spectroscopy. The study showed that milling of the CNTs alone introduces defects but preserves the tubular structure. When milling the CNTs with aluminum (Al) powder in order to produce a composite, Raman spectroscopy has shown that most of the nanotubes are destroyed. During sintering of the CNT/Al milled mixture, the carbon atoms available from the destruction of the nanotubes react with the Al to form aluminum carbide (Al₄C₃). The effect of milling on the Al matrix was also studied.     

Role of powder treatment and carbon nanotube dispersion in the fracture toughening of plasma-sprayed aluminum oxide-carbon nanotube nanocomposite

Al2O3 ceramic reinforced with 4-wt% multiwalled carbon nanotube (CNT) is plasma sprayed for improving the fracture toughness of the nanocomposite coating. Two different methodologies of CNT addition have been adopted in the powder feedstock to assist CNT dispersion in the nano-Al2O3 matrix. First, spray-dried nano-Al2O3 agglomerates are blended with 4 wt% CNT as powder-feedstock, which is subsequently plasma sprayed resulting in the fracture toughness improvement of 19.9%. Secondly, spray dried composite nano-Al2O3 and 4 wt% CNT powder was used as feedstock for attaining improved dispersion of CNTs. Plasma sprayed coating of composite spray dried powder resulted in increase of 42.9% in the fracture toughness. Coating synthesized from the blended powder displayed impact alignment of CNTs along splat interface, and CNTs chain loop structure anchoring the fused Al2O3 melt whereas coating synthesized from composite spray dried powder evinced anchoring of CNTs in the solid state sintered region and CNT mesh formation. Enhanced fracture toughness is attributed to significance of CNT dispersion.     

Properties of polypropylene composites containing aluminum/multi-walled carbon nanotubes

Polypropylene/aluminum–multi-walled carbon nanotube (PP/Al–CNT) composites were prepared by a twin-screw extruder. The morphology indicates that the CNTs are well embedded or implanted within Al-flakes rather than attached on the surface. During preparation of composites, the CNTs came apart from Al–CNT so that free CNTs as well as Al–CNT were observed in PP/Al–CNT composite. The crystallization temperatures of PP/CNT and PP/Al–CNT composites were increased from 111 °C for PP to 127 °C for the composites. The decomposition temperature increased by 55 °C for PP/CNT composite and 75 °C for PP/Al–CNT composite. The PP/Al–CNT composite showed higher thermal conductivity than PP/CNT and PP/Al-flake composites with increasing filler content. PP/Al–CNT composites showed the viscosity values between PP/CNT and PP/Al-flake composites. PP/Al–CNT composite showed higher tensile modulus and lower tensile strength with increasing filler content compared to PP/CNT and PP/Al-flake composites.     

Formation and mechanical characterisation of SU8 composite films reinforced with horizontally aligned and high volume fraction CNTs

Carbon nanotube (CNT) reinforced composites have been identified as promising structural materials for the mechanical components of microelectromechanical systems (MEMS), potentially leading to advanced performance. High alignment and volume fraction of CNTs in the composites are the prerequisites to achieve such desirable mechanical characteristics. In particular, horizontal CNT alignment in composite films is necessary to enable high longitudinal moduli of the composites which is crucial for the performance of microactuators. A practical process has been developed to transfer CNT arrays from vertical to horizontal alignment which is followed by in situ wetting, realign and pressurized consolidation processes, which lead to a high CNT volume fraction in the range of 46-63%. As a result, SU8 epoxy composite films reinforced with horizontally aligned CNTs and a high volume faction of CNTs have been achieved with outstanding mechanical characteristics. The transverse modulus of the composite films has been characterised through nanoindentation and the longitudinal elastic modulus has been investigated. An experimental transverse modulus of 9.6 GPa and an inferred longitudinal modulus in the range of 460-630 GPa have been achieved, which demonstrate effective CNT reinforcement in the SU8 matrix.     

Effect of size and shape of metal particles to improve hardness and electrical properties of carbon nanotube reinforced copper and copper alloy composites

Utilizing the extra-ordinary properties of carbon nanotube (CNT) in metal matrix composite (MMC) for macroscopic applications is still a big challenge for science and technology. Very few successful attempts have been made for commercial applications due to the difficulties incorporating CNTs in metals with up-scalable processes. CNT reinforced copper and copper alloy (bronze) composites have been fabricated by well-established hot-press sintering method of powder metallurgy. The parameters of CNT–metal powder mixing and hot-press sintering have been optimized and the matrix materials of the mixed powders and composites have been evaluated. However, the effect of shape and size of metal particles as well as selection of carbon nanotubes has significant influence on the mechanical and electrical properties of the composites. The hardness of copper matrix composite has improved up to 47% compared to that of pure copper, while the electrical conductivity of bronze composite has improved up to 20% compared to that of the pure alloy. Thus carbon nanotube can improve the mechanical properties of highly-conductive low-strength copper metals, whereas in low-conductivity high-strength copper alloys the electrical conductivity can be improved.     

Effect of ball-milling time on mechanical properties of carbon nanotubes reinforced aluminum matrix composites

Carbon nanotubes reinforced pure Al (CNT/Al) composites were produced by ball-milling and powder metallurgy. Microstructure and its evolution of the mixture powders and the fabricated composites were examined and the mechanical properties of the composites were tested. It was indicated that the CNTs were gradually dispersed into the Al matrix as ball-milling time increased and achieved a uniform dispersion after 6 h ball-milling. Further increasing the ball-milling time to 8–12 h resulted in serious damage to the CNTs. The tensile tests showed that as the ball-milling time increased, the tensile and yield strengths of the composites increased, while the elongation increased first and then decreased. The strengthening of CNTs increased significantly as the ball-milling time increased to 6 h, and then decreased when further increasing the ball-milling time. The yield strength of the composite with 6 h ball-milling increased by 42.3% compared with the matrix.     

Effect of mechanical alloying time and carbon nanotube (CNT) content on the evolution of aluminum (Al)–CNT composite powders

One of the major obstacles to the effective use of carbon nanotubes as reinforcements in metal matrix composites is their agglomeration and poor distribution/dispersion within the metallic matrix. In the present work, we use mechanical alloying (MA) to mechanically mix CNT (2 and 5 wt.%) with Al powders. These powders would be used as precursors for subsequent consolidation to generate bulk CNT-Al composites. Hence controlling the initial powder characteristics prior to high temperature consolidation is important. Up to 48 h of milling was employed to investigate the effect of milling time on the particle size, morphology and CNT dispersions. The results show that particle size and morphology vary with milling time and CNT content. Also the addition of process control agents such as methanol can aid in controlling the powder characteristics.     

碳纳米管对激光选区熔化成形Al基复合材料的影响

基于激光选区熔化（SLM）方式,通过改变扫描速度,制备不同碳纳米管（CNTs,质量分数分别为0、0.5wt%、1.0wt%、1.5wt%、2.0wt%）含量的CNTs/Al复合材料试件,探究不同CNTs含量与激光扫描速度对试件性能的影响。结果表明,CNTs含量小于1.0wt%时,分散效果较好,大部分CNTs以单根状态黏附于Al粉表面;含量大于1.0wt%时,CNTs团聚尺寸增大、数量增多。相同SLM成形工艺下,低CNTs含量的CNTs/Al复合材料试件内部孔隙较少,致密度较高;高CNTs含量的CNTs/Al复合材料试件内部孔隙逐渐增多,致密度降低。激光扫描速度为1 300 mm/s工艺下,随着CNTs质量分数的增加,CNTs/Al复合材料试件硬度呈先上升后下降趋势,在CNTs含量为1.0wt%显微硬度达到最高。CNTs/Al复合材料试件平均晶粒尺寸相对于铝合金试件更加细化,在CNTs含量大于1.0wt%时,尽管晶粒依然细化,但试件致密度降低造成显微硬度下降明显。     

High-temperature properties of extruded titanium composites fabricated from carbon nanotubes coated titanium powder by spark plasma sintering and hot extrusion

Pure titanium matrix composite reinforced with carbon nanotubes (CNTs) was prepared by spark plasma sintering and hot extrusion via powder metallurgy process. Titanium (Ti) powders were coated with CNTs via a wet process using a zwitterionic surfactant solution containing 1.0, 2.0 and 3.0 wt.% of CNTs. In situ TiC formation via reaction of CNTs with titanium occurred during sintering, and TiC particles were uniformly dispersed in the matrix. As-extruded Ti/TiCs composite rods were annealed at 473 K for 3.6 ks to reduce the residual stress during processing. After annealing process, the tensile properties of the composites were evaluated at room temperature, 473, 573 and 673 K, respectively. Hardness test was also performed at room temperature up to 573 K with a step of 50 K. The mechanical properties of extruded Ti/CNTs composites at elevated temperature were remarkably improved by adding a small amount of CNTs, compared to extruded Ti matrix. These were due to the TiC dispersoids originated from CNTs effectively stabilized the microstructure of extruded Ti composites by their pinning effect. Moreover, the coarsening and growth of Ti grain never occurred even though they were annealed at 573, 673 K for 36 ks and 673 K for 360 ks, respectively.     

Synthesis,microstructure and mechanical properties of Yttria Stabilized Zirconia (3YTZP) – Multi-Walled Nanotube (MWNTs) nanocomposite by direct in-situ growth of MWNTs on Zirconia particles

In this research, Yttria Stabilized Zirconia (3YTZP) – carbon nanotube (CNT) composites are fabricated by direct in-situ growth of CNTs on the Zirconia particles, followed by densification via the Spark Plasma Sintering (SPS) technique. Scanning electron microscopy analysis of the 3YTZP-CNT powders shows uniform distribution of CNTs without the formation of agglomerates frequently seen with the traditional ex-situ mixing of CNTs in ceramic compositions. The samples were sintered to nearly 100% theoretical density and with a finer grain size microstructure. High Resolution Transmission Electron Microscopy (HRTEM) and Raman Spectroscopy confirm CNT retention in the sintered nanocomposites up to 1600 °C. The flexural strength increases from ∼260 MPa for samples without CNTs sintered at 1600 °C to ∼312 MPa for samples with ∼4 wt.% CNTs sintered at the same temperature. A corresponding increase in the indentation fracture toughness is also observed for samples with ∼4 wt.% CNTs sintered at 1600 °C as compared to samples sintered at the same temperature without CNTs.