Thermo-physical properties and TEM analysis of silver based MMCs utilizing metallized multiwall-carbon nanotubes

Metal matrix composites with embedded multiwall-carbon nanotubes (MWNT) are attractive because MWNTs exhibit high intrinsic thermal conductivity. Thus to improve the thermal conductivity of a metal matrix, silver matrix composites with MWNT were prepared by “chemical” mixing, different active elements were introduced enhancing the bonding between inclusions and matrix. The evolution of the thermal conductivity and the coefficient of thermal expansion CTE as a function of the MWNT concentration and the presence of active elements cobalt, molybdenum or nickel in the silver matrix in Ag–X/MWNT composites are presented. A transition from weak to strong matrix/MWNT bonding is observed by adding active elements, the latter leading concomitantly to an increase in thermal conductivity and a decrease in CTE. The thermal conductivity was found to increase by up to 10% for a composition of 0.2 wt.% MWNT and cobalt as active element and a 6% decrease in CTE compared to a pure silver reference.     

Thermal expansion behaviors of aluminum composite reinforced with carbon nanotubes

The coefficient of thermal expansion (CTE) of aluminum matrix composite reinforced with 1.0wt.% multi-wall carbon nanotubes (MWNTs) fabricated by cold isostatic pressing and hot squeeze technique was measured between 25 and 400 °C with a high-precision thermomechanical analyzer, and compared with those of pure aluminum and 2024Al matrix fabricated under the same processing. The results show that the CTE of the composite obviously reduces in relation to those of pure aluminum and 2024Al matrix due to the introduction of MWNTs. The addition of 1.0wt.% MWNTs to 2024Al matrix decreases the CTE by as much as 12% and 11% compared with those of pure aluminum and 2024Al matrix at 50 °C, respectively, which indicates that carbon nanotube reinforced metal matrix composite may be a promising materials with low CTE.     

Effect of filler geometry on coefficient of thermal expansion in carbon nanofiber reinforced epoxy composites

This study involves the investigation of the geometry effect of nano-fillers on thermally induced dimensional stability of epoxy composites by experimentally evaluating the linear coefficient of thermal expansion (CTE). Carbon nanofibers (CNF) were chosen as the filler in epoxy matrix to investigate the effect of an aspect ratio on the CTE of the nanocomposites at three different volume fractions of 0.5, 1, and 2% of the nano-filler. The composites were fabricated using a mechanical mixing method. The CTE values were evaluated by measuring thermal strains of the composites and also compared with a micromechanics model. It was observed that the composites with short CNF (average L/d = 10) show better thermal stability than one of the composites with long CNF (average L/d = 70), and the thermal stability of the composites was proportional to the volume fraction of the filler in each composite. In addition, the CTE of mutliwalled carbon nanotubes (MWNT) reinforced epoxy composites was evaluated and compared with the CTE of the CNF reinforced composites. Interestingly, the MWNT reinforced composites show the greatest thermal stability with an 11.5% reduction in the CTE over the pure epoxy. The experimental data was compared with micromechanics model.     

Study on the thermal expansion properties of C/C composites

Two different woven (2D and 3D) carbon/carbon composites (C/C) and a block carbon have been prepared by chemical vapor infiltration (CVI). The effects of the density and porosity of composites, preform architectures and heat treatment on the thermal expansion properties of the C/C composites were investigated. It is revealed that the coefficient of thermal expansion (CTE) of C/C composites is negative below 100 °C, and the CTE values are inversely proportion to its porosity. Comparing with 2D C/C composites, 3D C/C composites have a better thermal stability. Heat treatment can increase the thermal stability of composites by changing interfacial thermal stress. The thermal expansion behavior of C/C composites is considered as the result of interaction between fibers and matrix.     

Thermische Ausdehnung,innere Spannungen und Porenverteilung in AlSiCp Metallmatrix‐ verbundwerkstoffen

Thermal expansion, internal stresses and porosity distribution in AlSiCp MMC AlSi7Mg/SiC/70p (AlSiC) is used for heat sinks because of its good thermal conductivity combined with a low coefficient of thermal expansion (CTE). These properties are important for power electronic devices where heat sinks have to provide efficient heat transfer to a cooling device. A low CTE is essential for a good surface bonding of the heat sink material to the isolating ceramics. Otherwise mismatch in thermal expansion would lead to damage of the bonding degrading the thermal contact within the electronic package. Therefore AlSiC replaces increasingly copper heat sinks. The CTE mismatch between isolation and a conventional metallic heat sink is transferred into the metal matrix composite (MMC). The stability of the external and internal interface bonding is essential for the heat sink function of AlSiC. In situ thermal cycling (RT – 400 °C) measurements of an AlSi7Mg/SiC/70p MMC are reported yielding the pore volume fraction and internal stresses between the matrix and the reinforcements in function of temperature. The changes in pore volume fractions are determined by synchrotron tomography and residual stresses by synchrotron diffraction at ESRF‐ID15A. The measurements show a relationship between thermal expansion, residual stresses and pore formation in the MMC. The results obtained from the in situ measurements reveal a thermo elastic range with inversion of the dominant tensile stresses in the matrix into compressive up to 200 °C followed by plastic matrix deformation reducing the volume of pores during heating. A reverse process takes place during cooling from 500 °C starting with elastic matrix strains converting into tensile stresses increasing the pore volume fraction again. Below 200 °C, the CTE behaves again according to thermo elastic calculations. Damage like in low cycle fatigue could be observed after multiple extreme cooling‐heating cycles between –100 °C and +400 °C, which increase the volume fraction and the size of the voids.     

Thermal expansion of cross-ply and woven carbon fibre–copper matrix composites

This paper presents thermal expansion data for cross-ply and woven copper matrix–carbon fibre composites (Cu–C_f MMCs) that were prepared by diffusion bonding. Thermal expansion was measured in two perpendicular in-plane directions of plate samples. For cross-ply samples (57 vol.%fibres) the mean coefficient of thermal expansion (CTE) between −20 and 300°C changed from approximately 6.5×10⁻⁶/°C to 3.5×10⁻⁶/°C during heating/cooling. The in-plane CTE increases with decreasing fibre content. Composites with woven arrangement of carbon fibres show a slightly higher CTE at elevated temperature.     

The effect of phase transformation on the thermal expansion property in Al/ZrW2O8 composites

This article studied the effect of phase transformation on the thermal expansion property in Al/ZrW₂O₈ composites. The Al/ZrW₂O₈ composites of low-thermal expansion were fabricated by a squeeze casting method. The coefficient of thermal expansion (CTE) of as-made composites was discovered sharply increased at around 130 °C. The X-ray diffraction (XRD) spectra showed the existence of high-pressure γ-phase in the as-made composites. This high-pressure γ-phase was considered to be induced by the compressive residual stress originated from the thermal mismatch between Al matrix and ZrW₂O₈ particles. The in situ high-temperature XRD and the differential scanning calorimetry technique were used to study this thermally expanded abruption phenomenon. It was found that the phase transformation from high-pressure γ-phase to the low-pressure phases (α/β phase) in the composites should be responsible for fluctuation in the CTE of composites. Furthermore, using a proper heat treatment to eliminate the high-pressure phase in the composite, the Al/ZrW₂O₈ composites of low and uniform CTE (from 20 to 200 °C) could be achieved. And when temperature increased again, the thermal mismatch stresses between the metal matrix and ceramic particles in the composite were not large enough to re-induce the α-γ transformation.     

Thermal expansion responses of pressure infiltrated SiC/Al metal-matrix composites

Aluminium-matrix composites containing thermally oxidized and unoxidized SiC particles featuring four average particle diameters ranging from 3 to 40 μm were produced by vacuum assisted high pressure infiltration. Their thermal expansion coefficient (CTE) was measured between 25 and 500°C. Oxidation of the SiC particles in air produces the formation at their surface of silicon oxide in quantities sufficient to bond the particles together, and confer strength to preforms. After infiltration with pure aluminium, the composites produced showed no sign of significant interfacial reaction. The CTE of the composite reinforced with unoxidized SiC particles featured an abrupt upward deviation upon heat-up near 200°C, and a second abrupt decrease near 400°C. The first transition is attributed to an inversion of stress across particle contact points. When composites are produced with oxidized SiC particles, these two transitions were removed, their CTE varying smoothly and gradually from the lower elastic bound to the upper elastic bound as temperature increases. With both composite types, the CTE decreased as the average particle size decreased. This work illustrates the benefits of three-dimensional reinforcement continuity for the production of low-CTE metal matrix composites, and shows a simple method for producing such composites. This revised version was published online in November 2006 with corrections to the Cover Date.     

高温处理对3D C/SiC复合材料热膨胀性能的影响

研究了不同高温处理前后3D C/SiC复合材料热膨胀系数(CTE)的变化规律,从材料内部热应力变化及结构改变的角度定性地分析了其变化机理。研究发现,3D C/SiC复合材料的热膨胀系数受界面热应力的影响,其变化规律是纤维和基体相互限制、相互竞争的结果;高温处理可提高材料的热稳定性,并通过改变界面热应力及材料内部结构,来影响材料热膨胀系数的变化规律;通过增加基体裂纹来降低复合材料的低温热膨胀,但不影响其变化规律;通过改变材料内部结构,使热应力发生变化并重新分布,对复合材料的高温热膨胀产生显著影响。但高温处理没有改变3D C/SiC复合材料的基体裂纹愈合温度(900℃)。      

Microstructure and thermal expansion behavior of spray-formed Al–27Si alloy used for electronic packaging

The hypereutectic Al–27Si (mass fraction) alloys are prepared by spray deposition and extrusion. The effect of thermal aging process on the coefficient of thermal expansion (CTE) and microstructure of the Al–27Si alloys are investigated. The results show that the distribution of Si particles in α-Al matrix is uniform, and the primary Si phase grows gradually during the process of thermal aging. The CTE between room temperature to 100 °C increases gradually with the ascending of aging temperature, attributed to the relaxation of residual thermal stress and the coarsening of primary Si phases in the alloys. On the other hand, the CTE increases linearly as the cycling temperature increases up to 500 °C, and the measured values are in good agreement with the Kerner model.     

Comparison of Structure and Conductivity of Multiwall Carbon Nanotubes Obtained over Ni and Ni/Fe Catalysts

Abstract

Multiwall carbon nanotubes (MWNT) were produced by pyrolysis of acetonitrile (CH₃CN) on metallic particles of Ni and Ni/Fe at 850°C. The special program for statistical treatment of electron micrograph images was developed. Research of diameter distribution of MWNT grown over different catalysts was carried out. Two kinds of carbon nanotubes with different diameter and microstructure are formed on Ni catalyst. The MWNT with smaller diameter and cylindrical packing of layers were found to have the higher conductivity.     

The effect of microstructure on thermal expansion coefficients in powder-processed Al2Mo3O12

Orthorhombic Al₂Mo₃O₁₂ was investigated as a model anisotropic phase to understand the influence of powder preparation routes and bulk microstructure (mean grain size) on the bulk coefficient of thermal expansion (CTE) and to compare it to the intrinsic CTE of powder samples. A co-precipitation route was used for the synthesis of pure single-phase nanopowders, while a polyvinyl alcohol-assisted sol–gel method was utilized for the synthesis of micron-sized powders. Sintered samples prepared from both powders exhibited different microstructures in terms of mean crystal sizes and porosity. Bulk samples obtained from nanopowders were highly porous and contained crystals of approximately 100-nm diameter, while the bulk pieces produced from the micron-sized powders were denser, contained crystals larger than 5 μm, and showed occasional intergranular and transgranular microcracks. Such different microstructures hugely impact the bulk CTE: the nanometric sample possesses a bulk CTE (0.9 × 10^?6 °C^?1, from 200 to 700 °C) closer to the instrinsic CTE (2.4 × 10^?6 °C^?1) than for the micrometric sample, which showed a negative CTE (?2.2 × 10^?6 °C^?1) from 200 to 620 °C, and an even more negative CTE above 620 °C (?35 × 10^?6 °C^?1). A finite element analysis showed that the local maximum thermal tensile stresses could be as high as 220 MPa when simulating a temperature drop of 700 °C as an example of thermal treatment following sintering. This tensile stress is expected to exceed the tensile strength of Al₂Mo₃O₁₂, explaining the origin of microcracks in bulk samples prepared from the micron-sized powders. The thermal behavior of the microcracks leads to differences between the intrinsic and bulk thermal expansion; we show experimentally that such differences can be reduced by nanostructuring.     

Thermal stability and thermal expansion behavior of FeCoCrNi2Al high entropy alloy

Present work reports the thermal stability and thermal expansion behavior of dual-phase FeCoCrNi₂Al HEA prepared by Mechanical Activated Synthesis and consolidated by hot pressing. The thermal stability of the phases present in FeCoCrNi₂Al HEA has been extensively studied using in-situ high-temperature X-ray diffraction (HT-XRD) in conjunction with dilatometry and differential scanning calorimetry (DSC). The DSC thermogram shows a single endothermic peak at 1430 °C (1703 K) which belongs to the melting point of the alloy. HT-XRD and dilatometry experiments were carried out from room temperature to 1000 °C (1273 K). HT-XRD study has shown that the room temperature FCC + BCC (face-centred cubic + body-centred cubic) phases remains stable up to 1000 °C (1273 K). Although the amount of BCC phase has increased above 800 °C (1073 K), no additional phase formation was observed in HT-XRD. The coefficient of thermal expansion (CTE) curve shows linear increment up to 1000 °C (1273 K) with a slight change in slope beyond 800 °C (1073 K). Theoretical CTE was computed using the lattice parameter of the FCC phase, obtained from HT-XRD, as a function of temperature and compared with experimental CTE. Third-order polynomial equation was fitted to the experimental CTE data and the constants were evaluated which can be used to predict the coefficient of thermal expansion of the alloy.     

On CTE of SPS consolidated SiCp/Al composites with various particle size distributions

Abstract

The coefficient of thermal expansion (CTE) of spark plasma sintering consolidated SiC_p/Al composites with various size distributions was investigated with the combination of experimental measurements and modelling analyses. The CTE of the composites decreased with increasing particle volume fraction, and large particles played a major role in the decline of CTE. The measured CTE lay between the predictions of Kerner model and Schapery lower bound, but the possible formation of percolating particle network and the influence of matrix plasticisation led to the slight deviation of the experimental values from model predictions. A CTE peak appeared for all the composites with increasing temperature to about 250–300°C due to the action of matrix plasticisation filling the microvoids in the composites. The composites with mixed particles of substantially different sizes were prone to concentrate thermal stresses on large particles, which induced an early appearance of matrix plastic deformation that can result in a comparably low CTE peak temperature.     

Low-temperature sintered pollucite ceramic from geopolymer precursor using synthetic metakaolin

In this article, pollucite ceramic with high relative density and low coefficient of thermal expansion (CTE) was prepared from Cs-based geopolymer using synthetic metakaolin. Crystallization and sintering behavior of the Cs-based geopolymer together with thermal expansion behavior of the resulted pollucite ceramic were investigated. On heating at 1200 °C for 2 h, the amorphous Cs-based geopolymer completely crystallized into pollucite based on crystal nucleation and growth mechanism. Selected area diffraction analysis and XRD results confirmed the resulted pollucite ceramic at room temperature was pseudo-cubic phase with superlattice structure. Compared with Cs-based geopolymer using natural metakaolin, geopolymer using synthetic metakaolin in this article showed a much lower viscous sintering temperature range, which started at 800 °C, reached a maximum value of ?7.47 × 10^?4/°C at 1121.9 °C, and ended at 1200 °C. Cesium volatilization appeared only when temperature was above 1250 °C. Therefore, densified pollucite ceramic can be prepared from Cs-based geopolymer using synthetic metakaolin without cesium volatilization. Abnormal thermal shrinkage of pollucite ceramic was observed at temperature range from 25.3 to 54.6 °C because of pseudo-cubic to cubic phase transition, and its average CTE was 2.8 × 10^?6/°C from 25 to 1200 °C.     

Effect of ZnO coating of whiskers on thermal expansion properties of aluminium borate whisker reinforced aluminium composites

Abstract

The pure aluminium composites reinforced by ZnO coated aluminium borate whiskers were fabricated by squeeze casting. The microstructure of the composite was observed using an optical microscope and the thermal expansion behaviours of the composites were investigated in the range from 50 to 400°C. In addition, the effects of heat treatment and thermal cycling on the thermal expansion behaviours of the composite were also investigated. The results show that the coefficient of thermal expansion of as cast composites decreases with the ZnO coating content increasing. However, heat treatment time and thermal cycling lead to an increase in the CTE of the composite.     

Thermal expansion behaviour of barium and strontium zirconium phosphates

Ba_1.5-xSr_xZr₄P₅SiO₂₄ compounds withx = 0, 0.25, 0.5, 0.75, 1.0, 1.25 and 1.5, belonging to the low thermal expansion NZP family were synthesized by the solid state reaction method. The XRD pattern could be completely indexed with respect to space group indicating the ordering of vacancy at the divalent cation octahedral sites. The microstructure and bulk thermal expansion coefficient from room temperature to 800°C of the sintered samples have been studied. All the samples show very low coefficient of thermal expansion (CTE), withx = 0 samples showing negative expansion. A small substitution of strontium in the pure barium compound changes the sign of CTE. Similarly,x = 1.5 sample (pure strontium) shows a positive CTE and a small substitution of barium changes its sign.X = 1.0 and 1.25 samples have almost constant CTE over the entire temperature range. The low thermal expansion of these samples can be attributed to the ordering of the ions in the crystal structure of these materials     

碳纳米管的表面改性对环氧树脂低温(77 K)冲击性能及热膨胀系数的影响

采用混酸氧化及表面接枝改性的方法制备了表面含不同官能团的多壁碳纳米管(MWCNTs), 并研究了不同MWCNTs对环氧树脂的低温(77 K)抗冲击性能及热膨胀系数(CTE)的影响。结果表明: 通过接枝反应将—NCO基团封端的PEO齐聚物引入MWCNTs表面, 可提高MWCNTs在环氧树脂基体中的分散性, 加强MWCNTs与环氧树脂的界面作用; 相对于纯环氧树脂, 添加质量分数为0.5%的纯MWCNTs、 氧化MWCNTs和表面接枝MWCNTs改性后的环氧树脂的低温冲击强度分别升高了10.27%、 26.13%和32.95%, 而CTE则分别降低了14.79%、 29.59%和40.29%。这表明表面接枝改性MWCNTs可明显提高环氧树脂基体的低温抗冲击性能并降低环氧树脂在玻璃化转变温度下的CTE。     

Effect of sintering temperatures on properties of BaO–B<Subscript>2</Subscript>O<Subscript>3</Subscript>–SiO<Subscript>2</Subscript>–Al<Subscript>2</Subscript>O<Subscript>3</Subscript> glass/silica composites for CBGA package

BaO–B₂O₃–SiO₂–Al₂O₃ (BBSA) glass/silica composites synthesized by solid-state reaction method were developed for CBGA packages, and the effects of sintering temperature (900–950 °C) on the phase transformation, microstructure, thermal, mechanical and electrical properties were investigated. XRD results show that the major phases quartz and cristobalite, and the minor phase BaSi₂O₅ are detected in BBSA composites. Furthermore, it was found that the quartz phase transforms to cristobalite phase at 930–940 °C. The formation of cristobalite phase with higher coefficient of thermal expansion (CTE) led to the increase of CTE value of BBSA composites. However, excessive cristobalite phase content would degrade the mechanical properties and the linearity of thermal expansion of the ceramics. BBSA composites sintered at 920 °C exhibited excellent properties: low dielectric constant and loss (ε_r = 6.2, tanδ = 10^?4 at 1 MHz), high bending strength (179 MPa), high CTE (12.19 ppm/°C) as well as superior linearity of the thermal expansion.     

3D C/C复合材料的热膨胀性能

通过测定热膨胀系数(CTE),分析了不同密度以及高温处理前后热解炭基三维编织炭/炭复合材料(3DC/C复合材料)的热膨胀行为,并与PAN基炭纤维以及热解炭的热膨胀性能作了比较。结果表明:PAN基炭纤维在1200℃以后,出现明显的负膨胀。从室温到100℃,C/C复合材料呈负膨胀状态,CTE与密度成正比;从100℃到1000℃,C/C复合材料的CTE-温度曲线基本遵循热解炭基体的热膨胀规律变化;超过1000℃以后,CTE-温度曲线出现峰值,表明热解炭的膨胀受纤维的限制。复合材料的热膨胀行为由纤维和基体二者决定。