Cure processing modeling and cure cycle simulation of epoxy-terminated poly(phenylene ether ketone). V: Estimation of temperature distribution during cure process

A numerical method to estimate temperature distribution during the cure of epoxy-terminated poly(phenylene ether ketone) (E-PEK)-based composite is suggested. The effect of the temperature distribution on the selection of cure cycle is evaluated using a suggested alternation criterion. The effect of varying heating rate and thickness on the temperature distribution, viscosity distribution and distribution of the extent of cure reaction are discussed based on the combination of the here-established temperature distribution model and the previously established curing kinetics model and chemorheological model. It is found that, for a thin composite (<=10mm) and low heating rate (<=2.5K/min), the effect of temperature distribution on cure cycle and on the processing window for pressure application can be neglected. Low heating rate is of benefit to reduce the temperature gradient. The processing window for pressure application becomes narrower with increasing thicknesses of composite sheets. The validity of the temperature distribution model and the modified processing window is evaluated through the characterization of mechanical and physical properties of E-PEK-based composite fabricated according to different temperature distribution conditions.

Cure processing modeling and cure cycle simulation of epoxy-terminated poly(phenylene ether ketone) .1. DSC characterization of curing reaction

The curing reaction process of epoxy-terminated poly(phenylene ether ketone) (E-PEK) with 4,4'-diaminodiphenyl sulfone (DDS) and hexahydrophthalic acid anhydride (Nadic) as curing agents was investigated using isothermal differential scanning calorimetry (IDSC) and nonisothermal differential scanning calorimetry (DDSC) techniques. It was found that the curing reactions of E-PEK/DDS and E-PEK/Nadic are nth-order reactions but not autoaccelerating. The experimental results revealed that the curing reaction kinetics parameters measured from IDSC and DDSC are not equivalent. This means that, in the curing reaction kinetics model for our E-PEK system, both isothermal and nonisothermal reaction kinetics parameters are needed to describe isothermal and nonisothermal curing processes, The isothermal and nonisothermal curing processes were successfully simulated using this model. A new extrapolation method was suggested. On the basis of this method the maximum extent of the curing reaction (A(ult)) that is able to reach a certain temperature can be predicted. The A(ult) for the E-PEK system estimated by the new method agrees well with the results obtained from another procedure reported in the literature. (C) 1997 John Wiley & Sons, Inc.

The effect of curing on the performance of ACF bonded chip-on-flex assemblies after thermal ageing

Purpose – Anisotropic conductive film (ACF) is now an attractive technology for direct mounting of chips onto the substrate as an alternative to lead-free solders. However, despite its various advantages over other technologies, it also has many unresolved reliability issues. For instance, the performance of ACF assembly in high temperature applications is questionable. The purpose of this paper is to study the effect of bonding temperatures on the curing of ACFs, and their mechanical and electrical performance after high temperature ageing. Design/methodology/approach – In the work presented in this paper, the curing degree of an ACF at different bonding temperatures was measured using a differential scanning calorimeter. The adhesion strength and the contact resistance of ACF bonded chip-on-flex assembly were measured before and after thermal ageing and the results were correlated with the curing degree of ACF. The ACF was an epoxy-based adhesive in which Au-Ni coated polymer particles were randomly dispersed. Findings – The results showed that higher bonding temperatures had resulted in better ACF curing and stronger adhesion. After ageing, the adhesion strength increased for the samples bonded at lower temperatures and decreased for the samples bonded at higher temperatures. ACF assemblies with higher degrees of curing showed smaller increases in contact resistance after ageing. Conduction gaps at the bump-particle and/or particle-pad interfaces were found with the help of scanning electron microscopy and are thought to be the root cause of the increase in contact resistance. Originality/value – The present study focuses on the effect of bonding temperatures on the curing of ACFs, and their adhesion strength and electrical performances after high temperature ageing. The results of this study may help the development of ACFs with higher heat resistance, so that ACFs can be considered as an alternative to lead-free solders.

Multiphysics simulation of microwave curing in micro-electronics packaging applications

Purpose – This paper aims to present an open-ended microwave curing system for microelectronics components and a numerical analysis framework for virtual testing and prototyping of the system, enabling design of physical prototypes to be optimized, expediting the development process. Design/methodology/approach – An open-ended microwave oven system able to enhance the cure process for thermosetting polymer materials utilised in microelectronics applications is presented. The system is designed to be mounted on a precision placement machine enabling curing of individual components on a circuit board. The design of the system allows the heating pattern and heating rate to be carefully controlled optimising cure rate and cure quality. A multi-physics analysis approach has been adopted to form a numerical model capable of capturing the complex coupling that exists between physical processes. Electromagnetic analysis has been performed using a Yee finite-difference time-domain scheme, while an unstructured finite volume method has been utilized to perform thermophysical analysis. The two solvers are coupled using a sampling-based cross-mapping algorithm. Findings – The numerical results obtained demonstrate that the numerical model is able to obtain solutions for distribution of temperature, rate of cure, degree of cure and thermally induced stresses within an idealised polymer load heated by the proposed microwave system. Research limitations/implications – The work is limited by the absence of experimentally derived material property data and comparative experimental results. However, the model demonstrates that the proposed microwave system would seem to be a feasible method of expediting the cure rate of polymer materials. Originality/value – The findings of this paper will help to provide an understanding of the behaviour of thermosetting polymer materials during microwave cure processing.

Microwave curing for high density package

Summary form only given. Currently the vast majority of adhesive materials in electronic products are bonded using convection heating or infra-red as well as UV-curing. These thermal processing steps can take several hours to perform, slowing throughput and contributing a significant portion of the cost of manufacturing. With the demand for lighter, faster, and smaller electronic devices, there is a need for innovative material processing techniques and control methodologies. The increasing demand for smaller and cheaper devices pose engineering challenges in designing a curing systems that minimize the time required between the curing of devices in a production line, allowing access to the components during curing for alignment and testing. Microwave radiation exhibits several favorable characteristics and over the past few years has attracted increased academic and industrial attention as an alternative solution to curing of flip-chip underfills, bumps, glob top and potting cure, structural bonding, die attach, wafer processing, opto-electronics assembly as well as RF-ID tag bonding. Microwave energy fundamentally accelerates the cure kinetics of polymer adhesives. It provides a route to focus heat into the polymer materials penetrating the substrates that typically remain transparent. Therefore microwave energy can be used to minimise the temperature increase in the surrounding materials. The short path between the energy source and the cured material ensures a rapid heating rate and an overall low thermal budget. In this keynote talk, we will review the principles of microwave curing of materials for high density packing. Emphasis will be placed on recent advances within ongoing research in the UK on the realization of "open-oven" cavities, tailored to address existing challenges. Open-ovens do not require positioning of the device into the cavity through a movable door, hence being more suitable for fully automated processing. Further potential advantages of op- - en-oven curing include the possibility for simultaneous fine placement and curing of the device into a larger assembly. These capabilities promise productivity gains by combining assembly, placement and bonding into a single processing step. Moreover, the proposed design allows for selective heating within a large substrate, which can be useful particularly when the latter includes parts sensitive to increased temperatures.

Comparison of encapsulant curing with convention and microwave systems

Comparison of the performance of a conventional convection oven system with a dual-section microwave system for curing thermosetting polymer encapsulant materials has been performed numerically. A numerical model capable of analysing both the convection and microwave cure processes has been developed and is breifly outliines. The model is used to analyse the curing of a commercially available encapsulant material using both systems. Results obtained from numerical solutions are presented, confirming that the VFM system enables the cure process to be carried out far more rapidly than with the convection oven system. This capability stems from the fundamental heating processes involved, namely that microwave processing enables the heating rate to be varied independently of the material temperature. Variations in cure times, curing rates, maximum temperatures and residual stresses between the processes are fully discussed.

Advanced microwave oven for rapid curing of encapsulant

The curing of a thermosetting polymer materials utilized on micro-electronics packaging applications can be performed using microwave systems. The use of microwave energy enables the cure process to be completed more rapidly than with alternative approaches due to the ability to heat volumetrically. Furthermore, advanced dual-section microwave systems enable curing of individual components on a chip-on-board assembly. The dielectric properties of thermosetting polymer materials, commonly used in microelectronics packaging applications, vary significantly with temperature and degree of cure. The heating rate within a material subjected to an electric field is primarily dependant on the dielectric loss properties of the material itself. This article examines the variation in dielectric properties of a commercially available encapsulant paste with frequency and temperature and the resulting influence on the cure process. The 'FAMOBS' dual section microwave system and its application to microelectronics manufacture are described. The measurement of the dielectric properties of 'Henkel EO1080' encapsulant paste uses a commercially available 'dielectric probe kit' and is described in this paper. The FAMOBS heating system is used to encapsulate a small op-amp chip. A numerical model formulated to assess the cure process in thermosetting polymer materials under microwave heating is outlined. Numerical results showing that the microwave processing systems is capable of rapidly and evenly curing thermosetting polymer materials are presented.

Role of bonding time and temperature on the physical properties of coupled anisotropic conductive–nonconductive adhesive film for flip chip on glass technology

Using thermosetting epoxy based conductive adhesive films for the flip chip interconnect possess a great deal of attractions to the electronics manufacturing industries due to the ever increasing demands for miniaturized electronic products. Adhesive manufacturers have taken many attempts over the last decade to produce a number of types of adhesives and the coupled anisotropic conductive-nonconductive adhesive film is one of them. The successful formation of the flip chip interconnection using this particular type of adhesive depends on, among factors, how the physical properties of the adhesive changes during the bonding process. Experimental measurements of the temperature in the adhesive have revealed that the temperature becomes very close to the required maximum bonding temperature within the first 1s of the bonding time. The higher the bonding temperature the faster the ramp up of temperature is. A dynamic mechanical analysis (DMA) has been carried out to investigate the nature of the changes of the physical properties of the coupled anisotropic conductive-nonconductive adhesive film for a range of bonding parameters. Adhesive samples that are pre-cured at 170, 190 and 210°C for 3, 5 and 10s have been analyzed using a DMA instrument. The results have revealed that the glass transition temperature of this type of adhesive increases with the increase in the bonding time for the bonding temperatures that have been used in this work. For the curing time of 3 and 5s, the maximum glass transition temperature increases with the increase in the bonding temperature, but for the curing time of 10s the maximum glass transition temperature has been observed in the sample which is cured at 190°C. Based on these results it has been concluded that the optimal bonding temperature and time for this kind of adhesive are 190°C and 10s, respectively.

Microwave curing of thermosetting polymer materials in microelectronics applications

Thermosetting polymer materials are widely utilised in modern microelectronics packaging technology. These materials are used for a number of functions, such as for device bonding, for structural support applications and for physical protection of semiconductor dies. Typically, convection heating systems are used to raise the temperature of the materials to expedite the polymerisation process. The convection cure process has a number of drawbacks including process durations generally in excess of 1 hour and the requirement to heat the entire printed circuit board assembly, inducing thermomechanical stresses which effect device reliability. Microwave energy is able to raise the temperature of materials in a rapid, controlled manner. As the microwave energy penetrates into the polymer materials, the heating can be considered volumetric – i.e. the rate of heating is approximately constant throughout the material. This enables a maximal heating rate far greater than is available with convection oven systems which only raise the surface temperature of the polymer material and rely on thermal conductivity to transfer heat energy into the bulk. The high heating rate, combined with the ability to vary the operating power of the microwave system, enables the extremely rapid cure processes. Microwave curing of a commercially available encapsulation material has been studied experimentally and through use of numerical modelling techniques. The material assessed is Henkel EO-1080, a single component thermosetting epoxy. The producer has suggested three typical convection oven cure options for EO1080: 20 min at 150C or 90 min at 140C or 120 min at 110C. Rapid curing of materials of this type using advanced microwave systems, such as the FAMOBS system [1], is of great interest to microelectronics system manufacturers as it has the potential to reduce manufacturing costs, increase device reliability and enables new device designs. Experimental analysis has demonstrated that, in a realistic chip-on-board encapsulation scenario, the polymer material can be fully cured in approximately one minute. This corresponds to a reduction in cure time of approximately 95 percent relative to the convection oven process. Numerical assessment of the process [2] also suggests that cure times of approximately 70 seconds are feasible whilst indicating that the decrease in process duration comes at the expense of variation in degree of cure within the polymer.

Residual stress due to curing can initiate damage in porous bone cement: experimental and theoretical evidence

Residual stress due to shrinkage of polymethylmethacrylate bone cement after polymerisation is possibly one factor capable of initiating cracks in the mantle of cemented hip replacements. No relationship between residual stress and observed cracking of cement has yet been demonstrated. To investigate if any relationship exists, a physical model has been developed which allows direct observation of damage in the cement layer on the femoral side of total hip replacement. The model contains medial and lateral cement layers between a bony surface and a metal stem; the tubular nature of the cement mantle is ignored. Five specimens were prepared and examined for cracking using manual tracing of stained cracks, observed by transmission microscopy: cracks were located and measured using image analysis. A mathematical approach for the prediction of residual stress due to shrinkage was developed which uses the thermal history of the material to predict when stress-locking occurs, and estimates subsequent thermal stress. The residual stress distribution of the cement layer in the physical model was then calculated using finite element analysis. Results show maximum tensile stresses normal to the observed crack directions, suggesting a link between residual stress and preload cracking. The residual stress predicted depends strongly on the definition of the reference temperature for stress-locking. The highest residual stresses (4-7 MPa) are predicted for shrinkage from maximum temperature, in this case, magnitudes are sufficiently high to initiate cracks when the influence of stress raisers such as pores or interdigitation at the bone/cement interface are taken into account (up to 24 MPa when calculating stress around a pore according to the method of Harrigan and Harris (J. Biomech. 24(11) (1991) 1047-1058)). We conclude that the damage accumulation failure scenario begins before weight-bearing due to cracking induced by residual stress around pores or stress raisers. (C) 2002 Elsevier Science Ltd. All rights reserved.

Development of Polybutadiene (BR)-Polyethylene (LDPE) Blend Based Microcellular Soles for Low-Temperature Applications

Microcellular (MC) soles based on polybutadiene (BR) and low-density polyethylene (LDPE) blends for low-temperature applications were developed. A part of BR in BR-LDPE blend was replaced by natural rubber (NR) for property improvement. The BR-NR-LDPE blend-based MC sole shows good technical properties. Sulphur curing and DCP curing were tried in BR-LDPE and NR-BR-LDPE blends. Study shows that sulphur-cured MC sheets possess better technical properties than DCPcured MC sheets. 90/10 BR-LDPE and 60/30/10 BR-NR-LDPE blend combinations are found to be suitable for low-temperature applications.

Curing studies of elastomer blends with special reference to NR/ NBR and NR/BR blends

There are a large number of commercial examples and property advantages of immiscible elastomer blends.73 Blends of natural rubber (NR) and polybutadiene (BR) have shown various advantages including heat stability, improved elasticity and abrasion resistance. Ethylene-propylene-diene-rubber (EPDM) blended with styrene-butadiene rubber (SBR) has shown improvements in ozone and chemical resistance with better compression set properties. Blends of EPDM and nitrile rubber (NBR) have been cited as a compromise for obtaining moderate oil and ozone resistance with improved low temperature properties. Neoprene (CR)/BR blends offer improved low temperature properties and abrasion resistance with better processing characteristics etc. However, in many of the commercial two-phase elastomer blends, segregation of the crosslinking agents, carbon black or antioxidants preferentially into one phase can result in failure to attain optimum properties. Soluble and insoluble compounding ingredients are found to be preferentially concentrated in one phase. The balance of optimum curing of both phases therefore presents a difficult problem. It has been the aim of this study to improve the performance of commercially important elastomer blends such as natural rubber (NR)/styrene-butadiene rubber (SBR) and natural rubber/polybutadiene rubber (BR) by industrially viable procedures

Effect of Pre-Heating Resin Composite and Light-Curing Units on Monomer Conversion

The purpose of this study was to evaluate the effect of pre-heating resin composite photo-cured with light-curing units (LCU) by FT-IR. Twenty specimens were made in a metallic mold (4 mm diameter x 2 mm thick) from composite resin-Tetric Ceram (R) (Ivoclar/Vivadent) at room temperature (25 degrees C) and pre heated to 37, 54, and 60 degrees C. The specimens were cured with halogen curing light (QTH) and light emitted by diodes (LED) during 40 s. Then, the specimens were pulverized, pressed with KBr and analyzed with FT-IR. The data were submitted to statistical analysis of variance and Kruskal-Wallis test. Study data showed no statistically significant difference to the degree of conversion for the different light curing units (QTH and LED) (p > 0.05). With the increase of temperature there was significant increase in the degree of conversion (p < 0.05). In this study were not found evidence that the light curing unit and temperature influenced the degree of conversion.

Influence of pre-heat treatment and different light-curing units on Vickers hardness of a microhybrid composite resin

The aim of this study was to evaluate the hardness of a dental composite resin submitted to temperature changes before photo-activation with two light-curing unite (LCUs). Five samples (4 mm in diameter and 2 mm in thickness) for each group were made with pre-cure temperatures of 37, 54, and 60A degrees C. The samples were photo-activated with a conventional quartz-tungsten-halogen (QTH) and blue LED LCUs during 40 s. The hardness Vickers test (VHN) was performed on the top and bottom surfaces of the samples. According to the interaction between light-curing unit and different pre-heating temperatures of composite resin, only the light-curing unit provided influences on the mean values of initial Vickers hardness. The light-curing unit based on blue LED showed hardness mean values more homogeneous between the top and bottom surfaces. The hardness mean values were not statistically significant difference for the pre-cure temperature used. According to these results, the pre-heating of the composite resin provide no influence on Vickers hardness mean values, however the blue LED showed a cure more homogeneous than QTH LCU.

Degree of Conversion and Temperature Increase of a Composite Resin Light Cured with an Argon Laser and Blue LED

Different light sources and power densities used on the photoactivation process may provide changes in the degree of conversion (DC%) and temperature ( T) of the composite resins. Thus, the purpose of this study was to evaluate the DC (%) and T (degrees C) of the microhybrid composite resin (Filtek (TM) Z-250, 3M/ESPE) photoactivated with one argon laser and one LED (light-emitting diode) with different power densities. For the KBr pellet technique, the composite resin was placed into a metallic mould (2-mm thickness, 4-mm diameter) and photoactivated as follows: a continuous argon laser (CW) and LED LCUs with power density values of 100, 400, 700, and 1000 mW/cm(2) for 20 s. The measurements for DC (%) were made in a FTIR spectrometer Bomen ( model MB 102, Quebec, Canada). Spectroscopy ( FTIR) spectra for both uncured and cured samples were analyzed using an accessory of the reflectance diffusion. The measurements were recorded in absorbance operating under the following conditions: 32 scans, 4 cm(-1) resolution, 300 to 4000-cm(-1) wavelength. The percentage of unreacted carbon double bonds (% C=C) was determined from the ratio of absorbance intensities of aliphatic C=C (peak at 1638 cm(-1)) against an internal standard before and after the curing of the specimen: aromatic C-C (peak at 1608 cm(-1)). For T (degrees C), the samples were created in a metallic mould (2-mm thickness, 4-mm diameter) and photoactivated for 20 s. The thermocouple was attached to the multimeter allowing temperature readings. The DC (%) and T (degrees C) were submitted to ANOVA and Tukey`s test (p < 0.05). The degree of conversion values varied from 35.0 to 50.0% ( 100 to 1000 mW/cm(2)) for an argon laser and from 41.0 to 49% (100 to 1000 mW/cm(2)) for an LED. The temperature change values varied from 1.1 to 13.1 degrees C (100 to 1000 mW/cm(2)) for an argon laser and from 1.9 to 15.0 degrees C (100 to 1000 mW/cm(2)) for an LED. The power densities showed a significant effect on the degree of conversion and changes the temperature for both light-curing units.