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Polymer Analysis

Development Of A Gas-Based Temperature Control System For Injection Molds - Gasmold
Alexander Paskowski, Ruben Schlutter, June 2022

The paper describes the development of a variothermal process, which increases the mold surface temperature during the injection molding process without significantly extending the cycle time and minimizes unintentionally heated mold areas. To this end, the possibility of achieving the desired effects by direct introduction of heated gases into the mold cavity is being investigated. By addressing central issues such as gas distribution geometry, injection possibilities, required gas temperatures or the possibility of process implementation in a demonstrator mold, it was possible to develop a process with which it is possible to achieve temperature optimization for visually appealing parts within seconds. This means that weld lines, streaks or uneven mold impressions can be concealed even on flat parts.

Part 1: Ultraviolet-C (UVC) Exposure And Its Effect On Color Change For Polystyrene
Kristen Chang, June 2022

Due to the recent and ongoing pandemic – COVID-19 – there was an urgency to determine a method to delay the continuously rapid development of the new virus. As a result, Ultraviolet-C (UVC) light, also known as Ultraviolet Germicidal Irradiation (UVGI), has been in higher demand because of its known ability to disinfect quickly and effectively. However, because of its short wavelength/higher energy, either 222nm or 254nm, material degradation is usually much more accelerated than Ultraviolet-A (UVA) or Ultraviolet-B (UVB). At this moment, this study only observed color change when exposing polystyrene to UVC light, and it is believed that this is one of the first studies, if not the first, conducted with this material. Polystyrene was selected because of its availability, abundance of relevant research (ie. UVA/UVB exposure results), and its use in weathering standards. Additionally, since there are no standards specifically about UVC exposure, this preliminary research may provide some direction.

Analytical Method Development For Additive Analysis In Polyethylene
Praveenkumar Boopalachandran, Jörg Theuerkauf, Alexander Williamson, Jorge Gomes, Avery Brown, June 2022

The overall goal of the project targets the development of a product containing a rheology modifier additive in polyethylene (PE). This product is being sold to film converters for addition to the extruders of blown-film lines together with LLDPE resins. This increases the melt-strength during processing and the shrink tension for collation shrink films, enabling reduction in LDPE content and resultant tougher films. A tougher film will allow down-gauging and hence reduce material consumption, increasing the sustainability component for customers. This study focuses on the development of an analytical method at Dow to measure the concentration of the rheology modifier additive in PE. The method was validated and implemented successfully.

Development Of A Non-Destructive Measurement Method For Quality Assessment Of Foamed Plastic Parts
Ruben Schlutter, Alexander Paskowski, Manuel Schneider, Rainer Jahn, Joshua Voll, Thomas Seul, Andreas Wenzel, Gerd Telljohann, June 2022

Foamed parts are being produced in ever greater quantities. This is done, on the one hand, to save weight and, on the other hand, to take advantage of the greater design freedom in the layout of foamed components. Until now, quality control of the foam structure has hardly been possible without destructive testing methods. Therefore, a test method is presented to qualitatively evaluate the foam structure of foamed components without destruction.

Thermal and Mechanical Techniques for Troubleshooting Polylactic Acid Processing Issues
Tianhong (Terri) Chen | Louis Waguespack | Gregory W Kamykowski, May 2021

This paper describes the use of differential scanning calorimetry (DSC), modulated DSC, and dynamic mechanical analysis to characterize different regions of thermoformed beverage cups made from polylactic acid. These techniques demonstrated the differences in crystallinity and mechanical strength of the cup based on the location of the specimen. These techniques can guide the processor in resin selection and processing conditions.

Method to Evaluate Shrink Film Material Properties
Masoud Allahkarami | Michael Rector | Sudheer Bandla | Jay C. Hanan, May 2021

Understanding heat shrink film properties and behavior will help optimize shrink wrap formation in packaging applications. Two experiments were conducted to better understand shrink properties of PE film. The first experiment was to collect data on film shrink ratios. The second experiment was an attempt to compare film preshrunk and post-shrunk mechanical properties. For this, a fixture was developed to quantify film shrink under isothermal heating. The film submersion tool successfully yielded films that were shrunk at different temperatures and demonstrated a method applicable for analyzing properties of heat shrink film at various stages of the shrinking process. Further work is focused at developing correlations between preshrunk properties to post-shrunk properties.

Optimization of PVDF Extrusion to Produce Electroactive Filament for FFF
Aya A. Saleh | Garrett W. Melenka | Siu Ning Leung, May 2021

The development of Poly(vinylideneflouride) (PVDF) material with high electroactive properties is of great interest for its use in energy harvesting. This study is concerned with producing PVDF filaments to be fed into a Fused Filament Fabrication (FFF) 3D printer to broaden the horizon for printing complex energy harvesters. An extrusion process followed by post treatments was applied and the processing conditions were varied as they play a crucial role in altering the phases within PVDF and its crystallinity. The correlation between the parameters and the resultant properties of the PVDF filament was made using combination of Fourier-transform infrared spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC) characterization techniques. The optimized processing conditions were found to be 230 ᴼC for extrusion temperature and 4.5 – 6.5 stretching ratio. This led to the fabrication of an electroactive PVDF filament with 80% β-phase content and 50 to 55% degree of crystallinity.

Analytical Characterization of Acid Copolymers and Ionomers
Praveenkumar Boopalachandran | Yongfu Li | Steve Rozeveld | Barry Morris | Leslie O’Leary | Josh Enokida, May 2021

Ethylene-methacrylic acid (EMAA) copolymers are converted to ionomers (ionic functionality) through the partial neutralization of their carboxylic acid groups. These ionic groups are randomly distributed along the polymer backbone, and various cations (i.e., Na, Zn, Mg, Li, etc.) can be incorporated into the ionic functionality to modify their properties. Some unique properties that these ionomers exhibit include high melt strength, excellent toughness and optical clarity. These desired properties make the ionomers ideal for applications that include packaging, decorative perfume and spirit caps and capstock decking. This study was focused on the use of Fourier-Transform Infrared (FTIR) spectroscopy to study EMAA copolymers partially neutralized with Zn cations. FTIR was also used to measure the degree of neutralization of ionomers. The % neutralization method was developed internally, and it was applied to extract the experimental neutralization values with comparison to theoretical values for EMAA–Zn ionomers. The values were in good agreement with the expected neutralization levels. Chemical mapping of the acid band (C=O stretch) and carboxylate band (COO- stretch) in EMAA–Zn ionomer indicated that their distribution on a micro-scale in the selected cross-section were homogeneous. The FTIR method was also used to study EMAA copolymers neutralized by mixed metal Zn and Na cations and compare with EMAA ionomers neutralized by single metal cation. For the mixtures, a new carboxylate band appeared around 1569 cm-1, which was assigned to the COO- stretch. Based on the unique peak position, it suggests that there are interactions between the zinc and sodium cations.

Monitoring Degradation of Nuclear Cable Insulation Subjected To Sequential And Simultaneous Thermal
Madhusudhan R. Pallaka | Mychal P. Spencer | Tucker T. Bisel | Yelin Ni | Mark K. Murphy |Leonard S. Fifield, May 2021

Predicting useful remaining life of cables in nuclear power plants is a topic of growing interest as plants continue to age. A typical electrical cable consists of polymeric materials, such as the cable jacket and insulation, which are susceptible to degradation due to exposure to both elevated temperatures and gamma irradiation over decades of service. In this work two insulation materials, crosslinked polyethylene (XLPE) and ethylene propylene diene (EPDM) elastomer, were characterized to quantify aging using total color difference and indenter modulus. Since the effects of thermal and gamma radiation are not additive but coupled, the effects of different aging scenarios including sequential and simultaneous aging were also evaluated. In the case of sequential aging, two aging scenarios were explored where the order in which thermal and gamma radiation received were altered. Total color difference of XLPE showed that sequentially aged insulation specimens, which received radiation first, degraded slightly more at maximum exposure than specimens which received thermal first. Similarly, in the case of EPDM, the extent of degradation evaluated using total color difference was found to be most severe in the case of sequentially aged insulation specimens which received radiation first. Indenter modulus was found to be insensitive to aging for XLPE but trended for EPDM. The largest variations were observed for the sequentially aged insulation specimens which received radiation first, similar to what was observed for total color difference.

Fused Filament Fabrication Feedstock Characterization via In-Line Rheology
A.R. Colon | D.O. Kazmer | A. Peterson, May 2021

An instrumented hot end has been developed to monitor the pressure in Fused Filament Fabrication, and is used as an in-line rheometer to characterize the viscosity of an acrylonitrile butadiene styrene (ABS) material. Additional analysis was performed on the transient pressure data to consider compressibility effects and nozzle drool. The range of flow rates was identified at which the pressure in the hot end was most stable. Stabilization time given compressibility effects was also evaluated.

Research on Transfer Learning Applied to Characteristic Prediction of Injection Molded Products
Yan-Mao Huang | Wen-Ren Jong | Shia-Chung Chen, April 2021

With advances in computing technology, applications of computer-aided engineering (CAE) technology are becoming widespread in diverse industries. Specifically, machine learning is now being applied to fields such as that of materials design and production which is the field within which this study focuses. However, problems in implementing this technology arise in regard to lengthy analysis times and a lack of suitability in regard to on-site, real-time judgments during some production processes. This study addresses these issues in regard to the problems of applying CAE to the injection molding production process where quite complex factors inhibit its effective utilization. In this study, an artificial neural network, namely a Back Propagation Neural Network (BPNN), is utilized to render results predictions for the injection molding process. By inputting the plastic temperature, mold temperature, injection speed, holding pressure, and holding time in the molding parameters, these five results are more accurately predicted: EOF pressure and maximum cooling time, warpage along Z-axis, shrinkage along X-axis and shrinkage along Y-axis. This study first uses CAE analysis data as training data and reduces the error value to less than 5% through the Taguchi Method and the Random Shuffle Method which we introduce herein, and then successfully transfers the network which CAE data analysis has predicted to the actual machine for verification with the use of transfer learning. Of particular interest, is this study's use of a Back Propagation Neural Network (BPNN) to train a dedicated prediction network through using different, large amounts of data for training the network, which is proven fast and that can predict results accurately using our optimized model.

Failure Analysis of Products with Plastic to Metal Threaded Connections
Gaurav Nagalia | Anand R. Shah, April 2021

Many products and assembled systems of different products require the use of threaded plastic to threaded metal connection to provide the mechanical integrity required for the service application. While there are design guidelines and industry acceptable standard specifications related to the design of the different thread profiles used in the connection of plastic to plastic or connection of metal to metal threaded components, there is very limited information available for designing a plastic to metal threaded connection. Generally, designing a mechanical connection between a plastic threaded component and a metal threaded component is discouraged. However, in some applications this cannot be avoided and as such the lack of understanding related to plastic to metal threaded connection leads to product failures when such connections are made or designed improperly into products. This paper reports two case studies of product failures where plastic to metal threaded connections contributed to product failure that caused either personal injury or personal property loss. A failure analysis investigation was conducted to evaluate the thread design in two products in which plastic to metal threaded connections were involved in the product failure. In the first case-study, the thread connection was found to be insufficient in the mechanical strength and in the second case study the root cause of failure was determined to be excessive tightening of the female threaded plastic component onto a male threaded metal component.

Failure Analysis Case Study: The Good and the Bad PVC Cable Coatings
Sergey Shilov, April 2021

Polyvinylchloride (PVC) is the most commonly used thermoplastic resin for electrical cable coatings. PVC that hardens after polymerization is not suitable for insulating and protecting wires and cables. The necessary mechanical, thermal, and electrical levels can only be reached with the addition of softeners, stabilizers, and fillers. Composition of the good and the bad PVC samples were analyzed using FTIR spectroscopy and TG analysis.  It was found that ditridecyl phthalate was used as a softener in both samples. Magnesium oxide was used as a filler in one sample. The higher amount of water that present in the sample at room temperature and evolves during the first stage of PVC decomposition might be responsible for the low heat resistance of one sample.

Analytical Characterization of Commercial Foams for Consumer Bedding Applications
Praveen Boopalachandran, May 2020

The objective of this study was to characterize popular commercial bed-in-a-box mattress and visco topper foams, which are the benchmark bedding products in the market. These products were advertised as gel infused foams that offer superior thermal conductivity and support. Multiple techniques were utilized to identify the composition of the foams. In summary, the commercial “green” and “gray” bedding polyurethane (PU) foams were similar in composition, and they were made of glycerin-initiated PO/EO based polyols. It also showed the incorporation of styrene-acrylonitrile (SAN) in the polymer backbone. The isocyanate part was consistent with an aromatic isocyanate identified as methylene diphenyl diisocyanate (MDI). In addition, the blue gel polymers that were infused to these foams were polyurethane based material. Furthermore, the black particle in the “gray” foam that was advertised as heating wicking material was graphite-based additive.

Foaming of PVC Using Ultra High Molecular Weight Acrylic Processing Aids
Manoj Nerkar, May 2020

Polyvinyl Chloride (PVC) foaming was studied as a function of high molecular weight acrylic processing aids. It was demonstrated that an ultra-high molecular weight processing aid is 25-30% more efficient than relatively lower, but still high, molecular weight acrylic processing aids. The higher Mw processing aid provided similar foaming performance at lower loading levels. Foaming reduced the density of PVC compounds to 0.32-0.34 g/cc. More than 1000% expansion was achieved in the melt extrusion process using a chemical blowing agent. Fusion characteristics were also studied. Fusion times for initial fusion peaks were in the range of 42-44 seconds while the fusion times of the second fusion peaks were in the range of 74-94 seconds. The higher molecular weight processing aid maintained fusion characteristics of PVC compounds, warranting no significant changes in extrusion process.

Morphology and Mechanical Performance of Pipe Grade HDPE Exposed to Chlorinated Water
Andrew Hagen, May 2020

Thin samples of a pipe-grade polyethylene with a bimodal molecular weight distribution were exposed to 5ppm 70C chlorinated water for up to 3000 hours. The samples were characterized by tensile tests, size-exclusion chromatography, infrared spectroscopy, and differential scanning calorimetry. Throughout exposure, the molecular weight data showed evidence of degradation: weight-average molecular weight was reduced, and a shift in the molecular weight distribution from a bimodal to a unimodal distribution (decreased dispersity). After 2250 hours of exposure, brittle behavior was observed, in which the average elongation at break was 12%. At this level of degradation, the weight-average molecular weight was 9 % of its undegraded value, and the crystallinity had increased from 70% to 85%. Average tensile strength was reduced from 31.8 to 16.6 MPa. The data imply that the presence of short-chain branching may inhibit chemicrystallization and subsequently delay the onset of brittle behavior.

Novel Method of Compounding Cellulose Nanocrystal Suspensions into Polylactic Acid and Polyvinyl Acetate Blends
Ronald Sabo, PhD, May 2020

Cellulose nanocrystal (CNC) suspensions were compounded into blends of poly(lactic acid)(PLA) and poly(vinyl acetate)(PVAc) using a novel wet compounding approach in which drying and compounding werecarried out simultaneously. The resulting CNC/PLA composites were compared with those produced using a more traditional method of freeze-drying CNC suspensions followed bymelt-blending into PLA. CNCs in wet compounded composites appeared to be well-dispersed in the PLA/PVAc blends, and films extruded from these compounds exhibited high transparency compared with melt-blended composites. Gel permeation chromatography indicated that molecular weight degradation due to wet compounding was comparable to that from melt blending. The formulation, including surfactant modified CNCsand PVAc processing aids, played a significant role in the dispersion and properties of the nanocomposites. The elimination of a stand-alone drying stepfor cellulose nanomaterials can potentially overcome some of the challenges associatedwith producing thermoplastic cellulose nanocomposites and help advance commercialization of these materials.

Reverse Engineering and Failure Analysis of Materials and Polymers Using Infrared and Raman Spectroscopy
Sergey Shilov, May 2020

Failure analysis and reverse engineering can greatly expedite product development. Infrared and Raman spectroscopy is the among the most powerful tools for this application because each molecule has a unique infrared and Raman signature. Infrared and Raman microscopy was successfully used to identify foreign particles on elastomers and to depth profile multilayer polymer film. Details of the measurement techniques are discussed.

Reduced Order Kinetic Model for Corrosion of High-Density Polyethylene in Bleach Solutions
Susan Mantell, May 2020

A reduced order kinetics model is proposed for the corrosion of polyethylene in bleach solution. Hypochlorous acid (ClOH) is considered as the oxidizing agent which is formed from the hydrolysis of bleach. The model simulates the diffusion of ClOH into the non-polar polymer matrix followed by its dissociation into radicals. The reaction between the radicals and the polymer is phenomenologically modeled using an ordinary differential equation. The model is suitable for coupling with mechanical models for life-time analyses of polymers members under mechanical loading and exposure to corrosion. The model captures the effect of the chain oxidation process which causes the accelerated aging of the polymer.

Studies of Material Properties of Htpb- Based Composite Under Aging Conditions
Jaehee Jeong, May 2020

Hydroxyl-terminated polybutadiene (HTPB)-based rubber composite is usually used for solid propellant binder. In order to investigate the long-term material properties in the storage environment, it is recommended to set up the conditions refer to MIL-STD-810G. After aged for 100, 200, 300 hours with different temperature and humidity conditions, the key properties, i.e. tensile test, Fourier transform infrared spectroscopy (FTIR), and surface morphologies were examined. Also, by using these experimental data, diffusion model using finite element method suggested. This study will be useful for the life evaluation of HTPB-based composites considering diffusion.









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