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3D Printing Polymers Using Pyrolysis-GC/MS

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3D Printing Polymers Using Pyrolysis-GC/MS Material Characterization of 3D Printing Polymers Using Pyrolysis-GC/MS FRONTIER LAB Why Pyrolysis GC/MS? Manufacturers are always seeking new technologies and developments that increase production efficiency and the quality of the produced parts. Many analytical protocols used to analyze 3D printing and coating components require multi-step sample preparation prior to chromatographic analysis. These procedures often include solvent extraction, filtration, and concentration. These traditional techniques are cumbersome, time-consuming, and suffer from analyst-to-analyst variability while producing data of limited value. Samples are analyzed “as is” when using the Frontier pyrolyzer. No sample preparation is needed. Eliminating the solvent extraction process enhances the precision of quantitative analysis while virtually prevent sample contamination and improves analytical efficiency. These are three of the primary reasons many manufacturing and polymer development laboratories utilize the Frontier Pyrolyzer. The Frontier Multi-Shot Pyrolyzer can be configured in a number of different ways, so that a sample can be characterized using various analytical techniques, including evolved gas analysis, thermal desorption, flash pyrolysis, double-shot, Heart-Cutting of individual EGA thermal zones, and reactive pyrolysis. Initially, such diversity may be perceived as a complicated decision process: what analytical mode will give us the most insight into the nature of the sample in the least amount of time? To assist, Frontier scientists have created a “method map”. An overview of the “method map” is provided on page 45. FRONTIER LAB Table of Contents Polylactic acid (PLA) for 3D Printing 4 Epoxy Adhesives and Resins as Thermosets 8 Polysiloxane - PDMS and Adhesive Compositions 12 Polyphenylene Ether (PPE) Plastic Resins 16 Polyphenyelene Sulfide (PPS) Resins and Filaments 20 ULTEM or Polyetherimide (PEI) High Performance Polymer 23 Polyetheretherketone (PEEK) High Performance Polymers 26 Nylon 12 Powder Resins and SLS 3D Printing 29 Polycarbonate (PC) Plastic Resins 32 Nylon 6 and Polyphenylene sulfide (PPS) Blended Polymers 35 Thermoset Polymer Resin Coated Proppant 38 What is Pyrolysis GC/MS Technique? 42 Simplify and Improve Data Interpretation by F-search 44 “Method Map” Providing Direction 45 Pyrolysis-GC/MS System Configuration 47 FRONTIER LAB Polylactic acid (PLA) for 3D Printing Background: There is a high interest in bio-derived Plastics. Polylactic acid or polylactide (PLA or PLLA) is a thermoplastic polyester derived from renewable biomass (monomer) from fermented plant starch such as corn, cassava, sugarcane or sugar beet pulp. They range from amorphous glassy polymer to semi-crystalline and highly crystalline polymer with a glass transition temperature (Tg) of 60 °C and melting points of 130-180 °C. It is one of the most produced bioplastics. The mechanical properties of PLA are between those of polystyrene and PET. The melting temperature, Tm, of PLA can be increased by 40– 50 °C and its heat deflection temperature can be increased from approximately 60 °C to up to 190 °C by physically blending the polymer with PDLA (poly-D-lactide). Polylactic acid can be processed like most thermoplastics into fiber (for example, using conventional melt spinning processes) and film. With high surface energy, PLA has easy printability which makes it widely used as a filament in 3-D printing. Problem: Although PLA is commonly used as a 3D Printing polymer filament material, the composition in most filaments is unknown, including the presence of PDLA or any compatible additives or modifiers. While IR spectroscopy can be used for screening, it is not sufficient for composition determination or distinguishing between other types of polyester blends or PLA sources. Solution: Using Pyrolysis-GC/MS techniques, perform Evolved Gas Analysis (described in page 46) followed by a single shot/flash pyrolysis to confirm the presence of the PLA or its monomer and the general absence of other additives. FRONTIER LAB 4 [%] 110 Experimental: Evolved Gas Analysis 100 90 (EGA) was performed to identify the 80 thermal composition of a 3D printed PLA 70 sample. To perform EGA, around 100 µg 60 was cut from a 3D printed dogbone 50 40 shape specimen and placed into the inert 30 Flash Pyrolysis 500°C Eco-Cup. The micro-furnace was then 20 programmed from 100 to 700°C 10 0 100 300 500 700 (20°C/min). The GC oven was kept Temperature (oC) isothermal at 320°C. Compounds [%] 110 100 56 “evolved” continuously from the sample 90 as the temperature increases. The 80 EGA-MS result (9.949 to 14.987 min) 70 2943 obtained EGA-MS was summarized from 60 10 min to 15 min (300-400 oC), and the 50 40 reference was directly suggested by the 30 200 128 20 272 F-Search EGA-MS library. 100 344 10 72 416 145 217 488 0 173 243 289 441 471 532 560 604 632 m/z -->0 100 200 300 400 500 600 Results: The EGA thermogram indicated [%] 110 o 100 56 that the PLA starts to degrade at 300 C 90 and will be totally degraded at 400oC. 80 Reference of Poly(lactic acid) 70 (F-search library result) Library search is done by F-search 60 (interpretation library described in page 50 45 40 44) , which fits well with the EGA-MS of 30 29 sample, giving a result that the 3D printed 20 10 128 200 73 100 272 dogbone is consist of PLA. 0 173 217 344 416 m/z -->0 100 200 300 400 500 600 FRONTIER LAB 5 Flash pyrolysis was then performed at 500°C. By extracting the chromatogram of typical ion of compounds, they are obviously observed out of all peaks. For additives which has minor fraction in the material, they can be detected by scaling up the sample to 10 times and refocus the peak in Thermal Desorption (TD) or Heart-cut (HC). [%] 100 [%] 100 Thermal Desorption(TD) 100-300˚C 80 80 Single shot at 500˚C 60 60 40 40 20 20 0 10 times more sample 0 min --> 0 5 10 15 20 25 min --> 0 5 10 15 20 25 [%] 100 [%] 100 Extracted ion chromatogram m/z: 646 Extracted ion chromatogram m/z: 646 80 80 60 60 40 40 20 20 0 0 5 10 15 20 25 min --> 0 min --> 0 5 10 15 20 25 110 110 [%] [%] 441 100 441 100 90 Mass Spectrum of Single Shot 90 Mass Spectrum of TD 80 peak @ 20.726 min 80 peak @ 20.747 min 70 70 60 60 50 50 40 40 57 57 30 30 20 20 147 207 147 646 10 646 10 41 191 281 308 41 91 191 237 308 73 91 133 237 329 355 385 29 69 105 131 281 329 355 385405 474 506 540 589 0 405 479 508 540 589 631 0 m/z -->0 100 200 300 400 500 600 700 m/z -->0 100 200 300 400 500 600 700 110 110 [%] [%] 441 100 441 100 90 Reference of Irgafos 168 90 Reference of Irgafos 168 80 80 70 57 70 57 60 60 50 50 40 40 30 30 20 147 20 147 41 646 41 646 10 10 29 91 308 29 91105 131 191 308 69 105 131 191 219237 329 385 69 219237 273 329 385 0 273 533 589 0 533 589 m/z -->0 100 200 300 400 500 600 700 m/z -->0 100 200 300 400 500 600 700 FRONTIER LAB 6 [%] For the Thermal Desorption 100 (TD) analysis, the heating 80 Thermal Desorption(TD) 100-300˚C occurs below 300˚C, thus the 60 majority peaks are ascribed to 40 small molecules in their original 20 form without chemical 0 decomposition. min --> 0 5 10 15 20 25 [%] 100 Monomers, additives and 80 Extracted ion chromatogram m/z: 239 solvent residue are always 60 shown in this part. 40 20 Here, the Palmitic acid 0 monoglyceride is isolated by min --> 0 5 10 15 20 25 TD-GC/MS and its mass [%] 100 43 98 239 spectrum is highly consistent Mass Spectrum of TD 80 57 with the reference. 74 peak @ 15.852 min 60 84 134 69 40 257 29 112 20 129 299 61 154 168 182 227 270 196 213 283 343 371 396 m/z --> 0 100 200 300 400 [%] 100 98 239 Reference of Palmitic 43 80 57 acid monoglyceride 74 60 84 69 134 40 112 257 29 129 20 61 154 182 227 270 299 168 199 213 283 313 331 m/z --> 0 100 200 300 400 FRONTIER LAB 7 Epoxy Adhesives and Resins as Thermosets Background: Epoxy resins are a class of reactive prepolymers and polymers which contain epoxide (oxirane) groups. Reaction is based on either catalytic homopolymerization, or with a wide range of co- reactants including polyfunctional amines, acids (and acid anhydrides), phenols, alcohols and thiols (usually called mercaptans)- Part A & B. These co-reactants are often referred to as hardeners or curatives (Part B), and the cross-linking reaction is commonly referred to as curing. This results in a thermosetting polymer, often with favorable mechanical properties and high thermal and chemical resistance. Epoxy has a wide range of applications, including metal coatings, use in electronics/electrical components/LEDs, high tension electrical insulators, paint brush manufacturing, fiber-reinforced plastic materials (composites) and structural adhesives. Problem: Although Epoxy is a commonly used resin and adhesive material, their commercial compositions vary enormously, and the determination of the reactive equivalent is of then the only quantifiable reaction parameter. Moreover, their use as a 3D printing material is only currently being studied. To study the composition and additives of a 3D printed objective, normal method could be destructive and requires a larger sample and preparation methods.
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