Page 68 - Plastics News October 2018
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tEChnoLogy



         New NIST method measures 3D polymer processing precisely



             he  National  Institute  of  Standards  and Technology   printed  parts.  Instead,  the  performance  of  fabricated
          T(NIST) have derived methods to measure 3D polymer    parts depends on printing conditions. NIST's new method
          processing precisely Recipes for three-dimensional (3D)   measures how materials evolve with submicrometer
          printing, or additive manufacturing, of parts have required   spatial resolution and submillisecond time resolution
          as much guesswork as science. Until now. Resins and other   -- thousands of times smaller-scale and faster than bulk
          materials that react under light to form polymers, or   measurement techniques. Researchers can use SCRPR to
          long chains of molecules, are attractive for 3D printing   measure changes throughout a cure, collecting critical
          of parts ranging from architectural models to functioning   data for optimizing processing of materials ranging from
          human organs. But it's been a mystery what happens to   biological gels to stiff resins.The new method combines
          the materials' mechanical and flow properties during the   AFM with stereolithography, the use of light to pattern
          curing process at the scale of a single voxel. A voxel is a   photo-reactive materials ranging from hydrogels to
          3D unit of volume, the equivalent of a pixel in a photo.   reinforced acrylics. A printed voxel may turn out uneven
          Now, researchers at the National Institute of Standards   due to variations in light intensity or the diffusion of
                                                                reactive molecules. AFM can sense rapid, minute changes
                                                                in surfaces. In the NIST SCRPR method, the AFM probe is
                                                                continuously in contact with the sample. The researchers
                                                                adapted a commercial AFM to use an ultraviolet laser to
                                                                start the formation of the polymer ("polymerization")
                                                                at or near the point where the AFM probe contacts
                                                                the sample.The method measures two values at one
                                                                location in space during a finite timespan. Specifically,
                                                                it measures the resonance frequency (the frequency of
                                                                maximum vibration) and quality factor (an indicator of
                                                                energy dissipation) of the AFM probe, tracking changes
                                                                in these values throughout the polymerization process.
                                                                These data can then be analyzed with mathematical
                                                                models to determine material properties such as stiffness
                                                                and damping. The method was demonstrated with two
          and  Technology (NIST) have demonstrated a novel      materials. One was a polymer film transformed by light
          light-based atomic force microscopy (AFM) technique --   from a rubber into a glass. Researchers found that the
          sample-coupled-resonance photorheology (SCRPR) -- that   curing process and properties depended on exposure
          measures how and where a material's properties change   power and time and were spatially complex, confirming the
          in real time at the smallest scales during the curing   need for fast, high-resolution measurements. The second
          process. "We have had a ton of interest in the method   material was a commercial 3D printing resin that changed
          from industry, just as a result of a few conference talks,"   from liquid into solid form in 12 milliseconds. A rise in
          NIST materials research engineer Jason Killgore said. He   resonance frequency seemed to signal polymerization
          and his colleagues have now published the technique   and increased elasticity of the curing resin. Therefore,
          in the journal  Small Methods. 3D printing, or additive   researchers used the AFM to make topographic images of
          manufacturing, is lauded for flexible, efficient production   a single polymerized voxel.  Surprising the researchers,
          of complex parts but has the disadvantage of introducing   interest in the NIST technique has extended well beyond
          microscopic variations in a material's properties. Because   the initial 3D printing applications. Companies in the
          software renders the parts as thin layers and then    coatings, optics and additive manufacturing fields have
          reconstructs them in 3D before printing, the physical   reached out, and some are pursuing formal collaborations,
          material's bulk properties no longer match those of the   NIST researchers say.





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