Micophotometric Control of Particles and Inhomogeneities in Flowing Polymer Melts during Extrusion Processing

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1 M.Stephan, S.Große: Micophotometric Control of Particles and Inhomogeneities in Flowing Polymer Melts during Extrusion Processing Workshop January, 28 th -29 th 2005, Dresden

2 Particulate Heterogeneities in Polymer Melts unmolten granules processing conditions black spots degraded polymer extrusion start-up s gels / fisheyes crosslinked + ultra high molecular gas bubbles overheating, humidity additive agglomerates, environmental dust, insects

3 State of the Art - Determination of Melt Homogeneity Extrusion?Quality? buffer store!quality! final product injection molding sample offline analysis lab-extruder + film observation microscopy dead-times between taking a sample and getting a quality result large low quality batches possible generation of plastics waste time and cost consuming procedure

4 Objective - Real-time Determination of Melt Homogeneity Extrusion!Quality! final product injection molding inline/online analysis micro-photometric sensors continuous real-time data on melt quality low quality batches can be detected immediately application at processing conditions (p, T) technological and economical benefits increased level of process-/quality control (new applications of high performance polymers)

5 Measuring Principle Photometry - Light Extinction Lambert Beer: E = ln 1 T = A V c V L light source detector Mie: A V = f ( d, λ, m) setup parameters (Lambert-Beers-Law): reflection particle size d, concentration c V, shape of the particles incident light beam absorption deflection detector refractive indices particles/polymer matrix m optical path length L laser wavelength λ limitations (Lambert-Beers-Law): acceptance of spherical particles refraction no multiple scattering appears Extinction E = absorption + scattering (reflection, deflection, refraction)

6 2 Modes of Signal Evaluation by variation of time resolution of data recording (min.. ms-range) integral signal analysis: - shift of mean signal level - for nm-scaled particles (>300nm) - limitation on low concentrations (< 5Vol.%) (multiple scattering effects) - determination of mean particle sizes or particle concentrations (Lambert Beer) U [V] U t [min] single particle counting: - single particle impulses - for µm-scaled particles (>20µm) - limitation on lowest particle concentrations - determination of mean particle sizes and particle concentrations (calibration needed) U [V] t [ms] U

7 Sensor Setup beam splitter Backscatter- Detector Extinction- Detector Laser 660nm melt flow

8 Sensor Adaptation to Extrusion Processing inline screw-in EXTRUDER single screw / twin screw inline main melt flow online bypass melt flow sensors can be adapted to various positions of different extruders inline or online different sensor types are available

9 Sensor Adaptation to Extrusion Processing inline mode - extinction online mode - extinction main melt flow Laser inline mode backscattering Laser Extinction Laser bypass melt flow Extinction extruder barrel

10 Sensor Adaptation to Extrusion Processing Animation

11 Transparency Control in Molten State pure polymer polymer-blend (nm-particles) transmission signal time 400 [ms] integral signal analysis - classical turbidimetry light extinction by nm-particles - decrease of signal level by turbid melt applicable to polymer blending and control of batch changes

12 Determination of Mean Blend Particle Diameters integral signal analysis (Lambert Beer calculation) particle x size 50,3 [µm] 0,9 0,83 0,79 PMP 0,8 SEM 0,7 0,6 0,5 0,4 0,34 0,3 0,2 Extinktion [/] extinction 0, Lambert-Beer PMMA / PS m=1,0578 PS / PA6 m=0,9638 multiple scattering c V [%] 0,1 0,0 1 wt.% PS / PA6 1 wt.% PMMA / PS limitation on maximum blend concentrations of about 5 wt.% also applicable to low concentrated composites

13 Real-Time Monitoring of Pellets Melting first step of extrusion processing, detection of unmolten granules optimization of extrusion parameters (energy costs - melt quality) improved pellets melting with an increasing screw speed n=50 min -1 T melt =252 C n=100 min -1 T melt =256 C n=200 min -1 T melt = 261 C transmission signal Time [ms] transmission signal Time [ms] transmission signal Time [ms]

14 Real-Time Observation of Additive Dispersion during Extrusion Processing Sensor 1 Sensor 2 Sensor 3 inline backscatter or online extinction sensors can be applied additive- agglomerates (µm-range) dispersion process dispersed additives (nm-range) single particle analysis >20µm, lowest concentrations particle size and particle concentration integral particle analysis >300nm, low concentrations (<5 vol.-%) particle size or particle concentration inline measurements at various extruder position changes in particle situation can be observed (disagglomeration of nanoparticle agglomerates)

15 Summary Application PMPxyz sensors on nanocomposites extrusion processing may be usefull applicable to a direct monitoring of nanoparticle agglomerates in a flowing polymer melt from inside a twin screw extruder get in-process realtime informations about dispersion progress of nanoparticle agglomerates (µm-range observation by single particle counting) get in-process realtime informations about primary nanoparticle size (nm-range observation by turbitity analysis) get both particle informations simultaneously

16 Contact Leibniz - Institute of Polymer Research stephan@ipfdd.de our partners: Dresden University of Technology TOPAS

17 APPENDIX

18 Sensor Configuration Users Input: particle type (gels, black spots, unmolten granules, gas bubbles) particle size particle concentration access to extruder (inline, bypass) Sensor Setup: extinction / backscatter measurement optical setup (measuring volume, layer thickness, focus) signal processing Sensor Output: particle size detection limit sampling statistics

19 Sensor Overview several sensors with different setups for various applications developed + tested optimization of a sensor for each special application necessary

20 Co-Operating Partners high performance polymers cellulosic fibers polymer producer multilayer pipes colored masterbatches plastics recycling machines labscale extruders industrial extruders melt filters

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