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In Cooperation with DSM NeoResins by Sylvia Hanke
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Outline Differential scanning calorimetry (DSC) Atomic force microscopy (AFM) Magnetic resonance profiling Gravimetry Tacking / Blocking Sliding Final summary table Sylvia Hanke, 17.03.20082
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Differential scanning calorimetry Sylvia Hanke, 17.03.20083 baseline Temperature/Time melting decomposing cristallization TgTg Heat flow
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4Sylvia Hanke, 17.03.2008 A1A2B1B2 good/fast Low T g -17.7 °C-3.7 °C-10.7 °C2.4 °C High T g 117.1 °C123.0 °C102.7 °C92.1 °C A1A2B1B2 good/fast Low T g -17.7 °C-3.7 °C-10.7 °C2.4 °C High T g 117.1 °C123.0 °C102.7 °C92.1 °C MFFT (°C)6 - 12 < 0 => very soft and hard phases less soft and hard phases very soft and hard phases most similar phases
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Atomic Force Microscopy Sylvia Hanke, 17.03.20085
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6 Height Phase PS (nm) A1 A2 40 - 75 50 - 65 14 nm r.m.s. roughness 35 nm r.m.s. roughness A2 has larger and harder particles, but differs not much from A1
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7Sylvia Hanke, 17.03.2008 Height Phase PS (nm) B1 B2 100 - 120 90 - 105 35 nm r.m.s. roughness 25 nm r.m.s. roughness B1 has harder particles in a distinct matrix, B2 shows coalecsence
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Sylvia Hanke, 17.03.20088 Gravimetry measurements Measurement of fraction of initial mass at RT, under static air. (thickness of the coatings d = 200 m) Solid content (130 min)Solid content (1 day)Solid content (DSM) A10,4530,4500,44 A20,4520,4460,44 B10,4600,4590,45 B20,4490,4460,45 Obviously, the loss of water takes a long time. A1 and B1 dry faster than the other components, but between B1 and B2 is just a very small difference.
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Magnetic resonance profiling Sylvia Hanke, 17.03.20089 Sample Coverslip RF Coil B0B0 Characteristics: 0.7 T permanent magnet (B 0 ) 17.5 Tm -1 gradient in the vertical direction (G) sample size: 2 * 2 cm static air G
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10Sylvia Hanke, 17.03.2008 A1 A2 B2B1
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11Sylvia Hanke, 17.03.2008 A1 A2 B2B1
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Skewness Sylvia Hanke, 17.03.200812 B1B2 Obviously, there is a skin formation in B2.
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Tacking and Blocking experiments Sylvia Hanke, 17.03.200813 glass plate latex probe (stainless steel) Test conditions: Pre-test speed 0.1 mm/s test speed 0.1 mm/s Post-test speed 1 mm/s Applied Force 4.9 N Contact time 1s Trigger Force 0.01 N Thickness 200 m
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Sylvia Hanke, 17.03.200814 B1 shows 2 peaks in tack but goes quickly to zero in the blocking. B2 shows higher values in tack but has a gradual fall in blocking. Tack Block B1B2
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Sylvia Hanke, 17.03.200815 A2 has no clear trend in tack but a peak in blocking and goes to zero in a longer time (<15‘). A1 has no clear trend in tack but a peak in blocking and goes quickly to zero (<10‘). Tack Block A1A2
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Sliding experiments Sylvia Hanke, 17.03.200816 Test conditions: test speed 1 mm/s Applied Force 10 N Contact time 1min Contact area 1 cm² Thickness 200 m foil latex F
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Sylvia Hanke, 17.03.200817 No clear trends because the measurement is very difficult. A2A1 B2B1
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Thanks for your attention Summary table Sylvia Hanke, 17.03.200818 A1A2B1B2 T g (°C)-77.7 / 117.1-3.7 / 123.0-10.7 / 102.72.4 / 92.1 MFFT (°C)6 – 12 < 0 AFMsmall and softlarger and hardharder particlescoalescense PS (nm)40 – 7550 – 65100 – 12090 - 105 Drying timefasterslowerfasterslower MRPuniform non-uniform Tackno trend 2 peakshigher values Block1 peak quickly to zerogradual fall Slidingno trend
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