In Cooperation with DSM NeoResins by Sylvia Hanke

Outline Differential scanning calorimetry (DSC) Atomic force microscopy (AFM) Magnetic resonance profiling Gravimetry Tacking / Blocking Sliding Final summary table Sylvia Hanke,

Differential scanning calorimetry Sylvia Hanke, baseline Temperature/Time melting decomposing cristallization TgTg Heat flow

4Sylvia Hanke, A1A2B1B2 good/fast Low T g °C-3.7 °C-10.7 °C2.4 °C High T g °C123.0 °C102.7 °C92.1 °C A1A2B1B2 good/fast Low T g °C-3.7 °C-10.7 °C2.4 °C High T g °C123.0 °C102.7 °C92.1 °C MFFT (°C) < 0 => very soft and hard phases less soft and hard phases very soft and hard phases most similar phases

Atomic Force Microscopy Sylvia Hanke,

6 Height Phase PS (nm) A1 A nm r.m.s. roughness 35 nm r.m.s. roughness A2 has larger and harder particles, but differs not much from A1

7Sylvia Hanke, Height Phase PS (nm) B1 B nm r.m.s. roughness 25 nm r.m.s. roughness B1 has harder particles in a distinct matrix, B2 shows coalecsence

Sylvia Hanke, 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.

Magnetic resonance profiling Sylvia Hanke, 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

10Sylvia Hanke, A1 A2 B2B1

11Sylvia Hanke, A1 A2 B2B1

Skewness Sylvia Hanke, B1B2 Obviously, there is a skin formation in B2.

Tacking and Blocking experiments Sylvia Hanke, 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

Sylvia Hanke, 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

Sylvia Hanke, 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

Sliding experiments Sylvia Hanke, Test conditions: test speed 1 mm/s Applied Force 10 N Contact time 1min Contact area 1 cm² Thickness 200  m foil latex F

Sylvia Hanke, No clear trends because the measurement is very difficult. A2A1 B2B1

Thanks for your attention Summary table Sylvia Hanke, A1A2B1B2 T g (°C)-77.7 / / / / 92.1 MFFT (°C)6 – 12 < 0 AFMsmall and softlarger and hardharder particlescoalescense PS (nm)40 – 7550 – – Drying timefasterslowerfasterslower MRPuniform non-uniform Tackno trend 2 peakshigher values Block1 peak quickly to zerogradual fall Slidingno trend