Modular Microscope Accessory

Transcription

1 Modular Microscope Accessory Modular Microscope Accessory SAMPLE STRUCTURE OBSERVATION

2 DHR MMA Key Features Compact, modular design that directly installs to the DHR frame for easy alignment and minimal vibration Micrometer-controlled x-y-z stage to change position of observation Fast speed camera for image capture up to 90 fps, 640 x 480 pixels Brightfield and polarization microscopy with optional fluorescence Active temperature control up to 100 C using UHP with 1.1. mm quartz plate TA Instruments MMA Advantage DHR MMA Key Features Accepts standard microscopy objectives for maximum flexibility. Tested with: 20, and 40x and 1.1mm quartz plate 20, 50, and 100x and 0.17mm coverslip plate Field of view: 20X objective 320 x 240 m 2 40X objective 160 x 120 m 2 Optional stage with counter-rotation to observe features at a stagnant, zero-velocity plane Optional Piezo device for fine adjustment of the objective position permits 3D slices of microstructure 100 micron travel distance with step resolution of 0.5 micron TA Instruments MMA Advantage

3 Modular Microscope Accessory: Optical Path DHR Modular Microscope Accessory (MMA) Upper Heated Plate CCD Camera Optics Plate with Optional Counter-rotation Microscope Objective 3D Stage Vertical Piezo Stage LED Light Source

4 Brightfield Microscopy Calibration Grid, 20X 7 m Fluorescent PS Spheres, 20X Scale bar = 50 m Glass Spheres in PDMS, 20X 3D scan of hollow glass spheres, 20X Brightfield Microscopy: Emulsions Under Shear PDMS-PIB blend sample tested at 80 C Sample sheared at low shear rate (0.3 s -1 ) for 1 hour High shear rate (50 s -1 ) applied for 1 s, and sample allowed to relax

5 Polarization Microscopy: Light Crude Oil Pennysylvania crude oil sample cooled at 1 C/min Oscillation temperature ramp monitors changes in material properties Polarization Microscopy: Light Crude Oil Timelapse video of sample recorded in an independent experiment under identical temperature conditions Wax appearance temperature is in agreement with onset point from bulk rheology

6 Brightfield Microscopy: Emulsion Sample Water-Olive oil emulsion (20/80) stabilized by Cremodan-30 Shear 1.0 1/s scanning from bottom plate 100 m into the sample. Relative Motion Standard Rheo-Microscopy Counter-rotation Rheo-Microscopy Optional Accessory with MMA Software controls relative velocity ratio of upper to lower plates Adjust ratio to move stagnation plane up or down

7 Emulsion Sample: Counter-rotation Water-Olive oil emulsion (20/80) stabilized by Cremodan-30 Shear 1.0 1/s scanning from bottom plate 100 m into the sample. Stagnation plane Fluorescence Microscopy: Cheese Sample American Cheese stained with Nile Red dye Temperature ramp. 5º C/min. 1 Hz. Strain 2 %. 10º C

8 Fluorescence Microscopy: Cheese Sample American Cheese stained with Nile Red dye Temperature ramp. 5º C/min. 1 Hz. Strain 2 %. 20º C Fluorescence Microscopy: Cheese Sample American Cheese stained with Nile Red dye Temperature ramp. 5º C/min. 1 Hz. Strain 2 %. 30º C

9 Fluorescence Microscopy: Cheese Sample American Cheese stained with Nile Red dye Temperature ramp. 5º C/min. 1 Hz. Strain 2 %. 40º C Fluorescence Microscopy: Cheese Sample American Cheese stained with Nile Red dye Temperature ramp. 5º C/min. 1 Hz. Strain 2 %. 50º C

10 Fluorescence Microscopy: Cheese Sample American Cheese stained with Nile Red dye Temperature ramp. 5º C/min. 1 Hz. Strain 2 %. 60º C Fluorescence Microscopy: Cheese Sample American Cheese stained with Nile Red dye Temperature ramp. 5º C/min. 1 Hz. Strain 2 %. 70º C

11 Fluorescence Microscopy: Cheese Sample American Cheese stained with Nile Red dye Temperature ramp. 5º C/min. 1 Hz. Strain 2 %. 80º C Polarization Microscopy: Starch Gelatinization Corn Starch gelatinization Temperature ramp. 5º C/min. 1 Hz. Strain 0.3 %. Brightfield

12 Polarization Microscopy: Starch Gelatinization Corn Starch gelatinization Temperature ramp. 5º C/min. 1 Hz. Strain 0.3 %. Polarization Fluorescence Microscopy: Image Processing Fluorescently-dyed, 7 micron diameter Polystyrene spheres mixed in with test samples Publicly available image processing routines used to identify particle locations (1) Particle locations in videos were linked over time to construct particle trajectories Particle location and trajectory information used to quantify sample dynamics 50 m Raw Image (1): Particle Tracking using IDL, Bandpassed Image Features identified and overlaid on original image

13 Image Processing: Quantitative Analysis Average particle velocity along shear direction: 1 1,,., = location of the i th particle at time t, along the shear direction (x) = total time of observation = time between two frames = total number of particles tracked at time t and t- t Test Sample: Newtonian Fluid Fluorescent sphere solution mixed with glycerol Constant shear rate test under isothermal conditions at three different shear rates Microscopy video recorded at different heights along the gradient direction (z) using the piezo-ceramic focusing device Average particle velocity along shear direction determined at each height All videos recorded at radial location corresponding to applied shear rate (76% of plate radius)

14 Test Sample: Newtonian Fluid 125 Applied Shear Velocity ( m/s) Rate (1/s) x z y z-height ( m) Z height = Distance from lower glass plate Linear velocity profile observed Test Sample: Yield Stress Fluid Fluorescent particles added to commercially available hair gel material Sample subject to series of creep-recovery tests Creep for 120 s, recover for 240 s Microscopy video recorded during creep step (120 s) was processed and analyzed to quantify particle dynamics

15 Test Sample: Yield Stress Fluid Bulk rheology reveals a yield stress of 13 Pa Test Sample: Yield Stress Fluid Creep-Recovery at 9 Pa Creep-Recovery at 13 Pa

16 Thank You The World Leader in Thermal Analysis, Rheology, and Microcalorimetry