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RheoSANS at the NIST-CNR...NIST, NG-7, stress control rheometer radial tangential The Guts •Quartz...

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RheoSANS at the NIST-CNR NG7 SANS Beam Line B Greenwald NIST/UMD, Gaithersburg MD, USA
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Page 1: RheoSANS at the NIST-CNR...NIST, NG-7, stress control rheometer radial tangential The Guts •Quartz windows •Temperature range –10 to 90 C •1.5 mm Gap •Sample loading The

RheoSANS at the NIST-CNRNG7 SANS Beam Line

B Greenwald NIST/UMD, Gaithersburg MD, USA

Page 2: RheoSANS at the NIST-CNR...NIST, NG-7, stress control rheometer radial tangential The Guts •Quartz windows •Temperature range –10 to 90 C •1.5 mm Gap •Sample loading The

The Rheometer

• Paar Physica USD200*• Radial and tangential

configuration• Quartz or titanium Couette

type flow cells• Gaps of 0.5 or 1mm• Temperatures ranging from

–20°C to 150°C• Solvent trap preventing

solvent evaporation

* The mention of commercial equipment does not imply endorsement by the National Institute of Standards and Technology

Page 3: RheoSANS at the NIST-CNR...NIST, NG-7, stress control rheometer radial tangential The Guts •Quartz windows •Temperature range –10 to 90 C •1.5 mm Gap •Sample loading The

Radial and Tangential?

Couette shear cell

NIST, NG-7, stress control rheometer

radial

tangential

• Radial: Perpendicular to Shear Velocity• Tangential: Parallel to Shear Velocity

Page 4: RheoSANS at the NIST-CNR...NIST, NG-7, stress control rheometer radial tangential The Guts •Quartz windows •Temperature range –10 to 90 C •1.5 mm Gap •Sample loading The

Quartz vs Titanium

Page 5: RheoSANS at the NIST-CNR...NIST, NG-7, stress control rheometer radial tangential The Guts •Quartz windows •Temperature range –10 to 90 C •1.5 mm Gap •Sample loading The

Slit Packages and Alignment

•Radial aperture and tangential slit package

•Boron Aluminum backed with Cadmium

•1 cm aperture for radial measurement

•0.3, 0.5, 0.6, 0.8 mm tangential slits

Page 6: RheoSANS at the NIST-CNR...NIST, NG-7, stress control rheometer radial tangential The Guts •Quartz windows •Temperature range –10 to 90 C •1.5 mm Gap •Sample loading The

Slit Packages and Alignment

•2 micrometer screws in the X and Y plane and 2 screws to adjust the tilt aid in alignment of cup with bob

Page 7: RheoSANS at the NIST-CNR...NIST, NG-7, stress control rheometer radial tangential The Guts •Quartz windows •Temperature range –10 to 90 C •1.5 mm Gap •Sample loading The

Slit Packages and Alignment

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

1.1

23 24 25 26 27 28

Tran

smis

sion

Cell rotation axis to beam (slit*) edge (mm)

air

out

slitedge*

slitwidth

slitwidth

•Transmission measurements across gap

•Changes are interception with material boundaries

•Alignment indicated by arrow marked “slit edge”

Page 8: RheoSANS at the NIST-CNR...NIST, NG-7, stress control rheometer radial tangential The Guts •Quartz windows •Temperature range –10 to 90 C •1.5 mm Gap •Sample loading The

Technical Attributes

Accuracy 1% of maximum value

Minimum Torque 150 mNm

Torque Resolution 0.01 µNm

Speed Range 10-4 to 1000 min-1

Shear Rate Range 1.3*10-4 to 4.8*103 s-1

Shear Stress Range 0.67 to 3.5*104 Pa

Viscosity Range 1.7*10-3 to 2.7*108 Pas

Temperature Range -20 to 90 °C

Volume 8, 12 mL

Gap Size 0.5, 1 mm

Technical Specifications

•Temperature control by passing heated N2 gas by the cell

•0.5 and 1 mm gaps requiring 8 and 12 mL respectively

•Solvent trap to prevent evaporation of solvent during experiment

Page 9: RheoSANS at the NIST-CNR...NIST, NG-7, stress control rheometer radial tangential The Guts •Quartz windows •Temperature range –10 to 90 C •1.5 mm Gap •Sample loading The

1-2 Plane Shear Cell

Page 10: RheoSANS at the NIST-CNR...NIST, NG-7, stress control rheometer radial tangential The Guts •Quartz windows •Temperature range –10 to 90 C •1.5 mm Gap •Sample loading The

1-2 Plane?

• Parallel to Vorticity direction• Degree of Structural Anisotropy• Direction of Anisotropy within the plane

Couette shear cell

NIST, NG-7, stress control rheometer

radial

tangential

Page 11: RheoSANS at the NIST-CNR...NIST, NG-7, stress control rheometer radial tangential The Guts •Quartz windows •Temperature range –10 to 90 C •1.5 mm Gap •Sample loading The

The Guts•Quartz windows

•Temperature range –10 to 90 C

•1.5 mm Gap

•Sample loading

Page 12: RheoSANS at the NIST-CNR...NIST, NG-7, stress control rheometer radial tangential The Guts •Quartz windows •Temperature range –10 to 90 C •1.5 mm Gap •Sample loading The

The Assembly and Technical Attributes

Technical specifications:- Path length 5 or 7mm- Gap 1.5mm- Sample volume ~10ml- Slit 0.2,0.4 mm x 3mm- Shear rate 0.01-500s-1

Page 13: RheoSANS at the NIST-CNR...NIST, NG-7, stress control rheometer radial tangential The Guts •Quartz windows •Temperature range –10 to 90 C •1.5 mm Gap •Sample loading The

Thanks!

www.ncnr.nist.gov/sans/programs/equipment/rheometer.html

L Porcar1,2, P D Butler2, N Wagner3

1University of Maryland; College Park, MD 207052NIST Center for Neutron Research; Gaithersburg, MD 20899

3University of Delaware; Newark, DE 19716


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