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NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES Jeff Shield Department of Mechanical & Materials Engineering Nebraska Center for Materials and Nanoscience National Nanotechnology Coordinated Infrastructure University of Nebraska March 22-23, 2016

NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

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Page 1: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

NEBRASKA NANOSCALE FACILITYCHARACTERIZATION FACILITIES

Jeff ShieldDepartment of Mechanical & Materials Engineering

Nebraska Center for Materials and Nanoscience

National Nanotechnology Coordinated InfrastructureUniversity of Nebraska

March 22-23, 2016

Page 2: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

NNF

NNF WORKSHOP

NEBRASKA NANOSCALE FACILITY

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Page 3: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

NNF WORKSHOP

NNF Core Facilities

• Nanoengineering Research

• Scanning Probe & Materials Characterization

• X-ray Structural Characterization

• Electron Microscopy

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Page 4: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

CSI: Lincoln

Utilize materials characterization capabilities to uncover the secrets of a material’s behavior

• Probe microstructure properties/behavior

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Within the Nebraska Nanoscale Facility, we have many tools to probe microstructures at our disposal

Page 5: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

Functionalized Surfaces

Scanning a femtosecond laser over a smooth surface creates various features that can alter behavior• Hydrophobic/hydrophyllic

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X-ray diffraction can be used to characterize the base material• The NNF has a number of x-ray

diffractometers capable of a wide range of measurement techniques

lase

r

Page 6: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

Functionalized SurfacesSurface structure characterization

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Scanning electron microscopy (SEM) reveals surface morphology• The NNF has a number

of SEM instruments, most with chemical analysis capabilities

100 μm 20 μm

Laser scanning confocal microscope (Keyence VK-X) provides quantification of surface• Surface morphology parameters

such as relative surface area, peak-to-valley height, peak-to-peak distance

Page 7: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

10 μm

Functionalized SurfacesSub-surface characterization

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Dual-beam FIB/SEM (FEI Helios 660)• The focused ion beam (FIB) removes material,

allowing cross-sectional imaging and a view of the effects of processing on the material

Page 8: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

3D Imaging

Nebraska Sample 3 Avizo Movie.avi

Page 9: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

Scanning/Transmission Electron Microscopy

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Dual-beam FIB/SEM (FEI Helios 660)• The focused ion beam (FIB) can be used to

selectively make transmission electron microscope samples, too

1 μm

S/TEM (FEI Osiris, JEOL 2010)• Probe microstructure at a high

magnification (grain structure, structural defects, chemistry)

Page 10: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

What’s inside these?

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Page 11: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

What’s inside these?

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ChemiSTEM—collect x-rays from small regions to determine (very) local chemistry

10 nm

1 m

Page 12: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

And structural imaging

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Page 13: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

Other Capabilities

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Stratasys Objet 500 Connex3 3D printer (polymers)

. . . and coming soon: Metal3D printing!

Atomic force microscopy(AFM)

MicrohardnessOptical MicroscopyDifferential Scanning Calorimetry(DSC)Thermal Gravimetric Analysis (TGA)Thin film processing (RF/DC magnetron sputtering)

Page 14: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

NNF WORKSHOP

We have a wide variety of state-of-the-art capabilities to both

fabricate and characterize materials at many length scales

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10 nm

Page 15: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

NNF Facility for Scanning Probe & Materials Characterization

Thermal Analysis- DSC Thermal Analysis- TGA

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Page 16: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

NNF Facility for Scanning Probe & Materials Characterization

Optical Microscopy Tukon 2500 Hardness Tester

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Polyhydroxyaalkanoate (PHA) Knoop and Vickers Hardness

NNF

Page 17: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

NNF Facility for X-ray Characterization

Rigaku D/Max BBragg-Brentano (BB), 0D, Co-radiation

Powder XRD: Phase ID & Quantification, Residual stress analysis, Ideal for Ferrous samples, vertical sample mount

PANalytical EmpyreanBragg-Brentano (0 – 2D) , Cu-radiation

Powder XRD: Fast data collection, sample spinner, Automatic sample batch processing, Horizontal sample mount

Bruker D8 DiscoverParallel Beam (PB), 2D Large Area Detector & 0D, Hi-res Optics, Cu-radiation

Powder and Hi-Res XRD, Fast data collection, High Temperature XRD, XRR, Pole-Figure, vertical sample mount, capillary diffraction

Rigaku SmartLabBB & PB, Ultra Hi-Res optics0D & 1D detector, Cu-radiation

Powder and Ultra Hi-Res XRD, XRR, Grazing incidence In-plane XRD, In-plane pole figure, Small Angle X-ray Scattering (SAXS), reciprocal space mapping

Bruker PhotonParallel beam, CMOS detector (2D),Mo-radiation

Small Molecular Crystallography withTemperature range T ~ 100 – 500 K

Rigaku MultiflexBragg-Brentano (0D), Cu-radiation

Powder XRD: Phase ID & Quantification, Horizontal sample mount

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Page 18: NEBRASKA NANOSCALE FACILITY CHARACTERIZATION FACILITIES · March 22-23, 2016. NNF NNF WORKSHOP NEBRASKA NANOSCALE FACILITY 2. NNF WORKSHOP ... 3D printer (polymers). . . and coming

NNF Facility for Scanning Probe & Materials Characterization

Bruker Dimension ICON SPM

• Quantitatively nanomechanicalproperties (modulus: 1MPa--50GPa; adhesion: 10pN--10μN.)

• Conductivity mapping : charge distribution, surface potential distribution, etc.

• Nanomanipulation (indentation and lithography)

• Heating and Cooling: –30°C to +250°C

Dimension 3100 SPM System

EnviroScope Atomic Force Microscope

NNF