Resident faculty with labs30

Affiliated faculty~70MATSE, Phys, Chem, MecSE, ECE, BioE, Aero

Business OfficeFinancial operationsGrants application / support

Computer FacilitiesEngineering IT

Store roomLab/office suppliesShipping/receiving

Lab safety engineerCoordination with CoE safety and DRS

MRL central research facilitiesOpen user access, 24/7/365Shared instrumentation20 staff140 instruments> $ 50M set of tools

Main instrumentation cores:• Electron Microscopy• Nanofabrication • Scanning Probe• Surface Science• Optical Spectroscopy• X‐ray• Soft Materials Lab

IllionoisMaterials Research Laboratory

College of EngineeringUniversity of Illinois at Urbana‐Champaign

NanoMFG nodeWorkshop

Feb 26‐27, 2019

MRL – Central Research Facilities instrumentation cores:

Electron Microscopy(including bio analysis services)

Micro/Nanofabrication facility(including mask fabrication services)

Scanning Probe 

Microscopy

X‐ray analysis

Laser and spectroscopy 

facility

Surface Analysis Thermal Properties and 

Soft Materials Analysis

MRL – Central Research Facilities:

FY 2018: • 949 active users• 76,646 hours of instrument time

Grad students(552)

Undergrad students

(142)

Senior researchers(255)

Educational missionResearch trainingResearch support

24/7 open accessTraining, staff assist20 research scientist, 3 engineersLowest user fees in the countryBioMaker, MRSEC, IQUIST

Laser & Spectroscopy: Keyence VX1000 Laser Confocal 3D optical profiler Neaspec AFM/IR System Nanophoton Confocal Raman Microscope Zeiss Live 7 high-speed scanning confocal microscope Woollam V-VASE Spectroscopic Ellipsometer Gaertner L116C Ellipsometer Ti: sapphire Laser Pump/probe systems for Time-Domain

Thermo Reflectance Witec AFM/SNOM/Confocal Microscope Thermo Nexus 670 FTIR Optronic Laboratories OL750 Spectroradiometer (solar cell

and light detector QE measurement system) Agilent Cary 5000 Spectrophotometer Varian Cary 5G Spectrophotometer Polarizing/DIC Inverted Materials Microscope Time-resolved/Low Temperature Photoluminescence Sum Frequency Generation Rame-Hart Model 260 Contact Angle Goniometer Solar Simulator (based on a 300W Xe lamp)

NanophotonConfocal Raman 11 Microscope

Neaspec AFM/FTIR NSOM

~ 10‐500 Mb

~ 3‐5 Mb

~ 1‐5 Mb

~ 0.1‐10 Mb

~ 0.5‐100 Mb

~ 10‐100 Kb

~ 100 Kb

<50 Kb

<5 Kb

<10 Kb

<300 Kb

Accelerators: NEC Pelletron (RBS analysis) HV van de Graaf (ion implantation)

Surface Analysis: Kratos AXIS ULTRA XPS (2 systems) PHI 5400 XPS PHI Trift III TOF-SIMS PHI 660 Auger Spectrometer CAMECA LEAP 5000 XS Atom Probe

Tomography (soon)

NEC Pelletron accelerator for RBS

PHI 660 Auger system

Kratos XPS

PHI TOF-SIMS

< 1 Mb

~ 500 Mb

Nd O

Nd distribution near grain boundary in CeO2:NdD.R. Diercks et al, J. Mat. Chem A4, 5167 (2016)

Coming soon to theMRL Central Research Facilities

CAMECA LEAP 5000XS

Atom Probe Tomography

• 3D image + chemical composition at atomic scale

• Resolution: 0.3‐0.5 nm lateral, 0.1‐0.3 nm depth

www.cameca.com

www.cameca.comNiFeAlCr‐based superalloy

Malvern Zetasizer633 nm laser, reflective lightparticle sizes 0.6 nm – 6 m (in solution)

TA Q50 Thermogravimetric Analysis (TGA)Weight change vs. temperature, timeBalance sensitivity 0.1 mg. capacity 1 gfrom RT up to 1000 oC, inert or reactive gas

TA D2500 Differential Scanning Calorimeter (DSC)Heat flow difference between sample and reference heated at same temperaturesPhase transitions, chemical reactions, glass transitions, crystallization, melting, cure kinetics-150 oC to 400 oC (TGA analysis required first)

Shimadzu DTA50 Differential Thermal Analyzer (DTA)Temperature difference between sample and reference, same heat conditionsfrom RT up to 1400 oC, under nitrogen gas(TGA analysis required first)

TA Q800 Dynamical Mechanical Analysis (DMA)Young’s module, viscosity vs. temperature, timeTensile or cantilever bending testing-150 oC to 600 oC

Tosoh HLC‐8320 Size Exclusion Chromatography (SEC, GPC)Molecular mass analysis, from RT up to 50oCRI refractive index change detectorSolvents THF, DMF, NMP, etc.

Bio services:microtoming, embedding, staining, sample prep including cryo EMOptical and electron microscopy

TA Instruments Discovery 2500 DSC

Soft Materials Analysis:

Malvern Zetasizer

TA Q800 DMA

Tosoh EcoGPC

~ 1 Mb

~ 100 Kb

~ 3 Mb

~ 1 Mb

~ 1 Mb

~ 1 Mb

Scanning Probe Microscopy:

Asylum Cypher AFM Max: lateral 30 x 30 m2, depth 5 mviscoelasticity maps, PFM, blueDrive photothermal, STM

Asylum Research MFP‐3D AFM (2)Max: lateral 90 x 90 m2, depth 15 mClosed fluid cell, heater up to 300 oC, scanning microwave impedance

Hysitron TI‐950 Tribo‐IndenterLoads: ~ mN to 2.8 N; displacements up to 90 mIndentation, scratch test, nanoECR, fractureRT up to 400 oC

Optics11 Piuma indenter for soft materialsLoads: ~ 10 Pa – 1 GPa, displacements up to 20 mOperates in air or in fluids

Sloan Dektak3 ST profilersurface profiler using a diamond-tipped stylusmeasurable height range: few nm to 105 m

Asylum Research Cypher AFM

< 5 Mb

PANalytical X’PertMRD XRD

X-ray Scattering:

Bruker D8 Advance with Eiger2 areal detector and HKT1200N hot stage RT to 1200oC

PANalytical X’pert MRD (2)

DHS900 dome hot stage for X’pert systems

Siemens/Bruker D5000 powder XRD

Dexco Multi-wire Real Time Laue

Forvis Small Angle X-ray Scattering with Pilatus 300 Detector and in-situ capabilities

Shimadzu 7000 ED x-ray fluorescence system

Bruker D8 Advance

Forvis SAXS/WAXS

< 1 Mb

Nanoscribe Photonic ProGT 3D printer

Micro/Nanofabrication facility: 1500 sq. ft. class-100 clean room with spinners, optical aligners

and facilities for optical lithography. Raith eLine e-beam lithography system 600 sq. ft. class-100 clean room for e-beam lithography preparation Nanoscribe 3D printer with sub-micron resolution Sputtering deposition systems (4) E-beam evaporators (3) ALD systems (2) PECVD (2) Reactive Ion Etching (4) Furnaces and RTA facilities Mask fabrication facilities and services Low-temperature device testing and parameter analyzer

AJA Orion-8 Magnetron Sputtering System

Kurt J. Lesker Nano36 thermal evaporator

Raith eLine E-beam Lithography System

< 10 Mb

< 10 Mb

< 20 Mb

~ 100 Kb

Transmission Electron Microscopy: FEI Themis Z analytical (S)TEM Hitachi H-9500 DE-TEM JEOL 2200FS (S)TEM JEOL 2010F STEM JEOL 2100 Cryo TEM JEOL 2010 LaB6 TEM Hitachi H600 TEM

Scanning Electron Microscopy: JEOL 6060LV SEM Hitachi S-4800 SEM Hitachi S-4700 SEM JEOL 7000F Analytical SEM FEI Helios Nanolab 600i Dual Beam FIB FEI Scios 2 Dual Beam FIB FEI Strata 235 Dual Beam FIB

Sample Prep tools: Gatan PECSII Pro ion beam polisher Gatan PIPS ion miller (2) FEI Vitrobot Leica Cryo Ultramicrotome UC6/FC6 Ultramicrotomes and bio services SEM/TEM sample prep labs (3)

Hitachi H9500 DETEM

ThermoScios 2DB FIB

ThermoThemis Z TEM/STEM

~ Tb

~ 1 – 30 Mb

~ 10 – 100 Mb

Microfluidics synthesis of gene silencing cubosomes 

Lipide/ethanol

Staggered Herringbone Mixer Microfluidics device fabricated in the MRL Microfab(MRL in‐house mask fabrication service, then cleanroom work using Su‐8 photoresist, MJB3 mask aligner, UV exposure, Harrick Plasma cleaner, PDMS mold, etc.)

EthanolRemoval 

~ 200 m

Small monodisperseethanol‐in‐water droplets

Monodisperse small ~ 200 nm cubosomes in t<15min

H. Kim, J. Sung, Y. Chang, A. Alfeche, C. Leal ACS Nano (2018)

Cubosomes: lipid‐based NPs where membranes and pores form a cubic lattice

Cryo‐EM of gene silencing cubosomes H. Kim, J. Sung, Y. Chang, A. Alfeche, C. Leal ACS Nano (2018)

MRL Cryo TEM images for various times “t” of ethanol removal:

50 nm dropletsmonodispersive

emulsion

Droplets fusingin strings and 

clusters

Membranes fused. NPs rim of lipid bilayer structure

Ethanol‐depleted membranes in primitive cubic 

structure.

Cubosomes: cubic cell in a lipid leafletYellow: bilayer midplanesBlue: water channels

SAXS

Cryo‐EM of gene silencing cubosomes H. Kim, J. Sung, Y. Chang, A. Alfeche, C. Leal ACS Nano (2018)

MRL Cryo TEM: gene‐silencing siRNA with Au NP conjugates (markers)

Cryo‐TEM images and electron density maps show that cubosomes can be loaded with siRNA without disrupting the structure. Au‐NP used as markers to 

Ordered liquid membrane (green) in a square lattice, and water channels (red)

siRNA‐AuNP

siRNA‐AuNP

Detection limits vs. spot size

Detection limits vs. spot size

Multi‐tools, techniques challenges & opportunities:

‐ Work flow starting from design‐ Integration of steps: design, fabrication, processing, modification and analysis‐ Complementarity of techniques: wider view vs. potential conflicts