STM-ProGold

Slide 1: 

Material Science and Technology Research Group (STM) Dipartimento di Ingegneria Meccanica e Industriale Università Roma TRE Introducing STM to Progold Emailed – 25/01/2011 Edoardo Bemporad

Where is the University “Roma Tre”? : 

Where is the University “Roma Tre”? 30 min from Fiumicino airport 10 min walkpath from Metro B 20 min from railway station 35 min from the center of Rome (by taxi) E. Bemporad, gennaio 2011 Introducing STM to Progold 2

LIME from Google Earth : 

LIME from Google Earth E. Bemporad, gennaio 2011 Introducing STM to Progold 3

Roma Tre, some numbers… : 

Roma Tre, some numbers… Founded in 1992. One of the 4 State University in Rome (9 in total). 175.000 m2. More than 40.000 students (4.100 enrolled in Engineering) More than 700 Researchers and Professors. Faculty of Engineering: Civil Computer Science Electronic Mechanical Materials Science and Technology research group (STM Group) www.uniroma3.it E. Bemporad, gennaio 2011 Introducing STM to Progold 4

Slide 5: 

www.stm.uniroma3.it STM Roma TRE channel on YouTube: http://www.youtube.com/user/STMRomaTRE Image Gallery on flickr http://www.flickr.com/photos/stmdimiuniroma3/ E. Bemporad, gennaio 2011 Introducing STM to Progold 5

Slide 6: 

www.lime.uniroma3.it E. Bemporad, gennaio 2011 Introducing STM to Progold 6

Mission : 

Study of surface properties of systems for advanced mechanical engineering and micro-devices applications, through numerical and analytical modeling, advanced characterization methods, technological, mechanical, tribological and chemical tests. Development of advanced multi-scale methodology related with morphological, micro-structural and micro-analytical characterization of materials through optical, ionic, electronic and contact probes. Mission E. Bemporad, gennaio 2011 Introducing STM to Progold 7

Vision : 

Coupling nano-mechanical testing with high resolution microscopy High-resolution depth-resolved nano-scale mechanical characterization of engineered surfaces and multiphase materials; (Sub)microscale analysis of residual stress and stress gradients in thin coatings and complex structures FIB-SEM-TEM-AFM investigation of nano-scale deformation mechanisms and influence of microstructures on mechanical and functional behavior; Roughness and inducing roughness methods Vs surface energy: measurement and dependence with surface chemistry Future: expanding to processing MS-PVD enhanced: effect of deposition parameters on performances (adhesion, wear, bio, others..) Vision E. Bemporad, gennaio 2011 Introducing STM to Progold 8

STM Group: Vision : 

Product/process optimization (service) Improving of understanding capabilities STM Group: Vision E. Bemporad, gennaio 2011 Introducing STM to Progold 9

STM Group: Research Strategy : 

STM Group: Research Strategy Development of methodologies for materials processing optimisation by the use of the paradigm: nanostructure-microstructure–properties-performances Multiscale and multidisciplinaryapproach Modelling and simulating inservice behaviour, reliabilityand degradation modes (materials oriented) Optimization and failure analysis Material system Design E. Bemporad, gennaio 2011 Introducing STM to Progold 10

We keep attention to: : 

We keep attention to: Workflow concerns Privacy Timing Cost control Reporting Data and samples handling concerns Redoundancy Affordability Accessibility Privacy Report standardization (Corporate Identity) Everything is managed inside our intranet using Microsoft Sharepoint™ CMS E. Bemporad, gennaio 2011 Introducing STM to Progold 11

STM Group: : 

2 Full professors 5 researchers 1 graduated technicianmechanical engineer 2 Ph.D Studentsmaterials science and engineering 1 fellowships(1 Jr mechanical Engineers) 1 staff 4 undergraduate (average) doing their “Laurea” thesis STM Group: E. Bemporad, gennaio 2011 Introducing STM to Progold 12

STM Facilities: 4 laboratories (500m2 tot) : 

STM Facilities: 4 laboratories (500m2 tot) 1. LIME, Electron Microscopy lab Ion / Electronic / Stylus / Optical 2. MatEDP, Materials Modeling lab 15 PC stations, Thermocalc, ANSYS, ABAQUS, Elastica, EFS,… 3. MaTec, Materials Technology lab Mechanical characterization (Hardness, Micro-hardness, Abrasive Wear, Scratch), Salt Spray 4. MaDep, Coating technologies Lab 2 equipments (in development) based on High Power Impulse Magnetron Sputtering for residual stress investigation (duty cycle, bias, thicknesses, chemistry, process gases…) E. Bemporad, gennaio 2011 Introducing STM to Progold 13

Slide 14: 

Imaging, milling and deposition E. Bemporad, gennaio 2011 Introducing STM to Progold 14

Lime Lab: SEM (FEI) : 

Lime Lab: SEM (FEI) 30 Kv LaB6 filament Secondary electrons Backscattered electrons EDS to B, line & maps Cathode luminescence Specimen Current E. Bemporad, gennaio 2011 Introducing STM to Progold 15

Lime Lab: TEM (FEI) : 

Lime Lab: TEM (FEI) 120kV LaB6 filament Double tilt EDS to B, point & line nanoprobe E. Bemporad, gennaio 2011 Introducing STM to Progold 16

Lime Lab: AFMs (1 NT-MDT + 1 DI) : 

Lime Lab: AFMs (1 NT-MDT + 1 DI) 50x50x5 microns range All modes (contact, non contact, lateral force,…) E. Bemporad, gennaio 2011 Introducing STM to Progold 17

Lime Lab: DualBeam (FEI) Helios 600 Nanolab : 

Lime Lab: DualBeam (FEI) Helios 600 Nanolab early 2008 - Omnprobe - GIS (4 gases) - STEM - EDS (Oxford) E. Bemporad, gennaio 2011 Introducing STM to Progold 18

DualBeam (FEI) : 

DualBeam (FEI) SEM Column: spatial resolution 0,69 nm @ 15 kVFIB Column: spatial resolution5 nm @ 30 kV E. Bemporad, gennaio 2011 Introducing STM to Progold 19

Principal FIB modes: : 

Principal FIB modes: Milling Imaging Deposition E. Bemporad, gennaio 2011 Introducing STM to Progold 20

Lime Lab: DualBeam (FEI) : 

Lime Lab: DualBeam (FEI) 0,69 nm res E. Bemporad, gennaio 2011 Introducing STM to Progold 21

FIB modes: Ion imaging : 

FIB modes: Ion imaging Voltage contrast: insulators appear dark while grounded conductors are bright. Materials contrast: differences in yield of secondary particles due to the way energy is lost in the material. Crystallographic orientation contrast (channeling contrast): incident ions are channeled down between lattice planes of the specimen. E. Bemporad, gennaio 2011 Introducing STM to Progold 22

FIB modes: Ion Milling : 

FIB modes: Ion Milling E. Bemporad, gennaio 2011 Introducing STM to Progold 23

Using a DualBeam to characterize samples; what is new with respect to conventional characterization route? : 

Accurately localize the region of interest(within few nanometers) Possibility to reveal microstructure beneath the surface with very little or practically no artifacts Time to produce a TEM lamellae(within a couple of hours) EDS and Scanning Transmission Imaging within the DualBeam also available Using a DualBeam to characterize samples; what is new with respect to conventional characterization route? E. Bemporad, gennaio 2011 Introducing STM to Progold 24

Cross sections : 

Cross sections 25 E. Bemporad, gennaio 2011 Introducing STM to Progold

Hard inclusion in a soft metal : 

Hard inclusion in a soft metal E. Bemporad, gennaio 2011 Introducing STM to Progold 26

Characterization with Dual Beam Microscopy : 

Characterization with Dual Beam Microscopy 27 E. Bemporad, gennaio 2011 Introducing STM to Progold

Characterization with Dual Beam Microscopy : 

Characterization with Dual Beam Microscopy 28 Rockwell C adhesion test Multiscale and multitechnique approach to mechanical characterization of tribological coatings E. Bemporad, gennaio 2011 Introducing STM to Progold

Characterization with Dual Beam Microscopy : 

Characterization with Dual Beam Microscopy 29 Multiscale and multitechnique approach to mechanical characterization of tribological coatings Scratch test Lc3 failure E. Bemporad, gennaio 2011 Introducing STM to Progold

TEM sample preparation with FIB : 

TEM sample preparation with FIB The sample surface is investigated before cutting to determine the area of interest. Then the sample is milled and polished with predefined milling patterns Time for a lamella preparation: less then 2hours with expert operator 30 E. Bemporad, gennaio 2011 Introducing STM to Progold

TEM lamellae extraction : 

TEM lamellae extraction 31 E. Bemporad, gennaio 2011 Introducing STM to Progold

Site specific TEM X-View : 

Site specific TEM X-View E. Bemporad, gennaio 2011 Introducing STM to Progold 32

Site specific TEM X-View : 

Site specific TEM X-View E. Bemporad, gennaio 2011 Introducing STM to Progold 33

Slide 34: 

34 Site specific TEM X-View E. Bemporad, gennaio 2011 Introducing STM to Progold

Slide 35: 

35 Roughness E. Bemporad, gennaio 2011 Introducing STM to Progold

Slide 36: 

36 AFM (contact mode) Monolayer ZrN PVD magnetron sputtering Ra=14,6nm E. Bemporad, gennaio 2011 Introducing STM to Progold

Roughness : 

Roughness 37 E. Bemporad, gennaio 2011 Introducing STM to Progold

Differenti tecniche di analisi della topografia superficiale : 

Differenti tecniche di analisi della topografia superficiale 38 E. Bemporad, gennaio 2011 Introducing STM to Progold

Profilometer (non contact, both confocal and interferometric) : 

Profilometer (non contact, both confocal and interferometric) 39 Interferometric head: (sub)nanometer resolution in roughness analysis Confocal head: analysis of complex shapes with high z-range E. Bemporad, gennaio 2011 Introducing STM to Progold

Lime-lab Self-producing of standard samples for instruments calibration : 

Lime-lab Self-producing of standard samples for instruments calibration E. Bemporad, gennaio 2011 Introducing STM to Progold 40

Lime-lab Self-producing of standard samples for instruments calibration : 

Calibration of the profilometer Lime-lab Self-producing of standard samples for instruments calibration E. Bemporad, gennaio 2011 Introducing STM to Progold 41

Atomic Force Microscopy (AFM) : 

Atomic Force Microscopy (AFM) AFM of a Ag-Cu-Ge ternary system showing the two main phases of the alloy (dark and brighter zones) Principles of Atomic Force Microscopy GeOx layer on metal alloy E. Bemporad, gennaio 2011 Introducing STM to Progold 42

Atomic Force Microscopy (AFM) : 

Atomic Force Microscopy (AFM) SPM (contact mode) Peak to peak, Rmax = 137.592 nm Mean, Rmean=567.860 nm Roughness, Ra = 22.367 nm Root-Mean-Sq, Rq = 27.541 nm Skewness, Rsk = 0.036 Kurtosis, Rku = 2.642 E. Bemporad, gennaio 2011 Introducing STM to Progold 43

Slide 44: 

Wear and corrosion test E. Bemporad, gennaio 2011 Introducing STM to Progold 44

MaTec Lab: Wear test : 

MaTec Lab: Wear test Wear test device (prototype) Dynamic measurement of wear and friction coefficient at the micron scale E. Bemporad, gennaio 2011 Introducing STM to Progold 45

MaTec Lab: Wear test : 

MaTec Lab: Wear test E. Bemporad, gennaio 2011 Introducing STM to Progold 46

MaTec, Wear Tests : 

MaTec, Wear Tests E. Bemporad, gennaio 2011 Introducing STM to Progold 47

MaTec Lab: Salt Spray 1m3 chamber : 

MaTec Lab: Salt Spray 1m3 chamber E. Bemporad, gennaio 2011 Introducing STM to Progold 48

Slide 49: 

Lab scale small deposition plants E. Bemporad, gennaio 2011 Introducing STM to Progold 49

MaDep, deposition equipments: first steps : 

MaDep, deposition equipments: first steps E. Bemporad, gennaio 2011 Introducing STM to Progold 50

MaDep, deposition equipments: first steps : 

MaDep, deposition equipments: first steps E. Bemporad, gennaio 2011 Introducing STM to Progold 51

Slide 52: 

Micro and Nano mechanical test E. Bemporad, gennaio 2011 Introducing STM to Progold 52

MaTec Lab: Scratch tester : 

MaTec Lab: Scratch tester Depth profiling Applied force feedback controlled Acoustic emission sensor Friction force measurement E. Bemporad, gennaio 2011 Introducing STM to Progold 53

Macro-scale Instrumented spherical indentation : 

Macro-scale Instrumented spherical indentation Prototipal instrument for macro-scale spherical indentation The stress-strain curve is obtained by least-square fitting of exp data with a FEM-modelled database of L-h curves E. Bemporad, gennaio 2011 Introducing STM to Progold 54

MaTec Lab: Hardness Testers : 

MaTec Lab: Hardness Testers Vickers Knoop E. Bemporad, gennaio 2011 Introducing STM to Progold 55

Roma TRE nanohardness tester : 

Roma TRE nanohardness tester E. Bemporad, gennaio 2011 Introducing STM to Progold 56

Roma TRE nanohardness tester : 

Roma TRE nanohardness tester Berkovich tip E. Bemporad, gennaio 2011 Introducing STM to Progold 57

Slide 58: 

Physico-chemical surface properties E. Bemporad, gennaio 2011 Introducing STM to Progold 58

MaTec Lab: Contact Angle and Wettability : 

MaTec Lab: Contact Angle and Wettability Uni en 828 and ASTM D5725 - 99 E. Bemporad, gennaio 2011 Introducing STM to Progold 59

semi-automated instrument for contact angle measurement and surface free energy models : 

semi-automated instrument for contact angle measurement and surface free energy models SFE models: Zisman Neumann Girifalco Fowkes Owens-Wendt Van Oss-Chaudhury-Good E. Bemporad, gennaio 2011 Introducing STM to Progold 60

Pendant drop method : 

Pendant drop method This method allows to measure surface tension of: Liquids Resins Polymers Varnishes Glues Hu-Reed equation Bashfort-Adams equation Where: E. Bemporad, gennaio 2011 Introducing STM to Progold 61

Slide 62: 

Stress trasmission in adhesive joint is due to interface properties. The interface represent a critical zone because of the presence of the weak forces (adhesive force): Composite material-metal Composite material-composite material Composite material-ceramic E. Bemporad, gennaio 2011 Introducing STM to Progold 62

Improvement of equipment & new procedure to measure wettability : 

Improvement of equipment & new procedure to measure wettability On tilted surfaces (feasibility to measure dynamic contact angle) 20° 25° 30° Measure of shape drops E. Bemporad, gennaio 2011 Introducing STM to Progold 63

Dynamic contact angle : 

Energy adhesion Hysteresis of the liquid drop Dynamic contact angle E. Bemporad, gennaio 2011 Introducing STM to Progold 64

Why to study dynamic contact angle? : 

Why to study dynamic contact angle? Microfluidic systems Hydrophilic/Hydrophobic coatings E. Bemporad, gennaio 2011 Introducing STM to Progold 65

Slide 66: 

Captive Bubble Alternative way to measure wettability and surface free energy. Components in contact with more liquids (es. microfluidic systems). Measures of wettability of gas bubbles (es. air behavior around wings and other lifting surfaces in aeronatical applications). Measures of adhesion phenomena concerning liquid nanofiltration device (es. polymeric membranes having both low adhesion phenomena in order to reduce their contaminations and able to have a hydrophilic behavior in order to have high level of liquid permeation) Measures of the wettability of hydrophilic polimers with high water absorption (es. idrogel). E. Bemporad, gennaio 2011 Introducing STM to Progold 66

Surface Treatments : 

Polymeric surfaces have low surface free energy, therefore it is necessary to use surface treatments that allow to improve this surface property. The surface treatments involve: Surface Treatments New functional groups (typically O-radical groups); Morphological changes; Improvement of the surface free energy; Improvement of the wettability; Increase of the bonding, printability, paintability, ecc… Preventive activation before metallization E. Bemporad, gennaio 2011 Introducing STM to Progold 67

Methods of the surface modifications : 

The treatments of organic surfaces are more complex respect to those inorganic. Low surface free energy Presence of di lubricants, plasticizers, ..…. High number of polymers with different properties. Mixing of the different polymers (es: blend, compound, ecc..) Methods of the surface modifications Meccanichal Chemical Physical Sandblast Grinding Polishing Sanding Acid etching Plasma Corona Flame UV-Ozone E. Bemporad, gennaio 2011 Introducing STM to Progold 68

Flame treatment : 

Flame treatment a - oxygen and propane pressure vessel, b - valves, c - flowmeters, d - no return flame valves, e - premixing chamber, f - nozzle, g - sliding alumina screen, h - sample holder disc, i - magnetic sensor, l - speedometer. E. Bemporad, gennaio 2011 Introducing STM to Progold 69

Slide 70: 

Process parameters: Propane/oxygen ratio Time of exposure Frequency of exposure Distance flame-sample Total flow rate Propane/oxygen ratio Total flow rate Frequency of exposure Time of exposure E. Bemporad, gennaio 2011 Introducing STM to Progold 70

Improvement and optimization of the surface free energy of polymeric substrates by Flame treatment : 

Improvement and optimization of the surface free energy of polymeric substrates by Flame treatment Surface Free Energy Wettability Optimization phase Errore:- < 2% su Wtot- < 1% su Wp - < 9 % su θ E. Bemporad, gennaio 2011 Introducing STM to Progold 71

Multiscale anaysis of Surface Free Energy without to alter the moprhology : 

Multiscale anaysis of Surface Free Energy without to alter the moprhology MACRO MICRO NANO Contact angle measurements Nanoindentation equipment Atomic Force Microscopy (AFM) Contact area = mm2 Contact area = µm2 Contact area = nm2 E. Bemporad, gennaio 2011 Introducing STM to Progold 72

Applications of surface free energy measurements at the micro & nanoscale : 

Applications of surface free energy measurements at the micro & nanoscale Debonding of reinforced fiber, fillers, boundles, ecc… in composite materials Debonding of fiber optic sensors in composites materials PROBLEM SOLUTION Chemical modification (grafting, etching, ecc…) Morphological modification (micro e nano-texturing, patterning, ecc….) Fiber optic within composite materials MMT Nanoparticles within epoxy foam E. Bemporad, gennaio 2011 Introducing STM to Progold 73

Slide 74: 

E. Bemporad, gennaio 2011 Introducing STM to Progold 74