Presentation of the
Material Science and Technology Research Group
University Roma TRE
Roma,, Italy
y
WEB SITE: www.stm.uniroma3.it and www.lime.uniroma3.it
Address: Via Vasca Navale
Navale,, 79 00146 – Roma
28/07/2009
Edoardo Bemporad
WHERE IS THE UNIVERSITY “ROMA TRE”?
2
ROMA TRE, SOME NUMBERS…
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www.uniroma3.it
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Founded in 1992.
One of the 4 State University in
Rome (9 in total).
175.000 m2.
More than 40.000
40 000 students
(4.100 enrolled in Engineering)
More
o e than
t a 700
00 Researchers
esea c e s and
a d
Professors.
Faculty of Engineering:
y
y
y
y
Civil
Ci
il
Computer Science
Electronic
Mechanical
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Materials Science and Technology
research group (STM Group)
3
MORE
INFO..
www.stm.uniroma3.it
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4
MORE
INFO..
www.lime.uniroma3.it
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5
OUTLINE
Research Group presentation
y People and research Partners
y Vision
y Facilities
| Ongoing
g
g research
| Research topics on surface mechanical
measurements and microstructure concerns,
future activities
|
6
STM GROUP:
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2 Full professors
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1 researcher
|
1g
graduated technician
mechanical engineer, Graduate Technician
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3 Ph.D Students
materials science and engineering
2 fellowships
(1 Sr + 1Jr mechanical Engineers)
| 1 staff
|
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3 undergraduate (average) doing their
“Laurea” thesis
7
PRINCIPAL RESEARCH PARTNERS (CUSTOMERS)
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Private Firms
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INFN – Laboratori Nazionali di
L
Legnaro
(Pd)
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ENEA Casaccia dipartimento
Materiali ((RM))
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Centro Sviluppo Materiali (RM)
National Universities
y Ancona
y Brescia
y Cagliari
y Firenze
y Milano
y Modena
y Napoli
y Roma 1
y Roma 2
y Torino
T i
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National Research Council
(CNR)
y Department of Molecular
Design
y Others involved in surface
engineering
University of Oxford
Department of Engineering
Science
SIO and Technische Universität
Chemnitz (Germany)
Central University of
Venezuela School of Metallurgy
Venezuela,
and Materials Science
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Lille University Laboratoire de
Mécanique
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University of Rosario
(Argentina)
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Karlsruhe Forschungszentrum
(Germany)
8
STM GROUP: VISION
Product/process
optimization
p
Improving off
understanding
capabilities
Characterization
methods: tuning
and/or specific
development
Needs of
phenomena
p
explanation
Development
Advanced
d
d use
Routine use
9
STM GROUP: RESEARCH STRATEGY
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Development of methodologies for materials
processing
p
g optimisation
p
by
y the use of the paradigm:
p
g
Coated system Design
nanostructure--microstructure–
nanostructure
microstructure–propertiesproperties-performances
Optimization and failure analysis
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Multiscale and multidisciplinary
p
y
approach.
Modelling and simulating in
service behaviour,, reliability
y
and degradation modalities (materials oriented)
10
WE
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KEEP ATTENTION TO:
Workflow concerns
y
y
y
y
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Privacy
Timing
Cost control
Reporting
D
Data
and
d samples
l handling
h dli
concerns
y
y
y
y
y
Redoundancy
Affordability
Accessibility
Privacy
Report standardization (Corporate Identity)
11
STM FACILITIES: 3 LABORATORIES + 1 (IN DEV.)
1. LIME, Electron Microscopy lab
y
Optical / Electronic / Stylus / (Ion Probing)
2. MatEDP,, Materials Modeling
g lab
y
10 PC stations, Thermocalc, ANSYS, ABAQUS,
Elastica, EFS,…
3. MaTec, Materials Technology lab
y
Mechanical
h
l characterization
h
((Hardness,
d
Microhardness, Abrasive Wear, Scratch), Salt Spray,
Fretting
g
4. CoaTec, Coating technologies Lab
y
Work in p
progress,
g
coating
g facility
y to be acquired
q
within year 2010 (enhanced PVD process)
12
STM FACILITIES: CONNECTION LAYOUT
Building one
Internet
Offices 2° floor
WAN Roma TRE
EXTRANET
HTTPS - Certificates
Building two
MatEDP 1° floor
PHILIPS XL 30 LaB6 ANALYTICAL
LIME
and
MaTec
PHILIPS CM 120 TEM
EDX (EDAX 134 E
Ev))
CoaTec base floor
Optic Fibers
13
LIME AND MATEC, FROM THE VERY BEGINNING…!
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LIME
AND
MATEC: LAB
Digital Optical
Microscopy,
Macro-Micro-Nano
Indenters
Macro-nano-scratch
LAYOUT
Classroom
Prep line
SEM
TEM
Prep room
AFM
Dualbeam
15
LIME LAB: SEM (FEI)
„
„
„
„
„
„
30 Kv LaB6 filament
Secondary electrons
Backscattered electrons
EDS to B, line & maps
Cathode luminescence
Specimen Current
16
LIME LAB: TEM (FEI)
„
„
„
„
120kV LaB6 filament
Double tilt
EDS to B, point & line
nanoprobe
17
LIME LAB: AFMS (1 NT-MDT + 1 DI)
g
microns range
„All modes (contact, non
contact, lateral force,…)
„50x50x5
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LIME LAB: DUALBEAM (FEI) HELIOS 600 NANOLAB
early 2008
-
Omnprobe
GIS ((4 g
gases))
STEM
EDS (Oxford)
19
19
DUALBEAM (FEI)
SEM Column: spatial resolution
0,76 nm @ 15 kV
FIB Column: spatial resolution
5 nm @ 30 kV
20
PRINCIPAL FIB MODES:
Deposition
Imaging
Milling
21
LIME LAB: DUALBEAM (FEI)
|
0,76 nm res
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LIME LAB: DUALBEAM (FEI)
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LIME LAB: NON-CONTACT PROFILOMETRY (TALYSURF
CCI LITE)
24
LIME-LAB SELF-PRODUCING OF STANDARD
SAMPLES FOR INSTRUMENTS CALIBRATION
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Calibration of the profilometer
25
LIME-LAB SELF-PRODUCING OF STANDARD
SAMPLES FOR INSTRUMENTS CALIBRATION
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Calibration of the profilometer
26
MATEC LAB: HARDNESS TESTERS
Vickers
K
Knoop
27
MATEC LAB: SCRATCH TESTER
Depth profiling
Applied force feedback controlled
Acoustic emission sensor
Friction force measurement
28
MATEC LAB: NANOINDENTATION – NANOSCRATCH
Agilent Nano Indenter
G200
End of 2007
29
29
MATEC LAB: SALT SPRAY 1M3
CHAMBER
30
30
MATEC LAB: CONTACT ANGLE
AND
WETTABILITY
Uni en 828 and ASTM D5725 - 99
31
SEMI-AUTOMATED INSTRUMENT FOR CONTACT ANGLE MEASUREMENT AND
SURFACE FREE ENERGY MODELS
SFE models:
1.
2.
3.
4.
5.
6.
Zisman
Neumann
Girifalco
Fowkes
Owens-Wendt
Van Oss-Chaudhury-Good
Light
source,
polarized
filter,
screen diffuser
Sample holder(three
axes movement)
12X objectives
Digital Camera to
acquire images on a
PC
32
IMPROVEMENT AND OPTIMIZATION OF THE SURFACE FREE
ENERGY OF POLYMERIC SUBSTRATES BY FLAME TREATMENT
Process parameters observed:
1.
1
2.
3.
4
4.
Total flow rate;
Oxygen/propane ratio;
Distance sample-tip nozzle;
Frequency of sample pass on
flame;
5. Total time treatment.
Some results obtained through
DOE Technique
33
MACRO-SCALE INSTRUMENTED SPHERICAL
INDENTATION
Prototipal
P
t ti l instrument
i t
t for
f macroscale spherical indentation
The stress-strain curve is obtained by
least-square fitting of exp data with a
FEM-modelled database of L-h curves
34
MATEC LAB: WEAR TEST
002
003
001
004
005
Campione 004
-502
60
-502,5
50
40
-503
R2=0,98
30
-503,5
20
-504
10
Affondamento
Carico
-504,5
Carico [g]
|
Wear test device (prototype)
Dynamic measurement of wear and friction coefficient at
the sub-micron
sub micron scale
Affondamento [
[um]
|
0
-505
505
10
-10
0
10
20
30
40
50
60
70
80
90 100 110 120 130 140 150
Tempo [s]
35
OUTLINE
Research Group presentation
y People and research Partners
y Vision
y Facilities
| Ongoing
g
g research
| Research topics on surface mechanical
measurements and microstructure concerns,
future activities
|
36
ONGOING
RESEARCH
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Residual stress: FIB & Digital Imaging Correlation, FIB & nanoindentation
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Analysis of wear mechanisms by FIB-SEM techniques
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The use of statistical nanoindentation techniques for the mechanical
characterization of cement pastes
FIB-based failure analysis and nano-mechanical characterization of MEMS
structures
Scratch testing of thin coatings: failure modes mapping by FIB-SEM
morphological analysis
Improvement and optimization of the surface energy of polymeric substrates
by Flame treatment
Development of a semi-automated instrument for surface energy
measurement
Microstructural and mechanical characterization of cellular ceramics obtained
by gel casting
Instrumented spherical indentation at the
macro-scale for the assessment the stress-strain curves of metals
Use of nano-silica for preventing expansive alkali-silica reaction in concrete
Microstructural and mechanical characterization of sputtered niobium thin
films for accelerating cavity applications
37
COATINGS: FAILURE
MODES STUDY
38
SCRATCH
TESTING OF THIN COATINGS:
MAPPING BY
|
FIB-SEM
FIB
SEM
FAILURE
MODES
MORPHOLOGICAL ANALYSIS
Wedge spallation
39
SCRATCH TESTING OF THIN COATINGS: FAILURE MODES MAPPING
BY FIB
FIB-SEM
SEM MORPHOLOGICAL ANALYSIS
|
Duplex Ti/TiN multilayer on WC-CO Planar:
Lc3: 38,5 N
y FIB section in correspondence of the first
chipping
pp g with substrate appearence
pp
40
SCRATCH TEST
|
„
Duplex Ti/TiN
multilayer on WC
WCCO Planar;
Adhesion can be worsen by an
hi h compressive
high
i
residual
id l
stress that is additive with the
scratch stress in front of the
contact area
41
ANALYSIS OF WEAR MECHANISMS BY FIB-SEM
TECHNIQUES
|
FIB analysis of mechanisms and crosssectional microstructural evolution during inservice wear of a Stellite 6B cobalt-based
alloy subjected to sliding contact conditions
FIB section of the worn surface
FIB section outside the worn surface 42
RESONANT CAVITIES
FOR PARTICLE ACCELERATORS
Niobium Coated (PVD)
Copper cavity
Bulk Niobium
Very low Surface
electrical
resistance
(∼nΩ a 1,8 K)
Lower costs
Higher thermal stability
But…
But
Significantly lower
superconducting properties
– WHY??
43
COATINGS
ON
COPPER
SUBSTRATE
| BIASED
(e-f) and
UNBIASED
(CERN, g-h)
type coatings
on QUARTZ
substrate
44
NANOINDENTATION
ON
NB
THIN FILMS
0,03
Load On S
Sample (mN)
Load On Sample (mN
N)
p
1
0,9
08
0,8
0,7
0,6
0,5
0,4
0,3
0,2
0,1
0
0,025
0,02
0,015
,
0,01
0,005
0
0
50
100
Displacement Into Surface (nm)
Niobium film load-depth
curve
0
5
10
15
20
25
Displacement Into Surface (nm)
Niobium film: Detail of a
load-depth curve
Indenter pop-in systematically observed
at depth ~ 10 nm
45
TEM
ANALYSIS OF THE OXIDE LAYER
TEM sample
p p
preparation
p
by
y
FIB lamella thinning
The control of surface oxide layer can be
very important in determining the
functional performances of Nb coatings
for superconducting applications
46
NANOINDENTATION ON MS-PVD NB THIN FILMS
500 nm
Partial recrystallization during
plastic deformation;
Relative sliding of
columnar grain
Measurement of
indenter contact
radius
Direct measurement of
piling-up
Evaluation of the effects
of roughness on contact
area
Analysis of deformation
mechanisms
47
MICRO
INDENTATION ON
MS-PVD NB
Biased MS E = 88,95 GPa
THIN FILMS
unbiased MS E = 54,33 GPa
48
NANOINDENTATION ON STRESS RELIEVED PILLARS
|
Compressive
stress in the
coating
49
RESULTS – STRESS
a) Pillar – stress free
CALCULATIONS
b) Halfspace stressed coating – as measured
c) Modelled: Halfspace coating + RS
50
CONTACT AREAS AND NANO STRUCTURAL EFFECTS
|
Pillar – no RS
|
Halfspace coating
51
RESIDUAL STREESS BY
FIB DIC TECHNIQUES
FIB-DIC
Z=0
vs
each step
|
Incremental Milling;
|
Steps of 200 nm
|
|
The pillar size d is
equal to the coating
thickness
hi k
The maximum milling
depth is equal to the
coating thickness
(3.8 µm)
52
EXPERIMENTAL
DATA
53
USE
OF STATISTICAL NANOINDENTATION TECHNIQUES FOR
THE MECHANICAL CHARACTERIZATION OF CEMENT PASTES
54
FIB-BASED
FAILURE ANALYSIS AND NANO-MECHANICAL
CHARACTERIZATION OF MEMS STRUCTURES
calculation of the stiffness of MEMS membrane by the use of a wedge
indenter – spring stiffness taken into account
55
MULTISCALE MECHANICAL CHARACTERIZATION OF
POROUS CERAMICS
FIB section and analysis
of sub-superficial
porosity
56
MULTISCALE MECHANICAL CHARACTERIZATION OF
POROUS CERAMICS
σ max
⎛
a⎞
⎟
= σ 0 ⎜⎜1 + 2
⎟
ρ
⎝
⎠
|
|
|
Radius of curvature
at the apex of this
pore is 55 nm!
High stress
intensification at
crack tip
Vertical drop in
Hardness/Modulus
is due to brittle
failure of subsurface porosity!
57
USE OF NANO-SILICA FOR PREVENTING EXPANSIVE ALKALISILICA REACTION IN CONCRETE
„
„
NS – SEM-FEG and TEM
Analysis
‹ No tendency to particle
agglomeration
‹ Particle dimension
10.5±2.3 nm
BET specific surface area
345 m2/g
TEM-BF 50000x
TEM-BF 380000x
58
USE OF NANO-SILICA FOR PREVENTING EXPANSIVE
ALKALI-SILICA REACTION IN CONCRETE
Nano-Silica
RILEM AAR-4 Expansion test at 60 °C - 150 days
RILEM AAR-4 Expansion test at 60 °C - 90 days
0,25
,
0 25
0,25
A ggregate A
A ggregate A
A ggregate B
0,2
A ggregate B
0,2
0,15
0,15
0,1
0,1
Expansion limit at 60 °C
Expansio n limit at 60 °C
0,05
0,05
0
0
0
0,2
0,4
0,8
2
0
5
0,2
0,4
0,8
2
5
N ano - sil ica co nt ent ( wt %)
N a no - s ilic a c o nt e nt ( wt %)
Berra et Al.
Al Expansion test at 150 °C - 21 days
Ultima
ate test expansion E90 (% l/l)
0,25
Aggregate A
Aggregate B
0,2
„
Expansion
limit a 150 °C
C
Aggregate A:
Deff = 0,56%
,
at 60°C - 0,03%
,
‹ Deff = 0,58% at 150 °C - 0,12%
The addition of NS is effective in
reducine the expansion of
concrete
‹
0,15
0,1
‹
0,05
0
0,2
0,4
0,8
Nano-silica content (wt %)
2
5
59
0
OUTLINE
Research Group presentation
y People and research Partners
y Vision
y Facilities
| Ongoing
g
g research
| Research topics on surface mechanical
measurements and microstructure concerns,
future activities
|
60
FUTURE RESEARCH ACTIVITIES
|
FIB + Nanoindents
Improving pillar and half space modeling: not only
the edges of the pillars must be taken into into
account but also the layered character of the
account,
sample. Taking into account properly the real
layered structure and reevaluate the real Young's
modulus
d l
off the
h coating can be
b crucial.
l
y A concept for direct access to the contact area
without guess work and / or tip calibration even in
the Angstrom scale (we give support to Norbert
Schwarzer work, Saxonian Institute of Surface
Mechanics)
y
61
FUTURE RESEARCH ACTIVITIES
|
FIB + DIC
Improving stress profiling method, which no other
method can in a site specific way by the use of a
more efficient correlation algorithms
y Extension of the method to different coated
systems, with different elastic and plastic behaviour
at different scale values (i.e. soft materials or
foams)
y
62
RELATED PUBLICATIONS: 2008-2009
1.
A. KORSUNSKY, M. SEBASTIANI, E. BEMPORAD,
Residual Stress Evaluation at the Micrometre Scale: FIB Ring-Drilling and Digital Image
Correlation Analysis,
Acta Materialia, submitted;
2.
A. KORSUNSKY, M. SEBASTIANI, E. BEMPORAD,
3.
4.
5.
6.
7.
8.
9.
10.
FIB Ring-Drilling
Ri
D illi
For
F Residual
R id l St
Stress E
Evaluation,
l ti
Materials Letters, in press, doi:10.1016/j.matlet.2009.06.020 ;
C. Bartuli, J.M. Tulliani, E. Bemporad, J. Tirillò, G. Pulci, M. Sebastiani, Mechanical properties of
cellular ceramics obtained by gel casting: characterization and modeling, Journal of the
European Ceramic Society, in press, doi:10.1016/j.jeurceramsoc.2009.04.035
Jean - Marc Tulliani,
ll
Cecilia
l Bartuli,
l Edoardo
d
d Bemporad,
d Valentina
l
Naglieri,
l
Marco Sebastiani,
b
Preparation and mechanical characterization of dense and porous zirconia produced by gel
casting with gelatin as a gelling agent, Ceramics International 35 (2009) 2481–2491
RIZZO A, SIGNORE MA, TAPFER L, PISCOPIELLO E, CAPPELLO A, BEMPORAD E, EBASTIANI M,
Graded selective coatings based on zirconium and titanium oxynitride, Journal of physics d:
apllied physics,
physics 42,
42 2009,
2009 1-10
1 10
Bemporad E. and Carassiti F. and Sebastiani M. and Lanza G. and Palmieri V. and Padamsee H.,
Superconducting and microstructural studies on sputtered niobium thin films for accelerating
cavity applications, SUPERCONDUCTOR SCIENCE AND TECHNOLOGY, 21, 2008
E. BEMPORAD, M. SEBASTIANI, F. CARASSITI, Tribological studies on PVD/HVOF duplex
coatings
ti
on Ti6Al4V substrate
b t t , Surface
S f
&C
Coatings
ti
Technology
T h l
203 (2008) 566–571
566 571
CARASSITI F. and SEBASTIANI M. and MANGIALARDI T. and PAOLINI A.E. and BERRA M. , USE
OF NANO-SILICA FOR PREVENTING EXPANSIVE ALKALI-SILICA REACTION IN CONCRETE,
proceedings of the ICAAR 2008 – 13th International Conference on Alkali-Aggregate
Reaction in Concrete
BEMPORAD E. , SEBASTIANI M., CASADEI F., CARASSITI F., Modelling, production and
characterisation of duplex coatings (HVOF and PVD) on Ti–6Al–4V substrate for specific
mechanical applications, Surface & Coatings Technology 201 (2007) 7652–7662
E. Bemporad, M. Sebastiani, F. Carassiti, R. Valle, F. Casadei, Development of a duplex coating
procedure (HVOF and PVD) on TI-6AL-4V substrate for automotive applications, Ceramic
Engineering and Science Proceedings 28 (3),
(3) pp.
pp 145
145-158
158 ISBN 978-0-470-24679-5
978 0 470 24679 5
64
[email protected]
[email protected]
b ti i@ t
i
3 it
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