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Experimental and theoretical characterization of
Li2 TiO3 and Li4 SiO4 pebbles
Donato Aquaro - Nicola Zaccari
Dipartimento di Ingegneria Meccanica , Nucleare e della Produzione
Universita' di Pisa (Italy)
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
• Content• experimental tests on single pebbles of Li2 TiO3
and Li4 SiO4 (compression tests)• numerical simulation of the pebble compression• comparison between numerical and experimental
results (assessment of the numerical model )• numerical simulation of a oedometer test on a
Li4 SiO4 pebble bed using the Cam-clay model. comparison with the experimental results
• conclusions
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
• Experimental set up
INSTRON Press
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
Pebble tested
Li2 TiO3 pebbles
maximum variation of the average diameter 4%
- 1.1-1.3 mm of diameter
Li4 SiO4 pebbles
- maximum variation of the average diameter 7.8%
0.55-0.6 mm of diameter
The tests were carried out at room temperature and atmospheric pressure
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
Some pebbles were loaded until they broke - other pebbles were subjected at several cycles of loading and unloading without reaching the failure.
Before the test
After the test
0
2
4
6
8
10
12
14
16
0 0.01 0.02 0.03 0.04 0.05 0.06
Piston Displacemnt (mm)
Load
(N) I cycle
II cycle
III cycle
Com
pres
sive
load
(N)
Before the test
After the test
0
5
10
15
20
25
30
35
40
45
0 0.02 0.04 0.06 0.08 0.1 0.12 0.14
Piston Displacement (mm)
Com
pres
sive
Loa
d (N
)Collapse
Loading phase
Li2 TiO3
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
Before the test
After the test
0
2
4
6
8
10
12
0 0.01 0.02 0.03 0.04 0.05
Piston displacement (mm)
Com
pres
sive
Loa
d (N
)
I cycle
II cycle
III cycle
0
2
4
6
8
10
12
14
16
0 0.01 0.02 0.03 0.04 0.05 0.06
Displacement (mm)
Com
pres
sive
Loa
d (N
)
I cycle
II cycle
Collapse
Before the test
After the test
Li4 SiO4
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
0
10
20
30
40
50
60
0 0.02 0.04 0.06 0.08
displacement (mm)
load
(N)
t37 t23t22 t28t17 t34t27 regression curve
0
10
20
30
40
50
60
70
0 0.05 0.1 0.15
displacem ent (m m )
load
(N)
t37t23t22t28t11t12t15t34t27regression curve
Li2 TiO3
loading unloadingRegression curvesP=687.55 s 1.257
r2=0.9917
P=-3.287 + 733.62 s
r2=0.9854
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
0
2
4
6
8
10
12
14
0 0.02 0.04 0.06
displacement (mm)
load
( N)
t412 t45t43 t48regression curve
0
2
4
6
8
10
12
0 0.01 0.02 0.03 0.04
displacement (mm)lo
ad (N
)
t44 t43t45 t412regression curve
Li4 SiO4
loading unloadingRegression curve
P=3613 s 1.9027
r2=0.927
P=7657 s 1.8922
r2=0.974
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
0
0.1
0.2
0.3
0.4
0.5
0.6
11 17 24 26 31 31 35 36 37 39 40 51fracture load (N)
colla
psed
peb
ble
frac
tion
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
1.06 6.97 7.29 7.67 9.77 10.16
load (N)
colla
psed
peb
ble
frac
tion
Collapsed fraction of Lithium- Metatitanate pebble
Collapsed fraction of Lithium- Orthosilicate pebble
No Li2 TiO3 pebbles collapsed under 25 N
1 N is the maximum load supported by the Li4 SiO4 pebbles without any rupture
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
NUMERICAL SIMULATION OF THE PEBBLE COMPRESSION
FEM code MSC-MARC
aim of the simulations: to understand the main phenomena which occur during the pebble compression
- Mesh: axial symmetric elements. - load applied by means of a rigid upper plate- pebble located on a rigid lower plate.
- constraints pebble - plates : unilateral contacts (reacting only to compression loads) without friction.
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
Material model : low tension material
ε+
σ+σtu
εcr
softening
Traction
Compression
E0
Es
σy
- linear elastic behaviour under tensile stress
- elastic- plastic behaviour under compressive stress
Failure: - if tensile stress overcomes the cracking stress value (σcr ) - if the plastic strain (under compressive stresses) reaches the crushing strain value (εu ).
Other parameters:softening module ( Es), - the shear retention (τ),
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
The material data for the lithium metatitanate and Lithium Ortosilicate are reported in:
- Lithium-Metatitanate : E= 200.6 GPa - ν= 0.27 - σu = 1113 MPa- Lithium-ortosilicate : E= 90 GPa - ν= 0.25 - σu = 880 MPa
1] W. Dienst, H. Zimmermann, Mechanical properties of ceramics breeder materials, J. of Nucl. Mat., 155-157 (1998) 476-479.[2] P. Gierszewski, Review of properties of lithium metatitanate, Fusion Engineering and Design 39–40 (1998) 739–743.[3] G. Schumacher at alii, Properties of Lithium Ortosilicate, J. of Nuclear Materials, 155-157 (1998) 451-454.
E Young module, ν
Poisson coefficient, σu ultimate compression stress.
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
If we use the previous data for obtaining the material parameters,
the numerical results do not fit the experimental results.
Considering the experimental results of oedometer tests or single pebble compression tests we can conclude that the Young module must
be two or three order of magnitude lower than the previous data.
The previous data could not refer to the tested pebbles
for the ceramic material, the thermal mechanical characteristics are strongly dependent on the production technology
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
This problem was overcame performing a parametric analyses varying the model parameters in manner that the load- displacement curves fitted
the experimental ones.
0
10
20
30
40
50
60
0 0.05 0.1 0.15
displacement (mm)
load
(N)
t22
regression curve
sy=200Mpa-E=3.5GPa-eu=0.3-sc=100MPa
sy=200MPa-E=5GPa-eu=0.15-sc=100MPa
0
2
4
6
8
10
12
0 0.02 0.04 0.06
displacement (mm)
load
(N)
t44
sy=250MPa-E=5.5GPa-eu=0.15-sc=139MPa
Li4 SiO4 pebble Li2 TiO3 pebble
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
9.5 N 19 N 28 N 47N
Lithium Metatitanate pebble- Plastic strain
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
9.5 N 19 N 28 N 47N
Lithium Metatitanate pebble- Von Mises stress
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
0.00
50.00
100.00
150.00
200.00
250.00
300.00
350.00
400.00
450.00
0.00 0.05 0.10 0.15 0.20
strain
vert
ical
str
ess
(- M
Pa)
d=0.5 mm
d=0.1 mm
d=0.0125 mm
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
Collapse of the pebble
0
0.0001
0.0002
0.0003
0.0004
0.0005
0.0006
-0.0006 -0.0004 -0.0002 0 0.0002 0.0004 0.0006
pebble
cracking in 1st princ. direction
0
0.0001
0.0002
0.0003
0.0004
0.0005
0.0006
-0.0006 -0.0004 -0.0002 0 0.0002 0.0004 0.0006
pebble
cracking in 2d princ. direction
0
0.0001
0.0002
0.0003
0.0004
0.0005
0.0006
-0.0006 -0.0004 -0.0002 0 0.0002 0.0004 0.0006
pebble
crushed point
Cracking in the 1st principal direction
Cracking in the 2nd principal direction
Integration points in which the plastic strain reaches the crushing strain
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
NUMERICAL SIMULATION OF AN OEDOMETER TEST ON LITHIUM ORTOSILICATE PEBBLE BED WITH AN
HOMOGENEOUS MODEL
Material model : Modified Cam-clay model of Roscoe and Burland
The main parameters of the Cam-clay model are the following:
- - M, the slope of the critical state line
- - pc , preconsolidation pressure ( a stress-like hardening variable)
- - K, the slope of the over consolidation lines
- λ, the slope of the normal consolidation line.
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
Modified Cam-clay model of Roscoe and Burland
Main relations :-elastic stress-strain law: non linear elastic law - bulk modulus function of the hydrostatic pressure, p : K=pν/k
- f(σ,pc )=q2/M2+p(p-pc)=0
- Yield criterion
q=Mp
-isotropic compression constitutive relations- elastic range : ν= νp -kln(p/po)
-elasto-plastic range: ν= νco - λln(p/pco )
ν=V/Vs specific volume
V=current soil volume, Vs, volume of the solid phase
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
A good agreement between the experimental curve and numerical one was obtained assuming the following values for the four parameters :
M=0.5; K=0.002; λ=0.006; pc = 0.9 MPa.Sensitivity analysis for the four parameters
M=0.5 - k=2e-3 - pc=0.9 MPa
0.E+00
1.E+04
2.E+04
3.E+04
4.E+04
5.E+04
6.E+04
0.00 0.10 0.20 0.30 0.40
displacement (mm)
load
(N)
lbd=5e-3
lbd=6e-3
exp.results
lbd=6.5e-3
– Influence of the parameter λ
M=0.5 - k=2e-3 lbd=6e-3
0.E+00
1.E+04
2.E+04
3.E+04
4.E+04
5.E+04
6.E+04
0.00 0.10 0.20 0.30 0.40
displacement (mm)
load
(N)
pc=0.9MPa
exp.results
pc=2 MPa
pc=0.7 MPa
Influence of the parameter pc
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
lambda=6e-3 - k=1e-3 - pc=0.9 MPa
0
10000
20000
30000
40000
50000
60000
0 0.1 0.2 0.3 0.4
displacement (mm)
load
(N)
exper. results
M=0.5
M=0.8
M=1.5
M=0.5 -lbd=6e-3-pc=0.9 MPa
0
10000
20000
30000
40000
50000
60000
0.00 0.10 0.20 0.30 0.40
displacement (mm)
load
(N)
exp.results
k=3e-3
k=2e-3
k=0.5e-3
Sensitivity analysis for the four parameters
Influence of the parameter k Influence of the parameter M
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
Conclusion
- The compression tests on single pebbles permitted to estimate the fracture load of Lithium-Metatitanate pebbles (1.1-1.3 mm of diameter) and of Lithium-Orthosilicate pebbles (0.55-0.6 mm of diameter).
- The numerical simulations of the pebble compression give results which agree very well with the experimental ones assuming values of the material characteristics different from those found in the technical literature for these materials. the mechanical characteristics of ceramic materials depend strongly on the production technology.
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Experimental and theoretical characterization of Li2 TiO3 and Li4 SiO4 pebbles Aquaro - Zaccari
Conclusion
- with an homogeneous model developed for soil , choosing appropriate values for the several constants it is possible to fit the experimental curves,
- the physical meaning of the parameter values are not immediately extrapolate to the pebble bed
.