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Researcher Team:
Post-doc
Rajalekshmi Pillai
Graduate Students
Qiao Huang
Gunes Yakaboylu
Steven Andryzcik
Priyashraba Misra
Undergraduate Students
Brian Armour
James Meyer
HWI Team
4/27/2016
Margaret Raughley
Joshua Sayre
Acknowledgements:
We would like to thank U.S. Department of Energy (DOE) for
funding the project under contract DE-FE0012383.
Dr. Maria Reidpath, U. S. Department of Energy, is greatly
appreciated for her insight and valuable guidance.
We also would like to acknowledge WVU Shared Facilities.
Thanks to HarbisonWalker International for the technical
staff.
Kindly acknowledge Faculty and staff of West Virginia
University for their support.
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4/27/2016
Technology Vision:
Item A represents the smart
refractory material.
Item B is an interconnection
(alignment) pin.
Item C is an interconnection brick,
which will permit transfer of the
signal to the exterior wall.
Item D is the sealed electrical
access port to connect to the
signal acquisition/processing units.
Item E is low-power electronics
and wireless communication.
4/27/2016
Program Objectives:
1) Investigate chemical stability, thermomechanical properties, and electrical
properties of refractory ceramic composites at temperatures between 7501450C.
2) Define processes to pattern and embed the conductive ceramic composites
within refractory materials to incorporate temperature and strain/stress
sensors into refractory bricks.
3) Develop methods to interface the electrical sensing outputs from the smart
refractory with an embedded processor and to design a wireless sensor
network to efficiently collect the data at a processing unit for further data
analysis.
4) Develop algorithms for model-based estimation of temperature profile in the
refractory, slag penetration depth, spallation thickness, and resultant health
by using the data from the wireless sensor network.
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Task Assignments:
Task 2: Fabrication and Characterization of
Oxide-Silicide Composites.
Task 3 and Task 4: Sensor Patterning and
Embedding and Static and Dynamic Sensor
Testing.
Task 5: Data Ex-Filtration Using a Wireless
Sensor Network.
Task 6: Model-Based Estimation of Refractory
Degradation/Temperature.
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Task 2:
Fabrication and Characterization of
Oxide-Silicide Composites.
(Sabolsky)
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4/27/2016
Y2O3
ZrO2
Cr2O3
MoSi2
MoSi2, Cr2O3,
Cr3Mo, SiO2
WSi2
ZrSi2
TaSi2
NbSi2
TiSi2
(Cr0.88Ti0.12)2O3,
Cr3Si, SiO2
CrSi2
CrSi2, ZrO2
Metal silicides show high stability in Al2O3 and ZrO2 matrix only with formation of different type
of silicides (Mo5Si3, W5Si3, Ta5Si3, Nb5Si3, Cr5Si3) and SiO2 (highlighted).
They partially react with Y2O3 and Cr2O3 to form undesired secondary phases.
4/27/2016
10
20 m
10 m
3 m
20 m
Secondary Phase
10 m
1 m
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3 m
Silicide/Oxide Properties:
CTE (100-1000C)
10
12.0
MoSi2-Al2O3 composites
10.0
9.5
9.0
8.5
30
40
50
60
70
10
10
10
80
10
~ 9.65x10-6K-1
20
MoSi2-based composites
100 200 300 400 500 600 700 800 900 1000
10
WSi2-Al2O3 composites
10
10
10
Silicide/Al2O3 composites
0
100 200 300 400 500 600 700 800 900 1000
MoSi2-Al2O3
at ~ 1000C
(S/cm)
WSi2-Al2O3
MoSi2-coarseAl2O3
Conductivity (S/cm)
-6 -1
Alpha (10 K )
11.0
10.5
10.0
9.5
9.0
8.5
~ 9.41x10-6K-1
8.0
7.5
10
Temperature (C)
Temperature (C)
12.0
11.5
Conductivity (S/cm)
10.5
7.5
11.0
8.0
Conductivity (S/cm)
-6 -1
Alpha (10 K )
11.5
10
20
30
40
50
60
70
80
10
TaSi2-Al2O3
TiSi2-Al2O3
MoSi2-ZrO2
WSi2-ZrO2
CrSi2-Cr2O3
10
10
60/40 vol%
MoSi2-Al2O3
43.6
WSi2-Al2O3
26.7
WSi2-ZrO2
20.7
MoSi2-c.Al2O3
20.5
100 200 300 400 500 600 700 800 900 1000
Temperature (C)
Key Parameters: (1) metal silicide type and fraction, (2) mixedness or level of homogeneity, (3)
relative density, and (4) particle size of the metal silicide and refractory oxide.
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12
MoSi2-Al2O3 composite
30000
27000
12
18000
10
24 hrs
15000
12000
9000
3000
0
20
30
40
50
60
2 ()
70
48 hrs
27000
24000
21000
24 hrs
18000
15000
12000
9000
6000
3000
20
30
Sintered
40
4/27/2016
50
60
2 ()
70
Precursor
MoSi2 Powder
90
MoSi2-ZrO2 composite
30000
80
80
Sintered
After annealing
Intensity (a.u.)
14
21000
6000
Intensity (a.u.)
18
16
48 hrs
24000
Pure MoSi2
20
90
Pure MoSi2
After Sintering
(1600C - 2h)
After Annealing
(1400C - 24h)
MoSi2-Al2O3
5 m
1 m
Future Work:
14
15
Task 3 Objectives:
To develop methods for patterning technology the ceramic
composites within the refractory matrix.
Task 4 Objectives:
To test the electrical performance of the smart refractory
brick (with embedded thermocouple or thermistor sensors).
To investigate corrosion/erosion kinetics in static and
dynamic tests on smaller prototype and full-size smart cups
and bricks (at WVU and HWI).
To implement and test methods for data collection on initial
prototypes.
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16
4/27/2016
17
High-Temperature Thermocouple
Performance:
WSi2// TaSi2
32
MoSi2// WSi2
MoSi2// NbSi2
24
MoSi2// TiSi3
16
9
8
0
0
400
800
1200
1600
Temperature (C)
Various thermocouple
compositions studied
at 1500 C
18
2nd cycle
10
1500
1350 C
8.3 mV
Temperature (C)
1200
1350 C
8.43 mV
5h
9
8
10 h
1050
900
6
5
750
600
450
300
150
1350
-1
0
12 15 18 21 24 27 30 33 36 39 42 45 48 51 54 57 60 63 66
Time (hours)
Experiment
Hold Time, h
EMF, mV
1350
Cycle # 1
8.3
1350
Cycle # 2
10
8.43
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19
Monoliths of sensors were fabricated via tape casting, laminated and sintered
at 1500 C. These laminates were embedded in the Cr2O3 brick while slip
casting and co-sintered at 1500 C in Argon atmosphere.
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20
21
1350 C
Resistance ( )
3.5
3.0
2.5
2.0
1.5
1.0
-10
30
70
110
150
190
230
270
Time (Hours)
22
Lignite Coal
(b)
(c)
23
Smart brick
K-Type Thermocouple
24
Future Work:
Optimize method to interconnect to embedded sensors (in
order to stabilize sensor signal and sensor long-term response).
Investigate the corrosion/erosion kinetics of sensor embedded
refractory bricks in static and dynamic mode with slag.
Scale-up all sensor preforms and smart refractory brick for
FULL-TECHNOLOGY DEMO IN TASK 7.
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25
Task 5:
Data Ex-Filtration Using a Wireless
Sensor Network.
(Graham/Kulathumani)
4/27/2016
26
Task 5 Objectives:
To develop methods to interface the electrical
sensing outputs from the smart refractory with an
embedded processor
To design a wireless sensor network to efficiently
collect the data at a processing unit for further data
analysis
Energy
Harvester
Sensor
4/27/2016
Interface
Circuit
WSN
Mote
27
Radio
Base
Station
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28
3
5
1. Cold-Junction Compensator
2. Thermocouple Amplifier
3. Capacitive Sensor
4. Thermocouple Amplifier V2
5. Wheat-Stone Bridge
Bridge Circuit Temperature vs Actual Temperature
120
Resistance-Based Sensor
110
Within 2% accuracy
100
Temperature(C)
90
80
70
60
50
40
Measured
Ideal
30
20
20
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29
30
40
50
60
70
80
Temperature(C)
90
100
110
120
1500
4
3
1
Error(%)
Temperature(C)
2
1000
0
-1
500
-2
-3
Measured
Ideal
500
1000
Temperature(C)
4/27/2016
30
-4
1500
-5
700
800
900
1000
1100
1200
Temperature(C)
1300
1400
1500
31
Data In
Command
Out
Base Station
Desktop/Laptop
Sensor
3
Master
Mote
Sensor
4
32
33
x 10
Resistance( )
3
2
1
0
0
10
15
Time(h)
WSN Full Run
20
150
100
50
0
25
6
8
Time(h)
WSN Half Run
10
12
10
12
200
Resistance( )
Output(V)
3
2
1
0
0
10
15
Time(h)
20
150
100
50
0
25
6
Time(h)
34
35
36
Task 6.0:
Model-Based Estimation of
Temperature Profile and Extent of
Refractory Degradation.
(Bhattacharyya, Huang)
4/27/2016
37
Task 6 Objectives:
To develop algorithms for model-based estimation of
temperature profile in the refractory, slag
penetration depth, spallation thickness, and
resultant health by using the data from the wireless
sensor network
4/27/2016
38
Motivation:
Typical correlation based approaches are inadequate
Stiff temperature gradient along the refractory
resulting in a large temperature change along the
sensor length
Change in thermal and electrical properties over time
due to slag penetration
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39
Property Models:
In order to build the model of smart refractory , several
temperature-dependent property models for refractory
or sensor material are needed:
The electrical resistivity model for refractory*
Specific heat
Emissivity
Thermal conductivity
Electrical conductivity
Thermal expansion
Dielectric constant
Youngs modulus
Poissons ratio
*Hensler J R, Henry E C. Electrical Resistance of Some Refractory Oxides and Their Mixtures in the
Temperature Range 600 to 1500 C[J]. Journal of the American Ceramic Society, 1953, 36(3): 76-83
4/27/2016
40
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41
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42
43
Sensor Models:
Resistive
circuit
sensor
Thermistor or
thermocouple
Strain
gauge
thermocouple
4/27/2016
44
Interdigital
capacitor
5.00E-12
Capacitance (F)
4.80E-12
4.60E-12
0 vol% slag
5 vol% slag
10 vol% slag
4.40E-12
15 vol% slag
20 vol% slag
4.20E-12
4.00E-12
0
0.005
0.01
0.015
0.02
Distance (m)
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45
Estimation:
Methods:
Traditional Kalman Filter (TKF)
Linear process model
Computationally cheap
Less accuracy for highly nonlinear process
Extended Kalman Filter (EKF)
Nonlinear process linearized at every time step
Computationally costlier than TKF
Higher accuracy than TKF for nonlinear process
Unscented Kalman Filter (UKF)
Nonlinear process
Computationally expensive
Superior accuracy
4/27/2016
58
46
Filter Algorithm:
Differential Algebraic Equations System
Nonlinear differential algebraic equations (DAE) system:
,
Augmented form:
4/27/2016
59
47
Estimation of capacitance
Temperature Estimation for Different
Extent of Slag Penetration are completed
4/27/2016
48
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61
4/27/2016
50
4/27/2016
51
Products:
1. Edward M. Sabolsky, R. Chockalingam, K. Sabolsky, G. A. Yakaboylu, O. Ozmena, B. Armour,
A. Teter, D. Bhattacharyya , David Graham , Vinod Kulathumani, Close Timothy and Marc
Palmisiano, Refractory Ceramic Sensors for Process and Health Monitoring of Slagging
Gasifiers, 227th ECS Meeting- Chicago, Illinois, USA, May 28th, (2015).
2. Edward M. Sabolsky , R. Chockalingam, K. Sabolsky, G. A. Yakaboylu, O. Ozmen, B. Armour,
A. Teter, D. Bhattacharyya, David Graham, Vinod Kulathumani, Close Timothy and Marc
Palmisiano, Conductive Ceramic Composites Used to Fabricate Embedded Sensors for
Monitoring the Temperature and Health of Refractory Brick in Slagging Gasifiers, XIVth
International Conference European Ceramic Society- Toledo, Espana 24th June, 2015
3. R. C. Pillai, E. Sabolsky, K. Sabolsky, G. Yakaboylu, B. Armour, J. Mayer, J. Bogan, M.
Raughley and J. Sayre Performance of high temperature ceramic-ceramic thermocouples
embedded within chromia refractory bricks to monitor the health and stability of industrial
gasifiers Materials Science and technology MS&T2015, Oct 4-8, 2015, Greater Columbus
Conventional Center, Columbus, Ohio, USA.
4. G. Yakaboylu, R. C. Pillai, B. Armour, K. Sabolsky, E. Sabolsky,Development of Refractory
Oxide/Metal Silicide Composites for High Temperature Harsh-Environment Sensor
Applications,Materials Science and technology MS&T2015, Oct 4-8, 2015, Greater Columbus
Conventional Center, Columbus, Ohio, USA.
5. G.A. Yakaboylu, R. C. Pillai, B. Armour, K. Sabolsky and E. M. Sabolsky, Conductive
Ceramic Composites for Fabricating High Temperature and Harsh Environment Sensors:
Thermal Processing, Stability and Properties, International Conference and Exposition on
Advanced Ceramics and Composites, January 24-29, 2016, Daytona Beach, Florida, USA.
4/27/2016
52
Products:
6. R.C. Pillai, G.A. Yakaboylu, K. Sabolsky and E. M. Sabolsky,J. Bogan, J. Sayre,
Composite Ceramic Thermocouples for Harsh-Environment Temperature
Measurements, International Conference and Exposition on Advanced Ceramics and
Composites, January 24-29, 2016, Daytona Beach, Florida, USA.
7. E. M. Sabolsky, R. C. Pillai, K. Sabolsky, G. A. Yakaboylu, B. Armour, A. Teter, M.
Palmisiano and T. Close, Refractory Ceramic Sensors for Process and Health
Monitoring of Slagging Gasifiers, ECS Trans., Vol 66(37) pp 43-53 (2015).
8. B. Rumberg, D. Graham, S. Clites, B. Kelly, M. Navidi, A. Diello, V. Kulathumani,
RAMP: Accelerating Wireless Sensor Design with a Reconfigurable Analog/MixedSignal Platform, Proceedings of the ACM/IEEE Conference on Information
Processing in Sensor Networks (ISPN15), pp. 47-58, Seattle, WA, April 13-16, 2015.
4/27/2016
53
Appendix:
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54
Thermocouple Microstructures:
Microstructure of ceramic-ceramic thermocouples sintered at 1500 C in argon
The SEM micrographs clearly shows that the thermocouples are fully dense and hence
improves the conductivity
4/27/2016
55
1.0
0.9
0.8
0.7
D index
0.6
0.5
0.4
0.3
0.2
0.1
5 m
Original image
4/27/2016
0.0
Binary image
56
8 10 12 14 16 18 20 22 24 26 28 30 32
Silicide Thermocouples:
Seebeck coefficients
Thermoelectric Voltage
T1
T2
T2
T1
E AB = A (T ) dT + B (T ) dT
Silicide Couples
30
25
20
(Mo or W)-Ti
(Mo or W)- Ta
15
10
Mo-W
5
0
0
500
1000
4/27/2016
S500 (V/C)
Reference
-3.0
T. Nonomura (2011)
-0.3
T. Nonomura (2011)
14
Kenneth Kreider (1995)
20.8
Kenneth Kreider (1995)
-3.3
Kenneth Kreider (1995)
35
Mo-Ti
W-Ti
Mo-Ta
W-Ta
Mo-W
Material
MoSi2
WSi2
TaSi2
TiSi2
Pt
1500
Dispersant
(Solvents and Dispersants)
Ultrasonic mixing
Tape casted, laminated
and laser cut alumina
green substrates
Screen printing
Curing at 50 C
4/27/2016
58
25
20
WSi2 // TaSi2
WSi2 // MoSi2
15
MoSi2 // ZrSi2
WSi2 // ZrSi2
10
NbSi2 // MoSi2
TiSi2 // WSi2
5
0
0
200
400
600
800
1000
1.
2.
3.
4.
5.
6.
59
[90-10]WSi2-Al2O3//[90-10]TaSi2-Al2O3
[90-10WSi2-Al2O3//[90-10] MoSi2-Al2O3
[90-10]MoSi2-Al2O3//[90-10] ZrSi2-Al2O3
[90-10]WSi2-Al2O3// [90-10] ZrSi2-Al2O3
[90-10]NbSi2-Al2O3//[90-10] MoSi2-Al2O3
[90-10] TiSi2-Al2O3//[90-10] WSi2-Al2O3
Thermocouple Microstructures:
[90-10] WSi2-Al2O3
Intensity (A.U.)
[90-10] TiSi2-Al2O3
[90-10] TaSi2-Al2O3
[90-10] NbSi2-Al2O3
Al O MoSi
2
20
[90-10] MoSi2-Al2O3
40
60
80
100
Angle 2 (Deg)
120
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60
V3
V4
V5
V6
V7
(mm)
40
40
40
40
40
(mm)
1.0
0.5
0.5
0.2
0.2
(mm)
1.0
1.0
0.5
1.0
0.5
A Sensor length
B Spacing between legs
C Leg width
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Design: V3
61
40.00 mm
0.50 mm
0.50 mm
55.00 mm
40.00 mm
55.00 mm
Design ID
1.00 mm
1.00 mm
Design: V5
8
38-114-11 Therm o Couple
[90-10] vol% M oSi2 -Al2 O 3 //TaSi2 -Al2 O 3
Pt lead
4
Thermocouple
0
0
300
600
900
1200
Temperature ( C)
62
Thermistor Preforms:
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63
900
1h
25
5h
1h
20
15
600
10
300
0
4
14
280
900
210
140
300
70
Resistance, k
Temperature, C
1200
0
10
15
1
Data Rail Out Points
20
25
10
12
14
16
18
20
350
Time, h
1500
19
Time, h
600
Volts(ADC\Resistance)
1200
Volts(ADC\Resistance)
1350 C
Resistance, k
Temperature, C
3.5
3
2.5
2
1.5
1
0.5
0
30
Time, h
8 10 12 14 16 18 20 22 24
Time, h
The analytical test results (Lab View) of Brick #10: [60-40] MoSi2-Al2O3 brick were correlated
with wireless data up to 1350 C isothermal hold and thereafter the data showed deviations.
This may be due to oxidation.
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