Sing Ray Transmission and Tomography To Image Ion Transport in Cement Based Materials

ACI CONVENTION, SPRING 2016, MILWAUKEE
USING X-RAY TRANSMISSION AND

TOMOGRAPHY TO IMAGE ION
TRANSPORT IN CEMENT-BASED
MATERIALS
AUTHORS:
MEHDI KHANZADEH MORADLLO, PHD CANDIDATE
M. TYLER LEY, PE, PHD
ACKNOWLEDGEMENTS
Funding:
 Oklahoma Department of Transportation (ODOT)
 US National Science Foundation CAREER Award
 FHWA EAR “Novel Alternative Cementitious

Materials (ACMs) for Development of the Next
Generation of Sustainable Transportation
Infrastructure”
 Dr. Qinang Hu for his assistance with analyzing of
the 3-D images
TABLE OF CONTENTS
Introduction
Method
Diffusion experiments
Verfication of the technique
3-D diffusion from tomography
Absorption experiments
Conclusions
CURRENT CHALLENGE
 Long-termdurability of structures made
with cement-based materials
The majority of concrete structures

require repair because of poor durability
and not poor strength
HOW CAN WE IMPROVE THIS?
 Many durability issues are caused by the
penetration of outside fluids.
 We need methods that can help us measure
this penetration that are fast and non-
destructive
 We need these tools to give us detailed
information about how aggregates, cracks,
etc. impact how these fluids travel in
concrete
X-RAY TRANSMISSION AND TOMOGRAPHY
 This is a technique to characterize the internal
structure of materials in a non-destructive manner at
micron-scale spatial resolution.
Skyscan 1172 µCT scanner

3-D Tomography
X-RAY TRANSMISSION AND TOMOGRAPHY TECHNIQUE
• The gray value is an indication of X-ray absorption of
the material, which is function of density and
chemistry.
• The difference in gray value means difference in
density or chemistry or both
Low X-ray
absorption
High X-ray
absorption
Using potassium iodide to trace fluid penetration
Water on top KI solution on top

DIFFUSION EXPERIMENTS
CONVENTIONAL DIFFUSION EXPERIMENT
 Apparent chloride diffusion coefficient (ASTM C1556)
Drawbacks:
 Destructive and requires a
significant mass of powder
 Time consuming and labor
intensive
 Slow because of the long
ponding period and the testing
procedure
 Poor spatial resolution and the
measurement based on average
section
DIFFUSION EXPERIMENT WITH X-RAY TRANSMISSION
 Cement pastes with w/s = 0.35, 0.40, and 0.45 were made.
 Samples were sealed cured for 28 days and then ponded
with 0.6 mol/L potassium iodide (KI) solution for 28 days.
 A radiograph was taken from the paste samples before the
ponding as reference radiographs and then again over time
to determine the changes in the sample (time-series
radiographs).
 After the ponding period, the sample was polished for further
analysis with µXRF.
DIFFUSION EXPERIMENT WITH X-RAY TRANSMISSION
Sample size: 9.5×35 mm

EXAMPLE OF TIME-SERIES RADIOGRAPHS
ATTENUATION DUE TO IODIDE
(∆µ)x = ln(Iref)x – ln(It)x Beer-Lambert Law
Through standards we can change ∆µ to concentrations.

EXAMPLE OF TIME-SERIES PROFILES
A Paste sample with w/s of 0.35 and 28 days sealed cure
Non-destructive & each graph within 60 seconds

APPLICATION OF X-RAY TRANSMISSION METHOD
 Comparison of different w/s ratios after 2 days ponding
APPLICATION OF X-RAY TRANSMISSION METHOD
 Comparison of different w/s ratios after 20 days ponding
SUMMARY
 X-ray transmission technique was successfully used to
image time-dependent iodide diffusion in cement paste
 Comparison of performance of different paste samples
with various w/s at early ages
 Imaging diffusion front
VERIFICATION OF THE TECHNIQUE
WITH MICRO X-RAY FLUORESCENCE
(ΜXRF)
ΜXRF TECHNIQUE DESCRIPTION
 Uses an X-ray optic to focus a stationary beam of X-rays onto a sample
 The interaction of the X-rays with the electrons emits a secondary
fluoresced X-ray
 Every element emits a unique signal
 Uses a polycapillary optic to focus X-rays to a size of approximately 50
µm in diameter
Orbis by EDAX
VALIDATION OF THE TECHNIQUE BY USING ΜXRF
 Comparison of X-ray transmission with µXRF
Takes 6
hours
Takes 60
seconds
COMPARISON BETWEEN CHLORIDE AND IODIDE
COMPARISON BETWEEN CHLORIDE AND IODIDE
 The mortar samples with w/c of 0.4 were investigated.
Samples were cured for 14 days. Then, they were
ponded with 0.6 M NaCl and 0.6 M KI for 28 days.
Diffusion Coefficient × 10-12 (m2/s)
chloride 12.2
iodide 15.8
SUMMARY
 A good agreement was found between results from X-ray
transmission and micro X-ray fluorescence methods
 Iodide showed a similar diffusion trend to chloride
3-D DIFFUSION FROM TOMOGRAPHY
APPLICATION OF X-RAY TOMOGRAPHY
 A single aggregate was embedded inside the paste sample with w/s
of 0.40. The sample was ponded with 0.6 M KI after 14 days
curing.
Diffusion
Diffusion front
2 mm
APPLICATION OF X-RAY TOMOGRAPHY
Before ponding 14 days from ponding 35 days from ponding
2 mm
Before ponding 14 days from ponding 35 days from ponding
2 mm
ABSORPTION EXPERIMENT
CONVENTIONAL ABSORPTION EXPERIMENT
 Measurement of Rate of Absorption (ASTM C1585)
Drawbacks:
 The results of this test are highly dependent on the initial
conditioning of the concrete
 This method does not measure the actual depth of penetration
ABSORPTION EXPERIMENT WITH X-RAY TRANSMISSION
 Paste samples with w/c ratio of 0.40 were investigated.
 Samples were cured for 35 days
 Samples were conditioned in different relative humidities
(0% and 100%)
 Then, samples were ponded with 0.6 mol/L potassium
iodide (KI) solution for 14 days.
 A radiograph was taken from the paste samples before the
ponding as reference radiographs and then again over time
to determine the changes in the sample (time-series
radiographs).
Sample size: micro cylinders with dimensions of 9.5×35 mm

 Comparison between subtracted images after 1 min ponding
Absorption
Absorption front
2 mm
0% RH 100% RH
 Comparison between subtracted images after 10 min ponding
0% RH 100% RH
 Comparison between subtracted images after 6 hours ponding
0% RH 100% RH
 Comparison between subtracted images after 1 day ponding
0% RH 100% RH
 Time-series attenuation profiles for 0% RH
Fluid
penetrated
region
Penetration
front
Non-penetrated
region
WHY DOES THIS HAPPEN?
 Sample with 0% RH is dominated by capillary suction
 Sample with 100% RH is dominated by diffusion

SUMMARY
 Useful to look at changes in geometry (aggregates, voids,
and cracks)
 Can study non steady state conditions
 Imaging absorption depth

FUTURE EFFORTS
 Alternative Cementitious materials performance against
ion penetration
 Modeling based on the findings from experiments
CONCLUSIONS
SUMMARY OF X-RAY TRANSMISSION AND TOMOGRAPHY
ADVANTAGES
 Non-destructive
 Fast (takes 60 sec for each 2D image)
 In-situ
 Less human effort
 High spatial resolution
 Large No. of data points (1500)
 Identify local abnormalities
Applications:
This technique can be quite useful to study ion transport as well
as different durability mechanisms such as freeze thaw attack,
alkali silica reaction, physical salt attack, salt scaling, sulfate
attack, and cracking from drying shrinkage
THANK YOU!
Email:
mehdi.khanzadeh_moradllo@okstate.edu
tyler.ley@okstate.edu

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ACI CONVENTION, SPRING 2016, MILWAUKEE

USING X-RAY TRANSMISSION AND

 US National Science Foundation CAREER Award

 FHWA EAR “Novel Alternative Cementitious

Verfication of the technique

3-D diffusion from tomography

The majority of concrete structures

Skyscan 1172 µCT scanner

Using potassium iodide to trace fluid penetration

Water on top KI solution on top

Sample size: 9.5×35 mm

(∆µ)x = ln(Iref)x – ln(It)x Beer-Lambert Law

Through standards we can change ∆µ to concentrations.

Non-destructive & each graph within 60 seconds

Diffusion Coefficient × 10-12 (m2/s)

Before ponding 14 days from ponding 35 days from ponding

Sample size: micro cylinders with dimensions of 9.5×35 mm

 Sample with 0% RH is dominated by capillary suction

 Sample with 100% RH is dominated by diffusion

 Imaging absorption depth

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