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 CT 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
X-RAY TRANSMISSION AND TOMOGRAPHY TECHNIQUE

Using potassium iodide to trace fluid penetration

Water on top KI solution on top

X-RAY TRANSMISSION AND TOMOGRAPHY TECHNIQUE
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 XRF.
DIFFUSION EXPERIMENT WITH X-RAY TRANSMISSION

Sample size: 9.535 mm

EXAMPLE OF TIME-SERIES RADIOGRAPHS
ATTENUATION DUE TO IODIDE

()x = ln(Iref)x ln(It)x Beer-Lambert Law

Through standards we can change to concentrations.

EXAMPLE OF TIME-SERIES PROFILES
A Paste sample with w/s of 0.35 and 28 days sealed cure
EXAMPLE OF TIME-SERIES PROFILES
A Paste sample with w/s of 0.35 and 28 days sealed cure
EXAMPLE OF TIME-SERIES PROFILES
A Paste sample with w/s of 0.35 and 28 days sealed cure
EXAMPLE OF TIME-SERIES PROFILES
A Paste sample with w/s of 0.35 and 28 days sealed cure
EXAMPLE OF TIME-SERIES PROFILES
A Paste sample with w/s of 0.35 and 28 days sealed cure
EXAMPLE OF TIME-SERIES PROFILES
A Paste sample with w/s of 0.35 and 28 days sealed cure
EXAMPLE OF TIME-SERIES PROFILES
A Paste sample with w/s of 0.35 and 28 days sealed cure
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
(XRF)
XRF 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
m in diameter

Orbis by EDAX
VALIDATION OF THE TECHNIQUE BY USING XRF
Comparison of X-ray transmission with XRF

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 9.535 mm

ABSORPTION EXPERIMENT WITH X-RAY TRANSMISSION
Comparison between subtracted images after 1 min ponding

Absorption
Absorption front

2 mm

0% RH 100% RH
ABSORPTION EXPERIMENT WITH X-RAY TRANSMISSION
Comparison between subtracted images after 10 min ponding

0% RH 100% RH
ABSORPTION EXPERIMENT WITH X-RAY TRANSMISSION
Comparison between subtracted images after 6 hours ponding

0% RH 100% RH
ABSORPTION EXPERIMENT WITH X-RAY TRANSMISSION
Comparison between subtracted images after 1 day ponding

0% RH 100% RH
ABSORPTION EXPERIMENT WITH X-RAY TRANSMISSION
Time-series attenuation profiles for 0% RH

Fluid
penetrated
region

Penetration
front
Non-penetrated
region
ABSORPTION EXPERIMENT WITH X-RAY TRANSMISSION
Time-series attenuation profiles for 0% RH
ABSORPTION EXPERIMENT WITH X-RAY TRANSMISSION
Time-series attenuation profiles for 0% RH
ABSORPTION EXPERIMENT WITH X-RAY TRANSMISSION
Time-series attenuation profiles for 0% RH
ABSORPTION EXPERIMENT WITH X-RAY TRANSMISSION
Time-series attenuation profiles for 0% RH
ABSORPTION EXPERIMENT WITH X-RAY TRANSMISSION
Time-series attenuation profiles for 0% RH
ABSORPTION EXPERIMENT WITH X-RAY TRANSMISSION
Time-series attenuation profiles for 100% RH
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