Paste Microstructure and Mechanical Properties of

1741 Whitehorse Mercerville Rd, Mercerville, NJ 08619
mail@jcms.com, 609-631-0700

Paste Microstructure and Mechanical Properties of

Concrete:
X-Ray Micro Computed Tomography (µ-CT) and
Fluorescence Microscopy
Achintyamugdha Sharma1 (Speaker), Benjamin Affum2, Todd Sirotiak3, Priyanka Deka4
1 Ph.D., Project Controls Engineer, JCMS, Inc., 1741 Whitehorse Mercerville Rd, Mercerville, NJ 08619, email: asharma@jcms.com
2 Graduate Research Assistant, Dept. of Construction Management and Engineering, North Dakota State University, ND 58105, email:
benjamin.affum@ndsu.edu
3 Ph.D., Associate Professor, Dept. of Construction Management and Engineering, North Dakota State University, ND 58105, email: todd.sirotiak@ndsu.edu
4 Ph.D., Project Controls Specialist, JCMS, Inc., 1741 Whitehorse Mercerville Rd, Mercerville, NJ 08619, email: pdeka@jcms.com
Abstract 2032122
1

What is Concrete?
Source: Google Images
Portland cement Chemical Admixtures Coarse Aggregates

Sand
Fly Ash Ground granulated

blast furnace slag
Water
2

What Happens When Concrete Cracks?

Chemical ions
Chloride based
Water Compound
Concrete
Structure
Calcium Hydroxide Calcium
Oxychloride
Water
Crack
Source: PCA
Sulfate based
Compound
Calcium Hydroxide
Ettringite
Source:
www.markhamglobal.com
Water
3

Introduction
• Durability and shrinkage of concrete are important
• Cement paste is vulnerable to micro-cracks and defects
• Laboratory tests for Hardened Concrete
• Electrical Resistivity (ASTM C1760)
• Drying Shrinkage (Un-restrained) (ASTM C157)
• Drying Shrinkage (Restrained) (ASTM C1581)
• Time Consuming
• Labor Intensive
Electrical Resistivity Length Change due to Drying

Source: Proceq Shrinkage (Unrestrained)
4

Drying Shrinkage (Restrained) – Ring Test (ASTM C1581)
Ring Test (Source: Lomboy et.al. 2010)

5

Objectives
• Detection and quantification of micro-cracks and defects in paste
• Develop methodology for characterization of micro-cracks and defects in paste
• X-Ray Micro-Computed Tomography (µ-CT)
• Fluorescence Microscopy
• Potential relationships between paste defects and bulk properties of concrete
• Investigate the effects of cementitious changes on potential relationships
6

Methodology: Paste Samples for µ-CT and Fluorescence Microscopy
Metal mold for paste sample Paste samples in PVC molds (black), and 3D printed molds
(white)
7

3D Printed Resin Based Mold for Paste Sample

8

End-to-end Rotator Test setup for epoxy impregnation
9

For detailed methodology: Sharma, A., Angadi,

P., Sirotiak, T., Wang, X., Taylor, P., Borowicz,
P., & Payne, S. (2020). Characterization of paste
microstructure for durability properties of
concrete. Construction and Building Materials,
248, 118570.
(a) 3D reconstruction of a paste sample (µ-CT) (b) 3D reconstruction of pore distribution inside a paste sample (µ-CT)
(c) typical micro-crack observed through fluorescence microscopy (d) binary format of a micro-crack
10

Fluorescence Microscopy: Quantification of Cracks / Defects by ImageJ
11

Phase I
Relationships between paste defects and bulk properties of concrete
X-Ray Micro-Computed Tomography (µ-CT)
12

Phase I: Mixture Proportions

Chopped
Class F Fly Class C Fly Basalt Air Light Weight Coarse
Cement Nano Silica Water Water Reducers Entraining Fine Aggregates
Mix Code Description (kg/m3) Ash Ash (kg/m3) Fiber (kg/m3) (ml/m3) Agent (kg/m3) Aggregates Aggregates
(kg/m3) (kg/m3) Addition (kg/m3) (kg/m3)
(ml/m )3
(% v/v)
CG-P Coarse Ground Cement 344 0 0 0 - 145 888 45 1061 0 768
TI-P Type I Cement 344 0 0 0 - 145 721 45 1061 0 768
Type I Cement, 30%
TI-FC replaced with Class C Fly 241 0 103 0 - 145 862 45 1061 0 768
Ash
Type I Cement, 20%
TI-FF replaced with Class F Fly 275 69 0 0 - 145 448 45 1061 0 768
Ash
TIL-P Type IL Portland 344 0 0 0 - 145 1457 45 1061 0 768
Limestone Cement
Type IL Cement, 30%
TIL-FC replaced with Class C Fly 241 0 103 0 - 145 971 45 1061 0 768
Ash
Type IL Cement, 30%
TIL-FC (B) replaced with Class C Fly 241 0 103 0 0.25 145 971 45 1061 0 768
Ash, 0.25% (v/v) basalt
fibers
Type IL Cement, 5%
TIL-NS replaced with Colloidal 327 0 0 17 - 145 4280 45 1061 0 768
Nanosilica
13

Phase I: Paste Microstructure (µ-CT) & Durability of Concrete

Resistivity Plots Degree of Hydration (Semi-adiabatic
20 Calorimetry)
CG-P TI-P TI-FC TI-FF 50
18
Temperature Change (F)

TIL-P TIL-FC TIL-FC (B) TI-NS CG-P TI-P TI-FC
Resistivity (kΩcm)
16 TI-FF TIL-P TIL-FC
TIL-FC (B) TI-NS
14 40
12
30
10
8 20
6
4 10
2
0 0
0 7 14 21 28 0 300 600 900 1200 1500
Elapsed Time (Days) Elapsed Time (min)
Total Defects Average Pore Diameter
35000 320
Average Pore Diameter (µm)

Frequency of Defects
30000 300
25000
280
20000
260
15000
240
10000
5000 220
0 200
CG-P TI-P TI-FC TI-FF TIL-P TIL-FC TIL-FC TI-NS CG-P TI-P TI-FC TI-FF TIL-P TIL-FC TIL-FC TI-NS
(B) (B)
Paste Designation Paste Designation
14

1
5

Smaller Void 1
CH + S = CSH Smaller
Larger Void Smaller
Void 3 Void 4
Smaller Void 2
CH: Calcium Hydroxide

Secondary CSH
CSH: Calcium Silicate Hydrate
S: Silicate (from pozzolan)
16

Phase I: Paste Microstructure (µ-CT) & Degree of Hydration of

Concrete Mixtures with SCMs Mixtures without SCMs
0.07 0.07
Slope of Calorimetry Peak

Slope of Calorimetry Peak
0.06 0.06
0.05 0.05
0.04 0.04
0.03 0.03
0.02 0.02
0.01 y = 2E-06x + 0.013 0.01 y = 8E-06x + 0.013

R² = 0.9264 R² = 0.9096
0 0
0 5000 10000 15000 20000 25000 30000 35000 0 5000 10000 15000 20000 25000 30000 35000
Total Defects (Count) Total Defects (Count)
Slope Determination for Calorimtery Peak of TIL-P

60
Temperature Change (F) y = 0.0511x - 2.8968
SCM: Supplementary 50 R² = 0.9658
Cementitious Materials 40
30
20
10
0
0 300 600 900 1200 1500
-10
Elapsed Time (min)
17

Phase I: Paste Microstructure (µ-CT) & Shrinkage of Concrete

Concrete Shrinkage - Paste Defect Relationship Restrained Drying Shrinkage
0.50 0 7 14 21 28
0.45 40 CG-P TI-P TI-FC
Average Stress Rate (MPa/day)
0.40 TI-FF TIL-P TIL-FC

20
TI-NS TIL-FC (B)
0.35
Microstrain, 10-6
0
0.30
-20
0.25
-40
0.20
-60
0.15
0.10 -80
0.05 y = 8E-10x2 - 1E-05x + 0.1712 -100

R² = 0.8652
0.00 -120
0 5000 10000 15000 20000 25000 30000 35000
-140
Total Defects (Count) Elapsed Time (days)
18

Phase I: Conclusions
• Paste defects (µ-CT) may provide an indirect assessment of durability of concrete
• Frequency & distribution of paste defects related to resistivity in concrete
• Mixtures with pozzolans have high frequency of defects with a wide range of sizes
• Additional hydration products from pozzolans fill larger voids into discontinuous smaller voids
• Discontinuous defects prevent transport of deleterious ions like Cl - and SO42- dissolved in pore fluids
• Past defects (µ-CT) directly proportional to degree of hydration
• Trends of relationships different for mixtures with or without SCMs
• Past defects (µ-CT) related to drying shrinkage under restrained conditions
• Paste microstructure may predict bulk properties of concrete
19

Phase II
Effects of cementitious changes on potential relationships
Fluorescence Microscopy
20
Crack Length (µm)
100
150
200
250
300
350
50
0
3.65
3.76
3.87
5.20
5.20
5.47
6.09
6.45
6.64
8.00
8.39
8.41
CG-P
8.66
9.68
10.32
Crack Width (µm)

10.40
10.99
11.63
– Width-Length Analysis
14.00
14.21
15.00
16.49
20.65
21.63
27.56
Crack Length (µm)

21
0
100
150
200
250
300
350
50
0.65
1.25
3.29
3.69
3.92
6.48
7.85
7.85

8.90
9.39
9.70
10.11
10.31
10.32
11.31
TI-NS
11.63
11.86
12.26
12.33
Crack Width (µm)
12.36
12.92
13.56
14.43
14.84
14.85
16.13
16.77
Phase II: Defect Detection & Quantification (Fluorescence Microscopy)
22.37
23.28
35.22
36.87
40.42


– Porosity Distribution Along Width Axis
CG-P TI-NS
9 7
8 6
Mean Porosity (%)
Mean Porosity (%)

7
5
6
5 4
4 3
3
2
2
1 1
0 0
-10 -5 0 5 10 -10 -5 0 5 10
Distance from the Center (mm) Distance from the Center (mm)
22
Phase II: Mixture Proportions

Supplementary Coarse Water Air

Type Mix Code Description Cement (lbs) Cementitious Aggregates Fine Aggregates Reducers Entraining Water (gal)
(lbs)
Materials (lbs) (lbs) (oz) Agen (oz)
TI/II Type I/II Cement 587 - 1584 1467 36 2 30
High Tricalcium Aluminate
Plain HTCA Cement 587 - 1584 1467 55 2 30
Cement
HA High Alkali Cement 587 - 1584 1467 55 2 30
CG Coarse Ground Cement 587 - 1584 1467 32 2 30
TI/II-SF Type I/II Cement, 5% replaced 508 56 1584 1467 56 3 30
with Silica Fume
Type I/II Cement, 35% replaced
TI/II-FA with Fly Ash 354 191 1584 1467 - 2 30
TI/II-MK with Metakaolin 517 57 1584 1467 56 3 30
Binary
Blends Type I/II Cement, 50% replaced
TI/II-S 285 285 1584 1467 33 2 30
with Slag
TI/II-Z with Zeolite 453 80 1584 1467 55 3 30
Type IL Portland Limestone
TIL 585 - 1584 1467 36 2 30
Cement
Type IL Cement, 5% replaced
TIL-SF 506 56 1584 1467 56 3 30
with Silica Fume
TIL-FA Type IL Cement, 35% replaced 354 190 1584 1467 - 2 30
with Fly Ash
Ternary Type IL Cement, 10% replaced
TIL-S 284 284 1584 1467 33 2 30
Blends with Metakaolin
TIL-MK Type IL Cement, 50% replaced 516 57 1584 1467 57 3 30
with Slag
TIL-Z Type IL Cement, 15% replaced 452 80 1584 1467 64 3 30
with Zeolite
23


Defect Quantification
2.00
% of Defects
1.50
1.00
0.50
0.00
Mixture
24

Phase II: Paste Microstructure (Fluorescence) & Concrete Durability

Mixtures Containing Type I/II Cement Mixtures Containing Type IL Cement
40.0 40.0
y = -21.929x + 37.409
y = -58.07x + 69.601
35.0 35.0 R² = 0.5019
R² = 0.8276
30.0 30.0
28 Day Resistivity
28 Day Resistivity
25.0 25.0
20.0 20.0
15.0 15.0
10.0 10.0
5.0 5.0
0.0 0.0
0.00 0.20 0.40 0.60 0.80 1.00 1.20 0.00 0.20 0.40 0.60 0.80 1.00 1.20
Average % of Defects Average % of Defects
Other Cementitious Combinations

40.0
y = -17.372x + 17.757
35.0 R² = 0.8629
30.0
28 Day Resistivity
25.0
20.0
15.0
10.0
5.0
0.0
0.00 0.20 0.40 0.60 0.80 1.00 1.20
Average % of Defects
25

Phase II: Conclusions

• Type of SCM influences the frequency of micro-cracks / defects
• Paste defects (Fluorescence) related to resistivity of concrete
26

Overall Conclusions
• Defect analysis of paste may predict bulk properties of concrete
• Future Work: Statistical models for type of mixtures
• Trailer based set-up for field implementation
27

Acknowledgement
• U. S. Department of Energy under Award Number DE-EE0007246
• North Dakota Department of Commerce ND Venture Phase I
• Parsons Corporation
• Iowa State University
• NDSU Core Laboratories
28

Disclaimer
Any findings, opinions, and conclusions or recommendations
expressed in this report are those of the author(s) and do not
necessarily reflect the views of the Department of Energy,
North Dakota Department of Commerce or their employers.
29

References
• Sharma, A., et al., Characterization of paste microstructure for durability
properties of concrete. Construction and Building Materials, 2020. 248: p. 118570.
• Sharma, A., et al., Portland limestone cement for reduced shrinkage and
enhanced durability of concrete. Magazine of Concrete Research, 2019: p. 1-16.
• ASTM, Standard test method for length change of hardened hydraulic-cement
mortar and concrete. In C157 / C157M - 17. 2017: West Conshohocken, PA, USA.
• ASTM, Standard Test Method for Determining Age at Cracking and Induced
Tensile Stress Characteristics of Mortar and Concrete under Restrained Shrinkage,
in C1581/C1581M-09a. 2009: West Conshohocken, PA
• ASTM, Standard Test Method for Bulk Electrical Conductivity of Hardened
Concrete, in C1760-12. 2012: West Conshohocken, PA.
30

Thank You!
31

Phase II: Paste Microstructure (Fluorescence) & Concrete Shrinkage

Mixtures Containing Type I/II Cement Mixtures Containing Type IL Cement
180 180
28 Day Unrestrained Drying Shrinkage

160 160
140 140
(Negative Microstrain)
120 120
100 100
80 80
60 60
40 40
20 20
0 0
0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40
Average % of Defects Average % of Defects
Other Cementitious Combinations

180
160
140
120
100
80
60
40
20
0
0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40
Average % of Defects
32

Phase II: Paste Microstructure (Fluorescence) & Degree of Hydration of

Concrete
33

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1741 Whitehorse Mercerville Rd, Mercerville, NJ 08619

Paste Microstructure and Mechanical Properties of

Portland cement Chemical Admixtures Coarse Aggregates

Fly Ash Ground granulated

What Happens When Concrete Cracks?

Electrical Resistivity Length Change due to Drying

Drying Shrinkage (Restrained) – Ring Test (ASTM C1581)

Ring Test (Source: Lomboy et.al. 2010)

Methodology: Paste Samples for µ-CT and Fluorescence Microscopy

Methodology: Paste Samples for µ-CT and Fluorescence Microscopy

3D Printed Resin Based Mold for Paste Sample

Methodology: Paste Samples for µ-CT and Fluorescence Microscopy

End-to-end Rotator Test setup for epoxy impregnation

Methodology: Paste Samples for µ-CT and Fluorescence Microscopy

For detailed methodology: Sharma, A., Angadi,

Methodology: Paste Samples for µ-CT and Fluorescence Microscopy

Fluorescence Microscopy: Quantification of Cracks / Defects by ImageJ

Phase I: Mixture Proportions

Phase I: Paste Microstructure (µ-CT) & Durability of Concrete

Temperature Change (F)

Average Pore Diameter (µm)

Phase I: Paste Microstructure (µ-CT) & Durability of Concrete

Phase I: Paste Microstructure (µ-CT) & Durability of Concrete

CH: Calcium Hydroxide

Phase I: Paste Microstructure (µ-CT) & Degree of Hydration of

Slope of Calorimetry Peak

0.01 y = 2E-06x + 0.013 0.01 y = 8E-06x + 0.013

Slope Determination for Calorimtery Peak of TIL-P

Phase I: Paste Microstructure (µ-CT) & Shrinkage of Concrete

0.40 TI-FF TIL-P TIL-FC

0.05 y = 8E-10x2 - 1E-05x + 0.1712 -100

Crack Width (µm)

Crack Length (µm)

Phase II: Defect Detection & Quantification (Fluorescence Microscopy)

Mean Porosity (%)

Phase II: Mixture Proportions

Supplementary Coarse Water Air

Phase II: Defect Detection & Quantification (Fluorescence Microscopy)

Phase II: Paste Microstructure (Fluorescence) & Concrete Durability

Other Cementitious Combinations

Phase II: Conclusions

Phase II: Paste Microstructure (Fluorescence) & Concrete Shrinkage

28 Day Unrestrained Drying Shrinkage

28 Day Unrestrained Drying Shrinkage

Other Cementitious Combinations

Phase II: Paste Microstructure (Fluorescence) & Degree of Hydration of

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Temperature Change (F)