Mechanical Properties and Autogenous

Shrinkage of Carbon Nanofiber(CNF)

Reinforced Cement Composites
Yuan Gao
David Corr
Maria S. Konsta-Gdoutos
Surendra P. Shah

Department of Civil Engineering, Northwestern Univerisity

ACI Spring Convention, Milwaukee, 2016 1

 Background

Concrete
Low flexural strength
Low modulus of elasticity
High autogenous shrinkage and shrinkage cracking
Carbon nanofiber
Youngs Modulus: 200-600 GPa1,2
Tensile Strength: 3-15 GPa1,2
1. Ozkan T, Naraghi M, Chasiotis I. Mechanical properties of vapor grown carbon nanofibers. Carbon
2010;48:23944.
2. Mordlkovich VZ. Carbon nanofibers: a new ultrahigh-strength material for chemical technology. Theor
Found Chem Eng 2003;37(5):42938. 2
 Material Properties

CNF: Cone shaped graphite planes canted with respect to the longitudinal fiber axis

Property CNF
Carbon Purity 98 wt%
Average Diameter 150 nm
Fiber Length 50-200 um
Bulk Density 0.03 g/cm3
Iron Content 11,096 ppm

Higher Resolution Image of Carbon Aspect ratio ~670

Nanofiber from Pyrograf Products Specific Surface Area 20-30 m2/g

3
 CNF Dispersion

A combination of the use

of superplasticizer and
ultrasonication

CNF Dispersion

TEM of Undispersed CNF SEM of CNF in Cement Matrix

Patent, US20090229494 A1, Shah, S., Konsta-Gdoutos, M.S., Metaxa, Z. S., 2008. 4
 CNF Dispersion

Good Dispersion Poor Dispersion

5
 CNF Reinforced Cement Composites

Mechanical Properties of Cement Paste and Mortar

Flexural strength3 point bending
Modulus of elasticity
Autogenous Shrinkage of Cement Paste and Mortar
Restrained Ring Test of Cement Mortar

6
 Fracture Mechanics Test

0.0127(V )
FC
Ld
2

Where:
FC= fiber count
V = fiber content, percent by volume,
L = fiber length,
d = equivalent fiber diameter

[1] ACI 544.1R-96: Report on Fiber Reinforced Concrete

ASTM C78 7
 Fracture Mechanics Test

Flexural Strength of Cement Paste with or without CNF

7
6.5
Flexural Strength(MPa)

6
5.5
5
4.5 Plain Cement
4 PC+0.05 wt%CNF
3.5 PC+0.1 wt%CNF
3
0 5 10 15 20 25 30
Time(days) w:c=0.5

Increased Flexural Strength Compared to Plain Paste

CNF Content Fiber Count 3 Day 7 Day 28 Day
0.05 wt% CNF 6.9*109 9% 10% 9%
0.1 wt% CNF 13.8*109 22% 20% 18% 8
 Modulus of Elasticity

Modulus of Elasticity of Cement Paste with or without CNF

11
Modulus of Elasticity(GPa)

10
9
8
7
6 Plain Cement
5 PC+0.05 wt%CNF
4 PC+0.1 wt%CNF
3
0 5 10 15 20 25 30
Time(days)
w:c=0.5
Increased Modulus of Elasticity Compared to Plain Paste
CNF Content Fiber Count 3 Day 7 Day 28 Day
0.05 wt% CNF 6.9*109 24% 15% 13%
0.1 wt% CNF 13.8*109 27% 22% 21% 9
 Fracture Mechanics Test

Flexural Strength of Cement Mortar with or without CNF

9
8
Flexural Strength(MPa)

7
6
5
4
3 Plain Mortar
2 PM+0.05 wt% CNF
1
PM+0.1 wt% CNF
0
0 5 10 15 20 25 30
Time(days) w:c:s=0.485:1:2.75
Increased Flexural Strength Compared to Plain Mortar
CNF Content Fiber Count 3 Day 7 Day 28 Day
0.05 wt% CNF 3.0*109 14% 18% 19%
0.1 wt% CNF 6.1*109 25% 28% 28% 10
 Modulus of Elasticity

Modulus of Elasticity of Cement Mortar with or without CNF

30
Modulus of Elasticity(GPa)

25
20
15
10 Plain Mortar
PM+0.05 wt% CNF
5
PM+0.1 wt% CNF
0
0 5 10 15 20 25 30
Time(days) w:c:s=0.485:1:2.75
Increased Modulus of Elasticity Compared to Plain Mortar
CNF Content Fiber Count 3 Day 7 Day 28 Day
0.05 wt% CNF 3.0*109 17% 17% 23%
0.1 wt% CNF 6.1*109 22% 29% 34% 11
Mechanical Properties of CNF/Cement Composites

CNFs Effect on Mechanical Properties of Cement Paste/Mortar

Modulus of
Flexural Strength
Fiber Count Elasticity
Improvement
Improvement
Cement Paste
+0.1 wt%CNF 13.8*109 18% 21%

Cement Mortar
+0.1 wt% CNF 6.1*109 28% 34%

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 CNF Reinforced Cement Composites

Mechanical Properties of Cement Paste and Mortar

Flexural strength3 point bending
Modulus of elasticity
Autogenous Shrinkage of Cement Paste and Mortar
Restrained Ring Test of Cement Mortar

13
Autogenous Shrinkage Measurement
Calibration Bar

About 43 cm

ASTM C1698 14
 A Parameter Affecting Dispersion Degree--
Concentration in Water

Cement Paste
w:c=0.4 W/C=0.4

Cement Mortar
water
0.4:1:2.75 CNF

0.34:1:1.75 Ultrasonication
Or
Superplasticizer

W/C=0.34

water

15
 Autogenous Shrinkage Measurement

Autogenous Shrinkage of Cement Paste with or without CNF

0
0 0.5 1 1.5 2 2.5 3
-500
Autogenous Shrinkage()

-1000
0.08 wt% CNF
-1500
-2000
-2500
-3000
Plain Paste 23% Reduction
-3500
Time(days)

w:c=0.4

16
 Autogenous Shrinkage Measurement

Autogenous Shrinkage of Cement Mortar with or without CNF

0
-50 0 0.5 1 1.5 2 2.5 3
Autogenous Shrinkage()

-100
-150 0.08 wt% CNF
-200
-250
-300
-350
Plain Mortar
-400 24% Reduction
Time(days)

w:c:s=0.4:1:2.75
17
 Autogenous Shrinkage Measurement

Autogenous Shrinkage of High Performance Mortar

with or without CNF
0
-100 0 0.5 1 1.5 2 2.5 3
Autogenous Shrinkage()

-200
-300 0.05 wt% CNF
-400
-500
-600
-700
-800 Plain Mortar
-900
25% Reduction
Time(days)

w:c:s=0.34:1:1.75
18
 CNF Reinforced Cement Composites

Mechanical Properties of Cement Paste and Mortar

Flexural strength3 point bending
Modulus of elasticity
Autogenous Shrinkage of Cement Paste and Mortar
Shrinkage Cracking of Cement MortarRestrained Ring Test

19
 Restrained Ring Test
Thickness of steel ring: 0.5 in(12.7mm)
Thickness of specimen: 1.5 in(38.1mm)
Steel Ring Specimen
4in

7in(177.8mm)
6in(152.4mm)

10in(254mm)
ASTM C1581
Wood Base
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Set up for the restrained ring test, including ring dimensions.
Restrained Ring Test

Seal after casting, and keep it in 23 C

chamber.

Demold, and apply the silicone gel to the

surface of the sample to prevent drying.

Specimen is kept in environmental

chamber(23 C, 50% RH) for 2 weeks.

21
 Restrained Ring Test

Restrained Ring Test of High Performance Mortar with or

without CNF
0.8
Plain Mortar Microscope
0.7

0.6
Crack Width(mm)

0.5

0.4 29% Reduction

0.3
0.05 wt% CNF
0.2

0.1
Start cracking w:c:s=0.34:1:1.75
0
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15
Time(days)
22
 Autogenous Shrinkage and Shrinkage Cracking of CNF/Cement
Composites

Autogenous Shrinkage Crack

Fiber Count
Shrinkage Reduction Width

PC+0.08 wt% CNF

12.6*109 23 --
(w:c=0.4)

PM+0.08 wt% CNF

5.1*109 24 --
(w:c:s=0.4:1:2.75)

HPM+0.05 wt% CNF

4.3*109 25 29%
(w:c:s=0.34:1:1.75)

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 Conclusions

CNF increases flexural strength and modulus of elasticity of

cement paste and mortar.

CNF reduces the autogenous shrinkage both in cement paste

and mortars.

CNF delays the shrinkage cracking and reduces the crack

width.

CNFs effect is more pronounced in mortar than in paste.

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 Future Research

Nanoindentation test why CNFs effect is stronger in mortar than

in paste
Corrosion resistanceProf. Konsta will present the preliminary
research
Explore the mechanism of CNFs interaction within cement matrix
Pore structure analysis
Internal humidity analysis
Chloride diffusion analysis
FTIR for hydration process

25
 Acknowledgement

This research was partially supported by Cemex.

We acknowledge the support and guidance of Olga Chowaniec and Nestor

Quintero of Cemex.

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Thank You

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