Presented in the Second World Congress on Microscopy: Instrumentation, Techniques and Applications in Life Sciences and Materials Sciences (WCM 2018) 10-12 August 2018, Kottayam, Kerala, India organised by Institute for Holistic Medical Sciences,Parumbaikadu P.O, Kottayam,Kerala ,India & Technical University of Gdansk, Gdansk, Poland & Beijing University of Chemical Technology,Beijing, China

1. - Mainak Ghosal* & Prof.Arun Kumar Chakraborty
*PhD. Research Scholar ,IIEST,Shibpur
MECHANICAL & MICROSTRUCTURAL
CHARACTERIZATION ON CEMENT MORTAR
WITH NANO-MATERIAL ADDITIONS

2. Hydration Process of Cement

3. Cement Hydration v/s Time

4. Typical Microstructure of Cement Paste
• Feature 1
• Feature 2
• Feature 3
• Feature 1
• Feature 2
• Feature 3
Sand

5. Looking for Origin of Hydration in Cement
(Nanomaterials)

6. Nanomaterials Used – (1) Nano Silica
Item Description
Active Nano Content 35-40%
Particle Size 5-40 nm
pH (20°C) 9-10
Specific Gravity 1.08-1.32

7. Nanomaterials Used – (2) Carbon Nanotubes
Item Description
Diameter 20-40nm
Length 25-45nm
Purity 80-85%(a/c Raman Spectrometer & SEM analysis)
Amorphous Carbon 5-8%
Residue( Calcination in Air) 5-6% by Wt.
Average interlayer distance 0.34nm
Specific surface area 90-220 m2/g
Bulk density 0.07-0.32gm/cc
Real density 1-8 gm/cc
Volume Resistivity 0.1-0.15 ohm.cm(measured at pressure in powder)

8. Nanomaterials Used -(3)Nano Titanium Dioxide
Item Description
Rutile content % 98
pH 7
Average particle size (TEM) 30-40 nm
Treatment Nil
Moisture % 1.75-2
Bulk Density 0.31gm/cc
Water Solubility In-soluble

9. Sample Preparation for XRD Analysis
• 1.Nano Silica –
• 2. Nano Titanium Dioxide –
• 3. Carbon Nanotubes –

10. Modern X-ray Diffractometer

11. XRD image of Nanomaterials used
RECORDING
2θ
2θ

12. Sample Preparation for Mechanical Testing
Nano-
materials
added here

13. How Nano MaterialsWork ???
- CNTs exist in Entangled Mass like
form -- like COTTON FIBRES
- Dispersion Agent(Poly Carboxylate
Ether(PCE)  ACTIVATE Nucleation
OR
OR

14. Mechanical Testing of Cement Composites Samples

16. % Nano
additions in
Cement
7 Days
Strength
(% incr.)
28 Days
Strength
(% incr.)
90 Days
Strength
(% incr.)
180 Days
Strength
(% incr.)
365 Days
Strength
(% incr.)
0% nS
21.08 MPa
(--)
31.89MPa
(--)
31.20MPa
(--)
30.01MPa
(--)
30.01MPa
(---)
0.5% nS
23.85MPa
(13.14% )
35.1MPa
(11 .35% )
41.30MPa
(32. 37% )
27.47MPa
(-9.24% )
26.76MPa
(-4.29%)
0.75% nS
27.73MPa
(31.54%)
42.27MPa
(32.55%)
49.85MPa
(59.78%)
32.52MPa
(8.36%)
31.5MPa
(4.96%)
1.0% nS
25.07MPa
(18.93%)
37.36MPa
(17.15%)
42.98MPa
(37.76%)
33.68MPa
(12.23%)
32.41MPa
(8.0%)
1.25% nS
23.17MPa
(9.91%)
30.85MPa
(-3.26%)
39.45MPa
(26.44%)
35.24MPa
(17.43%)
31.3MPa
(4.29%)
1.50% nS 23.81MPa
(12.95%)
37.79MPa
(18.50%)
33.42MPa
(7.12%)
31.23MPa
(4.07%)
29.12 MPa
(-2.96%)

17. % Nano additions
in Cement
7 Days
Compressive
Strength
(% incr.)
28 Days
Compressive
Strength
(% incr.)
90 Days
Compressive
Strength
(% incr.)
180 Days
Compressive
Strength
(% incr.)
365 Days
Compressive
Strength
(% incr.)
0% CNT/TiO2
21.08MPa
(--)
31.89MPa
(--)
31.20MPa
(--)
30.01MPa
(--)
30.01MPa
(--)
0.02%CNT 17.69MPa
(-16.08%)
43.75MPa
(37.19%)
35.59MPa
(14.07%)
30.89MPa
(0%)
28.53MPa
(-4.93%)
0.05%CNT
27.19MPa
(28.98%)
34.88MPa
(9.37%)
31.85MPa
(2.08%)
38.55MPa
(3%)
41.69MPa
(38.92%)
0.1%CNT 21.69MPa
(2.89%)
24.83MPa
(-22.14%)
31.50MPa
(0.96%)
30.16MPa
(0%)
50.78MPa
(69.21%)
1% TiO2
25.24MPa
(19.70%)
36.71MPa
(12.60%)
35.92MPa
(15.10%)
33.42MPa
(11.40%)
41.16MPa
(37.20%)
2.5% TiO2
20.34MPa
(-3.50%)
34.97MPa
(9.60%)
37.80MPa
(21.20%)
40.96MPa
(36.50%)
28.16MPa
(-3.20%)

18. OPTIMIZATION OF NANO-MATERIALS
27.73
42.27
31.5
17.69
43.75
28.53
25.24
36.71
41.16
21.08
31.89
30.01
0
5
10
15
20
25
30
35
40
45
50
7 day Strength 28 day Strength 365 day Strength
nS(opt.)
CNT(opt.)
n-TiO2(opt.)
Ordinary Cement
Mortar(opt.)

19. Sample Preparation for Scanning Electron Microscopy

20. Scanning Electron Microscope used

22. SEM Image of Ordinary Cement Composites @ 28 days

23. SEM Image of NanoSilica added Cement Composites @ 28 days

24. SEM Image of Nanotubes added Cement Composites @ 28 days

25. OPTIMIZATIONS for Nano Materials in Cement
Mortar -nS, CNT & TiO2 are 0.75%,0.02% & 1% w.r.to
Cement weight.

26.  From SEM images it is observed that, Nano-particles improved the
structure of the cement mortar matrix. 0.75% nS and 0.02% CNT
system has shown a dense, compact and uniform microstructure
indicating the uniform distribution of the Nano particles along with
good bonding between cement and sand particles. Also with nS there
is an increased concentration of HYDRATION products which is directly
responsible for its strength gain along with the PORE FILLING EFFECTS.
However, CNT particles could not be shown due to lack of TEM image
results.

27. Further research on micro structural studies like
XRD,SEM,AFM,TEM,STM are necessary for
characterization of nano materials in concrete.