IP Library › Granted Patent US 9,365,456
Granted Patent B2
US 9,365,456 · App. 12/322,842 · Granted Jun 14, 2016

Highly-dispersed carbon nanotube-reinforced cement-based materials

Inventors: Surendra P. Shah (Evanston, IL); Maria S. Konsta-Gdoutos (Wilmette, IL); Zoi S. Metaxa (Evanston, IL)
Assignee: Northwestern University
C04B28/02C04B2111/34
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Quick Facts
Patent No.
US 9,365,456
App. No.
12/322,842
Granted
Jun 14, 2016
Kind
B2
Abstract

A composite cement material is prepared from cement material and carbon nanotubes, wherein the carbon nanotubes are present from about 0.02 wt % to about 0.10 wt % based on weight of cement material. The process for preparing such cement compositions includes sonicating a mixture of a surfactant, water, and carbon nanotubes; and blending the dispersion and the cement material to form a cementitious paste. The process may also include curing the cementitious paste. The composite cement materials are useful in a variety of cement applications where a reduction in nanoscale flaws and fractures is desired.

Claims (21)

1. A method of making a nanocomposite cementitious material, comprising sonicating an aqueous solution containing surfactant and carbon nanotubes to form a dispersion of carbon nanotubes in the solution, and mixing the dispersion of carbon nanotubes and a cement to form a nanocomposite cementitious material wherein the carbon nanotubes are present in an amount of about 0.048% to about 0.08% by weight of the cement and further wherein the nanocomposite cementitious material exhibits a modified nanostructure so that the average values of stiffness and hardness of C-S-H, as determined by nanoindentation tests, are higher compared to the same cementitious material without carbon nanotubes.

2. The method of claim 1 wherein the carbon nanotubes have lengths of about 10 to about 100 m and diameters of about 20 to about 40 nanometers.

3. The method of claim 1 wherein a weight ratio of surfactant to carbon nanotubes is about 1.5 to about 8.0.

4. The method of claim 1 wherein dispersion of the carbon nanotubes in the aqueous solution containing surfactant occurs while sonicating the solution.

5. The method of claim 4 wherein the sonicating is conducted using an ultrasonic energy of about 700 to about 4200 kJ/l.

6. The method of claim 1 wherein the dispersion and cement are mixed at a water to cement ratio (w/c) of 0.2 to 0.6.

7. The method of claim 1 wherein the carbon nanotubes are dispersed in the aqueous solution that includes surfactant comprising polycarboxylate based superplasticizer.

8. A method of making a nanocomposite cementitious material, comprising sonicating an aqueous solution containing surfactant and carbon nanotubes to form a dispersion of carbon nanotubes in the solution, and mixing the dispersion of carbon nanotubes and a cement to form a nanocomposite cementitious material wherein the carbon nanotubes are present in an amount of about 0.02% to about 0.1% by weight of the cement including the further step of curing the nanocomposite cementitious material, wherein the cured nanocomposite cementitious material has a Young's modulus that is at least 15% higher than that of the cured nanocomposite cementitious material in the absence of the carbon nanotubes at the age of 28 days and further wherein the nanocomposite cementitious material exhibits a modified nanostructure so that the average values of stiffness and hardness of C-S-H, as determined by nanoindentation tests, are higher compared to the same cementitious material without carbon nanotubes.

9. The method of claim 8 wherein the nanocomposite cementitious material exhibits reduced autogenous shrinkage as compared to the same cementitious material without carbon nanotubes.

10. The method of claim 8 wherein the nanocomposite cementitious material exhibits increased flexural strength as compared to the same cementitious material without carbon nanotubes.

11. The method of claim 1 wherein sonicating is conducted using an ultrasonic energy of about 2800 kJ/l.

12. The method of claim 8 , wherein the cement is Portland cement and the carbon nanotubes are multiwalled carbon nanotubes.

13. The method of claim 12 , wherein sonicating the aqueous solution comprises sonicating the aqueous solution using an ultrasonic energy in the range from 700 to 3500 kJ/l; the surfactant to carbon nanotube weight ratio in the dispersion is in the range from about 4 to about 6.25; the surfactant comprises a polycarboxylate based superplasticizer; and the dispersion and cement are mixed at a water to cement ratio (w/c) of about 0.3 to about 0.5.

14. The method of claim 8 , wherein the carbon nanotubes are present in an amount of about 0.02% to about 0.08% by weight of the cement and the cured nanocomposite cementitious material has a Young's modulus that is at least 25% higher than that of the cured nanocomposite cementitious material in the absence of the carbon nanotubes at the age of 28 days.

15. The method of claim 8 , wherein the carbon nanotubes are present in an amount of about 0.02% to about 0.08% by weight of the cement and the cured nanocomposite cementitious material has a Young's modulus that is at least about 55% higher than that of the cured nanocomposite cementitious material in the absence of the carbon nanotubes at the age of 28 days.

16. The method of claim 12 , wherein the carbon nanotubes are present in an amount of about 0.02% to about 0.08% by weight of the cement and the cured nanocomposite cementitious material has a Young's modulus that is at least 25% higher than that of the cured nanocomposite cementitious material in the absence of the carbon nanotubes at the age of 28 days.

17. The method of claim 12 , wherein the carbon nanotubes are present in an amount of about 0.02% to about 0.08% by weight of the cement and the cured nanocomposite cementitious material has a Young's modulus that is at least about 55% higher than that of the cured nanocomposite cementitious material in the absence of the carbon nanotubes at the age of 28 days.

18. The method of claim 8 , wherein the carbon nanotubes in the aqueous solution have aspect ratios of greater than 1000, the carbon nanotubes are present in an amount of about 0.02% to about 0.08% by weight of the cement and the surfactant comprises a polycarboxylate based superplasticizer that is present in an amount of about 0.08 to about 0.25 by weight of the cement.

19. The method of claim 8 , wherein the carbon nanotubes in the aqueous solution have aspect ratios of less than 1000, the carbon nanotubes are present in an amount of about 0.05% to about 0.1% by weight of the cement and the surfactant comprises a polycarboxylate based superplasticizer that is present in an amount of about 0.23 to about 0.38 by weight of the cement.

20. The method of claim 12 , wherein the carbon nanotubes in the aqueous solution have aspect ratios of greater than 1000, the carbon nanotubes are present in an amount of about 0.02% to about 0.08% by weight of the cement and the surfactant comprises a polycarboxylate based superplasticizer that is present in an amount of about 0.08 to about 0.25 by weight of the cement.

21. The method of claim 12 , wherein the carbon nanotubes in the aqueous solution have aspect ratios of less than 1000, the carbon nanotubes are present in an amount of about 0.05% to about 0.1% by weight of the cement and the surfactant comprises a polycarboxylate based superplasticizer that is present in an amount of about 0.23 to about 0.38 by weight of the cement.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 26, 2009
From: SHAH, SURENDRA P.; KONSTA-GDOUTOS, MARIA S.; METAXA, ZOI S.
To: NORTHWESTERN UNIVERSITY
Reel/Frame 022754/0323 →
Continuity (2)
Provisional Application 61027160 · Feb 8, 2008
Related Publication 20090229494A1 · Sep 17, 2009