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AN INVESTIGATION OF NANO SILICA (SiO2) IN THE CEMENT HYDRATION PROCESS

Jon Belkowitz Stevens Institute of Technology Hoboken NJ Hoboken,

Dr Daniel Armentrout University of Denver Denver CO Denver,

2010 Concrete Sustainability Conference

National Ready Mixed Concrete Association

Overview
Introduction A Brief History of Concrete What Makes This Project j Unique? q
Comparing new vs old materials What has been investigated What worked What didnt work 5 Stages of the Heat of Hydration What Happened

Materials and Experiments The Cement Hydration Process Results and Analysis Summary y Questions References

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A Brief History of Concrete


Concrete Technology through time (Finding Solutions in the Face of Adversity)
Appian, Rome: Circa 125 BC First Concrete Roadway, Ohio: 1893 Confederation Bridge, Canada: 1993

Problems in Need of Solutions


Concrete/Cement Expensive ASR , Min. Fly Ash Req.
GAO 85 10R

Apian - Rome Courtesy of Univ of Knowledge, 1938.

1st Concrete Roadway Ohio 1893 Courtesy of Univ of Knowledge, 1938.

Engineering Responsibility
Preserving the Environment Economic Vitality Durable/Sustainable Roadways
Confederate Bridge Canada 1993 Courtesy of www.ConfederateBridge.com, 1995.

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What Makes this Project Unique?


Comparing old vs new materials
Silica, a pozzolanic material
Introduced in the 1970s

Nano Silica Silica, a pozzolanic material


Introduced in the new millennium

What has been investigated g


A nano silica changing a microscopic crystal structure which has macroscopic affects.

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Materials and Experiments p


Constituents
Type I/II Portland Cement Polycarboxylate Comb Polymer (HRWR) Silica

Mix Mi D Design i
No Aggregate w/c of 0.32

Preliminary P li i T Trials i l
Contamination Modifying the Standards

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Materials Silica Fume (SF) ( )


This byproduct is the result of the reduction of high-purity quartz and coal in an electric arc furnace in the manufacture of silicon or ferrosilicon alloy. (PCA 60). Commercialization ~ 1970s 1970 s Surface area of SF ~ 20,000 m2/kg
Cigarette smoke ~ 10,000 m2/kg

Size ~ Average 1.0 m


ST DEV of 0.5 m

Variability

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Materials Nano Silica


Less variability Size distribution
Mix 8, Size ~ Average 35 nm
Range of sizes: 2 to 100 nm

Mix 50, , Size ~ Average g 5.5 nm


Range of sizes: 4 to 6 nm

Mix 508: Combination of 8 and 50

Manufacturers Specification p
Diameter > 40 nm, Filler Diameter < 10 nm, Chemical
Micrograph of Nano Particles From Brian H. Green at the Army Corp of Engineers

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Experiments
With a Brief B i f Discussion Di i on Standards St d d

Calorimetry
Grace Adiacal, Semi-Adiabatic Calorimetric Chamber Specimens: p 76.2 mm ( (diam.) ) by y 152.4 mm (length) Standard: ASTM C 31-09

X-Ray Diffraction
Siemmins E500, X-Ray Diffractor Specimens: 25 mm by 50 mm by 10 mm Standard: N/A

Scanning Electron Microscopy


Jeoul 5800 LV, Scanning Electron Microscope Specimens: 25 mm by 50 mm by 10 mm Standard: N/A

Compressive Tests
Forney Pilot Pilot, Closed Loop Hydraulic Press Specimen: 50 mm by 50 mm by 50 mm Standard: ASTM C 109-08

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Cement Hydration y Process



C3 A + 6 H C3 AH6 Stage 1 Stage 2, 3, & 4 2 (C3S) + 6 (H2O) C3S2H3 + 3(Ca(OH)2 ) 2 (C2S) + 4 (H2O) C3S2H3 + Ca(OH)2 Stage 4, 5 Pozzolanic Reaction S + Ca(OH)2 C3S2H3 + Ca(OH)2

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Results Calorimetry

SF MIX, POZZ REACTION AT 120 Hr

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Results XRD

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Results - SEM

Mix ST CM

Mix SF

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Results SEM, Contd

Mix 8

Mix 50

Mix 508

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Results SEM, Contd

Mix 508

Mix 8

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Results Compressive Strength


Compressive Strength ( (MPa)
100.00 90.00 80.00 70.00 60.00 50.00 40.00 30.00 20.00

8 508 50 SF ST CMT

10

15

20

25

30

Time (Days)
ST DEV for all mixes conformed to the ASTM C 109-08
Did not exceed 3.5 MPa (500PSI) between samples

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Summary y
Thesis Goals
An Investigation of Nano Silica on The Cement Hydration Process

As the Size of the Nano Particle Decreases and the Distribution of Sizes Increases
Increase in Temperature Reduction in CH
Possibility of a Change in CSH

Increase in Compressive Strength SF Mix, Mix An Outlier

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QUESTIONS

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ASTM C 31-09. Standard Practice for Making and Curing Concrete Test Specimens in
the Field. ASTM International. 2009.

References

ASTM C 109 -08 08. Standard Standard Test Method for Compressive Strength of Hydraulic Cement Mortars. ASTM International. 2008. Balaguru, P., and Chong, K. Nanotechnology and Concrete: Research Opportunities. ACI SP-2008. Bentz, D.P. Influence of silica fume on diffusivity in cement-based materials. II. Multi-scale modeling of concrete diffusivity. National Institute of Standards and Technology. July 2000. B Berger, R R. and dM McGregor, G J J. Influence I fl of f Admixtures Ad i t on the th Morphology M h l of f Calcium C l i
Hydroxide Formed During Tricalcium Silicate Hydration. Cement and Concrete Research. 1972.

Bogue, Robert. Chemistry of Portland Cement. Reinhold. 1955. Christensen P. Structural and Ingredient Analysis of Concrete Methods, Results, and Experience. Nordisk Betong. 1984. Gartner, E., Young, J. Damidot, D. and I Jawed. Hydration of Portland Cement. Lafarge. 2000. Green, B. Development of a High-Density Cementitious Rock-Matching Grout using
Nano-Particles. SP-2548. Nanotechnology of Concrete: Recent Developments and Future Perspectives. ACI. K. Sobolev and S.P. Shah. 2008. pp. 121 132.

Holland, T. Silica Fume Users Manual. Silica Fume Association. April 2005. p. 4. Larsen, G. Microscopic Point Measuring: A Quantitative Petrographic Method of
Determining the Ca(OH)2 Content of the Cement Paste in Concrete. Magazine of Concrete Research. 1961.

Mindess, Sydney, J. Young, and, D, Darwin. Concrete. 2nd Edition. Prentice Hall. 2003. Neville, A. M. Properties of Concrete. 14th Edition. Prentice Hall. 2002. Reed, Matt. Nano Silica Particle Size and Distribution. Eka Chemicals. Email
Interview. 22 June 2009.

Sobolev, K., I. Flores, R. Hermosillo, and L.M. Torres-Martinez. Nanomaterials and Nanotechnology for High-Performance Cement Composites. SP-2548. Nanotechnology of Concrete: Recent Developments p and Future Perspectives. p ACI. K. Sobolev and S.P. Shah. 2008. pp pp. 93 120 Spinks, J.W.T., H. W. Baldwin, and T. Thorvaldson. Tracer Studies of diffusion in set Portland Cement. Can. J. Technol. Vol. 30. 1952. St John, Donald, Poole, A., and Ian Sims. Concrete Petrography. Elsevier. 1998.

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Acknowledgements g
Whitney Bitter Harry and Pearl Belkowitz Dr Daniel Armentrout Dr Maciej Kumosa Dr Paul Predecki Brian Burks James Middleton Daniel St-Pierre Matt Nilsen Matt McCombs Lafarge Asphalt Crew Peggy Martinez Kevin Sobczak Renee Teixeira The Folks at Chryso, Inc The Folks at Cemex The Folks at W.R. Grace The Best Family

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