Document 7226775

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Synthesis of Calcium Silicate
Hydrate/Polymer Nanocomposites
S. C. Mojumdar & L. Raki
Institute for Research in Construction
National Research Council Canada
2nd International Symposium on Nanotechnology in Construction
Bilbao, Spain, 13-16 November 2005
Outline
• Introduction
• Research approach
• Discussion of results
• Future prospects
• Summary
IRC: “Canada's
Construction
Technology Centre”
• Mission
– Develops core competencies, knowledge base critical to
construction needs
– Supports development, commercialization,
implementation of leading technologies
– Fosters safe, sustainable built environment through
development of codes and standards
IRC Services to
Construction Industry
• Contract Research
• Strategic Research
• Development of Model
Building Codes
• Evaluation of Innovative
Construction Products
• Dissemination of Technical
Information
Diversified Research
Services
• Laboratory research
(unique national
facilities)
• Computer Modelling
• Field Work
• Many national
and international
consortia
IRC Program Areas
• Indoor Environment
• Fire Research
• Urban Infrastructure
• Canadian Codes Centre
• Canadian Construction Materials Centre
• Building Envelope and Structure
Building Envelope
& Structure
• Objective
– Develop technologies for the design,
construction and operation of durable,
energy-efficient and cost-effective building
envelope systems and structures.
Building Envelope &
Structure
• Heat & Moisture Performance of Envelopes
• Performance of Roof Systems & Insulation
• Concrete Materials & Structural Technologies
CMST Sub-Program
Staff
Researchers
•
•
•
•
•
•
Dr. L. Raki
Mr. M. Arnott
Dr. J. Makar
Dr. L. Mitchell
Dr. G. Pernica
Dr. H. Rahman
Technical Officers
•
•
•
•
Mr.G. Chan
Mr. R. Glazer
Mr. G. Pye
Mr. K. Trishuk
Guests
• Dr. J. Beaudoin
• Dr. R. Ramachandran
• Mr. N. Mailvaganam
Students/visitors
•
•
•
•
Mr. T. Sato (PhD)
Dr. S. Mojumdar (PDF)
Dr. P. Mercier (PDF)
Ms. K. Essagheier (WES)
CMST’s Vision
To be considered the leading research group
in the development of innovative, durable,
eco-efficient construction materials and
repair technologies in partnership with
industry and universities through market
driven strategic and client supported
investigations.
CMST Sub-Program
Projects
• Sustainable Concrete
Technologies
• Safety & Security
of Buildings
• Innovative Materials
& Systems
Corrosion
Alkali-Silica Reaction (ASR)
Repair
Nanotechnology for
Construction at IRC
Research Approach
Materials (nm –mm)
Microstructure
Design
Properties
Structures
Mechanics
(m)
(mm-m)
Materials-Mechanics-Structures Interaction
Research Approach
Need to interface different disciplines
Chemistry
Materials
Science
Physics
Engineering
Research Facility (cont’d)
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Scintag XDS2000 XRD
Rigaku Geigerflex XRD
TA Instrument Q600
Jeol JSPM5200 AFM
Hitachi S4800 SEM
Bomem MB 100 FTIR
Research Facility (cont’d)
•
•
•
•
•
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Bruker S4 Pioneer XRF
Varian SpectrAA 250 Plus AA
Metrohn 808 Titrando
Mercury porosimeter
Particle analyzer
2 TAM air calorimeters
Projects
• Synthesis & Characterization of
Nanoparticles
• CNT/Cement Composites
• Cement-based Nanocomposites
– Organic-inorganic hybrids
– C-S-H:
 Volume stability
 Organic intercalates
Synthesis & Characterization of Nanoparticles
Highlights:
• Synthesis of nano-sized
cement phases (e.g.. low
energy C2S)
• Production of nanoscale
particle for use as rheology
modifiers, accelerators, and
shrinkage compensating
agents
Cementitious nanoparticles syntesized
by “Chimie douce” techniques
Rate of Heat Development, Cal/g/h
Calorimetry: Nano-CaCO3 – C3S Pastes
4
C3S, w/c = 0.50
15%
3.5
3
2.5
2
10%
1.5
5%
1
% CaCO3
0.5
0%
0
0
5
10
15
20
Time, h
25
30
35
40
Calorimetry: Nano-CaCO3 – OPC Pastes
Rate of Heat Development, Cal/g/h
4
OPC, w/c = 0.50
3.5
3
2.5
2
15%
1.5
10%
1
5%
0.5
0%
% CaCO3
0
0
10
20
30
40
Time, h
50
60
70
80
Carbon Nanotubes/Cement Composites
Highlights:
• Unique physical properties
– very high strength, thermal
conductivity
• Cement-carbon nanotube
composites
– toughening through control
of microcracking
Carbon nanotubes bridging
cracks in a cement composite
Controlled Release of Chemical
Admixtures
Highlights:
• Chimie douce technique
• New routes for
delivering and
controlling admixtures
• Provisional patent
C-S-H-Based
Nanocomposites
Man-made Nanomaterials: Nanostructure of C-S-H
Schematic of the nanostructure of the binding phase
within concrete,
Feldman Model, Concrete Science 1981
Cement at the
Nanoscale
• The hydrated cement binder in concrete has a
complex, nanoscale structure that is still not
fully understood
• Hydrated cement is porous, with a pore size
distribution that ranges from the nanometers
to millimeters
• Cement and its hydrates can be manipulated
and controlled through nanotechnology
Analogy with Clays
• Clay layers separated by an interlayer or gallery.
• Layers are ~ 1 nm thick, 300 nm to microns
laterally.
• Organics and inorganics as interlayers.
• Tailor structural, physical properties.
Clay
Nanocomposites
Phase separated
Intercalated
+
Layered
Silicate
Polymer
Exfoliated
XRD Analysis
400
350
d =1.40 nm
Intensity(Counts)
300
C-S-H/PVA (0.7/0.5)
250
200
150
d = 1.26 nm
100
C-S-H (0.7)
50
0
4
5
6
7
8
2-Theta(°)
9
10
11
12
FTIR
Assignments
-1)
(cm811
973,
C-S-H-PVA
(0.7-0.05)
-1)
(cm812
974,
C-S-H-PVA
(0.7-0.75)
-1)
(cm816
977,
(cm- -1)
Si-O-Si
670
673
673
-
Si-OH
3742
3741
3744
-
H-O-H
1645
1643
1651
-
OH
3390
3422, 3240
3339, 3281
3337
CH3
-
2936
2925
2934
CH2
-
2857
2876
2891
O=C-OR
-
1410
1434
1445
C-O-C
-
1036
1039
1093
CH
-
831
843
844
CO32-
1431
1410
1434
-
Other Bands
448
460
447
-
Si-O
C-S-H
PVA
TGA
100
80
Weight (%)
60
40
–––––––
––––
––––– ·
––– – –
––– –––
CSH(0.7)0
CSH-PVA(0.7-0.05)
CSH-PVA(0.7-0.5)
CSH-PVA(0.7-0.75)
PVA(Rep).001
20
0
0
200
400
600
Temperature (°C)
800
1000
1200
Universal V3.8B TA Instruments
Thermal
Conductivity
Sample
Average of the
Measured k
/ Wm-1 K-1
25 C
50 C
0.1063
0.11375
C-S-HPN
material
0.1650
0.1895
C-S-H
0.1012
0.1189
PVA
Increase
from 25 to 50
RSD / %
C / %
25 C
50 C
0.81
0.13
14.85
0.39
0.11
17.46
4.61
0.17
7.03
29Si
MAS-NMR
Q2
C-S-H (0.7)
Q1
ppm
-60
Q2
-70
-80
-90
-100
-110
Q2
Q2
CSH-PVA (0.7-0.50)
CSH-PVA (0.7-0.75)
Q1
Q1
Q1
ppm
ppm
ppm
-60
-70
-80
-90
-100
-110
-60
-70
-80
-90
-100
-110
13C
CP MAS-NMR
PVA
CH2
CHinter
CHinter
CHintra
30
40
50
60
70
80
90
CSH-PVA(0.7-0.5)
30
40
50
60
70
80
90
13C
DD MAS-NMR
30000
13C CP
25000
13CP DDP
Intensity
20000
15000
10000
5000
0
-5000 0
10
20
30
40
50
Chemical Shift /ppm
60
70
80
90
Synthetic C-S-H
Synthetic C-S-H
C-S-H-PVA
C-S-H
C-S-H PVA
Recent and Future
Developments
Development of sustainable products through
knowledge-based activities
• Engineering the formation of selected C/S ratio C-S-H
• Elucidate the interaction of “superplasticizers” and other types
of chemical admixtures with C-S-H and other nanoadditives
• Optimizing volume stability by controlling the interaction of
alkali ions and C-S-H
• Immobilizing environmentally unfriendly species in C-S-H
binding materials
• Superior extrudable cement boards/tiles
• Optimizing the use of MDM for maximizing the performance
of nano cement-based materials1
1
R.J. Kirkpatrick et al.
Workshop on Nanotechnology in Constryction, Ottawa, 2004
Other possible areas of
research in construction
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Rheology
Fire
FRP
Paint
Sensors
Insulation
Shrinkage
Coatings
Corrosion
Roads
Summary
• C-S-H/polymer
complexes
formation
opens up potentially new
routes to cement-based
nanocomposites
• Nanotechnology has the
potential to produce a
significant impact on the
construction industry
 Improved performance and
service life
 Stronger, tougher, lightweight
materials
Acknowledgments
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Dr. J. J. Beaudoin
Mr. G. Chan (XRD)
Mr. P. Collins (FTIR)
Mrs. A. Delgado (TGA)
Mr. S. Lang (NRC/SIMS, NMR)
Mr. J. Margeson (SEM, AFM)
Mr. D. Wang (NRC/ICPET, TEM)
• NRC-Major Initiative Committee
• NSERC for PDF grant