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Investigation of Cementitious Materials for Powder-based 3D Printing A Thesis Submitted in Fulfillment of the Requirements for the Degree of Doctor of Philosophy by Ming Xia Faculty of Science, Engineering and Technology Swinburne University of Technology Hawthorn, VIC, 3122 Australia March 2019
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Investigation of Cementitious Materials for Powder-based 3D Printing

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Investigation of Cementitious Materials for Powder-based 3D PrintingPowder-based 3D Printing
A Thesis Submitted in Fulfillment of the Requirements for the Degree of
Doctor of Philosophy
Swinburne University of Technology
ii
ABSTRACT
The construction industry is expected to go through large transformations since
construction automation is anticipated to drastically alter standard processing
technologies and could lead to possible disrupting technologies such as 3D Concrete
Printing (3DCP). 3DCP is a new and emerging technology that is set to revolutionize
construction by allowing ‘free-form’ construction without the use of expensive
formwork. 3DCP has been proved to be beneficial in terms of optimizing construction
time, cost, design flexibility, and error reduction, as well as being environmentally
friendly.
The powder-based 3D printing method is one of the most attractive 3DCP techniques,
which is capable of producing building components with complex geometries,
optimized topologies, and uniform surface finishes. Currently, this technique is in its
early stages of development and many hurdles are yet to be overcome. One of the main
challenges is the very limited scope of printable cementitious materials that can be used
for construction applications. This research aims to overcome the issues and barriers by
developing a systemic methodology to adapt conventional construction materials to the
powder-based 3D printing process.
In the first part of this research work, a Portland cement-based powder composed of
Portland cement, amorphous calcium aluminate and fine silica sand was developed for
the powder-based 3D printing process. Effects of different printing parameters on
dimensional accuracy and compressive strength of the ‘green’ specimens (before any
post-processing process) have been investigated. The results showed that the printing
parameters had significant effects on the final qualities of the 3D printed components.
Compressive strength of up to 8.4 MPa was achieved for the ‘green’ 3D printed
samples. Subsequently, the effects of post-processing methods on the compressive
strength of 3D printed specimens were also investigated. The results showed that the
compressive strength of the printed samples cured in either tap water or saturated
limewater was significantly higher than that of the ‘green’ samples. The 3D printed
samples cured in saturated limewater for 28 days showed the highest compressive
strength of 29.4 MPa. The degree of anisotropy in the compressive strength was reduced
with the increase of curing time.
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In the second part of this research work, an innovative methodology was presented to
develop geopolymer-based materials for the requirements and demands of the powder-
based 3D printing process, intended for broadening the scope of printable cementitious
materials. Geopolymer is an emerging OPC-less binder purported to provide a
sustainable alternative to OPC. Geopolymer may be manufactured by alkaline
activation of industrial by-products such as fly ash and slag that are rich in silica and
alumina. A geopolymer-based powder using slag-only formulation was developed
which can be used in commercially available powder-based 3D printers. The printed
samples exhibited the highest ‘green’ compressive strength of up to 1.3 MPa.
Subsequently, a series of post-processing methods were developed to enhance the
strength of 3D printed geopolymers. The influences of types of curing medium,
duration, and temperature of curing on the compressive strength of the printed samples
were investigated. Post-processing of the samples was carried out in tap water, three
alkaline solutions and three fly ash-based geopolymer slurries at different temperatures
(25°C, 40°C, 60°C and 80°C). The results showed that printed geopolymer samples
cured in a combination of 8.0 M sodium hydroxide solution (28.6% w/w) and sodium
silicate solution with SiO2/Na2O = 3.22 at 60°C for 7 days gained the highest
compressive strength of 30 MPa, which is sufficiently high for a wide range of
construction applications. The results also showed that the compressive strength of the
samples cured at ambient temperature (25°C) for 28 days was comparable to that of the
samples cured at 60°C for 7 days. The comparable strength of the ambient-temperature
cured samples significantly enhances the commercial viability of 3D printed
geopolymers since the developed ambient-temperature curing method is significantly
less energy- and emissions-intensive compared to the heat-curing method.
To expand the scope of printable geopolymer materials, the methodology developed in
the second part was extended to fly ash and slag combinations. The inclusion of fly ash
in the formulation is because it is more abundantly available than slag and a large
amount of it is still dumped in many parts of the world. The quantitative influences of
fly ash content on the printability of the geopolymer powder, as well as the dimensional
accuracy and compressive strength of the printed specimens were investigated. The
effect of type of alkaline solution used for the post-processing on the dimensional
accuracy and compressive strength of the post-processed specimens were also
evaluated. The results showed that the maximum fly ash content that can be
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incorporated in the developed 3D printable geopolymer powder is 50 wt%. The post-
processed samples printed with 50 wt% slag/50 wt% fly ash powder cured at 60°C for
7 days exhibited a compressive strength of up to 25 MPa.
The powder-based 3D printing process is likely to be used for highly detailed
ornamental shapes where the high accuracy will be demanded. Therefore, a novel
method based on image acquisition and processing system using a flatbed scanner was
developed to quantitatively evaluate the shape accuracy of the powder-based 3D printed
samples. A set of image processing algorithms was developed to extract useful shape
information from scanned images without any intervention. Centroid distance function
was used as the shape error representation under the polar coordinate system for the
shape error measurement. A color-labeled map in conjunction with root mean square
error (RMSE) were used to quantify the shape accuracy of the samples. The results
showed that the developed method can satisfactorily be used for shape accuracy
measurement of the powder-based 3D printed specimen. At the same time, this method
is cheaper, simpler and less time-consuming compared to the currently used techniques
such as computed tomography (CT) scan and coordinate measuring machine (CMM).
Overall, the novel methodologies developed in this doctoral research expand the
severely limited scope of cementitious materials that can be used in the powder-based
3D printing process for construction applications.
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ACKNOWLEDGEMENTS
The thesis was partly funded by Australian Research Council Discovery Grant
DP170103521 and Linkage Infrastructure Grant LE170100168 and Discovery Early
Career Researcher Award DE180101587. I also acknowledge Swinburne University of
Technology for supporting and funding this doctoral research through Swinburne
University Postgraduate Research Award (SUPRA) and ARC Discovery Scholarship.
First of all, and most importantly, I want to thank my family. I am eternally grateful to
my parents, Mr. Qingyuan Xia and Ms. Yan Zou, for setting the model of how to be the
person I am today. Their belief in me and unconditional support have always given me
the strength to follow my dreams.
I would like to express my deep gratitude to my principal coordinating supervisor,
Professor Jay Sanjayan for his patient guidance and valuable support on this journey,
and his valuable and constructive suggestions during this doctoral research. I would
also like to truly thank him for placing his confidence in my work which gave me the
strength to continue. This thesis would not have been possible without his support. I am
forever indebted for his great mentorship.
I am also grateful to my associate supervisor, Dr. Behzad Nematollahi for his
extraordinary help and support during my doctoral research, and for the many, many
encouraging talks he gave me on this journey. Without his support, I might never have
managed to believe this was possible.
I truly appreciate Dr. Vinh Dao (University of Queensland, Australia) and Prof. Paolo
Colombo (University of Padova, Italy) as my examiners for revising this manuscript
and for their help in getting it to its final shape.
I would especially like to thank Miss Meiyu Hu for being there for me for every up and
down in these 1400 days. Thank you came into my life, the beautiful, happy, thank you
for giving me cherish the memory forever.
I would like to acknowledge the people in the Digital Construction Laboratory, who
contributed in one way or another to this work. I am thankful to Dr. Ali Nazari and Dr.
Hongjian Du, Taylor Marchment, Shin-Hau Bong, Ravendran Arunothayan, Roshan
Jayathilakage Shiwei Yu for supporting me with experimental work, data analysis or
collection, and for engaging in insightful discussions. I am also grateful to Praful Vijay
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for being a wonderful friend. Especially thank Senior Laboratory Engineer Kia Rasekhi
for his invaluable technical assistance and guidance during the experimental work.
Every single person in the group contributed to making this journey a very special,
extremely enjoyable, and incredibly rewarding experience.
And lastly, from the bottom of my heart, I wish to express my sincere gratitude
everyone who has given me power, enthusiasm, and motivation throughout my life.
viii
DECLARATION
I declare that the thesis is my original work except for quotations and citations which
have been duly acknowledged. I also declare that it has not been previously, and is not
concurrently, submitted for any other degree at any other institutions. I hereby declare
that I am the sole author of this thesis.
Ming Xia
March 2019
Patent:
Provisional Patent No. 2018903373.
Peer-Reviewed Journal Papers:
(1) Xia, M., Nematollahi, B., and Sanjayan, J., 2019 Post-processing methods to
improve strength of particle-bed 3D printed geopolymer for digital construction
applications. Frontiers in Materials, 6:160.
(2) Xia, M., Nematollahi, B. and Sanjayan, J., 2019. Printability, accuracy and strength
of geopolymer made using powder-based 3D printing for construction applications.
Automation in Construction, 101, pp.179-189.
(3) Xia, M., Nematollahi, B. and Sanjayan, J., 2018. Influence of binder saturation level
on compressive strength and dimensional accuracy of powder-based 3D printed
geopolymer. In Materials Science Forum (Vol. 939, pp. 177-183). Trans Tech
Publications.
(4) Xia, M. and Sanjayan, J.G., 2018. Methods of enhancing strength of geopolymer
produced from powder-based 3D printing process. Materials Letters, 227, pp.281-
283.
(5) Xia, M. and Sanjayan, J., 2016. Method of formulating geopolymer for 3D printing
for construction applications. Materials & Design, 110, pp.382-390.
Book Chapters:
(1) Xia, M., Nematollahi, B. and Sanjayan, J.G., 2019. Properties of Powder-Based 3D
Printed Geopolymers. In 3D Concrete Printing Technology (pp. 265-280).
Butterworth-Heinemann.
x
(2) Xia, M., Nematollahi, B. and Sanjayan, J.G., 2019. Development of Powder-Based
3D Concrete Printing Using Geopolymers. In 3D Concrete Printing Technology
(pp. 223-240). Butterworth-Heinemann.
(3) Xia, M., Nematollahi, B. and Sanjayan, J., 2018, September. Compressive strength
and dimensional accuracy of portland cement mortar made using powder-based 3D
printing for construction applications. In RILEM International Conference on
Concrete and Digital Fabrication (pp. 245-254). Springer, Cham.
Peer-Reviewed Conference Papers:
(1) Xia, M. and Sanjayan, J., 2017. Post-processing methods for improving strength of
geopolymer produced using 3D printing technique. In International Conference on
Advances in Construction Materials and Systems, ICACMS, Chennai (pp. 2746-
2773).
(2) Nematollahi, B., Xia, M. and Sanjayan, J., 2017. Current progress of 3D concrete
printing technologies. In ISARC. Proceedings of the International Symposium on
Automation and Robotics in Construction (Vol. 34). Vilnius Gediminas Technical
University, Department of Construction Economics & Property.
Other publications during this doctoral research:
Peer-Reviewed Journal Papers:
(1) Bong, SH, Nematollahi, B, Nazari, A, Xia, M & Sanjayan, J 2019, Method of
Optimisation for Ambient Temperature Cured Sustainable Geopolymers for 3D
Printing Construction Applications, Materials, vol. 12, no. 6, pp. 902.
(2) Marchment, T., Sanjayan, J. and Xia, M., 2019. Method of enhancing interlayer
bond strength in construction scale 3D printing with mortar by effective bond area
amplification. Materials & Design, pp.107684.
(3) Nematollahi, B., Vijay, P., Sanjayan, J., Nazari, A., Xia, M., Naidu Nerella, V. and
Mechtcherine, V., 2018. Effect of Polypropylene Fibre Addition on Properties of
Geopolymers Made by 3D Printing for Digital Construction. Materials, 11(12),
pp.2352.
xi
(4) Nematollahi, B., Xia, M., Sanjayan, J. and Vijay, P., 2018. Effect of type of fiber
on inter-layer bond and flexural strengths of extrusion-based 3D printed
geopolymer. In Materials Science Forum (Vol. 939, pp. 155-162). Trans Tech
Publications.
(5) Sanjayan, J.G., Nematollahi, B., Xia, M. and Marchment, T., 2018. Effect of
surface moisture on inter-layer strength of 3D printed concrete. Construction and
Building Materials, 172, pp.468-475.
Under Review Journal Papers:
(1) Nematollahi, B., Vijay, P., Sanjayan, J., Xia, M., Nerella, VN.and Mechtcherine,
V., 2018. “Systematic Approach to Develop Geopolymers for 3D Concrete
Printing”. Archives of Civil and Mechanical Engineering, Under review.
Book Chapters:
(2) Nematollahi, B., Xia, M., Vijay, P. and Sanjayan, J.G., 2019. Properties of
Extrusion-Based 3D Printable Geopolymers for Digital Construction Applications.
In 3D Concrete Printing Technology (pp. 371-388). Butterworth-Heinemann.
(3) Marchment, T., Sanjayan, J.G., Nematollahi, B. and Xia, M., 2019. Interlayer
Strength of 3D Printed Concrete: Influencing Factors and Method of Enhancing. In
3D Concrete Printing Technology (pp. 241-264). Butterworth-Heinemann.
(4) Bong, S.H., Nematollahi, B., Nazari, A., Xia, M. and Sanjayan, J.G., 2018,
September. Fresh and hardened properties of 3D printable geopolymer cured in
ambient temperature. In RILEM International Conference on Concrete and Digital
Fabrication (pp. 3-11). Springer, Cham.
(5) Nematollahi, B., Xia, M., Bong, S.H. and Sanjayan, J., 2018, September. Hardened
Properties of 3D Printable ‘One-Part’Geopolymer for Construction Applications.
In RILEM International Conference on Concrete and Digital Fabrication (pp. 190-
199). Springer, Cham.
Peer-Reviewed Conference Papers:
(1) Marchment, T., Xia, M., Dodd, E., Sanjayan, J. and Nematollahi, B., 2017. Effect
of delay time on the mechanical properties of extrusion-based 3D printed concrete.
In ISARC. Proceedings of the International Symposium on Automation and
Robotics in Construction (Vol. 34). Vilnius Gediminas Technical University,
Department of Construction Economics & Property.
(2) Nematollahi, B., Xia, M. and Sanjayan, J., 2017. Current progress of 3D concrete
printing technologies. In ISARC. Proceedings of the International Symposium on
Automation and Robotics in Construction (Vol. 34). Vilnius Gediminas Technical
University, Department of Construction Economics & Property.
TABLE OF CONTENTS
1.3 Research Objectives .............................................................................................. 31
1.4 Research Methodology .......................................................................................... 32
1.5 The Scope of Work and Organization of Thesis ................................................... 33
1.6 References ............................................................................................................. 36
CHAPTER 2 .................................................................................................................. 39
LITERATURE REVIEW ............................................................................................. 39
2.1 Introduction ........................................................................................................... 39
2.2.3 Ceramics ......................................................................................................... 48
2.4 Current 3D Construction Printing Technologies ................................................... 55
2.4.1 Extrusion-based 3D printing technique .......................................................... 55
2.4.2 Current large-scale applications of extrusion-based 3D printing technique ... 63
2.4.3 Powder-based 3D printing techniques ............................................................ 71
2.4.4 Current challenges of adopting AM techniques in the construction industry 77
2.5 Geopolymer Technology ....................................................................................... 82
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................................................................................................................................. 94
2.5.5 The available literature on developing geopolymer for 3D printing .............. 96
2.6 Summary ............................................................................................................. 101
2.7 References ........................................................................................................... 103
CHAPTER 3 ................................................................................................................ 118
3.1 Introduction ......................................................................................................... 118
3.3.1 Results of Part I ............................................................................................ 124
3.3.2 Results of Part II ........................................................................................... 129
3.4 Conclusions ......................................................................................................... 134
3.5 References ........................................................................................................... 137
CHAPTER 4 ................................................................................................................ 139
CONCRETE PRINTING ........................................................................................... 139
4.1 Introduction ......................................................................................................... 139
4.2.1 Materials ....................................................................................................... 140
4.2.4 3D printed parts characterizations ................................................................ 146
4.3 Results and Discussions ...................................................................................... 147
4.3.1 Characterizations of powders ....................................................................... 147
4.3.2 Characterizations of 3D printed structures ................................................... 152
4.4 Conclusions ......................................................................................................... 159
4.5 References ........................................................................................................... 161
GEOPOLYMER ......................................................................................................... 165
5.2.3 Post-processing procedures .......................................................................... 168
5.2.4 Compressive strength .................................................................................... 170
5.3.1 Effect of curing temperatures ....................................................................... 170
5.3.2 Effect of curing mediums ............................................................................. 172
5.4 Conclusions ......................................................................................................... 175
5.5 References ........................................................................................................... 175
CHAPTER 6 ................................................................................................................ 178
6.1 Introduction ......................................................................................................... 178
6.2.1 Raw materials ............................................................................................... 179
6.2.3 Post-processing and testing methods ............................................................ 183
6.3 Results and Discussions ...................................................................................... 184
6.3.1 Heat curing group ......................................................................................... 184
6.3.2 Ambient temperature curing group ............................................................... 187
6.4 Conclusions ......................................................................................................... 191
6.5 References ........................................................................................................... 192
CHAPTER 7 ................................................................................................................ 198
7.1 Introduction ......................................................................................................... 198
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7.2.3 Powder-based 3D printing process ............................................................... 203
7.2.4 Post-processing procedure ............................................................................ 204
7.3.1 Linear dimensional accuracy ........................................................................ 205
7.3.2 Mechanical property ..................................................................................... 205
7.4.1 Powder characteristics .................................................................................. 205
7.5 The Merits and Demerits of the Approach .......................................................... 221
7.6 Conclusions ......................................................................................................... 222
7.7 References ........................................................................................................... 225
CHAPTER 8 ................................................................................................................ 229
SHAPE ACCURACY OF POWDER-BASED 3D PRINTING .............................. 229
8.1 Introduction ......................................................................................................... 229
8.1.2 Metrology ..................................................................................................... 231
8.2.1 Materials ....................................................................................................... 232
8.2.3 The powder-based 3D printing process ........................................................ 234
8.2.4 Image acquisition of test component ............................................................ 235
8.3 Image Processing Algorithms ............................................................................. 236
8.3.1 Grayscale conversion and contrast stretching ............................................... 237
8.3.2 Binary conversion and thresholding ............................................................. 238
8.3.3 Erosion, dilation, and border removal .......................................................... 240
8.3.4 Shape boundary and centroid detection ........................................................ 241
8.4 x-y plane Shape Accuracy ................................................................................... 242
8.4.1 Representation of shape errors in the x-y plane ............................................ 242
8.4.2 Measurement of the shape error in the x-y plane ......................................... 244
8.4.3 Assessment of the x-y plane shape accuracy ................................................ 245
8.5 Application of the Proposed Methodology ......................................................... 246
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8.5.1 Shape errors of test component printed by ZP powder ................................. 246
8.5.2 Shape errors of test component printed by GP powder ................................ 248
8.5.3 Shape Accuracy of Plate Component Printed from ZP And GP Powders ... 251
8.6 Conclusions ......................................................................................................... 253
8.7 References ........................................................................................................... 254
8.8 Appendix ............................................................................................................. 259
CHAPTER 9 ................................................................................................................ 267
RESEARCH ................................................................................................................ 267
9.2 Recommendations for Future Research .............................................................. 273
xviii
Figure 2-1. Schematic illustration of the SLA process ................................................ 41
Figure 2-2. Schematic illustration of the FDM process ............................................... 42
Figure 2-3. Schematic illustration of PolyJet printing process .................................... 43
Figure 2-4. Schematic illustration of the SLS process ................................................. 44
Figure 2-5. Schematic illustration of the DLP process ................................................ 45
Figure 2-6. Schematic illustration of the EBM process ............................................... 47
Figure 2-7. Schematic illustration of the LPF process ................................................. 48
Figure 2-8. Schematic illustration of the powder-based printing process ................... 49
Figure 2-9. The progression of 3DCP advancement since 1997 (Source: Buswell et al.
2018) ............................................................................................................................ 54
Figure 2-10. An example of an extrusion-based printing system ................................ 56
Figure 2-11. Contour Crafting. (a) The deposition system, (b) A printed dome structure.
(Source: Khoshnevis et al. 2006) ................................................................................. 57
Figure 2-12. Concrete Printing. (a) Printing system, (b) Printed bench structure.
(Source: Lim et al. 2011) ............................................................................................. 59
Figure 2-13. Schematic illustrations of CONPrint3D (a) Printing process (b) Essential
components and (c) Design of the printhead. (Source: Krause et al. 2018) ................ 61
Figure 2-14. Multifunctional wall element (Source Gosselin et al. 2016) ................... 62
Figure 2-15. Conceptual diagram of the production of SDC (left). A structure fabricated
by SDC (right) (Source: Lloret-Fritschi et al. 2018; Scotto et al. 2018) ..................... 63
Figure 2-16. WinSun Project. (Source: 3ders 2015) .................................................... 65
Figure 2-17. Huashang Luhai Project. (a) A two-story-tall printed villa, (b) Deposition
system. (Source: 3dprint 2015) .................................................................................... 66
Figure 2-18. WASP Project: (a) BigDelta printer, (b) Printed clay wall. (Source:3dwasp
2018) ............................................................................................................................ 66
Figure 2-19. The first 3D printed modular reinforced concrete beam with a variable
cross-section (Source: Asprone et al. 2018) ................................................................ 67
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3DCP (Source: 3ders 2017b) ....................................................................................... 68
Figure 2-21. On-site’ 3D printed house by Apis Core (a) A ‘mobile’ 3D concrete printer,
(b) Exterior of the printed house (Source: 3ders 2017a) .............................................. 69
Figure 2-22. Figure 2-22. 3D printed bicycle bridge by TU/E (Source: Dezeen 2017)
...................................................................................................................................... 70
Figure 2-23. (a) A single-arched pedestrian bridge, (b-d) Assembling and 3D printing
process (Source: Dezeen 2019) .................................................................................... 71
Figure 2-24. Schematic illustration of the powder-based 3D printing ......................... 72
Figure 2-25. (a) D-shape printer, (b) 3D printed Spiral Holes and (c) 3D printed footpath
bridge. (Source: D-shape 2018) ................................................................................... 73
Figure 2-26. Emerging Objects. (a) 3D Printed ‘Bloom’ structure, (b) ‘3D Printed
House 1.0’. (Source: EmergingObjects 2018) ............................................................. 74
Figure 2-27. Digital Grotesque-Grotto II (Source: DigitalGrotesque 2017) ............... 74
Figure 2-28. (a) The process of selective paste intrusion; (b) Printed pipe with double
bracing. (Source: Pierre et al. 2018; Weger, Lowke & Gehlen 2016a) ....................... 75
Figure 2-29. Schematic geopolymerization process (Source: Davidovits 1999) ......... 84
Figure 2-30. Geopolymer systems based on the number of siloxo Si-O units (Source:
Davidovits 1999) .......................................................................................................... 85
Figure 2-31. Glukhovsky model (Source: Duxson et al. 2006) ................................... 86
Figure 2-32. A descriptive model of the alkali…