Abstract
The addition of graphene and its derivatives can enhance the mechanical and functional properties of cement-based composites, but most of the current technologies have limited dispersion and are costly. The creation of a cost-effective graphene-reinforced cement material with uniform graphene dispersion remains difficult. We used glucose as an economical carbon source to induce the in-situ formation of graphene on cement particles. Our proposed method is approximately 80% less expensive than commercial techniques. Evaluation of the microscopic morphology demonstrated uniform distribution of graphene in the cement matrix, which improved the mechanical properties of the cement paste. The compressive strengths of the test groups with 3% carbon source improved by almostly 38% and 48.9%, respectively, compared with pure cement paste. This newly established technique is essential for the future design of excellent graphene-based cement materials and the achievement of multifunctional cementitious applications.
You have full access to this open access chapter, Download conference paper PDF
Keywords
1 Introduction
Over the past decades, a significant amount of research has been devoted to manipulating the structure of cement hyadration products and the mechanical properties of cement at the nanoscale by using a wide range of nanomaterials such as nanoscale silicon dioxide [1], carbon nanotubes (CNTs) [2], and graphene-based materials [3,4,5,6,7]). Because graphene-based materials are two-dimensional, they possesses good physical and chemical characteristics, making them a suitable option for the next generation of improved cement-based material [8,9,10,11,12]. Many studies [13,14,15,16,17] have demonstrated that graphene and its derivatives, such as graphene oxide (GO), can effectively improve the mechanical characteristics of cementitious materials by increasing the hydration process of the cement and altering the pore distribution in the matrix. Increased durability of GO-reinforced cement mortar can be achieved with only a small amount of additional GO [18]. However, the high cost and poor dispersion of graphene-based compounds prevent their future practical application. The dispersion of graphene materials in the cement matrix [19, 20] is the primary factor that determines how well graphene can reinforce cementitious materials.
It is possible to attribute the aggregation of graphene and its derivative GO to the powerful van der Waals force that exists between nanomaterials as well as the linking effect that Ca2+ and Mg2+ ions have on GO in the cement environment. This is because van der Waals forces are known to exist between nanomaterials [21,22,23]. Graphene and GO in aqueous solution have been prestabilized using a variety of chemical and physical techniques in order to address the issue of their poor dispersion. Graphene-modified cement can be manufactured by combining cement with the prestabilized aqueous solution [14, 23,24,25,26]. However, treatment with ultrasonication for extended periods of time and functionalization with strong acids have adverse impacts on graphene materials, which might cause flaws in the graphene structure.
Here, we describe a novel and uncomplicated technique for the synthesis of graphene–cement (GC) composite. This strategy involves the in-situ development of graphene in the cement matrix (Fig. 1) by carbonization and calcination [27, 28]. In the course of the synthesis procedure, the glucose used as the carbon source is thoroughly combined with the cement [27, 29]. In order to obtain advanced GC material, the mixture is heated further at 800 °C for 2 h, during which the glucose is converted into graphene on the cement particles, which inhibits aggregation and ensures well-dispersed graphene in the cementitious matrix.
2 Methods
2.1 Materials
Glucose (C6H12O6, 98%; Sigma Aldrich) and GO (Suzhou TANFENG graphene Tech) acted as the carbon source and reinforcement material, respectively. Ordinary Portland cement (P.O. 42.5; Jiuqi Building Components) and ethanol (C2H5OH, AR.; Sinopharm Chemical Reagent) were also used in this work.
2.2 Sample Preparation
It is a well known that incorporating a negligible quantity of GO (0.05% by weight) into cement materials can dramatically improve the mechanical characteristics of these materials [5, 13, 30,31,32]. As a result, we carried out a control experiment of adding 0.05 wt% of GO to 100 g of cement. After completely mixing the GO with water, the mixture was sonicated for 30 min by ultrasonic equipment at the highest possible power setting (500 W). Next, the GO solution was included in the cement mix. The production of the new cement paste infused with GO (GOP) followed the same procedure as that of the GC material. In terms of the overall weight of binder, the quantity of GO that was utilized was equal to 0.05 wt%. These techniques provide assurance that the cementitious materials will be capable of meeting the casting standards at the location of the construction project. The GO that is sold commercially has a thickness of roughly 1 nm and a diameter that may reach a maximum of 10 µm. The substance known as GC was created by heating a combination of cement and glucose (carbon source) as shown in Fig. 1. The ratio of cement to glucose powder varied as follows: 100:1, 100:3, and 100:6. The cement and glucose were homogeneously mixed manner at room temperature for 1 h at a rotational speed of 1000 rpm. The mixture was then placed in a furnace to undergo the reaction under a specified high-temperature program while being shielded by N2 as shown in Fig. 1. In this particular investigation, the oven was initially purged with nitrogen at a rate of 50 mL/min before being heated from 25 to 550 °C at a rate of 5 °C/min over 60 min. The temperature inside the furnace then increased by 5 °C every minute until it reached 800 °C, where it remained for 2 h before gradually decreasing to the temperature of the surrounding air. The amount of graphene could be changed by adjusting the bulk amount of glucose, and the yield of pure graphene was determined by using the same techniques. The percentage of graphene that can be yielded was 7%. In order to investigate the effect that in-situ grown graphene development had on the mechanical characteristics of cement paste, we divided the samples into 4 groups: GP-0, GP-1, GP-3 and GP-6 according to the addition amount of glucose before heat treatment as presented in Table 1. Fresh cement paste containing the in-situ growing graphene was pressed into plastic molds with dimensions of 50 × 50 × 50 mm (for the compressive test) and 40 × 40 × 160 mm (for the flexure test). The molds were removed after 24 h and the samples placed in an environment with a relative humidity of 95% for 3, 7, and 28 days, respectively.
2.3 Experimental Methods
In the current investigation, a porosimeter capable of detecting pores ranging in size from 5 nm to 100 μm was utilized (equivalent to pressures of 206 MPa and 345 kPa, respectively, which are the highest and minimum that were applied). Raman spectra were obtained with a Renishaw spectrometer that included an excitation laser wavelength of 532 nm. The instrument was also fitted with ×50 lens and was focused to a spot size that was 1 m in diameter. The scanning electron microscopy (SEM) examination was performed in order to investigate the microstructure. The compression test of cubic specimens with dimensions of 50 × 50 × 50 mm and the three-point flexure test of beam members with dimensions of 40 × 40 × 160 mm are both common methods for determining the mechanical properties of cementitious materials. Both of these tests were performed on specimens with dimensions of 50 × 50 × 50 mm. When calculating the amount of compressive stress, the applied force is divided by the area that is being loaded. The loading rate was set at 1.2 mm/min for the compressive strength test, and at 0.05 mm/min for the flexure test.
3 Results and Discussion
3.1 Characterization of GC Material
The conversion of glucose (carbon source) into graphene on cement particles, which took place during the manufacturing process of GC material, was an essential step in our process of dispersing graphene evenly throughout the cement composites. Figure 2 illustrates the morphology of graphene as well as GC. The results of tests using energy dispersive X-ray spectroscopy (EDS) showed a distinct distribution of carbon (Fig. 2b, c). EDS mapping of the GC material showed that the elements carbon, oxygen, calcium, and silicon were all equally distributed throughout the material (Fig. 2e). SEM and atomic force microscopy revealed that the wrinkled nanosheets of graphene generated by glocuse had a thickness of 1.1 nm (Fig. 2e, f). Very thin sheets were positioned on the surface of the cement particles and had a wrinkly appearance that was analogous to the morphology shown in Fig. 2e. Additional methods of characterization indicated beyond a shadow of a doubt that glucose was effectively transformed to graphene. The X-ray diffraction (XRD) patterns of the GC composite (Fig. 3a) revealed a new peak around 27° representing as-formed graphene sheets. According to the Raman spectra of the GC material, two additional peaks were discovered at 1578 and 1360 cm−1, corresponding to the G-peak and D-peak of graphene, respectively. These peaks are found at these specific frequencies. The development of graphitic carbon was further supported by the G-band of the samples’ 532 nm Raman spectra (Fig. 3b), which was located at 1578 cm−1. The sample displayed a wide D-band with its center at 1360 cm−1, which was indicative of nanoscale graphite particles and chemically modified graphene flakes. The center of the band was at 1360 cm−1. This property, representing the existence of disorder as well as the boundaries of graphene domains, was detected with high-resolution SEM. The results of the studies suggested that the GC composite was composed of cement and graphene. Additionally, the results indicated that the graphene was equally distributed throughout the cement matrix and was confirmed by the fact that the GC material passed the GC test.
3.2 Mechanical Properties of GC Material
After being cured for 28 days, the compressive strengths of GOP paste, GP-0, GP-1, GP-3, and GP-6 were evaluated, and the results are depicted in Fig. 4. When calculating each reported compressive strength, the average of three duplicate specimens was used as the basis for the calculation. The compressive strengths were affected by the different content of the reinforcing materials. The compressive and flexural strengths of the GC paste were superior to those of GP-0 and GOP. The compressive strength of GC paste increased in direct proportion to the graphene content. The GP-3 group demonstrated the strongest compressive strength of all of the groups. In comparison with the GC paste, GOP had a somewhat lower compressive strength. After curing for 28 days, the compressive of GP-3 rose by 38.18% in comparison with GP-0. In contrast, after curing for 28 days, the compressive strength of GOP fell by almost 0.75%, as shown in Fig. 4.
3.3 Dispersion Effect
The large-scale SEM study of GP-3 and GOP, as well as the related element scanning tests, were carried out as shown in Fig. 5 for the purpose of confirming consistent distribution of the graphene. The carbon element distribution map of GCP-3 is shown in Fig. 5b, d, and the element distribution map of GOP is shown in Fig. 5f, both at the same scale as Fig. 5b. As can be seen in Fig. 5f, the aggregation of GO resulted in the formation of carbon element facula. On the other hand, graphene with uniform dispersion does not create an aggregation zone at the same scale (Fig. 5b), which demonstrated that the graphene was uniformly disseminated throughout the cement matrix.
4 Conclusions
By heating a mixture of glucose powder and cement powder, a new in-situ growth approach has been devised with the goal of successfully dispersing graphene throughout the cement matrix in a homogeneous manner. In order to manufacture high-quality graphene in situ, glucose was used as the carbon source because it reduces the overall cost of the process. This recently developed synthetic technique is extensible to the rational design of additional cement-based materials, and it has already been done. The in-situ growing process that was developed may produce a low-cost product and improve the dispersion effect of graphene sheets in the cement matrix. This in turn improves the mechanical properties of cement paste and makes it more amenable for graphene-based reinforced cement composites to be used in civil engineering.
References
Rong Z, Sun W, Xiao H, Jiang G (2015) Effects of nano-SiO2 particles on the mechanical and microstructural properties of ultra-high performance cementitious composites. Cem Concr Compos 56:25–31. https://doi.org/10.1016/j.cemconcomp.2014.11.001
Isfahani FT, Li W, Redaelli E (2016) Dispersion of multi-walled carbon nanotubes and its effects on the properties of cement composites. Cem Concr Compos 74:154–163. https://doi.org/10.1016/j.cemconcomp.2016.09.007
Rafiee MA, Narayanan TN, Hashim DP, Sakhavand N, Shahsavari R, Vajtai R, Ajayan PM (2013) Hexagonal boron nitride and graphite oxide reinforced multifunctional porous cement composites. Adv Funct Mater 23:5624–5630. https://doi.org/10.1002/adfm.201203866
Dimov D, Amit I, Gorrie O, Barnes MD, Townsend NJ, Neves AIS, Withers F, Russo S, Craciun MF (2018) Ultrahigh performance nanoengineered graphene-concrete composites for multifunctional applications. Adv Funct Mater 28:1705183. https://doi.org/10.1002/adfm.201705183
Pan Z, He L, Qiu L, Korayem AH, Li G, Zhu JW, Collins F, Li D, Duan WH, Wang MC (2015) Mechanical properties and microstructure of a graphene oxide–cement composite. Cem Concr Compos 58:140–147. https://doi.org/10.1016/j.cemconcomp.2015.02.001
Jing G, Ye Z, Wu J, Wang S, Cheng X, Strokova V, Nelyubova V (2020) Introducing reduced graphene oxide to enhance the thermal properties of cement composites. Cem Concr Compos 109:103559. https://doi.org/10.1016/j.cemconcomp.2020.103559
Yao Y, Zhang Z, Liu H, Zhuge Y, Zhang D (2022) A new in-situ growth strategy to achieve high performance graphene-based cement material. Constr Build Mater 335:127451. https://doi.org/10.1016/j.conbuildmat.2022.127451
Sun C, Huang Y, Shen Q, Wang W, W. Pan, P. Zong, L. Yang, Y. Xing, C. Wan, Embedding two-dimensional graphene array in ceramic matrix, Sci Adv. 6 (2020) eabb1338. https://doi.org/10.1126/sciadv.abb1338.
Gómez-Navarro C, Burghard M, Kern K (2008) Elastic properties of chemically derived single graphene sheets. Nano Lett 8:2045–2049. https://doi.org/10.1021/nl801384y
Zhu Y, Murali S, Cai W, Li X, Suk JW, Potts JR, Ruoff RS (2010) Graphene and graphene oxide: synthesis, properties, and applications. Adv Mater 22:3906–3924
Hou D, Lu Z, Li X, Ma H, Li Z (2017) Reactive molecular dynamics and experimental study of graphene-cement composites: structure, dynamics and reinforcement mechanisms. Carbon 115:188–208
Liu C, Huang X, Wu Y-Y, Deng X, Zheng Z, Xu Z, Hui D (2021) Advance on the dispersion treatment of graphene oxide and the graphene oxide modified cement-based materials. Nanotechnol Rev 10:34–49. https://doi.org/10.1515/ntrev-2021-0003
Liu J, Li Q, Xu S (2019) Reinforcing mechanism of graphene and graphene oxide sheets on cement-based materials. J Mater Civil Eng. 31:04019014. https://doi.org/10.1061/(asce)mt.1943-5533.0002649
Lu Z, Hou D, Hanif A, Hao W, Li Z, Sun G (2018) Comparative evaluation on the dispersion and stability of graphene oxide in water and cement pore solution by incorporating silica fume. Cem Concr Compos 94:33–42. https://doi.org/10.1016/j.cemconcomp.2018.08.011
Roy R, Mitra A, Ganesh AT, Sairam V (2018) Effect of graphene oxide nanosheets dispersion in cement mortar composites incorporating metakaolin and silica fume. Constr Build Mater 186:514–524. https://doi.org/10.1016/j.conbuildmat.2018.07.135
Sun H, Ling L, Ren Z, Memon SA, Xing F (2020) Effect of graphene oxide/graphene hybrid on mechanical properties of cement mortar and mechanism investigation. Nanomater-Basel 10:113. https://doi.org/10.3390/nano10010113
Ho VD, Ng C-T, Coghlan CJ, Goodwin A, Guckin CM, Ozbakkaloglu T, Losic D (2020) Electrochemically produced graphene with ultra large particles enhances mechanical properties of Portland cement mortar. Constr Build Mater 234:117403. https://doi.org/10.1016/j.conbuildmat.2019.117403
Liu C, Huang X, Wu Y-Y, Deng X, Zheng Z (2021) The effect of graphene oxide on the mechanical properties, impermeability and corrosion resistance of cement mortar containing mineral admixtures. Constr Build Mater 288:123059. https://doi.org/10.1016/j.conbuildmat.2021.123059
Li X, Lu Z, Chuah S, Li W, Liu Y, Duan WH, Li Z (2017) Effects of graphene oxide aggregates on hydration degree, sorptivity, and tensile splitting strength of cement paste. Compos Part Appl Sci Manuf 100:1–8. https://doi.org/10.1016/j.compositesa.2017.05.002
Li X, Liu YM, Li WG, Li CY, Sanjayan JG, Duan WH, Li Z (2017) Effects of graphene oxide agglomerates on workability, hydration, microstructure and compressive strength of cement paste. Constr Build Mater 145:402–410. https://doi.org/10.1016/j.conbuildmat.2017.04.058
Wang M, Niu Y, Zhou J, Wen H, Zhang Z, Luo D, Gao D, Yang J, Liang D, Li Y (2016) The dispersion and aggregation of graphene oxide in aqueous media. Nanoscale 8:14587–14592. https://doi.org/10.1039/c6nr03503e
Lu Z, Chen B, Leung CKY, Li Z, Sun G (2019) Aggregation size effect of graphene oxide on its reinforcing efficiency to cement-based materials. Cem Concr Compos 100:85–91. https://doi.org/10.1016/j.cemconcomp.2019.04.005
Lin J, Shamsaei E, de Souza FB, Sagoe-Crentsil K, Duan WH (2019) Dispersion of graphene oxide–silica nanohybrids in alkaline environment for improving ordinary Portland cement composites. Cem Concr Compos 106:103488. https://doi.org/10.1016/j.cemconcomp.2019.103488
Sabziparvar AM, Hosseini E, Chiniforush V, Korayem AH (2019) Barriers to achieving highly dispersed graphene oxide in cementitious composites: an experimental and computational study. Constr Build Mater 199:269–278. https://doi.org/10.1016/j.conbuildmat.2018.12.030
Zhao L, Zhu S, Wu H, Zhang X, Tao Q, Song L, Song Y, Guo X (2020) Deep research about the mechanisms of graphene oxide (GO) aggregation in alkaline cement pore solution. Constr Build Mater 247:118446. https://doi.org/10.1016/j.conbuildmat.2020.118446
Wang J, Tao J, Li L, Zhou C, Zeng Q (2020) Thinner fillers, coarser pores? A comparative study of the pore structure alterations of cement composites by graphene oxides and graphene nanoplatelets. Compos Part Appl Sci Manuf 130:105750. https://doi.org/10.1016/j.compositesa.2019.105750
Li X, Kurasch S, Kaiser U, Antonietti M (2012) Synthesis of monolayer-patched graphene from glucose. Angewandte Chemie Int Ed. 51:9689–9692. https://doi.org/10.1002/anie.201203207
Zhang B, Song J, Yang G, Han B (2014) Large-scale production of high-quality graphene using glucose and ferric chloride. Chem Sci 5:4656–4660. https://doi.org/10.1039/c4sc01950d
Zhang Y, Zhang L, Zhou C (2013) Review of chemical vapor deposition of graphene and related applications. Accounts Chem Res 46:2329–2339. https://doi.org/10.1021/ar300203n
Krystek M, Pakulski D, Patroniak V, Górski M, Szojda L, Ciesielski A, Samorì P (2019) High-performance graphene-based cementitious composites. Adv Sci 6:1801195. https://doi.org/10.1002/advs.201801195
Wang B, Jiang R, Wu Z (2016) Investigation of the mechanical properties and microstructure of graphene nanoplatelet-cement composite. Nanomater-Basel 6:200. https://doi.org/10.3390/nano6110200
Han B, Ding S, Wang J, Ou J (2019) Nano-engineered cementitious composites. Princ Pract 459–518. https://doi.org/10.1007/978-981-13-7078-6_4
Author information
Authors and Affiliations
Corresponding author
Editor information
Editors and Affiliations
Rights and permissions
Open Access This chapter is licensed under the terms of the Creative Commons Attribution 4.0 International License (http://creativecommons.org/licenses/by/4.0/), which permits use, sharing, adaptation, distribution and reproduction in any medium or format, as long as you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons license and indicate if changes were made.
The images or other third party material in this chapter are included in the chapter's Creative Commons license, unless indicated otherwise in a credit line to the material. If material is not included in the chapter's Creative Commons license and your intended use is not permitted by statutory regulation or exceeds the permitted use, you will need to obtain permission directly from the copyright holder.
Copyright information
© 2023 The Author(s)
About this paper
Cite this paper
Zhang, Z., Yao, Y., Liu, H., Zhuge, Y., Zhang, D. (2023). A New Dispersion Strategy to Achieve High Performance Graphene-Based Cement Material. In: Duan, W., Zhang, L., Shah, S.P. (eds) Nanotechnology in Construction for Circular Economy. NICOM 2022. Lecture Notes in Civil Engineering, vol 356. Springer, Singapore. https://doi.org/10.1007/978-981-99-3330-3_23
Download citation
DOI: https://doi.org/10.1007/978-981-99-3330-3_23
Published:
Publisher Name: Springer, Singapore
Print ISBN: 978-981-99-3329-7
Online ISBN: 978-981-99-3330-3
eBook Packages: EngineeringEngineering (R0)