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Article

Red Mud in Combination with Construction Waste Red Bricks for the Preparation of Low-Carbon Binder Materials: Design and Material Characterization

by
Teng Qin
1,
Hui Luo
1,2,
Rubin Han
1,
Yunrui Zhao
1,
Limin Chen
1,
Meng Liu
1,
Zhihang Gui
1,
Jiayao Xing
1,
Dongshun Chen
1 and
Bao-Jie He
3,4,5,*
1
School of Civil and Ocean Engineering, Jiangsu Ocean University, Lianyungang 222005, China
2
Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071, China
3
Centre for Climate-Resilient and Low-Carbon Cities, School of Architecture and Urban Planning, Key Laboratory of New Technology for Construction of Cities in Mountain Area, Ministry of Education, Chongqing University, Chongqing 400045, China
4
School of Architecture, Design and Planning, University of Queensland, Brisbane 4072, Australia
5
CMA Key Open Laboratory of Transforming Climate Resources to Economy, Chongqing 401147, China
*
Author to whom correspondence should be addressed.
Buildings 2024, 14(12), 3982; https://doi.org/10.3390/buildings14123982
Submission received: 6 November 2024 / Revised: 2 December 2024 / Accepted: 9 December 2024 / Published: 15 December 2024
(This article belongs to the Section Building Materials, and Repair & Renovation)
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Abstract

The effective and safe treatment of red mud has become a pressing global issue in recent years. The purpose of this study is to prepare different systems of low-carbon cementitious materials by combining various solid wastes (slag powder, red brick of construction waste) with different systems of low-carbon cementitious materials and to observe the effects of different cementitious compositions on the construction performance, mechanical properties, freeze–thaw resistance, and heavy metal leaching properties by designing different systems of low-carbon cementitious materials, as well as to analyze the microscopic morphology, mineral composition, and strength-forming mechanisms of the different systems of low-carbon cementitious materials through the use of X-ray fluorescence (XRF), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR) techniques. The findings reveal that a ternary cementitious system containing 16% red brick powder exhibits the most favorable overall performance. Compared to a binary system, this mixture improves fluidity by 4.5%, increases compressive strength by 18.27%, reduces drying shrinkage by 39.56%, and lowers the mass loss rate during dry–wet cycling by 11.07%. Furthermore, the leaching levels of heavy metals such as Cr, As, Pb, Ni, and Cu in the red mud-based cementitious materials, combined with multiple solid wastes, are within the safe limits for non-hazardous environmental release, as specified by Chinese regulations, under both freeze–thaw and non-freeze–thaw conditions. This study demonstrates for the first time the potential of combining red mud with construction waste brick dust and provides a scientific basis and theoretical guidance for the synergistic utilization of alkaline solid waste, calcium solid waste, and silica–aluminum solid waste.

1. Introduction

Sustainability has emerged as a key focus worldwide [1]. However, rapid urbanization and industrialization have resulted in a substantial accumulation of industrial solid waste, posing a serious challenge to sustainable development [2]. Notably, the accumulation of red mud (RM), an industrial waste byproduct from alumina refining in bauxite mining, has become particularly concerning, with global reserves estimated to reach approximately 4 billion t [3]. Due to its high alkalinity and heavy metal content [4], the storage process can alter the pH of the soil in the area, leading to soil salinization; at the same time, the chloride ions in the alkali residue can also cause varying degrees of pollution in groundwater. As a result, the comprehensive management and reuse of RM have attracted considerable interest [5].
Currently, RM is primarily utilized as an absorbent in wastewater treatment [6], for extracting rare metals [7], and in the production of gelling materials [8]. Among these applications, its use in gelling material production has gained significant research traction in recent years [9]. The main chemical composition of RM includes Al2O3, SiO2, Fe2O3, and Na2O, indicating its potential for gelling material preparation [10]. Additionally, RM’s fine particle size and large surface area contribute to improving the mechanical characteristics of such materials [11]. However, using RM alone in alkali-activated materials results in a compressive strength of less than 5 MPa, limiting its effectiveness [12]. Methods such as applying pressure, high-temperature treatment, or activation of RM have been explored to improve its mechanical properties [13,14], but these processes are often energy-intensive and lead to increased carbon emissions [15]. To address these challenges, Lemougna et al. [16] modified RM using a sodium silicate solution, achieving a notable enhancement in the mechanical characteristics of the gelling material. However, the process may still intensify RM consumption and raise concerns about energy use and potential secondary pollution [17]. Thus, it is crucial to develop new approaches to optimize RM utilization. Recent research suggests that synergistic utilization strategies can be effective in reducing both energy consumption and carbon emissions [18].
Studies demonstrate that the synergistic combination of RM with other solid wastes can notably enhance the mechanical properties of gelling materials. In this context, Kardelen Kaya et al. [19] systematically investigated the effects of different RM contents on the microstructure and mechanical properties of cementitious materials, and the results showed that iron in RM was the main factor controlling the evolution of structural features and mechanical properties and the addition of iron made the compressive strength of cementitious materials reach 21.5 MPa at 28 days; in addition, Hao et al. [20] used RM and steel slag (SS) as raw materials to prepare composite cementitious materials, and the results showed that the synergistic effect of SS and RM significantly improved the mechanical properties of the cementitious materials and further increased the compressive strength to 22.7 MPa. Although a small amount of RM can be incorporated to improve the mechanical properties of the cementitious materials, there are still the problems of a low utilization rate and high alkalinity. Therefore, Pan et al. [21] prepared alkali-excited cementitious materials by combining RM, slag (MP), and an exciter and found that the material had a compressive strength of more than 24 MPa at 28 d and exhibited lower porosity and greater structural stability than conventional silicate cements; at the same time, Hou et al. [22] prepared RM, high-strength cement, and an exciter by using RM-based cementitious material, which was found to have a compressive strength of 25.6 MPa at 28 d. From this, it can be seen that the incorporation of alkali exciters can stimulate the activity of RM and effectively improve the mechanical properties of cementitious materials, but it still faces the problems of higher cost and poorer durability. In order to solve these problems, Zhang et al. [23] used sintered RM as the main raw ingredient, blended with MP and a 5% water glass solution (modulus 2.4), to produce a material with compressive strengths exceeding 40 MPa at 3 days and 60 MPa at 28 days. Kang et al. [24] integrated RM into an alkaline–MP system, obtaining a compressive strength of 72.05 MPa for the RM-MP-based gelling material at 28 days. Although the incorporation of active materials into RM-based systems can significantly enhance mechanical performance and reduce energy consumption, variations in experimental conditions and reaction products often lead to inconsistencies in mechanical property outcomes [25]. Therefore, more comprehensive research is necessary to evaluate the potential of producing low-carbon gelling materials using RM in combination with other solid wastes.
In conclusion, while numerous studies have investigated the potential of using RM in combination with steel slag (SS), slag (MP), and iron tailings (IRs) for gelling material production, research on the effects of construction waste red brick powder (RB) in such materials remains limited. Therefore, this study focuses on using RM as the primary raw material, designing various low-carbon gelling systems in conjunction with multi-source solid wastes, including RB and MP, sourced from Lianyungang City, Jiangsu Province, China. The purpose of this study is to analyze the physical and chemical properties of red mud, reveal its basic gelling activity and the excitation mechanism of gelling activity, obtain the synergistic mode between red mud and other types of solid waste, determine the ratio design method in the preparation of composite gelling materials, and analyze the effects of different preparation parameters on the hydration products in response to the defects of red mud, which has complex and variable components, as well as low gelling activity. In addition, this study also explores the effects of different gelling compositions on the physical properties (including fluidity, drying shrinkage, and wet/dry cycling), mechanical properties, anti-freeze–thaw properties, and heavy metal leaching properties of composite gelling materials, as well as the mechanism of the formation of the strength of alkali-inspired materials for the curing of multi-source solid wastes. It further analyzes the microscopic morphology and mineral compositions of different systems of low-carbon gelling materials through XRF, SEM, EDS, XRD, and FTIR techniques. This work aims to offer innovative strategies for the synergistic use of RM, MP, and RB in the development of composite gelling materials.

2. Materials and Methods

2.1. Raw Materials

The primary raw materials utilized in this research include RM, RB, and MP. The RM was sourced from a production facility in Liaocheng City, Shandong Province, China, while the RB originated from a construction waste site in Lianyungang. The MP was obtained from Lianyungang Hanjiang Mining Technology Co. Laboratory tap water was utilized for all experiments, and the chemical reagents, including sodium silicate (Na2SiO3·9H2O) and sodium hydroxide (NaOH), were of analytical grade (AR) and procured from Sinopharm Shanghai Co. (Shanghai, China).
The chemical compositions of the raw materials were determined using X-ray fluorescence spectrometry (XRF) (Horiba Scientific, Tokyo, Japan). Table 1 reveals that RM contains 10.95% Na2O, indicating high alkalinity, and 38.96% Fe2O3, which suggests slight magnetic properties. Meanwhile, the MP has a CaO content of 35.17%, highlighting its potential reactivity. In contrast, the RB exhibited a high SiO2 content of 52.37%, indicating its potential as a gelling agent. The loss on ignition (LOI) parameters indicated an ignition loss of 9.42% for RM, while RB showed a significantly lower ignition loss of 0.58%. This is consistent with the results of the Kaplan–Meier survival analysis and correlation analysis.
A more detailed analysis of the raw materials was performed using X-ray diffraction (XRD) (Rigaku Corporation, Tokyo, Japan), scanning electron microscopy (SEM, JSM-7200), and a laser particle size analyzer (Japan Electron Optics Laboratory Co., Ltd, Tokyo, Japan), with the results displayed in Figure 1. It is found that the primary mineral components of RM are hematite and quartz. The particle size distribution of RM ranges from 0.5 to 500 µm, with a peak at 0.77 µm, accounting for 2.86% of all particles. The microstructure of RM appears relatively loose, primarily consisting of irregularly shaped particle agglomerates. These RM agglomerates have a rich pore structure with a porosity of up to 42% and exhibit a high water absorption of 69% and a strong water holding capacity of 47% [26]. These properties are one of the key reasons for RM’s excellent water absorption and water holding properties.
The primary composition of RB is quartz-based crystalline compounds, as shown in Figure 1. It also contains minor amounts of minerals such as microplagioclase feldspar and hematite. The particle size of RB ranges from 0.1 to 900 µm, with a peak size of 93.5 µm, accounting for 1.78% of the total particles. The particles generally have an angular shape. On the other hand, MP mainly consists of quartz and exhibits an irregular block-like microstructure. Its particle size distribution falls between 0.2 and 350 µm, with a peak at 15.7 µm, making up 3.25% of the total particles.

2.2. Preparation Method of Gelling Materials

The preparation method of the cementitious materials in this study refers to the Guide for Design and Construction of Concrete Structures for Durability (CCES 01-2004) [27], and the production process of binary and ternary cementitious materials is shown in Figure 2. According to previous studies, the optimal dosing of RM is 4–20%, and the optimal dosing of RB is 5–25%. Initially, 20 g of sodium hydroxide was dissolved in 94.42 g of water with continuous stirring until fully dissolved and then set aside for 2 h to form a sodium hydroxide solution. Next, the amount of RM, RB, and MP raw materials was calculated according to predetermined ratios (detailed in Table 2) and placed into a mortar mixer for thorough blending, which lasted for 60 s. After the initial mixing, the sodium hydroxide solution was added to the mixer, followed by an additional 120 s of mixing. Subsequently, a water glass solution was added to the mixture, followed by stirring for an additional 120 s. The mixture was then poured into pre-greased molds and placed on a vibrating table for 60 s to eliminate air bubbles [28]. Following the vibration process, the specimens were left in a cool place for 12 h before demolding. Finally, the demolded specimens were stored in a curing room at a temperature of 20 ± 2 °C with a relative humidity of over 95%, where they underwent curing for 1, 3, and 28 days, respectively.

2.3. Test Methods

2.3.1. Fluidity

A truncated cone circular mold with dimensions of Φ36 × Φ60 × 60 mm was utilized to assess the fluidity of the gelling material. The process began by pouring the thoroughly mixed cementitious material into the mold, followed by leveling it off with a spatula. Within 2 s, the mold was lifted vertically upward by 5–10 cm and held in place for 10–15 s, allowing the material to flow freely. Afterward, a caliper was used to measure the maximum diameters in two perpendicular directions, and the mean values were recorded. The fluidity test was performed twice on the same product and the results of the two experiments were averaged and the flow rate was measured repeatedly by means of a Pressure Capillary Viscometer, ensuring that the data were accurate to 0.1 mm.

2.3.2. Compressive Strength

In this study, a SANS-type universal testing machine with a displacement accuracy of ±0.01 mm and a force measurement accuracy of ±0.5% was used, and the size of the test blocks used was 40 mm × 40 mm × 160 mm. The experiments were carried out in accordance with the ASTM C109 standard [29].

2.3.3. Drying Shrinkage and Mass Loss

The drying shrinkage test methods used in the research follow the standard requirements outlined in JGJ/T 70-2009 [30]. Initially, the specimens were placed in a standard curing room for 24 h. After curing, the initial length and mass of each sample were recorded. The specimens were then stored in a room with a constant temperature and humidity for drying. Finally, at T age (1d, 3d, 7d, 14d, 28d), the length of the specimens was measured by a vernier caliper to an accuracy of 0.1 mm. The drying shrinkage rate and mass loss rate at age T were obtained using Equations (2) and (3), respectively.
St = (L0 − Lt)/L × 100%,
M1 = (M0 − Mt)/M0 × 100%,
where St represents the drying shrinkage percentage (%), L0 is the specimen’s initial length (mm), Lt is the length of the specimen at age T (mm), and L denotes the specimen’s effective length, which is taken as 160 mm. Ml indicates the mass loss rate (%), M0 is the initial mass (g), and Mt is the mass of the specimen at age T (g).

2.3.4. Dry–Wet Cycle

The dry–wet cycle test methods in this study followed the standard requirements outlined in “GB/T 50082-2009” [31]. Initially, the specimen was placed in a constant-temperature (temperature rise rate of 1 °C/min, exposure time of 10 min) water tank for immersion. Once the immersion is complete, it was moved to an electric blast drying oven for drying. After drying, the specimen was then placed in a dry indoor area to dry naturally. After each cycle of drying and wetting, the specimen was allowed to dry naturally, then checked for any changes in appearance and weighed to calculate its mass loss rate using the following expression:
ΔMni = (M0i − Mni)/M0i × 100%,
where M0i and Mni are the mass (g) before and after the dry and wet cycle experiments, respectively, and ΔMni is the corresponding mass loss rate (%).

2.3.5. Microstructure Test

In this study, the microstructures of solid waste raw materials and composite cementitious materials were examined using a scanning electron microscope (SEM, JSM-7200) with a scanning speed ranging from 1 μs/pixel to 1000 μs/pixel; meanwhile, the chemical compositions of the composite cementitious materials were investigated by using energy spectrometry (EDS) with a spectral resolution of typically 130–200 eV and an energy spectrum ranging from 0 eV to 20 keV. XRD analysis was conducted with the Rigaku Ultima IV polycrystalline powder diffractometer (Cu target). The main operating parameters included a voltage of 40 kV, a current of 40 mA, and an incident wavelength λ = 0.154 nm to identify the physical phases of the composite cementitious materials. The Fourier transform infrared (FTIR) spectroscopy test was carried out using the Thermo Scientific Nicolet iS50 FTIR spectrometer with a resolution of 2 cm−1 and a wavenumber range of 400–4000 cm−1.

2.3.6. Freeze–Thaw Cycling Test

The freeze–thaw cycle tests in this study followed the guidelines set by the standard “GB/T 50082-2009”. Initially, the specimens were submerged in water for 2 h to achieve full saturation. Following this, they were placed into a rapid freeze–thaw testing machine to initiate the freeze–thaw cycle process. After each cycle, the samples were removed, surface water was drained, and the specimens were weighed to calculate the mass loss rate.
ΔWni = (W0i − Wni)/W0i × 100%,
where W0i and Wni are the mass (g) before and after the freeze–thaw cycle test, respectively, and ∆Wni is the corresponding mass loss rate (%).

2.3.7. Heavy Metal Leaching Characterization Test

In this experiment, inductively coupled plasma atomic emission spectrometry (ICP-OES) was employed to analyze the leaching characteristics of heavy metals in the composite cementitious materials. The procedure adhered to the requirements of the standard “HJ557-2010” [32]. After a curing period of 28 days, 100 g of dried and crushed RM-LWA samples (particle size < 3 mm) were placed into a glass bottle. Deionized water was added at a liquid-to-solid ratio of 10:1 (L/kg). The bottle was then securely placed on a reciprocating shaker (HDY-40) and agitated for 8 h at a frequency of 110 shakes per minute with an amplitude of 40 mm. Following this, the bottle was allowed to stand for 16 h. The resulting leachate was then extracted for heavy metal leaching analysis.

3. Results and Discussion

3.1. Fluidity

Figure 3 presents the fluidity results for both binary and ternary cementitious materials. As shown in Figure 3a, an increase in RM content results in a decline in the flowability of the binary binder. The cementitious material achieves its maximum flow of 172 mm when RM content is 0%. However, with a 20% RM content, the flowability decreases to 120 mm, indicating a total reduction of 30.23%. This reduction originates from the rough absorbent surface of RM. Additionally, the presence of CaO and amorphous phases in RM can impede the polymerization reaction [33], further diminishing flowability. Notably, when RM content is between 4% and 8%, the flow rate of the binary cementitious materials decreases by only 1.2%, likely due to the moderate calcium ions in RM slowing the curing rate of the gelling material [34]. Hence, RM content has a negative correlation with flowability, while MP content has a positive correlation, in line with findings reported by Li et al. [35].
Figure 3b indicates that the mobility of the ternary gelling material decreases as the RB content increases. At 4% RB, the flow reaches a maximum of 177 mm, but when RB content rises to 25%, the flowability drops to 129 mm, representing a total decrease of 27.11%. This decrease is due to the thin water film on the surface of RB particles, their rough texture, and the chemical reaction between RB and NaOH, which leads the three-dimensional cementitious material to absorb more water, further reducing mobility. However, compared to the binary system, the overall flow of the ternary system increases by 4.5%. This improvement can be explained by two main factors. First, the reduced RM content lessens the hindrance of calcium ions on the polymerization process [36]; second, the potential activity of RB is stimulated [37]. Thus, a suitable amount of RB can enhance the fluidity of the gelling material.

3.2. Compressive Strength

Figure 4 illustrates the mechanical properties of binary and ternary gelling materials at various curing ages. As depicted in Figure 4a, the highest compressive strengths at 1, 3, and 28 days were achieved with MP alone, measuring 30.53 MPa, 36.67 MPa, and 42.24 MPa, respectively. However, when RM was used at a 20% dosage, the compressive strengths dropped to 22.31 MPa, 27.17 MPa, and 33.72 MPa, reflecting overall reductions of 26.92%, 25.91%, and 20.17%. This indicates that incorporating RM reduced the compressive strength of the gelling material. It should be indicated that this observation aligns with the findings reported by Li et al. [38]. When RM content ranged from 4% to 8%, the changes in compressive strength were negligible. However, at RM dosages exceeding 16%, a significant decrease in compressive strength was observed, primarily due to excessive iron ions inhibiting silicate dissolution [39]. Additionally, a reduction in binder dosage also negatively affected compressive strength [40]. Despite this, the compressive strength at 3 and 28 days increased by 16.49% and 28.94% compared to 1 day, suggesting that RM’s high alkalinity contributes positively to gel formation over time.
For RB doping, Figure 4b reveals that the compressive strength increases first and then decreases. At 16% RB, compressive strengths were 32.37 MPa, 38.92 MPa, and 55.63 MPa at 1, 3, and 28 days, respectively, representing increases of 5.71%, 5.78%, and 24.07% compared to 4% RB. This suggests that RB’s potential activity was activated, improving the material’s compactness by filling system voids [41]. However, when RB content exceeded 16%, compressive strengths at 1, 3, and 28 days decreased by 1.72%, 3.02%, and 25.26%, respectively. This reduction may be due to RB’s large surface area and high water absorption capacity, which can interfere with the gelling material’s hydration reaction if present in excessive amounts. Despite this, compared to the 1-day compressive strength, strengths at 3 and 28 days increased by 16.28% and 33.83%, respectively. The overall compressive strength of the ternary cementitious material was improved by 13.54% and 18.27% compared to the overall compressive strength derived from the experiments of the binary cementitious material and that in [42]. Thus, moderate RB doping enhances the compressive strength of the gelling material.

3.3. Drying Shrinkage and Mass Loss

Figure 5 illustrates the drying shrinkage and mass loss rates of binary and ternary gelling materials. As shown in Figure 5a, incorporating RM into the gelling material resulted in reduced drying shrinkage. The specimens with 20% RM exhibited drying shrinkages that were 11.65%, 23.94%, 24.95%, 23.52%, and 16.09% lower at 1, 3, 7, 14, and 28 days, respectively, compared to the pure MP specimens. This reduction aligns with the findings reported by Ma et al. [43]. Additionally, Figure 5b indicates that the mass loss rate of the binary gelling material generally follows the same trend as the drying shrinkage, with an increasing mass loss rate as RM content rises. The presence of RM not only refines the pore structure and enhances micro-agglomeration effects but also reduces internal deformation by filling matrix voids with new hydration products generated from the active ingredients in RM. However, this process is accompanied by an increase in mass loss.
In contrast, the drying shrinkage of the ternary gelling material increases with higher RB content, as depicted in Figure 5c. For specimens with 24% RB, the drying shrinkage at 1, 3, 7, 14, and 28 days was 15.82%, 13.01%, 12.62%, 13.99%, and 9.96% higher than that of specimens with 4% RB, respectively. This increase may originate from the higher silica content in RB, which exacerbates drying shrinkage. Figure 5d shows that the mass loss of ternary cementitious materials mainly occurs in the first 14 days of drying shrinkage. Compared with the mass loss rate shown in [44] on day 7, the total loss rate decreased by 7.19%. Unlike drying shrinkage, the mass loss rate decreases as RB content increases. This observation suggests that drying shrinkage is influenced not only by the chemical composition of the raw materials but also by the microstructure of the samples.

3.4. Dry–Wet Cycle

Figure 6 demonstrates the mass loss and rate of loss for binary and ternary gelling materials during wet and dry cycling. It is observed that the mass of both binary and ternary gelling materials decreases progressively with an increasing number of wet and dry cycles. Initially, the mass loss across all specimens during the first 16 cycles was quite similar, with differences in adjacent loss rates being 0.31% and 0.65%, respectively. By the 28th cycle, the mass loss rates for CPM1, CPM2, and CPMB4 were 17.74%, 19.99%, and 8.92%, respectively, with differences in neighboring loss rates being 2.25% and 11.07%. The increased mass loss rate observed in the binary gelling materials incorporating RM may be attributed to the reduction in structural strength caused by RM. This reduction leads to the formation of more internal cracks under the stress of wet and dry cycling, which in turn causes the surface layer to chalk and results in greater mass loss [45]. However, the rate of mass loss of ternary cementitious materials incorporated with RB was reduced by 13.24% compared to the findings in [46]. This improvement is due to RB’s effective physical filling during dry and wet shrinkage and its role in reducing porosity through the generation of hydration products.

3.5. Mechanistic Analysis

3.5.1. Microstructure Test

The morphology of the binary and ternary gelling materials was analyzed using SEM coupled with energy-dispersive spectroscopy (SEM-EDS). Figure 7 illustrates that gelling materials prepared with MP alone exhibit a smoother surface and a denser internal structure with fewer pores, but some cracks also appeared under the influence of the alkaline environment [33]. In contrast, increasing the RM content results in a rise in flocculated loose hydrates, which enlarges the interstices between particles and increases the number of pores and the number of cracks, as shown in Figure 7b. This is accompanied by a rise in reactive Al-Si substances in RM, which heightens the alkalinity of the binary gelling material and promotes the formation of C-S-H gels. During this process, the number of cracks decreased but their depth increased [47]. This increase in pore size and the formation of C-S-H gels can help explain the observed decrease in compressive strength when RM is incorporated.
Compared with the binary gelling materials, the OH− ions inside the ternary gelling materials can stimulate the activity of the Al-Si substances, which are more likely to participate in the hydration reaction and accelerate the hydration process, resulting in the generation of more amorphous aluminosilicate gel phases (ASGs), as shown in Figure 7d. These gel phases fill the large pores between the particles, which leads to decreased porosity and shallower cracks with a more compact structure. In addition, with the increase in RB doping, the alkaline environment provided by the excess OH- ions in CPMB4 contributes to the generation of C-S-H gels, which further fill the small pores between the particles and make the cracks almost disappear. These gels can encapsulate the free heavy metal ions and sticky particles to form a dense crystalline mesh structure and a stronger skeleton, which plays a sealing role for the heavy metal ions, reduces the leaching of heavy metals, and forms a stable spatial structure, thus improving the strength of the cementitious materials. At the same time, the Ca2+ content also increases, which promotes the formation of calcium alumina [48]. This is consistent with the subsequent XRD and FTIR results.

3.5.2. XRD

Figure 8 presents the XRD patterns of the binary and ternary gelling materials, revealing three typical mineral phases, namely calcite (CaCO3), quartz (SiO2), and hematite (Fe2O3). A comparison of Figure 8a,b shows that the diffraction peak intensities of the binary gelling materials are significantly lower than those of the raw materials. This indicates that incorporating RM gradually increases the alkalinity of the binary cementitious material, promoting the rapid formation of initial gel products that coat the surface of the raw material particles. This coating effect hinders further dissolution, consequently reducing the hydration process in the binary cementitious material. In contrast, the diffraction peaks of the ternary gelling materials increase with the incorporation of RB, suggesting an enhancement in the quantity of gel phases formed during the polymerization reaction, as illustrated in Figure 8e. The synergistic use of RM, MP, and RB in the ternary gelling materials activates the Si-Al substances through the presence of OH- ions, forming aluminosilicate compounds such as ettringite and amorphous gels. Notably, all gelling materials display similar amorphous humps within the 27–32° range. Compared to the raw materials, the humps in the ternary gelling materials are broader, and the hump center shifts to the right. These observations align with previous research findings [49,50], confirming the formation of amorphous gels. Additionally, the ternary gelling materials exhibit a more extensive range of humps and a further rightward shift in the hump center compared to the binary materials. This suggests that a higher RB content in the gelling material promotes the generation of amorphous gels, thereby enhancing the material’s strength.

3.5.3. FTIR

Figure 8 displays the FTIR spectra of the binary and ternary gelling materials. The spectra show significant absorption peaks at 3442 cm−1 and 2056 cm−1, corresponding to the stretching and bending absorption of -OH groups, respectively [51]. The peak at 1638 cm−1 is associated with the asymmetric stretching vibration of the Si-O-Si bond. The absorption peak at 1405 cm−1 is attributed to the stretching vibration of the C-O bond, while the peak at 1089 cm−1 corresponds to the asymmetric stretching vibration of the Si-OH bond, indicating the presence of C-(A)-S-H gel [52]. Additionally, the absorption peak at 879 cm−1 is linked to the asymmetric bending vibration of the Al-O-H bond, and the peak at 564 cm−1 is associated with the asymmetric stretching vibration of the Al-O bond. These findings confirm the uniform distribution of silicon and aluminum oxides within the gelling material. In the binary system, the intensities of the absorption peaks at 879 cm−1 and 1089 cm−1 increase with a higher RM substitution rate, suggesting that RM facilitates the generation of C-S-H gels. In the ternary system, significant absorption peaks appear at 1638 cm−1 and 1405 cm−1 following the incorporation of RB, indicating that RB dissolution under highly alkaline conditions leads to the formation of amorphous aluminosilicate gels [53]. As the RB substitution rate increases, the intensities of the absorption peaks at 2056 cm−1, 879 cm−1, and 564 cm−1 decrease. This suggests that Al and Si from RB are more actively involved in the hydration reaction, resulting in a greater production of C-S-H gels. These observations are consistent with the XRD analysis results.

3.6. Freeze–Thaw Resistance

Figure 9 presents the mass loss of binary and ternary gelling materials during freeze–thaw cycles under standard curing conditions. It is observed that the mass loss of the gelling material prepared with MP alone decreased by 3.04% after 50 freeze–thaw cycles. However, with the addition of RM, the mass loss of the binary gelling material increased by 7.03%, 24.38%, 28.81%, 33.77%, and 39.56%, respectively. When subjected to 100 freeze–thaw cycles, the mass losses of CPM2, CPM3, CPM4, CPM5, and CPM6 were 5.25%, 6.21%, 6.47%, 6.79%, and 7.38%, respectively, showing an overall increase of 84.39% compared to CPM1. This increased mass loss may be attributed to the reduced frost resistance caused by the incorporation of RM, which led to the formation of macroscopic pores and microcracks on the surface of the binary gelling material.
The mass loss observed in ternary gelling materials was lower than that of binary materials under the same number of freeze–thaw cycles, suggesting that adding RB significantly enhances the freeze–thaw resistance of ternary gelling materials. CPMB5 and CPMB6 increased the mass loss of the ternary cementitious materials compared to previous findings, which suggests that excess RB reduces the freeze–thaw cycle resistance of ternary cementitious materials. For instance, after 100 freeze–thaw cycles, the mass loss of CPMB4 was limited to just 4.13%. This improvement may be attributed to the RB particles filling the micropores and microcracks in the gelling material, thereby reducing the amount of free water present in these spaces. Additionally, the macropores formed by RB contribute to a reduction in material density and water saturation, mitigating the effects of freezing and the resulting expansion forces, which ultimately boosts frost resistance.
However, introducing excessive amounts of RB, as seen in CPMB5 and CPMB6, actually increased the mass loss in the ternary material. This suggests that too much RB reduces the freeze–thaw resistance. This decline in performance may originate from the aggregation of excess RB particles, leading to the creation of weak and defective areas within the material’s structure. When exposed to ice expansion pressure, the matrix at these weak surfaces tends to separate, causing a significant loss of mass. Therefore, the inclusion of a balanced amount of RB is key to enhancing the frost resistance of gelling materials.

3.7. Heavy Metal Leaching

To evaluate the potential environmental impacts of binary and ternary cementitious materials, heavy metal leaching toxicity tests were conducted using ICP-OES on specimens exposed to both freeze–thaw cycling conditions and non-freeze–thaw conditions. The results are presented in Figure 10. Based on the standard “GB 5085.3-2007” [54], the leaching concentrations of heavy metals, including Cr (<15 mg/L), Zn (<5 mg/L), Pb (<5 mg/L), Ni (<5 mg/L), and Cu (<100 mg/L), in both binary and ternary cementitious materials under freeze–thaw and non-freeze–thaw conditions are lower than the specified limit values for releasing non-hazardous substances into the environment.
Figure 10a shows that under freeze–thaw cycling conditions, Cr exhibited the highest leaching concentration among the heavy metals in both binary and ternary cementitious materials, with values of 1.25 mg/L, 3.19 mg/L, 3.07 mg/L, and 2.15 mg/L, respectively. The lowest leaching content was observed for Cu. Conversely, as depicted in Figure 10b, under non-freeze–thaw conditions, Cr still had the highest leaching content; however, its leaching rate was relatively slower. Different from the freeze–thaw scenario, the lowest heavy metal leaching content under non-freeze–thaw conditions was Ni, with concentrations of 2.3 μg/L, 2.7 μg/L, 2.4 μg/L, 2.1 μg/L, and 2.7 μg/L, which were 14.81%, 6.89%, 11.11%, 22.17%, and 3.57% lower than the leaching concentrations detected in [55]. This could be related to the inherent heavy metal concentrations of the materials themselves. Additionally, the leaching concentrations of heavy metals (Zn, Cu, and Ni) from both binary and ternary cementitious materials were higher under freeze–thaw cycling conditions (0.015–1.07 mg/L) compared to non-freeze–thaw conditions (2.1–7.5 μg/L), indicating that the surrounding environment significantly influences the leaching characteristics of heavy metals.

4. Conclusions

In this study, 12 groups of low-carbon cementitious materials were formulated using RM combined with different solid wastes, including MP and RB. The microstructure and mineral compositions of the raw materials and the various cementitious systems were characterized using SEM, EDS, XRD, and FTIR analyses. The research investigated the physical and mechanical properties, freeze–thaw resistance, and heavy metal leaching behavior of the different cementitious material systems. The findings contribute valuable scientific and theoretical guidance for the synergistic utilization of alkaline, calcium, and silica–aluminum solid wastes, aligning with “low-carbon, green” sustainable development goals. The main achievements of the present study are as follows:
(1)
Under standard curing conditions, the ternary cementitious material with 16% RB performed the best, with a 4.5% improvement in fluidity, 18.27% increase in compressive strength, 39.56% increase in drying shrinkage, 45.91% reduction in mass loss, and 11.07% reduction in wet and dry cycle mass loss.
(2)
The incorporation of RB stimulates Al-Si activity, generates amorphous alumino-silicate gel phases and C-S-H gels, and also promotes the formation of chalcocite. XRD results show that the incorporation of RB reduces porosity and forms a dense structure, which enhances the mechanical properties of the cementitious materials.
(3)
Under standard curing conditions, the ternary cementitious material with 16% RB showed the best freeze–thaw resistance, with a mass loss of only 4.13% after 100 freeze–thaw cycles.
(4)
The results of the heavy metal leaching characterization test showed that the leaching concentrations of Cr, As, Pb, Ni, and Cu in the specimens were below the specified limits for the release of non-hazardous substances to the environment under freeze–thaw cycles and non-freeze–thaw conditions.
Although the composite cementitious materials prepared in this study are characterized by environmental protection and high efficiency, there are deficiencies in the upper limit of RB dosage and long-term durability. Future research can focus on optimizing the ratio, enhancing the long-term performance, and broadening the application areas to increase the RB dosage and further explore a wider range of application areas.

Author Contributions

Conceptualization, T.Q., H.L., L.C., M.L. and B.-J.H.; methodology, R.H., Y.Z., L.C., M.L., Z.G., J.X. and D.C.; software, Z.G., J.X., D.C. and B.-J.H.; validation, Y.Z., L.C., M.L. and B.-J.H.; formal analysis, T.Q., R.H., Y.Z., L.C. and M.L.; investigation, J.X., Z.G. and L.C.; resources, H.L., Z.G., J.X. and D.C.; data curation, R.H., Y.Z., L.C., Z.G. and D.C.; writing—original draft preparation, T.Q.; writing—review and editing, R.H., H.L. and Y.Z.; visualization, B.-J.H. and M.L.; supervision, H.L. and B.-J.H.; project administration, H.L. and B.-J.H.; funding acquisition, H.L. All authors have read and agreed to the published version of the manuscript.

Funding

This research was funded by the National Natural Science Foundation of China (52108322), the Xinjiang Biomass Solid Waste Resources Technology and Engineering Center of China (KSUGCZX2022), the Lianyungang Key Research and Development Plan (Social Development) project of China (SF2130), the Lianyungang Key Research and Development Plan (Industrial Outlook and Key Technology Core) project of China (CG2207), the Postgraduate Research & Practice Innovation Program of Jiangsu Province, grant numbers (SJCX23_1814, SJCX23_1816, and KYCX2023-24), the Natural Science Foundation of the Jiangsu Higher Education Institutions of China (22KJB560001), and the China Meteorological Administration “Research on value realization of climate ecological products” Youth Innovation Team Project (No. CMA2024QN15), and Chongqing Natural Science Foundation Project (No. CSTB2024NSCQ-MSX0670).

Data Availability Statement

The datasets used and/or analyzed during the current study are available from the corresponding author upon reasonable request.

Conflicts of Interest

The authors declare no conflicts of interest.

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Figure 1. XRD, particle size distribution, and SEM images of raw materials: (a,d,g) RM, (b,e,h) RB, (c,f,i) MP.
Figure 1. XRD, particle size distribution, and SEM images of raw materials: (a,d,g) RM, (b,e,h) RB, (c,f,i) MP.
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Figure 2. A flowchart of the preparation of low-carbon gelling materials.
Figure 2. A flowchart of the preparation of low-carbon gelling materials.
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Figure 3. Flowability of low-carbon gelling material: (a) binary system; (b) ternary system.
Figure 3. Flowability of low-carbon gelling material: (a) binary system; (b) ternary system.
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Figure 4. Mechanical properties of low-carbon gelling material: (a) binary system; (b) ternary system.
Figure 4. Mechanical properties of low-carbon gelling material: (a) binary system; (b) ternary system.
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Figure 5. Drying shrinkage and mass loss of low-carbon gelling material. (a) Drying shrinkage of binary gelling material; (b) mass loss rate of binary gelling material; (c) drying shrinkage of ternary gelling material; (d) mass loss rate of ternary gelling material.
Figure 5. Drying shrinkage and mass loss of low-carbon gelling material. (a) Drying shrinkage of binary gelling material; (b) mass loss rate of binary gelling material; (c) drying shrinkage of ternary gelling material; (d) mass loss rate of ternary gelling material.
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Figure 6. The mass loss and rate of loss for binary and ternary gelling materials during wet and dry cycling.
Figure 6. The mass loss and rate of loss for binary and ternary gelling materials during wet and dry cycling.
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Figure 7. Microanalysis of low-carbon cementitious materials: (a–e) SEM images of binary and ternary cementitious materials at different magnifications; (f–j) EDS images of binary and ternary cementitious materials showing the distribution of different elements.
Figure 7. Microanalysis of low-carbon cementitious materials: (a–e) SEM images of binary and ternary cementitious materials at different magnifications; (f–j) EDS images of binary and ternary cementitious materials showing the distribution of different elements.
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Figure 8. Microscopic analysis of low-carbon gelling material: (a–e) XRD patterns and FTIR spectra.
Figure 8. Microscopic analysis of low-carbon gelling material: (a–e) XRD patterns and FTIR spectra.
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Figure 9. Frost resistance of low-carbon gelling material: (a) binary system; (b) ternary system.
Figure 9. Frost resistance of low-carbon gelling material: (a) binary system; (b) ternary system.
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Figure 10. Heavy metal leaching characteristics of low-carbon cementitious materials: (a) freeze–thaw; (b) non-freeze–thaw.
Figure 10. Heavy metal leaching characteristics of low-carbon cementitious materials: (a) freeze–thaw; (b) non-freeze–thaw.
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Table 1. Chemical compositions of RM, RB, and MP.
Table 1. Chemical compositions of RM, RB, and MP.
Composition (wt%)CaOSiO2Al2O3Fe2O3SO3MgOTiO2Na2OLOI
RM1.1718.2323.9738.960.720.174.7110.959.42
RB10.1152.3724.432.142.432.180.792.040.58
MP25.1740.6716.520.282.748.751.090.77-
Table 2. The proportion design of the low-carbon-gelling material.
Table 2. The proportion design of the low-carbon-gelling material.
SampleNameMP (%)RMMP (%)Alkaline Activator Module (%)Water-to-Cement Ratio
Dualist systemCPM1100--1.30.35
CPM2964-
CPM3928-
CPM48812-
CPM58416-
CPM68020-
Three-component systemCPMB18415.360.641.30.35
CPMB28414.721.28
CPMB38414.081.92
CPMB48413.442.56
CPMB58412.803.20
CPMB68412.163.84
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Qin, T.; Luo, H.; Han, R.; Zhao, Y.; Chen, L.; Liu, M.; Gui, Z.; Xing, J.; Chen, D.; He, B.-J. Red Mud in Combination with Construction Waste Red Bricks for the Preparation of Low-Carbon Binder Materials: Design and Material Characterization. Buildings 2024, 14, 3982. https://doi.org/10.3390/buildings14123982

AMA Style

Qin T, Luo H, Han R, Zhao Y, Chen L, Liu M, Gui Z, Xing J, Chen D, He B-J. Red Mud in Combination with Construction Waste Red Bricks for the Preparation of Low-Carbon Binder Materials: Design and Material Characterization. Buildings. 2024; 14(12):3982. https://doi.org/10.3390/buildings14123982

Chicago/Turabian Style

Qin, Teng, Hui Luo, Rubin Han, Yunrui Zhao, Limin Chen, Meng Liu, Zhihang Gui, Jiayao Xing, Dongshun Chen, and Bao-Jie He. 2024. "Red Mud in Combination with Construction Waste Red Bricks for the Preparation of Low-Carbon Binder Materials: Design and Material Characterization" Buildings 14, no. 12: 3982. https://doi.org/10.3390/buildings14123982

APA Style

Qin, T., Luo, H., Han, R., Zhao, Y., Chen, L., Liu, M., Gui, Z., Xing, J., Chen, D., & He, B.-J. (2024). Red Mud in Combination with Construction Waste Red Bricks for the Preparation of Low-Carbon Binder Materials: Design and Material Characterization. Buildings, 14(12), 3982. https://doi.org/10.3390/buildings14123982

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