applied sciences Article Impact of Rice Husk Ash on the Mechanical Characteristics and Freeze–Thaw Resistance of Recycled Aggregate Concrete Wei Zhang, Huawei Liu and Chao Liu * College of Civil Engineering, Xi’an University of Architecture and Technology, Xi’an 710055, China * Correspondence: chaoliu@xauat.edu.cn Citation: Zhang, W.; Liu, H.; Liu, C. Impact of Rice Husk Ash on the Mechanical Characteristics and Abstract: With the accelerating growth of infrastructure construction, carbon emission and environmental pollution problems have become increasingly severe. In order to promote the sustainable development of the construction industry, using rice husk ash (RHA) in recycled aggregate concrete has aroused extensive interest. This study aims to investigate the impact of the partial replacement (0%, 10%, 20%, 30% of binder) of ordinary Portland cement (OPC) with RHA by equal mass on recycled concrete’s mechanical characteristics and freeze–thaw resistance. The workability, compressive strength, mass loss and dynamic elastic modulus of recycled concrete were tested, and the hydration products and microstructure were analyzed using scanning electron microscope (SEM) tests. The mechanism of the freeze–thaw damage deterioration of RHA recycled aggregate concrete was revealed. The results indicate that the incorporation of RHA has an adverse effect on the workability of fresh concrete. Its high specific surface area will provide a large number of nucleation sites for the hydration reaction, refining the pore structure in the paste and improving the weak bonding of the interfacial transition zone (ITZ) by enhancing the matrix’s pozzolanic reaction effect and filling effect, thus improving the compressive strength of concrete. Furthermore, the porous structure of the recycled aggregate attached mortar and mesoporous RHA will absorb a lot of water during the freeze–thaw cycles. With the continuous accumulation of expansion pressure, the interior pores and cracks will gradually expand and extend, leading to more severe damage to the concrete, and the degree of freeze–thaw damage deterioration grows as the RHA replacement ratios increase. Freeze–Thaw Resistance of Recycled Aggregate Concrete. Appl. Sci. 2022, 12, 12238. https://doi.org/10.3390/ Keywords: rice husk ash; recycled aggregate concrete; mechanical characteristics; freeze–thaw resistance; deterioration mechanism app122312238 Academic Editor: Laurent Daudeville Received: 9 November 2022 Accepted: 27 November 2022 Published: 29 November 2022 Publisher’s Note: MDPI stays neutral with regard to jurisdictional claims in published maps and institutional affiliations. Copyright: © 2022 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https:// creativecommons.org/licenses/by/ 4.0/). 1. Introduction With the continuous development of the construction industry, cement production has grown dramatically, resulting in increasingly aggravated carbon emissions and environmental pollution [1]. The main sources of carbon emissions in cement production are the chemical reaction of clinker components and the combustion of fossil fuels [2]. Based on the above two points, it is estimated that the total emissions from the cement industry are about 8% of global carbon emissions [3]. The partial replacement of cement with low-energy industrial and agricultural solid waste can reverse the rising carbon emissions trend, thus achieving energy efficiency and environmental protection [4–6]. Although using industrial solid wastes such as silica fume (SF), fly ash (FA) and ground granulated blast furnace slag (GGBFS) in concrete has the potential to reduce carbon dioxide emissions and contribute to the idea of sustainable development in the cement sector, their sources are limited by geographical conditions, technological conditions and economic costs [7,8]. Therefore, using agricultural solid wastes such as rice husk ash (RHA) in concrete has aroused extensive interest [9,10]. The rice husk is a broad source of agricultural waste collected during the grinding process from the surface layer of rice grains. In the field of green technology, rice husks are mainly used as fuel for processing rice grains, as boiler steam or as fuel for producing Appl. Sci. 2022, 12, 12238. https://doi.org/10.3390/app122312238 https://www.mdpi.com/journal/applsci Appl. Sci. 2022, 12, 12238 2 of 15 electricity in biomass power plants [11,12]. RHA is an agricultural residue generated by the incineration of rice husk [13]. Because of its high amorphous silica concentration, specific surface area and pozzolanic activity, it is regarded by many researchers as a cementitious material for increasing the properties of concrete [14–16]. Recycled concrete aggregate is an environmentally friendly material prepared from construction and demolition waste (CDW) by sorting, crushing, sieving and cleaning, which can be used in the construction sector to alleviate the gradually decreasing natural aggregate and solve the problem of the piling and disposal of construction solid waste, which is conducive to sustainable development [17,18]. Currently, the use of supplementary cementitious materials and recycled concrete aggregate for concrete preparation in the construction industry has attracted widespread attention. Therefore, many researchers have studied the mechanical characteristics and durability of concrete prepared synergistically from RHA and recycled aggregate. Qureshi et al. [19] studied the coupling effect of hook-ended steel fibers (HSF) and 15% RHA on the mechanical properties and durability of RAC. The results revealed that the joint action of RHA and fibers significantly enhanced the compressive strength, splitting tensile strength, impermeability and acid attack resistance (AAR) of RAC. Rattanachu et al. [20] evaluated recycled concrete’s mechanical properties, chloride penetration depth and steel corrosion using ground RHA. The findings revealed that using RHA had adversely affected the compressive strength of RAC, while greatly improving steel corrosion and chloride resistance. Alyousef et al. [5] studied the effect of waste mineral admixtures and glass fibers on the mechanical and permeability properties of recycled aggregate concrete. The results showed that the combined action of RHA and glass fibers resulted in recycled aggregate concrete exhibiting improved mechanical and durability properties compared to natural aggregate concrete. Nuaklong et al. [21] investigated the influence of RHA replacing silica nanoparticles on the mechanical and fire resistance properties of recycled concrete. The results showed that the addition of rice husk ash could lead to enhanced mechanical properties of recycled concrete by improving the microstructure of the paste, but RHA will adversely affect the post-fire residual strength of recycled concrete. Padhi et al. [22] investigated the engineering application effect of 0–35% RHA and recycled aggregate to prepare concrete. The findings revealed that incorporating RHA and recycled aggregate greatly enhanced the performance of concrete. When the replacement ratio of RHA and recycled coarse aggregate was 10–15% and 100%, respectively, the concrete mix ratio satisfied the engineering application requirements. Koushkbaghi et al. [23] investigated the impact of RHA and fibers on the mechanical properties and acid attack performance of recycled concrete. The results revealed that RHA could enhance the inferior properties of concrete by enhancing the bond between concrete and fibers, and the improvement effect increased with the rise in the RHA replacement ratio. Salahuddin et al. [24] studied the influence of temperature increases on RHA recycled concrete performance. The results showed that a 20% replacement ratio of RHA and a 100% substitution rate of recycled concrete aggregate resulted in a reduction of the compressive strength of concrete. Alnahhal et al. [25] investigated the influence of the partial replacement of cement by RHA on the engineering performance and environmental effects of recycled concrete. The results indicated that the partial replacement cement with RHA not only improved the performance of recycled concrete but also reduced carbon dioxide emissions during the cement production. Although previous studies have investigated the impact of RHA on various mechanical characteristics as well as the durability of recycled concrete, a mechanism analysis of the impact of RHA on the freeze–thaw resistance performance of recycled concrete has not been reported yet. Therefore, it is of great significance to carry out research on the frost resistance of RHA recycled concrete. In view of this, this research aims to investigate the impact of partially replacing Portland cement with RHA by equal mass on recycled concrete’s mechanical characteristics and freeze–thaw resistance. The workability, compressive strength, mass loss and dynamic elastic modulus of recycled concrete were determined. In addition, the paste’s hydration products and microscopic morphology were analyzed using Appl. Sci. 2022, 12, 12238 3 of 15 scanning electron microscope (SEM) tests. The deterioration mechanism of the freeze–thaw damage of RHA recycled concrete was revealed. The outcome of this research is expected to promote the application of RHA recycled concrete in severe cold regions. 2. Materials and Methods 2.1. Raw Materials Appl. Sci. 2022, 12, 12238 In this paper, the Shieldstone P.O 42.5 ordinary Portland cement (OPC) and untreated residual RHA were used as the cementitious materials, and the RHA was sourced from a biomass power factory in Nanjing. The microstructure of RHA is shown in Figure 1, which shows a honeycomb structure. The physicochemical characteristics of the cementitious materials are shown in Table 1, and it can be seen that the specific surface area of RHA is approximately 5–6 times that of cement, and its internal silica content is as high as 92.1%. 4 of 16 The particle size distributions of the cement and RHA are shown in Figure 2, which are 14.77 µm and 14.81 µm, respectively. Figure 1.1.Microstructure of RHA measured by scanning electron electron microscopy. Figure Microstructure of RHA measured by scanning microscopy. Table 1. The physicochemical characteristics of the cementitious materials used. Cementitious Materials Characteristics Cement RHA Physical properties Mean particle size (µm) 14.77 14.81 1.72 8.60 Specific surface area (m2 /g) Setting time (min) Initial time 202 Final time 258 Chemical composition (%) Silicon dioxide (SiO2 ) 21.07 92.08 Ferric oxide (Fe2 O3 ) 3.78 0.05 Aluminium oxide (Al2 O3 ) 4.91 0.11 Potassium oxide (K2 O) 0.59 3.50 Magnesium oxide (MgO) 1.43 0.49 Calcium oxide (CaO) 65.36 0.78 Sodium oxide (Na2 O) 0.39 Phosphorous oxide (P2 O5 ) 1.35 FigureSulfur 2. The particle size distributions of cement, RHA, river sand and RCA. trioxide (SO 2.45 0.92 3) Loss on ignition 4.52 1.83 The fine aggregate was river sand from the Shaanxi region, with a water absorption of 3%, a maximum particle size of 3 mm and an apparent density of 2640 kg/m3. The coarse aggregate was prepared from crushed and manufactured recycled concrete. The basic performance indexes were measured following GB/T 14685-2011 [26], as shown in Table 2. The mixing water was tap water, and the superplasticizer was the PCA polycarboxylic superplasticizer produced by Subot New Materials Co., Ltd. (Nanjing, China). Appl. Sci. 2022, 12, 12238 4 of 15 Figure 1. Microstructure of RHA measured by scanning electron microscopy. Figure2.2. The The particle particle size RHA, river sand andand RCA. Figure sizedistributions distributionsofofcement, cement, RHA, river sand RCA. Thefine fine aggregate aggregate was river sand The sand from from the theShaanxi Shaanxiregion, region,with witha awater waterabsorption absorption of 3 . The 3. The of 3%, a maximum particlesize sizeofof33mm mm and and an apparent 2640 kg/m coarse 3%, a maximum particle apparentdensity densityofof 2640 kg/m coarse aggregate was crushed andand manufactured recycled concrete. The basicThe per-basic aggregate wasprepared preparedfrom from crushed manufactured recycled concrete. formance indexes were measured following GB/T 14685-2011 [26], [26], as shown in Table 2. 2. performance indexes were measured following GB/T 14685-2011 as shown in Table The mixing water was tap water, and the superplasticizer was the PCA polycarboxylic The mixing water was tap water, and the superplasticizer was the PCA polycarboxylic superplasticizer produced produced by Co., Ltd. (Nanjing, China). superplasticizer bySubot SubotNew NewMaterials Materials Co., Ltd. (Nanjing, China). Table 2. The basic properties indexes of recycled concrete aggregate (RCA). Aggregate Type Grading (mm) Water Absorption (%) Apparent Density (kg/m3 ) Bulk Density (kg/m3 ) Crush Index (%) RCA 5–25 3.8 2458.0 1430.0 17.0 2.2. Mixture Proportions and Specimen Preparation The concrete design mix is shown in Table 3, in which RHA replaced cement with 0%, 10%, 20% and 30% replacement ratios, respectively. The designation of the specimens was sourced from the replacement ratios of RHA. An effective water-to-binder ratio of 0.4 was maintained by adjusting the amount of additional water to the system owing to the high water absorption of the recycled coarse aggregate. A target slump of 100–150 mm was kept for the fresh concrete by adjusting the superplasticizer amount due to the RHA’s high specific surface area [20]. Table 3. The mixture proportion of the RHA recycled concrete mixtures. Mixture Proportion (kg/m3 ) Specimen W/B 0% RHA 10% RHA 20% RHA 30% RHA 0.40 0.40 0.40 0.40 Cement RHA Sand RCA Water AW SP 410 369 328 287 41 82 123 825 825 825 825 1085 1085 1085 1085 164 164 164 164 22 22 22 22 8.5 9.5 11.5 12.0 Notes: W/B represents the water-to-binder ratio. AW represents the additional water amount. SP represents the superplasticizer amount. carried out. The mass loss and relative dynamic elastic modulus were also used to assess the degree of the macroscopic performance deterioration of concrete [31], which was calculated as follows: ∆𝑚 = Appl. Sci. 2022, 12, 12238 × 100%, (1) 5 of 15 where ∆𝑚 is the mass loss; ∆𝑚 and 𝑚 are the masses before and after n freeze–thaw cycles, respectively. × dry 100%, 𝐸 , = the (2) In order to prepare concrete specimens, solid components were taken following the mass in the mixture proportion, which was subsequently dumped into a blender and where 𝐸 , is the relative dynamic elastic modulus; 𝐸 and 𝐸 are the dynamic elastic mixed evenly for 2 min. Then, superplasticizer and water were used, and the mixture moduli of concrete before and after n freeze–thaw cycles, respectively, and the measuring was cast into cubic specimens for mechanical characteristics testing after mixing uniformly. instrument is the NELD-DTV dynamic elastic modulus testing machine. Finally, the fresh concrete mixtures were loaded into the mold and vibrated on a table for compacting. The demolding and curing of the specimens were conducted following 2.3.4. SEM Test GB/T 50081-2019 [27]. The small pieces of paste samples with different RHA replacement ratios were immersed in ethanolMethod solution to prevent further hydration [32], dried in a GZX-9030MBE 2.3. Experimental drying oven, coated with conductive tape and pasted on the specimens, and they were In this paper, the impact of RHA on recycled concrete’s mechanical characteristics and subsequently subjected to spray gold treatment using a Cressington 108 coater. The specfreeze–thaw resistance was investigated using experiments, and the hydration products imens were analyzed by a Gemini SEM 500 field emission scanning electron microscope and microstructure were analyzed in combination with scanning electron microscopy (SEM) with a resolution of 0.5 nm, an acceleration pressure of 0.02 KV to 30 KV, a probe-current experiments. The experimental procedure is presented in Figure 3, and the details of the of 3 pA to 20 nA and a magnification of 50 X to 20,000 KX. experiments are given below. Figure3.3.Experimental Experimentalprocedure. procedure. Figure 2.3.1. Workability 3. Results and Discussions According to GB/T 50080-2016 [28], the slump cone experiment was performed to 3.1. Workability of RHA Recycled Aggregate Concrete evaluate the workability of fresh concrete. The slump value is measured in mm, the The workability of fresh to concrete mixtures be reflected by the value measurements were accurate 1 mm and the testcan results were revised to slump 5 mm [29]. [33,34]. The impact of RHA with different replacement ratios on the workability of recycled concrete was investigated by means of a slump cone test, and the results 2.3.2.aggregate Mechanical Characteristics are shown in Figure 4. It is noteworthy that 0% RHA and 10% RHA showed the same According to GB/T 50081-2019 [27], the compressive strength of concrete specimens slump value, which may be due to the increase in the superplasticizer (Table 3), resulting with dimensions of 100 mm × 100 mm × 100 mm cubic specimens was tested, and the in improved concrete workability. However, the improvement degree of the superplastiYAW-3000 universal loading machine was used. The test ages for strength were 7d, 28d, cizer is similar to the reduction degree caused by the increase in RHA content. At the same 90d and 360d, and the experimental value is the average of three specimens. 2.3.3. Freeze–Thaw Cycling According to GB/T 50082-2009 [30], the concrete specimens were put into the TDR-28 concrete freeze–thaw cycle testing machine for a rapid freeze–thaw cycle experiment. The freeze–thaw medium was tap water supplied by the laboratory, and the control system was suspended after reaching 50, 100, 150, 200, 250 and 300 cycles. The surface water of the specimens was dried, followed by mass and dynamic elastic modulus tests being carried out. The mass loss and relative dynamic elastic modulus were also used to assess the degree of the macroscopic performance deterioration of concrete [31], which was calculated as follows: m0 − m n ∆mn = × 100% (1) m0 Appl. Sci. 2022, 12, 12238 6 of 15 where ∆mn is the mass loss; ∆mn and mn are the masses before and after n freeze–thaw cycles, respectively. E Er,n = dn × 100% (2) Ed0 where Er,n is the relative dynamic elastic modulus; Ed0 and Edn are the dynamic elastic moduli of concrete before and after n freeze–thaw cycles, respectively, and the measuring instrument is the NELD-DTV dynamic elastic modulus testing machine. 2.3.4. SEM Test The small pieces of paste samples with different RHA replacement ratios were immersed in ethanol solution to prevent further hydration [32], dried in a GZX-9030MBE drying oven, coated with conductive tape and pasted on the specimens, and they were subsequently subjected to spray gold treatment using a Cressington 108 coater. The specimens were analyzed by a Gemini SEM 500 field emission scanning electron microscope with a resolution of 0.5 nm, an acceleration pressure of 0.02 KV to 30 KV, a probe-current of 3 pA to 20 nA and a magnification of 50 X to 20,000 KX. 3. Results and Discussions 3.1. Workability of RHA Recycled Aggregate Concrete Appl. Sci. 2022, 12, 12238 The workability of fresh concrete mixtures can be reflected by the slump value [33,34]. The impact of RHA with different replacement ratios on the workability of recycled aggregate concrete was investigated by means of a slump cone test, and the results are shown 7 of 16value, in Figure 4. It is noteworthy that 0% RHA and 10% RHA showed the same slump which may be due to the increase in the superplasticizer (Table 3), resulting in improved concrete workability. However, the improvement degree of the superplasticizer is similar to theitreduction degree caused by the slump increase in RHA thesame sameworkabiltime, it is due time, is due to the modification of the value, thus content. resulting At in the to the modification of the slump value, thus resulting in the same workability [35]. ity [35]. Figure 4. The impact of RHA replacement ratios on the workability of fresh concrete mixtures. Figure 4. The impact of RHA replacement ratios on the workability of fresh concrete mixtures. With the RHA substitution rate,rate, the the slump value of 20% With the thegradual gradualincrease increaseinin the RHA substitution slump value of RHA 20% RHA and 30% RHA decreased by 15.38% and 23.08%, respectively, compared with 0% RHA. and 30% RHA decreased by 15.38% and 23.08%, respectively, compared with 0% RHA. This may be due to the increase in the RHA replacement ratio, leading to an increase in This may be due to the increase in the RHA replacement ratio, leading to an increase in the the porosity and total specific surface area of the cementitious material (Table 1). The sysporosity and total specific surface area of the cementitious material (Table 1). The system tem absorbs more water, thus causing a reduction in the free water within the paste, which absorbs more water, thus causing a reduction in the free water within the paste, which will will increase the mixtures’ friction and discourage the flow, which in turn leads to the increase the mixtures’ friction and discourage the flow, which in turn leads to the decrease decrease in the concrete slump and reduced workability. This finding is similar to that of in the et concrete and reduced This finding is similar to thatwith of Amin Amin al. [15], slump who reported that theworkability. slump of fresh concrete mixtures increased et al. [15], who reported that the slump of fresh concrete mixtures increased with increasing increasing RHA content, and the mixtures with 30% RHA content had the worst workaRHA bility. content, and the mixtures with 30% RHA content had the worst workability. 3.2. Compressive Strength of RHA Recycled Aggregate Concrete The impact of RHA with different replacement ratios on the compressive strength of recycled concrete is shown in Figure 5. As shown in the figure, the compressive strength of the recycled concrete gradually increased as the hydration reaction continued, and the Appl. Sci. 2022, 12, 12238 7 of 15 3.2. Compressive Strength of RHA Recycled Aggregate Concrete Appl. Sci. 2022, 12, 12238 The impact of RHA with different replacement ratios on the compressive strength of recycled concrete is shown in Figure 5. As shown in the figure, the compressive strength of the recycled concrete gradually increased as the hydration reaction continued, and the growth rate shows a trend of first being rapid, then slowing down and finally gradually stabilizing. For instance, the compressive strength of 30% RHA at 7 days, 28 days, 90 days and 360 days was 33.8 MPa, 42.9 MPa, 46.4 MPa and 48.3 MPa, which increased by 69.98%, 8 of 16 18.84%, 7.25% and 3.94%, respectively. The variation in recycled concrete’s compressive strength may be because, in the initial stage of curing, the strength growth of the concrete is mainly due to the RHA particle’s filling action. The fine RHA particles can fill the pores and microcracks of thegrowth paste and interface transition zone,ages reducing theby porosity to a certain [38]. The strength of concrete at different curing is caused a combination extent and increasing the bulk density of the concrete, significantly improving of the cement hydration reaction, the filling effect and thethereby pozzolanic effect of RHA parti- the early strength of concrete. cles [39,40]. Figure 5. The impact of RHA replacement ratios on the compressive strength of recycled concrete. Figure 5. The impact of RHA replacement ratios on the compressive strength of recycled concrete. Thecontrast, compressive recycledofconcrete shows a tendency first increase In the strength strengthofgrowth recycled concrete in thetolater stages ofand curing then decrease as the RHA replacement ratio increases. For instance, the compressive is primarily due to the RHA particle’s pozzolanic effect [36]. Although the pozzolanic strength between of 10% RHA, 20% RHA 30% RHA at 360 days 52.8 MPa andpaste reaction RHA and freeand calcium hydroxide (CH)was led51.9 to aMPa, reduction in the 48.3 MPa and 102.17%, 103.94% and 95.08% of 0% RHA, respectively. This is probably porosity [37], the existence of the porous structure of the recycled aggregate attached because the high silica content and high specific surface area of RHA particles, which can mortar led to the absorption of large amounts of water by the system and a reduction in contact and react with more CH and water, produce extra C-S-H gels to improve the mathe free water content of the matrix, resulting in a weakening of the pozzolanic effect of trix compactness, thus leading to the improvement of concrete compressive strength. the RHA particles, thus causing a reduction in the total volume of hydration products, However, when the strength loss due to the decrease in cement content was more signifiwhich leads to a slow strength growth of the concrete in the later curing period. This is cant than the compressive strength increment contributed by the RHA filling effect and similar to the results Salas the later variation of RHAofnatural pozzolanic effect, thisof will leadettoal.a on reduction in strength the compressive strength concreteaggregate at a concrete [38]. The strength growth of concrete at different curing ages is caused high RHA replacement ratio. According to the variation in the compressive strength of by a combination of the cement hydration reaction, the filling effect and the pozzolanic effect concrete with an RHA replacement ratio, it is clear that the optimum replacement ratio of of RHA [39,40]. RHA particles is 20%, which is similar to the report of RHA natural aggregate concrete. For inThe compressive of recycled shows a tendency to first increase stance, He et al. [32] andstrength Chao-Lung et al. [41]concrete found that the concrete specimens with a and then decrease as the RHA replacement ratio increases. For instance, the compressive 20% RHA replacement ratio resulted in the highest paste compactness due to the joint strength RHA, and 30% RHA 360 daysinwas 51.9 MPa, 52.8 MPa and action of of the10% filling effect20% andRHA pozzolanic effect, thusatresulting the optimum mechanical 48.3 MPa and of 102.17%, characteristics concrete.103.94% and 95.08% of 0% RHA, respectively. This is probably because the high silica content and high specific surface area of RHA particles, which can 3.3. Mass Loss of RHA Aggregate Concrete contact and react withRecycled more CH and water, produce extra C-S-H gels to improve the matrix compactness, to the improvement of concrete strength. However, The massthus lossleading is an essential indicator representing thecompressive damage degree of surface when theofstrength due to subjected the decrease in cement content wasFigure more 6significant spalling concreteloss specimens to freeze–thaw cycles [42]. shows the than the compressive strength increment contributed by theRHA RHAreplacement filling effect and during pozzolanic variation in recycled concrete’s mass loss with different ratios the freeze–thaw cycle. shown in in thethe figure, the mass strength loss tends decreaseatwith theRHA effect, this will lead to As a reduction compressive oftoconcrete a high increase in the number of cycles at the initial stage of the freeze–thaw cycle, and the re- with replacement ratio. According to the variation in the compressive strength of concrete duction amount increases with the rise in the RHA substitution rate. For instance, when concrete specimens were subjected to 100 freeze–thaw cycles, the mass losses of concrete with 0% RHA, 10% RHA, 20% RHA and 30% RHA were −0.48%, −0.71%, −0.73% and −0.83%, respectively. This could be attributed to the existence of the porous structure of the recycled aggregate attached mortar, which resulted in more external water transfer to Appl. Sci. 2022, 12, 12238 8 of 15 an RHA replacement ratio, it is clear that the optimum replacement ratio of RHA is 20%, which is similar to the report of RHA natural aggregate concrete. For instance, He et al. [32] and Chao-Lung et al. [41] found that the concrete specimens with a 20% RHA replacement ratio resulted in the highest paste compactness due to the joint action of the filling effect and pozzolanic effect, thus resulting in the optimum mechanical characteristics of concrete. 3.3. Mass Loss of RHA Recycled Aggregate Concrete Appl. Sci. 2022, 12, 12238 The mass loss is an essential indicator representing the damage degree of surface spalling of concrete specimens subjected to freeze–thaw cycles [42]. Figure 6 shows the variation in recycled concrete’s mass loss with different RHA replacement ratios during the freeze–thaw cycle. As shown in the figure, the mass loss tends to decrease with the increase in the number of cycles at the initial stage of the freeze–thaw cycle, and the reduction amount increases with the rise in the RHA substitution rate. For instance, when concrete specimens were subjected to 100 freeze–thaw cycles, the mass losses of concrete with 0% RHA, 10% RHA, 20% RHA and 30% RHA were −0.48%, −0.71%, −0.73% and −0.83%, respectively. This could be attributed to the existence of the porous structure of the recycled aggregate attached mortar, which resulted in more external water transfer to the internal pores and cracks. In addition, the high porosity of RHA particles will enhance 9 of 16 the permeability of the concrete; thus, it will also cause a large amount of water absorption. The synergistic effect of both will reduce the mass loss of the concrete. Figure6.6.The Therelationship relationshipbetween betweenthe themass massloss lossof ofrecycled recycledconcrete concrete and and the the number number of of freeze–thaw freeze– Figure thaw cycles with different RHA replacement ratios. cycles with different RHA replacement ratios. However,the the water water absorbed will lead to concrete freeze–thaw However, absorbedby bythe theRHA RHAparticles particles will lead to concrete freeze–thaw damage due to icing pressure and expansion pressure with the increase in the number of of damage due to icing pressure and expansion pressure with the increase in the number freeze–thaw cycles. During the freeze–thaw cycle, the original pore structure continuously freeze–thaw cycles. During the freeze–thaw cycle, the original pore structure continuously expands into visible pores and sprouts to generate microcracks. It then gradually develops expands into visible pores and sprouts to generate microcracks. It then gradually develops into macrocracks under repeated expansion pressure, which eventually leads to spalling into macrocracks under repeated expansion pressure, which eventually leads to spalling damage and aggregate loss on the concrete surface. When the mass loss of concrete caused damage and aggregate loss on the concrete surface. When the mass loss of concrete caused by surface damage is greater than the mass increment generated by the absorbed water of by surface damage is greater than the mass increment generated by the absorbed water of the concrete specimens, the mass of concrete will decrease, and the mass loss will increase. the concrete specimens, the mass of concrete will decrease, and the mass loss will increase. According to GB/T 50082-2009 [30], if the mass loss exceeds 5% as the basis of concrete According to GB/T 50082-2009 [30], if the mass loss exceeds 5% as the basis of concrete freeze–thaw resistance damage, the concrete specimens with 10% RHA and 20% RHA lose freeze–thaw resistance damage, specimens with 10% RHA and their freeze–thaw resistance afterthe 300concrete cycles, while the concrete specimens with20% 30%RHA RHA lose their resistance afterafter 300 only cycles, the concrete lose freeze–thaw their freeze–thaw resistance 250while freeze–thaw cycles.specimens with 30% RHA lose their freeze–thaw resistance after only 250 freeze–thaw cycles. 3.4. Relative Dynamic Elastic Modulus of RHA Recycled Aggregate Concrete The stiffness of concrete specimens subjected to the freeze–thaw cycles can be characterized by the variation in the relative dynamic elastic modulus [43]. Figure 7 shows the variation in the recycled concrete’s relative dynamic elastic modulus with different RHA replacement ratios during the freeze–thaw cycles. As shown in the figure, the relative dynamic elastic modulus of concrete decreases continuously with an increase in the number of freeze–thaw cycles. Specifically, the relative dynamic elastic modulus decreases slowly Appl. Sci. 2022, 12, 12238 9 of 15 3.4. Relative Dynamic Elastic Modulus of RHA Recycled Aggregate Concrete Appl. Sci. 2022, 12, 12238 The stiffness of concrete specimens subjected to the freeze–thaw cycles can be characterized by the variation in the relative dynamic elastic modulus [43]. Figure 7 shows the variation in the recycled concrete’s relative dynamic elastic modulus with different RHA replacement ratios during the freeze–thaw cycles. As shown in the figure, the relative dynamic elastic modulus of concrete decreases continuously with an increase in the number of freeze–thaw cycles. Specifically, the relative dynamic elastic modulus decreases slowly in the initial stage of the cycle, while it decreases rapidly in the later stage of the cycle, indicating that the internal damage of the concrete gradually increases, subjected to the freeze–thaw cycle. The variation in the relative dynamic elastic modulus is related to the number of cracks and pores in the concrete itself, as there are many unfavorable interfacial transition zones within the recycled concrete aggregate, thus resulting in a lower initial dynamic modulus of elasticity for the concrete. The higher the initial damage degree, the easier it is for the specimens to form new cracks [44]. Under the freeze–thaw cycling, the expansion and icing pressure of pore water inside the specimen will lead to numerous new pores and new microcracks in the unfavorable interfacial transition zone. The presence of 10 of 16 these discontinuities in the matrix increases the propagation time of the ultrasonic pulse velocity, which leads to a decrease in the relative dynamic elastic modulus. Figure7.7. The The relationship relationship between between the Figure the relative relative dynamic dynamic elastic elasticmodulus modulusofofrecycled recycledconcrete concreteand and the the number of freeze–thaw cycles with different RHA replacement ratios. number of freeze–thaw cycles with different RHA replacement ratios. In addition, addition, the relative dynamic elastic modulus increased In the decreasing decreasingdegree degreeininthe the relative dynamic elastic modulus increased with the increase in the RHA replacement ratio. This is probably because the addition of of with the increase in the RHA replacement ratio. This is probably because the addition RHA can enhance the pore structure within the concrete, reducing the freezing point and RHA can enhance the pore structure within the concrete, reducing the freezing point and pore connectivity, retarding the crack generation and water migration between the pores pore connectivity, retarding the crack generation and water migration between the pores inside the concrete. However, the introduction of the RHA mesoporous structure will lead inside the concrete. However, the introduction of the RHA mesoporous structure will lead to the expansion and extension of the pore structure under the action of expansion presto the expansion and extension of the pore structure under the action of expansion pressure, sure, resulting in the deterioration of the pore structure, which will adversely affect the resulting in the deterioration of the pore structure, which will adversely affect the concrete’s concrete’s freeze–thaw resistance, thus resulting in the freeze–thaw damage of concrete freeze–thaw resistance, thus resulting in the freeze–thaw damagethe of reduced concretecement specimens specimens with 20% RHA after 300 freeze–thaw cycles. In addition, with 20% RHA after 300 freeze–thaw cycles. In addition, the reduced cement content content at a high RHA replacement rate resulted in the poor filling of paste pores, thus at a high RHA resulted in the poor of paste thus leading to the leading to replacement the damage ofrate concrete specimens withfilling 30% RHA afterpores, only 250 freeze–thaw damage of concrete specimens with 30% RHA after only 250 freeze–thaw cycles. cycles. In introducingRHA RHAwill will reduce concrete freeze–thaw resistance In conclusion, conclusion, introducing reduce thethe concrete freeze–thaw resistance com-compared to ordinary concrete (without RHA), and the decreasing degree increases pared to ordinary concrete (without RHA), and the decreasing degree increases withwith the the increase replacementrate. rate.The The influence mechanism of the RHA substitution increase in in the the RHA RHA replacement influence mechanism of the RHA substitution rate on the freeze–thaw damage deterioration of recycled concrete will be analyzed in detail in Section 3.6. 3.5. Mechanistic Analysis of the Influence of RHA on the Microstructure of Recycled Aggregate Concrete Figure 8 shows the influence of different RHA replacement ratios on paste samples’ Appl. Sci. 2022, 12, 12238 10 of 15 rate on the freeze–thaw damage deterioration of recycled concrete will be analyzed in detail in Section 3.6. 3.5. Mechanistic Analysis of the Influence of RHA on the Microstructure of Recycled Aggregate Concrete Appl. Sci. 2022, 12, 12238 Figure 8 shows the influence of different RHA replacement ratios on paste samples’ microstructure and hydration products before the freeze–thaw cycles. As shown in Figure 8a, the 0% RHA paste is characterized by significant amounts of rod-shaped CH crystals and numerous pores in the matrix, and the surface microstructure is relatively loose. This is probably because the insufficient hydration of cement particles leads to a decrease in the degree of paste compactness, which agrees with previous research results [45,46]. The 10% RHA paste is characterized by a dense paste without obvious pores in the matrix, and cracks of significant width were found in the interfacial transition zone. The 20% RHA paste is characterized by dense paste at different locations in the matrix, small microcracks between the interfacial transition zone of the aggregate and mortar and no significant 11 of 16 CH crystals in the paste. This may be due to the smaller particle size of RHA particles, which can promote cement hydration due to their high specific surface, resulting in a pozzolanic reaction CH generated by the cement hydrationcompacting and the amorphous silica the RHAbetween to reach the a threshold value, leading to the optimum effect of the gen-of the RHA to reach a threshold value, leading to the optimum compacting effect of the generated erated C-S-H gels on the paste pores and enhancing the bonding of the interfacial transiC-S-H gelsreducing on the paste pores andofenhancing the will bonding of thetointerfacial transition tion zone, the formation cracks, which contribute the mechanical char-zone, reducing the formation of cracks, which will contribute to the mechanical characteristics acteristics of concrete enhancement [47,48]. As shown in Figure 8d, the 30% RHA paste is of concrete enhancement [47,48]. Asa shown in Figure 8d, the 30% RHA paste is characterized characterized by large pores and large number of randomly distributed needle-shaped by large pores and a large number of randomly distributed needle-shaped AFTs in the AFTs in the matrix. This may be due to the lower cement content, which leads to a reduced matrix. This may be due to the lower cement content, which leads to a reduced CH content CH content generated by cement hydration, which in turn leads to a weaker degree of generated cement hydration, which intoturn to a weaker degree of pozzolanic pozzolanic by reaction, which is not conducive poreleads compactness. In conclusion, the compactness degree samples an increase followed by a decrease with an reaction, which of is the notpaste conducive toshowed pore compactness. In conclusion, the compactness increasing RHA replacement ratio, which corresponds to its compressive degree of the paste samples showed an increase followed by a decreasestrength with anmagniincreasing tude. replacement ratio, which corresponds to its compressive strength magnitude. RHA Figure 8. 8. Microscopic Microscopic morphology ratios be-before Figure morphologyof ofthe thepaste pastesamples sampleswith withdifferent differentRHA RHAreplacement replacement ratios fore the freeze–thaw cycles. the freeze–thaw cycles. The microscopic microscopic morphology ra-ratios The morphologyof ofpaste pastesamples sampleswith withdifferent differentRHA RHAreplacement replacement tios after undergoing freeze–thaw cycles presentedininFigure Figure9.9. As As shown shown in after undergoing freeze–thaw cycles is is presented in Figure Figure9a, 9a, the the RHA 0% RHA paste shows a relativelydense densemicrostructure microstructure with ofof pores. 0% paste shows a relatively withaasmall smallnumber number pores. It It can seenfrom fromFigure Figure9b 9b that that aa penetrating was found on on the the surface of the can bebe seen penetratingcrack crack was found surface of10% the 10% RHA paste sample, which may be caused by human factors during the sample preparaRHA paste sample, which may be caused by human factors during the sample preparation tion process [40,49]. Figure showsthat that 20% 20% RHA characterized by aby noticeable process [40,49]. Figure 9c9c shows RHApaste pasteisis characterized a noticeable increase in the number of pores as well as a large number of staggered cracks in the cement paste matrix, which may be because, although the low content of RHA can improve the paste compactness and the bonding of the interfacial transition zone, it cannot compensate for the lack of its porous properties, which will cause a reduction in the freeze–thaw resistance of the concrete. Appl. Sci. 2022, 12, 12238 Appl. Sci. 2022, 12, 12238 11 of 15 increase in the number of pores as well as a large number of staggered cracks in the cement paste matrix, which may be because, although the low content of RHA can improve the paste compactness and the bonding of the interfacial transition zone, it cannot compensate 12 of 16 for the lack of its porous properties, which will cause a reduction in the freeze–thaw resistance of the concrete. Figure 9. ofof thethe paste samples with different RHARHA replacement ratiosratios after after Figure 9. Microscopic Microscopicmorphology morphology paste samples with different replacement the freeze–thaw freeze–thaw cycles. the cycles. 3.6. Mechanistic the the Influence of RHA the Mechanical and significantly Freeze– As shown Analysis in Figureof9d, surface of theon30% RHA pasteCharacteristics sample showed Thaw Resistance of Recycled Concrete porous characteristics, andAggregate the mortar matrix appeared brittle, indicating that the addition of a large number of RHA process would further deteriorate compactness degree of the cement During the hydration of cement paste, thethe RHA particle’s high specific surpaste. This is probably because of the recycled structure, face area will promote the hydration reaction of aggregate cement. Atattached the samemortar’s time, theporous amorphous which increases the water absorption the the concrete. In addition, reductionof inthe cement silica within the RHA particles will reactofwith CH generated by thea hydration cement to produce gel. The C-S-Hdensification. gels and the incompletely content leads to a C-S-H weakening ofextra the paste This leads hydrated to a morecement significant and RHA particles will refine thethe pore structure in the paste improve the bonding of icing pressure generated inside concrete subjected to theand freeze–thaw cycles, an increase thethe interfacial which in leads a densified consequently in numbertransition of pores zone, and cracks thetopaste due tomicrostructure the expansionand pressure and further has a positive contribution to the development of the compressive strength ofby thethe concrete. damage to the internal structure, which is macroscopically manifested increase in However, under the condition of a high RHA replacement rate, the reduced free water mass loss and the decrease in dynamic elastic modulus. content leads to a weaker hydration reaction, less CH generation and a reduced poz- zolanic reaction Analysis between of CH amorphous silica, leading to a reduction in C-S-H 3.6. Mechanistic theand Influence of RHA on the Mechanical Characteristics andgel Freeze–Thaw Resistance of conducive Recycled Aggregate Concretecompactness of the paste pore and production, which is not to the improved the interfacial transition zone, thus leading to apaste, loose the microstructure of the cement paste During the hydration process of cement RHA particle’s high specific surface and a weaker bonding of the interfacial transition zone, which will have a negative impact area will promote the hydration reaction of cement. At the same time, the amorphous silica on the load-bearing capacity the concrete. within the RHA particles willofreact with the CH generated by the hydration of the cement to When recycled coarse aggregate is added to incompletely concrete, two hydrated types of interfaces areRHA produce C-S-H gel. The extra C-S-H gels and the cement and formed inside the concrete: the attached mortar–old aggregate interface and the new morparticles will refine the pore structure in the paste and improve the bonding of the interfacial tar–attached mortar interface, as shown in Figure 10a. The recycled aggregate attached transition zone, which leads to a densified microstructure and consequently has a positive mortar’s porous structure will make the concrete absorb a large amount of water during contribution to the development of the compressive strength of the concrete. However, the process of the freeze–thaw cycle. The RHA particle’s high specific surface area will under the condition of a high RHA replacement rate, the reduced free water content leads cause water enrichment to occur on its surface and enter the interface transition zone of to a weaker hydration reaction, less CH generation and a reduced pozzolanic reaction the new mortar–attached mortar interface of the recycled aggregate through cracks and between CH and amorphous silica, leading to a reduction in C-S-H gel production, which is pores. When the pore water inside the concrete is in the process of repeated freeze–thaw, not conducive to the improved compactness of the paste pore and thepores interfacial it causes the continuous accumulation of the expansion pressure of the withintransition the zone, thus leading to a loose microstructure of the cement paste and a weaker concrete, which consequently leads to the gradual transformation of the tiny pores inbonding the of the interfacial zone, pores whichunder will have a negative impact interface transitiontransition zone into larger the action of tensile stress on andthe theload-bearing gradual capacity of the development ofconcrete. microcracks into macrocracks, which will provide a channel for the miWhen recycled coarse aggregate to concrete, types of interfaces gration of water. The more water retainedisinadded the pores and crackstwo inside the concrete, the are formed inside the the attached mortar–old aggregate and the new more significant theconcrete: volume increase when freezing, which leads to ainterface higher expansion pressure inside the concrete and accelerates the formation of cracks [50]. The interface transition zone, as the strength-limiting phase of concrete, makes the concrete reach an Appl. Sci. 2022, 12, 12238 Appl. Sci. 2022, 12, 12238 12 of 15 mortar–attached mortar interface, as shown in Figure 10a. The recycled aggregate attached mortar’s porous structure will make the concrete absorb a large amount of water during the process of the freeze–thaw cycle. The RHA particle’s high specific surface area will cause water enrichment to occur on its surface and enter the interface transition zone of the new mortar–attached mortar interface of the recycled aggregate through cracks and pores. When the pore water inside the concrete is in the process of repeated freeze–thaw, it causes the continuous accumulation of the expansion pressure of the pores within the concrete, which consequently leads to the gradual transformation of the tiny pores in the interface transition zone into larger pores under the action of tensile stress and the gradual development of microcracks into macrocracks, which will provide a channel for the migration of water. 13 of 16 The more water retained in the pores and cracks inside the concrete, the more significant the volume increase when freezing, which leads to a higher expansion pressure inside the concrete and accelerates the formation of cracks [50]. The interface transition zone, as the strength-limiting phase ofunder concrete, makes the concrete reachwhich an ultimate ultimate tensile strength a slight expansion pressure, resultstensile in the strength freeze– under a slight of expansion which results in the thaw damage concrete pressure, due to stress concentration [51].freeze–thaw damage of concrete due to stress concentration [51]. Figure10. 10. (a) (a)Schematic Schematicdiagram diagramofofthe thecomponent componentphases phasesofofRCA; RCA;(b) (b)Schematic Schematicofofthe the deterioraFigure deterioration tion mechanism of RHA on recycled aggregate concrete freeze–thaw damage. mechanism of RHA on recycled aggregate concrete freeze–thaw damage. Meanwhile, as as the the bond bond is is the the weakest weakest at Meanwhile, at the the interface interface transition transitionzone zonebetween betweenthe the new mortar and the attached mortar, the transverse tensile stress continues new mortar and the attached mortar, the transverse tensile stress continuestotoincrease, increase, whichwill willcause cause the the rapid rapid expansion expansion and which and extension extension of of cracks cracksin inthe thenew newmortar–attached mortar–attached mortarinterface interface transition transition zone, zone, and mortar and the the attached attached mortar–old mortar–oldaggregate aggregateinterface interfacewill willalso also generatecracks cracks until until the the concrete concrete specimen generate specimen is is destroyed. destroyed. The Theeffect effectmechanism mechanismofofrecycled recycled concretefreeze–thaw freeze–thawdamage damage deterioration deterioration by by RHA concrete RHA is is shown shown in inFigure Figure10b. 10b.In Inthe theprocess process of freeze–thaw cycles, with the increase in the RHA replacement ratio, the degree of ceof freeze–thaw cycles, with the increase in the RHA replacement ratio, the degree of cement ment paste compactness decreases. In addition, the introduction of a large amount of the paste compactness decreases. In addition, the introduction of a large amount of the RHA RHA mesoporous structure causes a significant increase in the porosity and the number mesoporous structure causes a significant increase in the porosity and the number of cracks of cracks the concrete, and the increase pore connectivity to the enhance-of inside theinside concrete, and the increase in pore in connectivity leads toleads the enhancement ment of specimen permeability, whichthe makes the concrete more sensitive to freeze–thaw specimen permeability, which makes concrete more sensitive to freeze–thaw cycles. cycles. Overall, the freeze–thaw resistance of recycled a decreasing trend Overall, the freeze–thaw resistance of recycled concreteconcrete shows ashows decreasing trend with the with the increase in the RHA replacement ratio. increase in the RHA replacement ratio. Conclusions 4.4. Conclusions In this this paper, paper, the the impact impact of RHA on the mechanical In mechanical characteristics characteristicsand andfreeze–thaw freeze–thaw resistance of of recycled recycled concrete was investigated, resistance investigated, and and the the mechanism mechanismofofthe thefreeze–thaw freeze–thaw damage deterioration deterioration of RHA was revealed by combining SEMSEM exdamage ofrecycled recycledconcrete concretebyby RHA was revealed by combining periments. The main conclusions areare as as follows: experiments. The main conclusions follows: (1) The gradual increase in the RHA replacement ratio increased the cementitious material’s total specific surface area and porosity, which will increase the mixtures’ friction resistance and discourage the flow, which in turn leads to the decrease in the concrete slump and the reduced workability. (2) With the continuous hydration reaction process, the compressive strength of recycled concrete increased with the growth of the curing age, and the growth rate shows a Appl. Sci. 2022, 12, 12238 13 of 15 (1) (2) (3) (4) (5) The gradual increase in the RHA replacement ratio increased the cementitious material’s total specific surface area and porosity, which will increase the mixtures’ friction resistance and discourage the flow, which in turn leads to the decrease in the concrete slump and the reduced workability. With the continuous hydration reaction process, the compressive strength of recycled concrete increased with the growth of the curing age, and the growth rate shows a trend of first being rapid, then slowing down and finally gradually stabilizing. In addition, the optimum compressive strength of recycled concrete is observed with a 20% RHA replacement ratio. With the gradual increase in the number of freeze–thaw cycles, the mass loss of recycled concrete showed a tendency to first decrease and then increase, while the relative dynamic elastic modulus showed a continuous decreasing trend. Compared with ordinary concrete (without RHA), the RHA particle’s high specific surface area will promote the cement hydration and the formation of C-S-H gel by providing nucleation positions before the freeze–thaw cycle. During the process of the freeze–thaw cycle, the existence of the recycled aggregate attached mortar’s porous structure will cause a large amount of water absorption. With the continuous accumulation of expansion pressure, the internal pores and microcracks will gradually expand and extend, which will provide a channel for water migration, thus resulting in recycled concrete undergoing more severe freeze–thaw damage, and the degree of freeze–thaw damage deterioration grows as the RHA replacement ratio increases. In addition, more exploration and experimentation in other durability aspects are needed to expand the application of RHA in recycled aggregate concrete. Author Contributions: Conceptualization, W.Z. and H.L.; methodology, W.Z. and H.L.; software, W.Z.; validation, W.Z.; investigation, W.Z.; resources, W.Z.; writing—original draft preparation, W.Z.; writing—review and editing, C.L.; visualization, W.Z.; supervision, W.Z.; project administration, W.Z. and C.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 (Grant NO. 51878546, Grant NO. 52178251), the Science Foundation Project for Outstanding Youth of Shaanxi Province (Grant NO. 2020JC-46), the Key Research and Development Projects of Shaanxi Province (Grant NO. 2020SF-367) and the Xi’an Science and Technology Plan Key Industrial Chain Core Technology Project (Grant NO. 2022JH-ZCZC-0026). Data Availability Statement: Not applicable. Acknowledgments: The authors thank the editor and reviewers very much for their comments and helpful suggestions. Conflicts of Interest: The authors declare that they have no conflict of interest to report regarding the present study. References 1. 2. 3. 4. 5. 6. 7. Yan, K.; Lan, H.; Li, Q.; Ge, D.; Li, Y. Optimum utilization of recycled aggregate and rice husk ash stabilized base material. Constr. Build. Mater. 2022, 348, 128627. [CrossRef] Benhelal, E.; Zahedi, G.; Hashim, H. A novel design for green and economical cement manufacturing. J. Clean. Prod. 2012, 22, 60–66. [CrossRef] Andrew, R.M. Global CO2 emissions from cement production. Earth Syst. Sci. Data 2018, 10, 195–217. [CrossRef] Kurda, R.; de Brito, J.; Silvestre, J.D. Water absorption and electrical resistivity of concrete with recycled concrete aggregates and fly ash. Cem. Concr. Compos. 2019, 95, 169–182. [CrossRef] Alyousef, R.; Ali, B.; Mohammed, A.; Kurda, R.; Alabduljabbar, H.; Riaz, S. Evaluation of Mechanical and Permeability Characteristics of Microfiber-Reinforced Recycled Aggregate Concrete with Different Potential Waste Mineral Admixtures. Materials 2021, 14, 5933. [CrossRef] Fu, Q.; Zhang, Z.; Zhao, X.; Xu, W.; Niu, D. Effect of nano calcium carbonate on hydration characteristics and microstructure of cement-based materials: A review. J. Build. Eng. 2022, 50, 104220. [CrossRef] Wang, J.; Xiao, J.; Zhang, Z.; Han, K.; Hu, X.; Jiang, F. Action mechanism of rice husk ash and the effect on main performances of cement-based materials: A review. Constr. Build. Mater. 2021, 288, 123068. [CrossRef] Appl. Sci. 2022, 12, 12238 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 14 of 15 Hu, L.; He, Z.; Shao, Y.; Cai, X.; Zhang, S. Microstructure and properties of sustainable cement-based materials using combustion treated rice husk ash. Constr. Build. Mater. 2021, 294, 123482. [CrossRef] Yao, W.; Bai, M.; Pang, J.; Liu, T. Performance degradation and damage model of rice husk ash concrete under dry–wet cycles of sulfate environment. Environ. Sci. Pollut. Res. 2022, 29, 59173–59189. [CrossRef] Abolhasani, A.; Samali, B.; Aslani, F. Rice Husk Ash Incorporation in Calcium Aluminate Cement Concrete: Life Cycle Assessment, Hydration and Strength Development. Sustainability 2022, 14, 1012. [CrossRef] Bie, R.-S.; Song, X.-F.; Liu, Q.-Q.; Ji, X.-Y.; Chen, P. Studies on effects of burning conditions and rice husk ash (RHA) blending amount on the mechanical behavior of cement. Cem. Concr. Compos. 2015, 55, 162–168. [CrossRef] Chalee, W.; Sasakul, T.; Suwanmaneechot, P.; Jaturapitakkul, C. Utilization of rice husk–bark ash to improve the corrosion resistance of concrete under 5-year exposure in a marine environment. Cem. Concr. Compos. 2013, 37, 47–53. [CrossRef] Liu, C.; Zhang, W.; Liu, H.; Lin, X.; Zhang, R. A compressive strength prediction model based on the hydration reaction of cement paste by rice husk ash. Constr. Build. Mater. 2022, 340, 127841. [CrossRef] Vieira, A.P.; Filho, R.D.T.; Tavares, L.; Cordeiro, G.C. Effect of particle size, porous structure and content of rice husk ash on the hydration process and compressive strength evolution of concrete. Constr. Build. Mater. 2020, 236, 117553. [CrossRef] Amin, M.; Abdelsalam, B.A. Efficiency of rice husk ash and fly ash as reactivity materials in sustainable concrete. Sustain. Environ. Res. 2019, 29, 30. [CrossRef] Kang, S.-H.; Hong, S.-G.; Moon, J. The use of rice husk ash as reactive filler in ultra-high performance concrete. Cem. Concr. Res. 2019, 115, 389–400. [CrossRef] Liu, H.; Liu, C.; Bai, G.; Wu, Y.; He, C.; Zhang, R.; Wang, Y. Influence of pore defects on the hardened properties of 3D printed concrete with coarse aggregate. Addit. Manuf. 2022, 55, 102843. [CrossRef] Liu, H.; Liu, C.; Wu, Y.; Bai, G.; He, C.; Zhang, R.; Wang, Y. Hardened properties of 3D printed concrete with recycled coarse aggregate. Cem. Concr. Res. 2022, 159, 106868. [CrossRef] Qureshi, L.A.; Ali, B.; Ali, A. Combined effects of supplementary cementitious materials (silica fume, GGBS, fly ash and rice husk ash) and steel fiber on the hardened properties of recycled aggregate concrete. Constr. Build. Mater. 2020, 263, 120636. [CrossRef] Rattanachu, P.; Toolkasikorn, P.; Tangchirapat, W.; Chindaprasirt, P.; Jaturapitakkul, C. Performance of recycled aggregate concrete with rice husk ash as cement binder. Cem. Concr. Compos. 2020, 108, 103533. [CrossRef] Nuaklong, P.; Jongvivatsakul, P.; Pothisiri, T.; Sata, V.; Chindaprasirt, P. Influence of rice husk ash on mechanical properties and fire resistance of recycled aggregate high-calcium fly ash geopolymer concrete. J. Clean. Prod. 2020, 252, 119797. [CrossRef] Padhi, R.S.; Patra, R.K.; Mukharjee, B.B.; Dey, T. Influence of incorporation of rice husk ash and coarse recycled concrete aggregates on properties of concrete. Constr. Build. Mater. 2018, 173, 289–297. [CrossRef] Koushkbaghi, M.; Kazemi, M.J.; Mosavi, H.; Mohseni, E. Acid resistance and durability properties of steel fiber-reinforced concrete incorporating rice husk ash and recycled aggregate. Constr. Build. Mater. 2019, 202, 266–275. [CrossRef] Salahuddin, H.; Nawaz, A.; Maqsoom, A.; Mehmood, T.; Zeeshan, B.U.A. Effects of elevated temperature on performance of recycled coarse aggregate concrete. Constr. Build. Mater. 2019, 202, 415–425. [CrossRef] Alnahhal, M.F.; Alengaram, U.J.; Jumaat, M.Z.; Abutaha, F.; Alqedra, M.A.; Nayaka, R.R. Assessment on engineering properties and CO2 emissions of recycled aggregate concrete incorporating waste products as supplements to Portland cement. J. Clean. Prod. 2018, 203, 822–835. [CrossRef] GB/T 14685-2011; Pebble and Crushed Stone for Construction. Chinese National Standard: Beijing, China, 2011. GB/T 50081-2019; Standard for Test Methods of Concrete Physical and Mechanical Properties. Chinese National Standard: Beijing, China, 2019. GB/T 50080-2016; Standard for Test Method of Performance on Ordinary Fresh Concrete. Chinese National Standard: Beijing, China, 2016. Liu, C.; Zhang, W.; Liu, H.; Zhu, C.; Wu, Y.; He, C.; Wang, Z. Recycled aggregate concrete with the incorporation of rice husk ash: Mechanical properties and microstructure. Constr. Build. Mater. 2022, 351, 128934. [CrossRef] GB/T 50082-2009; Standard for Test Methods of Long-Term Performance and Durability of Ordinary Concrete. Chinese National Standard: Beijing, China, 2009. Zhang, W.; Pi, Y.; Kong, W.; Zhang, Y.; Wu, P.; Zeng, W.; Yang, F. Influence of damage degree on the degradation of concrete under freezing-thawing cycles. Constr. Build. Mater. 2020, 260, 119903. [CrossRef] He, Z.-H.; Li, L.-Y.; Du, S.-G. Creep analysis of concrete containing rice husk ash. Cem. Concr. Compos. 2017, 80, 190–199. [CrossRef] Antiohos, S.; Papadakis, V.; Tsimas, S. Rice husk ash (RHA) effectiveness in cement and concrete as a function of reactive silica and fineness. Cem. Concr. Res. 2014, 61–62, 20–27. [CrossRef] Zhang, S.; Cao, K.; Wang, C.; Wang, X.; Deng, G.; Wei, P. Influence of the porosity and pore size on the compressive and splitting strengths of cellular concrete with millimeter-size pores. Constr. Build. Mater. 2020, 235, 117508. [CrossRef] Msinjili, N.S.; Schmidt, W.; Rogge, A.; Kühne, H.-C. Performance of rice husk ash blended cementitious systems with added superplasticizers. Cem. Concr. Compos. 2017, 83, 202–208. [CrossRef] Jamil, M.; Khan, M.; Karim, M.; Kaish, A.; Zain, M. Physical and chemical contributions of Rice Husk Ash on the properties of mortar. Constr. Build. Mater. 2016, 128, 185–198. [CrossRef] Appl. Sci. 2022, 12, 12238 37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 15 of 15 Van Tuan, N.; Ye, G.; van Breugel, K.; Copuroglu, O. Hydration and microstructure of ultra high performance concrete incorporating rice husk ash. Cem. Concr. Res. 2011, 41, 1104–1111. [CrossRef] Salas, A.; Delvasto, S.; DE Gutierrez, R.M.; Lange, D. Comparison of two processes for treating rice husk ash for use in high performance concrete. Cem. Concr. Res. 2009, 39, 773–778. [CrossRef] Alex, J.; Dhanalakshmi, J.; Ambedkar, B. Experimental investigation on rice husk ash as cement replacement on concrete production. Constr. Build. Mater. 2016, 127, 353–362. [CrossRef] Venkatanarayanan, H.K.; Rangaraju, P.R. Effect of grinding of low-carbon rice husk ash on the microstructure and performance properties of blended cement concrete. Cem. Concr. Compos. 2015, 55, 348–363. [CrossRef] Chao-Lung, H.; Le Anh-Tuan, B.; Chun-Tsun, C. Effect of rice husk ash on the strength and durability characteristics of concrete. Constr. Build. Mater. 2011, 25, 3768–3772. [CrossRef] Kessler, S.; Thiel, C.; Grosse, C.U.; Gehlen, C. Effect of freeze–thaw damage on chloride ingress into concrete. Mater. Struct. 2016, 50, 121. [CrossRef] del Bosque, I.S.; Heede, P.V.D.; De Belie, N.; de Rojas, M.S.; Medina, C. Freeze-thaw resistance of concrete containing mixed aggregate and construction and demolition waste-additioned cement in water and de-icing salts. Constr. Build. Mater. 2020, 259, 119772. [CrossRef] Tam, V.W.Y.; Gao, X.F.; Tam, C.M. Microstructural analysis of recycled aggregate concrete produced from two-stage mixing approach. Cem. Concr. Res. 2005, 35, 1195–1203. [CrossRef] Zhan, B.J.; Xuan, D.X.; Poon, C.S.; Scrivener, K.L. Characterization of interfacial transition zone in concrete prepared with carbonated modeled recycled concrete aggregates. Cem. Concr. Res. 2020, 136, 106175. [CrossRef] Miyandehi, B.M.; Feizbakhsh, A.; Yazdi, M.A.; Liu, Q.-F.; Yang, J.; Alipour, P. Performance and properties of mortar mixed with nano-CuO and rice husk ash. Cem. Concr. Compos. 2016, 74, 225–235. [CrossRef] Wang, D.; Zhou, X.; Fu, B.; Zhang, L. Chloride ion penetration resistance of concrete containing fly ash and silica fume against combined freezing-thawing and chloride attack. Constr. Build. Mater. 2018, 169, 740–747. [CrossRef] Gencel, O.; Benli, A.; Bayraktar, O.Y.; Kaplan, G.; Sutcu, M.; Elabade, W.A.T. Effect of waste marble powder and rice husk ash on the microstructural, physico-mechanical and transport properties of foam concretes exposed to high temperatures and freeze–thaw cycles. Constr. Build. Mater. 2021, 291, 123374. [CrossRef] Pawluczuk, E.; Kalinowska-Wichrowska, K.; Jiménez, J.R.; Fernández-Rodríguez, J.M.; Suescum-Morales, D. Geopolymer concrete with treated recycled aggregates: Macro and microstructural behavior. J. Build. Eng. 2021, 44, 103317. [CrossRef] Peerzada, M.; Naqash, J.A. Amelioration of freeze thaw damage of concrete with multi-walled carbon nano tubes. World J. Eng. 2020, 18, 58–65. [CrossRef] Mehta, P.K.; Monteiro, P.J.M. Concrete Microstructure, Properties and Materials; McGraw-Hill Education: San Francisco, CA, USA, 2001; pp. 1–239.