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    Modification Mechanism of Combined Nanomaterials On High Performance Concrete and Optimization of Nanomaterial Content - Elsevier Enhanced Reader

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    Jounal of ding Engineesing 64 (2023) 105643 ‘Contents lists available at ScienceDirect Journal of Building Engineering ELSEVIER journal homepage: www.elsevier.com/locatesjobe Modification mechanism of combined nanomaterials on high Lae performance concrete and optimization of nanomaterial content Xiaogi Du", Yanlong Li®’, Binghui Huangfu”, Zheng Si*, Lingzhi Huang *, Lifeng Wen“, Meiwei Ke® * sae Ke Labora of yds a Noes Ard Region of China, an Unvsiy of Tela, Xan, 72048, China ° Sean Wane Reirces and Hydrelerc vegan & Design hate Ca,L, China « Sham Xt Wee Eclogeal Group Ca Utd china ARTICLE INFO ABSTRACT Komente ‘With the increasing quality of concrete constuction, che vequtements for conetete performace High pesfrmance concrete have also giacially increased. n this paper, the effect of nanomaterials on concrete performace Nanomateria ‘was investigated by incorporating nanomavetals(nano-Si0, and nano-Fe,0s) into conerete to concrete performance prepate high performance concrete (HPC). The optimum content of nanomaterials was deter Response surface opemizaion nee mined by response surface method (RSM), whieh revealed the influence mechanism of nano- matciial on concrete petformance. Results showed that adding nanomaterials remaskably enhanced the mechanical properties of concrete. When the dosage of nano-SiOa Was 3.54% and the dosage of nano. FeO was 4.24%, which was the optimum dosage of nanomaterials. Concrete ‘with this dosage had compressive, spliting tensile, and flexural stength of 67.27 MPa, 8.05 MPs, and 9.50 MPa, lespectively. The neo types of nanomaterials can achieve excellent coupling efect. Nano SiO, acted as an ausiliary cementing material, and nano FeO, accelerated the hydration reaction rate of cementing materials. According fo the mictostructure of nanoconerete, ener sy dispetsive specttometer (EDS) elemental analysis and thermogravimetry analysis (TGA), i was concluded that the incorporation of nanomaterials cannot produce new Kinds of hydvation products in conesete but ean produce mote hydiation products. These results can seve as theo Tetial seference for HPC preparation 1. Introduction ‘With the high speed development of the water conservancy industry, the requirements for the performance of hydraulic concrete are gradually improving. The construction of water conservancy project differs from that of conventional project. The force of water ‘conservancy project is more complicated, which requires high stability [1]. Meanwhile, avoiding the adverse effects of seepage on the stability of the building Is necessary [2,5]. Therefore, to ensure the quality of hydraulic engineering, high performance conerete (HPC) is the current development trend of hydraulic concrete, HPC has good mechanical properties, The application of HPC can significantly Improve the bearing eapacity of the dam, extend the service life, reduce the amount of concrete, and reduce the project cost [4,5]. HPC ‘also has high workability in the fresh state to achieve the effect of no initial cracks and low permeability after hardening [6]. HPC is ‘extensively studied, and the fields involved are relatively wide (7,8) Sone mineral powder can be incorporated into concrete to prepare HPC [9]. Among mineral powder admixtu for concrete, = Conesponding auhoe mal eden liyalong@xau.eduen (Y. Ui). _nps//dol.org/10.1016/3jobe.2022.105648 Received § October 2022; Received ia revised fo1m 18 November 2022: Accepted 28 Noveatber 2022 Available online 1 December 2022 2352.7102/0 2022 Elsevier Led All rights reserved. X Ducal Journal of Bune Brainerne 64 (2023) 105648 ‘nanomaterials are increasingly being favored by researchers. Nanomaterials are known as new materials in the 21st century [10]. The electronic structure of their interior surface and the erystal structure have undergone tremendous changes due to their small size ‘compared with the corresponding macroscopic material, with a macroscopic material having incomparable stall size effect, surface effect, quantum effect, and macroscopic quantum tunneling effect [11,12]. Therefore, nanomaterials can effectively improve the meclnieal properties of concrete. With the reduction in che manufacturing cost of wanomaterials, thelr application flelds can become more extensive. Particularly, in the production of auxiliary cementitious materials, nanomaterials have been regarded as a promising research direction [1], which ean improve the mix design and performance of conerete [14,15]. 1 provides a breakthrough in ma: terials for HPC preparation, Research shows that incorporating nanomaterials into HPC production could improve its workability and mechanical properties [16-16], At present, the main nanomaterial incorporated into HPC is nano-SiOs, Compared with other mineral admixtures, nano-Si0 has obvious advantages in improving the strength of conerete. For instance, compared with the addition with silica fume, the addition ‘of nano-Si0> could increase the early strength by two timtes [19]. This is due to nano-Si0y’s large specific surface area, which eam accelerate early hydration and inezease the an.ount of hydration produets [20,21], Moreover, nao SiO, asa filler in the cement mateix ‘can reduce the porosity of concrete, debase the erosion of harmful ions, and improve the performiance of concrete [22,2]. According to the workability test of fresh concrete, Givi et al. [24] demonstrated that the nano-Sid» content obviously influences the slump of ‘concrete when the water-to-binder ratio remains vnchanged and nano-SiO. reduces the sump. To maintain the workability of con: crete, a large amount of water needs to be added during concrete mixing. Salemi et al. [25] found that after incorporating an appropriate amount of nano SiO» into concrete, the compressive strength increases by 30%, Liet al, [26] demonstrated that nano-SiO, incorporation ean evidently enhance the flexural strength and fatigue life of concrete, but the flexural strength gradually deereases ‘with inereased nano SiO. Veerendrakumar etal. [27] analyzed the effect of incorporating nano-SiO, on the mechanical properties of concrete. Results showed that the compressive strength obviously improves after incorporating 5% nano-SiO>, Het al. [28] found that the penetration depth of water into concrete is significantly reduced, and the microstructure of the interface transition zone (ITZ) becomes denser by incorporating the right amount of nano-SiOs, Kong et al, [29] found that nanoconerete has good resistance to chloride penetration by incorporating nano-SiO2 into concrete. Liet al. [30-82] analyzed the effect of incorporating nano-Si02 on the properties of concrete, They found that nano SiO» particles are small and have hiigh specific surface area, which can improve grain gradation in concrete. In rermis of nano-Fe20s, Li et al (33) found that a higher nano-Fes0s content corresponds with stronger com ‘rete, The compressive strength of concrete can increase by 264% when the content of nano-Fep0 is:3%, Khoshakhlagh etal [34] found that when the water-to-binder ratio is 0.4, the incorporation of 1%-5% nano-FezOs significantly improves the mechanical properties of| self compacting concrete at all ages, and the maximum enhancement effect is 93.75%. The optinvum nano-Fe0s content is 43 Liet al: [85,86] found thet when the water-to-binder ratio is 0.5, the compressive strength of concrete increases by 3.7% when 10% nano- Fe,0s Is incorporated. Hovrever, the optimum content of nano-Fe.03 is 3%. Wu et al. [37] investigated the influence of nano-Al0s, rnano-CuO, nano-MgO, nanoFe;O4, and nano-Fe0s on the mechanical properties of cement based materials. Results show that nanometer oxides can improve the flexural and compressive strength of cement-based materials. However, compared with other ‘nanomaterials, nano-e;0 has a higher surface activity on the mechanieal properties of eoncrete greater impact. In terms of combined nanomaterials, Riahi et al [38] found that incorporating 2% nano-Si0z, nano-CuO and nano-AlzQg into concrete indifferent curing media (water and saturated lime water) increases the compressive strength of concrete. When cured in water, the compressive strength ‘of concrote increases initially and then decreases with increased content of nanomaterials. The compressive strength of eonerete gradually increases during saturated lime water curing with increased content of nanomaterials. Meamshile, compared with nano-CuO ‘and nano-AlsOs, nano-SiO2 can improve the mechanical properties of concrete more effectively. Mastali et al. [39] found that incorporating 1% nano.SiO2 and 7% sila fume into self-compacting concrete can improve Its impact resistance and mechanical properties. Jalal etal. [40] investigated the effect of two materials on the rheological and mechanical properties of self-compacting ‘concrete by incorporating nano-SiOz and silica fume. Results show that when the nano-SiO, content is 10% and the siliea fume content is 2%, the theological and mechanical properties of concrete improve significantly. ‘The effects of single incorporated nano SiQ2, single incorporated nano-Fe,03 and nano-SiO» combined with other nanomaterials on the properties of conerere have been extensively studied. However, the optinnim nanomacerial content determined by different re searchers varies, and research on the effect of combining nano-SiO, and nano-Fe,0, on the performance of concrete is relatively few, Nano-Feg0s has higher surface activity than other nanomaterials and can improve concrete performance. Accordingly, this paper investigated the effects of single incorporated nano-SiO» (1.5%, 3.096, and 4.5%), single incorporated nano-Fe,0s (1.5%, 3.0%, and 4.5%), and combined nano-Si0> (1.5%, 3.09%, and 4.59%) and nano-Fe,0, (1.5%, 3.036, and 4.5%) on the performanees of concrete tduough macrophysical tests, The optimum content of nanomaterials In concrete was obtained by respouse surface method (RSM) ruult-goal optimization. The modification mechanism of nanomaterials on the performance of concrete was revealed based on scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), ad thermogravimetry analysis (TGA). The results ean serve as a theoretical basis for HPC preparation, 2. Test process 2.1, Materials: 2.11. Cement, aggregates, and admixtures ‘The cement adopts P.O 42.5 R ordinary silicare cement with a specific surface area of 330 m:7/kg, loss on ignition ratio of 2.596, ingtial setting time of 87 min, and final setting time of 270min. The sand was medium sand produced by Weihe River in Shaanxi Province, China, with particle size of 0.15-4.75 mim and fineness modulus of 2.5. The natural aggregate was a continously graded 2 X Ducal Journal of Bune Brainerne 64 (2023) 105648 ‘rushed stone purchased from Tongehwan, Shaanxi Province, China with a partile sizeof 5-20 mum, The basie properties of aggregate are shiown in Table 1, The additive was polycarboxylate superplasticizer with water reducing rate of 26%. 21.2, Nanomaterial ‘Two types of nanomaterials were incorporated in this study, namtely, nano-SIO3 and nano-FezOs. Nano-SiO; was a white powder (Pig. 16), and nano-Fe,03 was a reddish brown powder (Fig. 1(b)). The two types of nanomaterials had the characteristics of high pureness, large specific surface area, high surface activity, and easy dispersion. ‘The performance indicators of nanomaterials are shown in Table 2 2.2, Mix ratio design ‘The mix ratio design of nanoconerete was based on relevant standard specifications [41] to obtaine a group of reference mix ratio (ater to binder ratio, 0.42; water, 157.9 kg/m; cement, 376 kg/m; sand, 679 kg/m®; gravel, 1157 kg/m). The nanomaterials were miixed into the reference mix ratio (S0-FO, S = SiO2, F = Fe2Os) [421 ‘The effect of single incorporated nano-SiOz, single incorporated nano-Fe,0s, and combined nano-SiOy and nano-Fe,0s on the properties of concrete was investigated by setting three different contents, accounting for 1.5%, 3.0%, and 4.5% of the cement quality, respectively. We established 16 groups of nanoconcrete mix ratios (Table 9), in which $1.5-F3.0 indicated that the nano-Si0, content ‘was 1.5% and the nano-Fe,03 content was 3.0%. 2.3. Specimen preparation Nanomaterials have the features of large specific surface area and easy agglomeration. Therefore, nanomaterials should be dispersed before they are incorporated into the mixture, The specific measures are as follows. First, the nanomaterials to be incor porated were evenly mixed with water. Then, the suspension was stirred with magnetic stirring for 1 min, Finally, the nanoparticle suspension was ultrasonically crested for 30 min to reduce nanomaterial agglomeration [43]. When the nanoparticle suspension was allowed to stand for more than 24 h, the nanoparticles gradually precipitated and agglomerated, and the upper liquid became clea. ‘Therefore, when preparing nanoconcrete, allowing the nanoparticle suspension to stand for too long was critical to avoid. ‘The nanoconerete preparation method was essentially the same as that of ordinary concrete. Nanoconerete specimens were pre pared and cured according to relevant standard specifications [44]. The specific manufaeturing steps of nanaconerete specimens were as follovis. (1) The mixer was londed with sand, gravel, and cement and mixed for 2min (2) The nanoparticle suspension and water ‘were poured into the blender and mixed for about Smin (9) The slump experiment was conducted on concrete to determine its ‘workability [45]. (4) The mixture was filled into the mold and vibrated on a vibrating table. (5) The vibration specimens were placed in the external environment for 24 before demolding. (6) The prepared specimens were cured for 28 dina stancard curing enviroment (20°C curing temperature and 95% curing umidity). In tls experiment, sixteen groups of nanoconerete were produced based on the mix ratios (Table 8) 10 investigate the effect of rnanomaterial content on concrete performance. 24, Test methods According (0 the GB/T 50081-2019 specification, the compressive strength of nanoconcrete was calculated [46]. The cube nnanoconcrete (150 x 150 x 150 mm°) was taken out for compressive strength test after 28 days of curing in a standard curing room, During the cest, te now-pouring surface of the nanoconcrete was placed at the center of the pressure plate of the universal testing machine. The loading speed was set to S KN/s. The mean of the three spocimens was taken as the compressive strength of this group. ‘The GB/T 50081-2019 specification was used to determine its spliting tensile strength [46]. The eube nanoconerere (290 x 150 x 150mm!) was taken out for spitting tensile strength test after 28 d of curing in a standard curing room. The loading speed was ser to 0.5KN/s. The mean of the three specimons was taken as the splitting tensile strength of this group. ‘The flexural strength of nanoconcrete was determined on the basis of relevant specifications [46]. The nanoconerete (100 x 100 x 400mm:) was taken out for flexural strength test after 28 days of curing in a standard curing room. During the test, the hon-pouring surface of the nanoconerete specimen was placed atthe center of the pressure board of the universal testing machine (0 ‘ensue that the two positioning lines in the middle of the specimen coineided with the two upper steel bars, and two locating lines ‘outside of the specimen coincided with the two lower steel bars, Then, the flexural strength test was performed. The loading speed of the flexural strength test was 0.2 mni/min. The flexural strength of this group of concrete was determined to be the average ofthe three specimens. The calculation formula was as follows: am bie h o ‘where f isthe flexural strength (MPa), isthe fathure load of specimen (N), lis the span between supports (mm), 1 = 3b, bis the section Tbe 1 Properties of astepatee. ‘Auwegate category ‘Bulk density kg/m") Appatent easy w/a) Clusbindex (90) Water coment (@)___ Mua content) ‘Conse egeregate 1390 2788 7 085 08 X Ducal Journal of Bune Brainerne 64 (2023) 105648 @ ) Fig. 1. (6) Nano S02 (8) Nano Fe.Os ‘able? Pesformance lndleetors of nanomaterials Nenomaicials Aveige paride Palenes@) Speciiesuisceaica(a/ Buk dauiyig? _—Datyig/ Gaal fomm/ensul sae 2 a) ee) phase NenosiO; 200m 999 240 006 2a ‘Sphevieat Nano FeO, 20am, 999 30 036 54 Phase ‘Tables Mix rei umber ‘ane S102 (6) Nano F050) Superpascian (8) stun (a) ‘00 ° o rr 170 soon a0 6 oat 162 S45 F0 45 6 28 169 sons: ° 18 0.22 m1 0-790 ° 30 a2 169 S05, ° 45 023 166 S15i5 15 15 025 178 Sons a0 1s 2s mn 30780 a0 30 a2 Ww S0RS a0 45 025 ye S45FIS 45 18 2s 78 ‘width of concrete (mm), b = 100mm, and ft is the section height of concrete (mm), it = 100mm, ‘The microstructure of nanoconerete was examined by SEM, chemical elements were studied by EDS, The large specimen must be eut due to the small size of the specimen used for SEM observation. The huge specimen was divided into smaller ones (44% 4 mm®) for this test. To avotd SEM contamination, the sample surface had to be cleaned before observation. The cleaning sample was processed with spray gold and vacuum to improve the observation, and SEM was performed to examine the sample ricrostructure [47]. Finally, the chemical element was investigated by EDS to reveal the influence mechanism of nanomaterials on ‘concrete performance. ‘The hydration products of nanoconcrete were quantitatively analyzed by TGA to better understand the influence of different nanomaterials on the hydration produets of conerete. TGA of concrete was performed in saturated nitrogen, and the mass Toss of ‘conerete was obtained by heating from 50°C to 1000°C at a rate of 20 °C/min, 3. Results and discussion 3.1. Workabilty ‘The slump of conerete typically serves as @ measure of its workability. According co the actual project, the conerete slump is Set berween 160 mm and 180 mm to meer the conerete construction requirements [49,49]. The incorporation of nanomaterials lessens the ‘hump of the conerete [12,16,42,50). As the amount of nanomaterials increases, she slump progressively decreases, Nano-particles have a large specife surface area, and incorporating them into conerete increases the amount of water requited to wer the pack: age, thereby reducing the amount of water needed to wrap the cementitious material [42,51]. Conerete has poor workability and fluidity. inthis test, the slump of nanoconcrete ranged within 160 mm-180 mm by varying the superplasticizer amount. The fluidity of ‘concrete gradually increased with ineroased superplasticizer dosage. This result was essentially in line with the eonerete workability X Ducal Journal of Bune Brainerne 64 (2023) 105648 test results obtained by Chithra et al. [52]. Consequently, the mix ratio of nanoconerete provided in this paper can serve as.a guidance for HPC preparation. 3.2, Compressive strengte The compressive strength of nanoconcrete is an important parameter to evaluate its basic mechanical performances. Table 4 shows the different mechanical properties of nanoconerete, Fig. 2 displays the compressive strength of eonerete under different nanomaterial ‘contents. The single incorporated nano-Si02 into conerete significantly improves its compressive strength compared with ordinary ‘concrete, as shown in Fig, 2. The compressive strength gradually increases with increased nano-SiO, dosage. The compressive strength (of nan0-SiOg dosages at 1.5%, 3.036, and 4.5% increased by 10.03%, 21.30%, and 35.46%, respectively, compared with ordinary ‘concrete. This finding was due to nano-SiOy's ability to react with calcium hydroxide in concrete to produce calelum silicate hydrate (C-S-# [40,59], thereby inereasing the amount of hydration products [28,54,55]. Accordingly, nano-SiO, can be used as an auxiliary ‘cementing material to significantly improve the compressive strength of concrete. The conipressive strength of conerete increased after single incorporated nano-Fe,0s, but the improvement was minimal. The compressive strength initially increased upward and then downward with increased nano-Fez03 dosage. The compressive strength of nano-Fe,03 content at 1.5%, 3.0%, and 4.5% increased by 5.51%, 7.9%, and 1.56%, respectively, compared with that of regular concrete. The reason was the high surface activity of nano~ Fe,0s that promoted the hydration reaction of cementitious materials through auileation and increased the hydration reaction speed [97,50]. When the curing age reached 284d, the hydration of cementitious materials was basically completed [40]. The ability of nnano-Fe,0; to promote the hydration of cementitious materials did not significantly ineresse the amount of hydration products ‘Therefore, the nano-Fe,Os content had little effect on the compressive strength. However, with inereased nano-FesOs content, the particle gradation of the conerete material significantly decreased [57], thereby further reducing the improvement effect of nano- FFe,03 on concrete compressive strength, ‘The compressive sirength of concrete was significantly improved by the combined nanomaterials. The compressive strength of ‘combined nanomaterials inereased by 19,06%-52.74% compared with that of regular conerete, Meanwhile, the influence of combined nanomaterials on the improvement in concrete compressive strength was significantly superior chan that of single incorporated nanomaterials. When the dosage of nemo-SiO was3.0% and the dosage of natto-Fe,0, was 4.5% (S9.0-F4.5), the compressive strength ‘was the greatest, i, 67.62MPa, This compressive strength was 12.76% and 42.24% higher than those of single incorporated nao SiOz with a content of 4.5% ($4.5-PO) and single incorporated nano-FezOs with a content of 3.0% ($0-F3.0), respectively. When the dosage of nano-Si0» in combined nanomaterial approached 3.0%, the strength declined but it remained much higher than that of regular concrete. This reason was that when two different types of nanomaterials were combined, neno-SiOg can serve as at auxiliary ‘cementing material [40,53], whereas nano-e203 can promote the hydration of the cementing material via nucleation [37,56]. The ‘wo types of nanomaterials played « good coupling role, increasing the content of hydration products aud improving the strength of 3.3, Splicing tensile strength “The results of the spliting tensile strength test on nanoconcrete are shown in Table 4. fig. 9 displays the splitting tensile strength of ‘concrete with various nanomaterial contents, The splitting tensile strength was greatly boosted by a single incorporation of nano-SiOo ‘The splitting tensile strength increased initially and then decreased with increased nano-SiO, dosage. The spitting tensile strength nproved by 29.459, 61.85%, and 52.15% when nano-SiO2 was incorporated at 1.5%, 3.096, and 4.5%, respectively, compared with that of regular concrete, The reason was thar the appropriate amount of nano-SiO2 as an auxiliary cementitious material for concrete Increased the amount of hydration products and splitting tensile strength [40,53]. When excessive nano-SiO was incorporated, the Table Mechanical properties of manoconcrete Number Compressive suength Spling tense sueagt leu suengt| Asai) SD(MP) CVO) ASIP) SDI) CVO) —_—AS(NPS) —SDGI) CV) 70 ar 486 rer) 026 3a 3a 016 300 Sisko 4871 a4 978 633 047 748 695 oat 302 Sur sa74 392 729 799 oat 266 8.02 0.29 262 SSR) 5897 3.06 510 744 032 430 oat 361 sisms S27 416 789 24s 028 300 020 875 SISFRO S61 $53 °7 a2 0s 638 037 419 SISRS 57.29 sat °”7 805 047 5a oat 461 S45F65 6169 349 566 893 036 03 038 394 Nowe: -S represents average song; SD represent standard dvlaon; C-V represents coffins of vavetion s X Ducal Journal of Bune Brainerne 64 (2023) 105648 z & 2 % 5 SESS menredorntgreinre hen? Site tenets SSS eee Fig. 2. Compressive strength of nsnoconerte particle distribution of concrete was severely affected, resulting in reduced splitting tensile strength [58-60]. The splitting tensile strength with single Incorporated nano-Fe,O5 increased, but only slightly. The splitting tensile strength gradually inereased with increased nano-Fe,0s dosage. When the nano-Fe,0, dosage was 1.5%, the spitting tensile strength was 4.86 MPa, which was basically the same as that of ordinary concrete. The splitting tensile strength improved by 7.169 and 10.22% when nano-Fe,0s was incor: porated at 3.0% and 4.5%, respectively, compared with that of normal conerete. This finding was due to the gradually increased promoting effeet on the hydration reaction of cement with increased nano-Fez0s dosage [97,5661], resulting in increased splitting Tensile strength. However, when the curing age reached 284, the cement hydration was basically completed (62). When nano-FesOs ‘was incorporated into eonerete, the amount of hydration products only slightly increased, Therefore, the splitting tensile strength increased only slightly ‘The splitting tensile strength significantly increased when two types of nanomaterials were combined. The effect of double incorporated nsnomaterials on splitting tensile strength was clearly superior to that of single incorporated nanomaterials. The splitting tensile strength was 9.17 MPa when the dosage of nano-Si02 was 3.0% and the dosage of nano-Fe0s was 4.5% (S3.0-F4.5), respectively, which was 16.22% and 70.13% higher than that of single incorporated nano-SiO2 content of 3.0% ($3.0-FO) and single incorporated nano-Fe03 content of 4.5% (S0-F4.5), respectively. When the dosage of nano-Sidg in double incorporated nan materials exceeded 3.0%, the splitting tensile strength decreased but remained remarkably higher than that of regular concrete. This finding can be explained similarly to the change in compressive strength, Nano-SiO, ean be used as auxiliary cementitious material to increase the hydration products content of concrete [63,644], whereas nano-Fey02 can improve the hydration reaction rate of ‘cementitious materials through nucleation [37,61,65]. The two types of nanomaterials exerted an excellent coupling effect to inerease the spliting tensile strength. Swe s Fig. 2, Spliting tose stength of nnoconcrets 6 X Ducal Journal of Bune Brainerne 64 (2023) 105648 94, Flexural strength ‘The flexural strength of nanoconerete is key indicator of eonerete structure that can accurately mirror the flexural and censile performances, The results of the flexural strength test on nanoconerete are shown in Table 4. The flexural strength of concrete with varying nanomaterial dosage is presented in Fig. 4, Pig, 4 depiets that single incorporated nano-Si0g can greatly increase the flexural strength. The flexural strength gradually increased with increased nano SiO dosage. When the nano-SiO. content was 1.5%, 3.0% and 4.5%, the flexural strength was 30.159, 50.19%, and 60.86% greater than that of regular conerete, respectively, The reason was that the proper amount of uano-SiO remarkably increased with the amount of hydration products inside the concrece and thus the flexural strength [40, 53,66]. When excessive nano-Si02 was incorporated, the particle gradation of concrete was seriously affected, resulting in decreased rate of flexural strength growth (67,68). As with the compressive and splitting tensile strength of nanaconerete, the flexural strength improved somewhat when nano-Pe05 was single incorporated to the conerete. The flexural strength inereased by 4.68%, 11,6196, and 13.11% when nano-Fe,03 was incorporated at 1.5%, 3.0%, and 4.5%, respectively, compared with that of normal concrete. This finding was due to nano-Fe,03 being able promote only the hydration of cementitious materials and accelerate the hydration reaction speed [37,56,61,67]. After the curing age of 28d, the coment hydration was basically completed [40,62]. Nano-Fe20. promoted more thorough hydration of cementitious materials and increased the amount of hydration products. However, the increase in hyération products rarely led to a small increase in its flexural strength. ‘The Mexural strength of conerote significantly improved hen two types of aanomaterials were incorporated. Meanwhile, the effect ‘of double incorporated nanomaterials on the flexural strength was significantly greater than that of single incorporated nanomateral When the dosage of nano-SiQ2 was 4.5% and the dosage of nano-Fe,03 was 4.5% (S4.5-F4,5), the flexural strength was the greatest, with a value of 9.89 MPa, which was 15.1396 and 63.749 higher than that of single incorporated nano-SiO. dosage of 4.5% ($4.5-FO) and single incorporated nano Fe,03 dosage of 4.5% (S0-F4.5). This finding was similar co the change in compressive and splitting tensile strength. In other words, the coupling effect of combined nanomaterials significantly Increase the flexural strength of eoncrete 35, Relationship between different mechanical properties ‘Numerous scholarshave obtained the mechanical properties of different types of concrete through experiments and then associated. them together to derive the functional relationship between different mechanical properties of conerote [69-72]. This research method ccan effectively reduce the cost and time ofthe test. The relationship between compressive and spliting tensile strength, as well as ‘compressive and flexural strength of nanoconcrete, are displayed in Fis, 5. Fig. 5 depiets a good correlation between the compressive and splitting tensile strength of nanoconerete, as well as between the ‘compressive and flexural strength, This finding was consistent with the change rule berween different mechanical properties of fiber reinforced recycled aggregate concrete obtained by Du etal. (49]. Thus, the spitting tensile and flexural strength of nanoconcrete can be inferred from its compressive strength an had high reliability. Meanwhile, the slope of the linear equation between compressive ‘and spliting tensile strength of nanoconerete was the same as that berween compressive and flexural strength, This esult showed that ‘when nanomaterials were incorporated into concrete to improve the compressive strength of concrete, the splitting tensile an flexural strength also linearly increased, and the increase speed was essentially the same, Therefore, a linear function can be used to describe the relationship between the compressive and splitting tensile strength of nanoconerete, as well as the compressive and flexural strength. The specific functional relations were y; = 0.19 ~ 3.34 and yp = 0.19x ~ 2.44, respectively. 3.6, Microstructure analysis ‘To investigate the effect of nanomaterials on the microstructure of concrete, the microstructure of hardened concrete specimens ($0-F0, $3.0.F4.5, and 84.5 F4.5) was observed by SEM. The observations of these specimens are shown in Fig. 6, Fig. 6(a)-(€) show lexus strengh (MPa) 8 POPPA, Siere Seleraioragie? SOS IE PS Fig. 4, Flexural strength of nanoconcree X Ducal Journal of Bune Brainerne 64 (2023) 105648 fo : » go] nmmametingatt 7 i g z BY sons on Par fed g wow sg . Sa t "4 : H ‘ i a , o & & 8 @ «Ww Compressive strength MPs) Fig. 5, Relationship between diferent meshanial properties of nanoconcet, the observation results of the ITZ becween aggregate and mortar at 500 x magnification to evaluate the bonding effect of the ITZ. According to the observation results, the microstructure in the ITZ of $3.0-F4.5 was denser than that of SO-FO and S4.5-F4.5. In terms ‘of the number of eracks, SO-FO had the most, followed by $4.5-F4.5, and 53.0-F4.5 had te least. n ters of crack size, SO-FO had ‘wider micro cracks ia ITZ and cement paste matrix, followed by $4.5-F4.5, and $3.0-P4.5 had che natrowest. Therefore, adding an appropriate amount of nanomaterials was considered to be helpful in improve the bonding effect of the ITZ, However, ifthe content of nanomaterials was too large, itcould adversely affect the bonding effect ofthe ITZ. The reason was thatthe incorporation of nano-SiO increased the amount of hydration products in conerote [40,53], whereas nano-Pe0 played a role in promoting the hydration re action, helping to accelerate the hydratfon reaction speed [37,56,611. The two types of nanomaterials exerted an excellent coupling effect at an appropriate content, generating more liydration products to improve the bonding effect ofthe ITZ. [22,28]. However, the ‘excessive content of nanomaterials led to insufficient space required (0 generate hydration products, which adversely affected the hydration reaction of cementitious material [73]. Meanwhile, the incorporation of excessive nanomaterials results in difficult dispersion and affected the particle gradation of concrete [74], Therefore, the ITZ showed a slight erack and a reduction in the binding effect. ‘ig. 6(4)-() show the observation results of hydration products of nanoconcrete at 3000 % magnification to evaluate the micro: scople pores and the compactness of hydration produets. Although the control specimen (S0-FO) produced a certaln amount of hy: ration products under the action of cement hydration, numerous microscopic pores remained (Fig. 6 (4)). When nanomaterials were incorporated, the hydration prodnets increased and the number of microscopic pores decreased (Fig. 6(€) and (®). However, ifthe content of nanomaterials was too large, the hydration products decreased and the number of microscopic pores increased (Fig. 6 (). “Therefore, in terms of the compactness of hydration products, thar of S3.0-F4.5 was the best, followed by that of $4.5-F4.5, and that of S0-FO was the worst. In terms of the number of mieroscopie pores, $3.0-F4.5 had the least, followed by S4.5-F4.5, and $0-FO had the most. This finding demonstrated that explaining the two types of nanomaterials had a strong coupling effect. The incorporation of an appropriate amount of double incorporated nanomaterials into concrete can generate more hydration produets to form an imper meable gel network [24,75,76]. Meanwhile, an appropriate amount of nanomaterials ($3.0.F4.5) can also fil the remaining micro scopic pores in the concrete. However, excessive nanomaterials can affect the particle gradation of conerete and the generation of hydration products, thereby increasing the internal pores [52,58], 4. Optimization of nanomaterial content 41. Model building ‘The above test results showed that the amount of nanomaterials added to achieve the maxinium value of different properties of nanoconcrete varied. In other words, when the dosage of nano-SiO was 3.0% and the dosage of nano-Fez0s was 4.5% (S9.0-F4.5), its ‘compressive and splitting tensile strength were the largest. When the dosage of nano-SiO, was 4.5% and the dosage of nano-Pe 05 was 4.5% (S4.5-F4.5), the flexural strength was the maximum, Therefore, Investigating the simultaneous maximization of different properties of concrete with the same nanomaterial content was necessary to determine the optimum nanomaterial content. ‘The current extensively applied optimization design methods include orthogonal design method snd factor design method [77] Although these methods can identify the direction of the next optimization, it cannot quickly identify the optimization area by sgraphies. The response surface method (RSM) can take the response ofthe system as a function of one or more factors and use graphical skills to depict this functional relation so that the optimum solution can be observed visually [78]. In addition to obtaining a continuous functional relation [7°], the RSM can investigate the interaction between different factors [49]. Compared with the previous optimization design methods, the RSM has more obvious advantages. Therefore, the RSM was applied to optimize the content ‘of nanomaterials in this paper. ‘The RSM was used to build the mathematical model between the nanomaterial dosage as a factor and the different properties of nanoconcrete asa response indicator. The models for diferent properties of nanoconcrete are shown in Eqs. (2)-(4). Table 5 plots the X Ducal Journal of Bune Brainerne 64 (2023) 105648 Sens co euitenty ees Ce eect mawiification oe ae ay . (c) S4.5-P4.5 specimen at SO0x (€) $3.0-F4.5 specimen at 3000x (1) S4.5-F4.5 specimen at 3000x ig 6, Seb of conc Tables Fetes and level of ranoconcet, Facor Coe lel Nano Si0s dosage x ° 13% 308) 45% Nano FeO snge y ° 136 30% 1596 X Ducal Journal of Bune Brainerne 64 (2023) 105648 factors and level settings for nanoconerete, 33—187X + 119 + L.23KY + 356K 40.66 o4siey + o24xv* 084%" 0.207" 7 51 +206% + 0.407 + 0.03xY —0.32x* — 0.08 @ 5.264219 poy -021xY —0.73x2 + 0.2097 a = 0.04N°Y —0.01XY? + 0.09X" — 0.037" ‘where My, Ma, and Mg are the prediction of compressive, splitting tensile, and flexural strength models of nanoconcrete, respectively. (MPa); X is the nano-SiO2 dosage (96); and Y is the nao-Fe20s dosage (90), 42. Mode inspection ‘The ANOVA results of Mf. MB, and Mare plotted in Table 6, The prominence ofthe model was decided by the F-value test (79) In ‘other words, a higher P-value and a lower P-value corresponded with a more prominent model. Table 6 displays thatthe F-values of models Mj, Mp, and Ms were 31.12, 92.98, and 75.39, respetively, and the corresponding P-values were all less than 0.0001. This finding expressed thet the three models had high prominence and statistical significance. The P-values inthe lack of fit were greater than 0.05. 8 other words, the proportion of abnormal error betwoon the three models ad the actual ficing was smal, andthe R1cing accuracy of the model was extremely high, which can well describe the relationship between the dosage of nanomaterials and the performance of concrete ‘The fing accuracy statistics ofthe model is plored in Table 7.The R2, Ray, and RR, oF models My, Ma, and Ms were il else 10 1, and the difference between the corresponding Ri, and R,. was es than 0.2 The coefficients of variation (C.V) were al ess than 1036, and theadeq precision (A.P.) was much greater than 4 [49,78]. This finding showed thatthe three models had high iting accuracy and sll error with the actual data points, and they can be used forthe subsequent optimization of nanomaterial dosage ‘The RSM model and contours ofthe mechanical properties of nanoconerete are shown in Fig. 7. The mechaniesl performances of concrete dramatically increased with increased nano-SiO» dosage. However, with inereased nano-Fe,0s dosage, the mechanical properties slightly changed. This finding demonstrated that the influence of nano-Si0z on concrete performances was much greater than that of nano-Fe05, tn terms of mechanieal properties of concrete, dhe combined nanomaterials were abviosly superior to tha of single incorporated nanomaterials, This finding indicated that double incorporated nano-Si0, and nano-PezOs can exert & good coupling effect to improve concrete performance 4.3. Mul goal optimization ‘The craving function was used to optimize the nanoconcrete performance based on the RSM model, The optimization goal was to seek the ideal dosage of nano-SiO, and nano-Fe,0s to maximize the different properties of nanoconcrete atthe same time. Assuming that the desired value b, ofa single goal was berween 0 and 1.0, when the desired value ofthe j — eh target was within this range, then > =1. When this target was outside this range, then Dy =0. The algorithm of the naxinnum value ofthe target by is displayed in Eq. (9) ‘The craving function @ is the product ofthe power exponent of the maximum Value of each target, as displayed in Eq. (6). Multi-goal ‘optimization was used to maximize Q. Each optimization goal and boundary scopes are displayed in Table 7

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