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Article

Enhancing Metakaolin-Based Geopolymer Mortar with Eggshell Powder and Fibers for Improved Sustainability

Department of Civil Engineering, Faculty of Engineering, University of Van Yüzüncü Yıl, Van 65080, Turkey
Buildings 2025, 15(14), 2526; https://doi.org/10.3390/buildings15142526
Submission received: 26 June 2025 / Revised: 10 July 2025 / Accepted: 13 July 2025 / Published: 18 July 2025
(This article belongs to the Section Building Materials, and Repair & Renovation)

Abstract

This research explores the effectiveness of eggshell powder (ESP) and polypropylene (PP) fiber in geopolymer (GP) mortars. It examines how various doses of ESP, ranging from 0% to 25%, and two volumes of PP fibers, at 0.1% and 0.2% (by volume), impact the workability, mechanical and physical characteristics, and microstructure of GP mortars. Assessments were made for workability, apparent porosity, water absorption, and flexural and compressive strengths, along with microstructural evaluations. Using ESP as a substitute for metakaolin (MK) at 15% and 25% (by weight) improved the flexural and compressive strengths by 22.9%, 22.5%, 37.1%, and 50.7%, respectively. Using PP fiber resulted in flexural strength improvements of up to 97%. These findings deepen the understanding of ESP’s potential as a partial replacement for MK in geopolymer mortar, provide insights on material enhancement, and demonstrate superior mechanical and durability properties.

1. Introduction

During the production of cement used in concrete, an average of 0.80 to 0.95 tons of CO2 is released into the atmosphere per ton [1]. It is reported that the cement industry is responsible for 5–7% of the amount of CO2 released into the atmosphere [2]. The rising levels of CO2 in the atmosphere harm all living beings and lead to numerous negative environmental consequences, particularly greenhouse gas. For this reason, researchers have developed geopolymer (GP) concretes that can be produced without the use of cement. These concretes are obtained by activating an aluminosilicate source used as a binder with alkali activators [3]. GP concretes have gained prominence in recent years as an environmentally friendly alternative to traditional concrete due to the limitations of cement use. Industrial wastes such as fly ash (FA), granulated blast furnace slag (GGFS), and metakaolin (MK) are commonly used in the production of GP concrete.
In recent years, GP concretes have been produced using various binders, and their properties, including their mechanical properties, physical properties, and durability, have been investigated [4]. Researchers have recommended curing geopolymer concretes made with FA and MK in an oven at temperatures ranging from 50 °C to 140 °C [5]. In addition, recent reports have indicated that GP concretes and mortars can gain strength within 1–2 min by using microwave curing [6,7]. Unlike concretes produced using cement, GP concretes have advantages over traditional concretes because they can set and gain strength quickly, as mentioned above. Apart from this, GP concretes are more economical, can be produced with low energy consumption, are more thermally stable, and can be made with waste materials, making them quite environmentally friendly [8].
MK is produced by calcining kaolin at temperatures ranging from 500 to 900 °C, and it can be used to make GP concrete due to its high silica and alumina content [9]. MK demonstrates superior bond strength to other binding materials, producing GP [10]. When studies on GP concretes produced using MK are examined, it is seen that researchers have obtained higher compressive strengths of MK-based GPs compared to mixtures using cement [11]. It is reported that compressive strengths of 100 MPa can be achieved with GP concretes produced using MK [12]. It has been stated that workability decreases in MK-based GPs. It has been reported that this behavior is due to MK being thinner, and its internal structure consists of plate-like shapes [13,14]. Pouhet and Cyr [15] stated that the total porosity values of GP concretes obtained using flash MK varied between 10.5% and 18.9% for an average density of 2180 kg/m3. The researchers also stated that the effect of total porosity on mechanical properties in GP concretes was negligible.
Utilizing waste materials as binders in conventional and green concrete production is significant for waste utilization. In addition to industrial wastes such as ground granulated blast slag (GGFS) and fly ash (FA), eggshell powder (ESP), a byproduct of egg production, has also attracted the attention of researchers due to its high calcium content. ESP generally contains around 94% CaCO3, and it is stated that when used as an alternative to cement, it accelerates hydration and provides early strength gain in concrete [16,17]. Considering that an average of 10,000 million eggshells are produced annually in India alone [18], using ESP instead of cement not only enhances the mechanical properties of concrete but also aids in waste disposal.
Workability in concrete decreases when ESP is used instead of cement [19]. This behavior results from ESP absorbing the mixing water [20]. Researchers state that using ESP increases the compressive strength of concretes up to a specific rate and decreases it after this optimal value. Many researchers have noted that using more than 10% ESP reduces the compressive strength of concrete [21,22]. Parthasarathi et al. [18], in a study where ESP was used at 5, 10, and 15% instead of cement, stated that the compressive strength of concrete also increased with increasing ESP dosage. In addition to using ESP alone in concrete production, studies have also been conducted on its use with waste materials, such as GGBS and FA. Gajjar and Zala [23] reported that compressive strength improved by 33–35% with 5% GGBS and 15% ESP in their study, where they used GGBS and ESP together.
On the other hand, the use of fibers in GP mortars and concretes creates a bridging effect, which limits crack formation and propagation. Polypropylene (PP) fibers resist harmful chemicals, such as acids and alkalis, and are frequently used in conventional concrete and GP applications [24]. As mentioned above, PP fibers prevent the spread of micro- and macro-cracks and reduce concrete permeability. Thus, a more compact internal structure can be obtained. In addition to the improvements mentioned, it is reported that the use of PP fibers increases impact resistance in concrete [25], improves durability [26,27], and provides abrasion resistance [28].
MK-based GP concretes are a type of concrete that can replace cement-based concretes, producing a more environmentally friendly solution. Researchers have utilized MK in GP concrete/mortar production, and it is reported that PP-fiber-reinforced ESP in GP concrete/mortar production remains an area that has not been sufficiently researched. It is seen that there are a limited number of studies related to GP concretes produced using ESP with different binders [29,30,31,32]. However, there is limited information about the use of fiber in these studies. The investigation of the usability of ESP, a biological waste, in GP concretes is crucial, as it enables waste disposal and reduces dependence on traditional binders. Based on the deficiencies explained in the literature, this study aims to examine the physical and mechanical properties of geopolymer mortars produced using PP-fiber-reinforced MK and ESP. For this purpose, geopolymer mortars were made by replacing MK with ESP at 0%, 15%, and 25% of the binder weight. In addition, PP fibers were added to the GP mixture at 0.1% and 0.2% (by volume) to investigate the effect of PP fibers on GP mortars’ properties. The spreading table, water absorption, porosity, flexural, and compressive strengths of GP mortars were investigated. Additionally, the internal structures of the selected samples were examined using a scanning electron microscope (SEM).

2. Test Materials and Methods

2.1. Test Materials

MK and ESP were used as binders to prepare GP mortars. CEN standard sand, 99.3% pure solid sodium hydroxide (NaOH), and liquid sodium silicate (Na2SiO3) were used. The chemical and physical properties of MK and ESP are shown in Table 1; their external appearances are shown in Figure 1, and their internal structures obtained with an SEM are shown in Figure 2. Standard CEN sand with a specific gravity of 2.63 and a maximum grain size of 4 mm was used to produce GP mortars. The MK used as a binder had 63.51% SiO2, while the main component in ESP was 53.4% CaO. ESPs were collected locally, washed to remove organic matter, and dried in a laboratory environment. Then, they were ground to a particle size of below 75 µm using a ball mill. The total grinding time of ESP was 5 min. Polypropylene (PP) fibers, 27 mm in length, were also used in the mixture, and their properties, as obtained from the manufacturer, are listed in Table 2.

2.2. Mix Design and Preparation

A total of 6 different mixtures were prepared within the scope of the study, including a control sample. MK replaced ESP with 0, 15, and 25% by weight. PP fibers were added to the mixture at 0.1% and 0.2% (by volume). Three samples were produced for each experiment, and the average of the results was taken. The strength and durability properties of GP concrete and mortars depend on many parameters, especially the activator/binder ratio, the NaOH molarity used, and the sodium silicate/sodium hydroxide ratio. Researchers generally state that increasing the molarity of NaOH increases the strength of GP mortars, and values between 8 and 12 are considered ideal. It is also recommended to use a Na2SiO3/NaOH ratio between 2 and 3 [33,34]. In line with the specified recommendations, the NaOH solution was prepared at a concentration of 10 M in this study, while the Na2SiO3/NaOH ratio was determined to be 2.5. The mixture ratios determined for the control and MK–ESP-based samples are listed in Table 3. In this study, low fiber dosages were used, considering that high fiber dosages could lead to fiber clustering and reduced processability, resulting in lower mechanical properties.
A solid 400 g of NaOH was added to 1 L of water to prepare the alkali activator, and the mixture was mixed at a constant speed. The NaOH solution prepared at 10 M was left to rest at room temperature for 24 h. Dry materials (MK, ESP, CEN standard sand, and fibers) were mixed in a mixer for one minute. Then, alkali activators NaOH and Na2SiO3 and extra water were added to the mixture, and mixing was continued for 2 min. A polycarboxylate-based plasticizer additive was added to the mixture with water and mixed at a dosage of 0.2% of the binder to ensure fluidity in mixtures containing fibers. After 3 min of mixing, the spreading diameters of the samples were determined and placed in the relevant molds in 3 stages. The samples were compressed using a shaking table for each stage. Then, the samples were cured in an 80 °C oven for 24 h without removing them from the molds. The samples were not placed directly in an 80 °C oven to prevent thermal shock. Instead, the samples were placed in an oven at room temperature, and then the oven was turned on and set to 80 °C. The time it took for the oven to reach 80 °C from room temperature was determined and added to the total curing time.

2.3. Testing

The spreading diameters of fresh GP mortars were measured in accordance with ASTM C1437-15 [35]. Water absorption and apparent porosity values were determined from cube samples with a side length of 70 mm, while flexural strength tests were conducted on prismatic samples measuring 40 mm × 40 mm × 160 mm. After the flexural strength tests, the fractured samples were used to assess their compressive strength. The ASTM C642 [36] standard was followed for evaluating water absorption and porosity, with calculations performed using Equations (1) and (2), respectively. Additionally, the internal structure of the samples from the selected mixtures was examined using a scanning electron microscope (SEM).
W A = W d W k W k × 100
A P = W d W k W d W w × 100
Here, WA is the water absorption rate of the GP mortars, AP is the apparent porosity, Wd represents the weight of specimens when they are in a saturated surface dry state, Wk represents the dry weight of the specimens when placed in the oven, and Ww is the weight of the saturated GP samples in water.

3. Results and Discussion

3.1. Flowability (Spreading Diameters)

Within the scope of this study, the spreading diameters (SDs) of the samples produced were measured, and their changes with increasing ESP and PP fiber amounts are reported and listed in Figure 3. While the SD value was 185 mm in the control mixture using 100% MK, the increase in ESP use resulted in a decrease of 2.2% and 4.3% in the MK85ESP15 and MK75ESP25 mixtures, respectively. In the MK100ESP0%0.1PP-MK75ESP25%0.1PP mixtures using 0.1% PP fiber, they decreased by 7.6% to 13.5% compared to the control mixture. When the fiber volume was increased to 0.2%, the MK100ESP0%0.2PP-MK75ESP25%0.2PP mixtures decreased by 16.2% to 22.7% compared to the control mixture. As can be understood from Figure 3, the SD values of the GP mortars decreased with the use of ESP. Since ESP has a finer grain structure than MK, it causes a decrease in workability [37]. In addition, the SD values decreased with the inclusion of PP fibers in the mixture. With the increasing use of fibers, they may tend to cluster and accumulate in a specific region [38,39,40]. In the MK100ESP0%0.1PP-MK75ESP25%0.1PP blends, where 27 mm long PP fibers were used at a rate of 0.1%, the SD values varied between 160 and 171 mm, while in the MK100ESP0%0.2PP-MK75ESP25%0.2PP blends, where PP fibers were utilized at a rate of 0.2%, these values were 143–155 mm. The lowest SD results were obtained in each group using 0.2% PP fibers. This results from the overlapping and agglomeration of fibers, characterized by increased fiber density. It has also been reported that a water film can form on the surfaces of PP fibers, leading to a decrease in the mixing water in GPs and negatively affecting workability [41]. Additionally, ESP typically comprises angular and uneven particles because of its brittle characteristics. This uneven structure heightens internal friction between the particles, making it more difficult for them to slide over each other and reducing the flowability of fresh concrete.

3.2. Water Absorption and Apparent Porosity

Penetration of harmful liquids into concrete causes deterioration of the internal structure of the concrete and consequently decreases its strength. Aggressive liquids (such as acids) penetrate the concrete through the voids inside it. Therefore, it is necessary to detect the voids in the concrete, determine their void sizes, frequency of formation, and connections with each other [42,43,44]. As the number of interconnected voids in the concrete increases, harmful substances can penetrate the concrete more easily and negatively affect its durability [45,46]. The WA and AP values of the samples obtained at room temperature within the scope of this study are given in Figure 4 and Figure 5, respectively. When Figure 4 and Figure 5 are examined, it is observed that the WA and AP values decrease with the use of ESP instead of MK. A tighter internal structure was obtained, and a decrease in the number of voids was achieved by using waste ESP with a finer grain structure in GP mortars [47,48]. While the WA and AP values in the control sample were 3.12 and 5.25, respectively, in the MK85ESP15 mixture in which 15% ESP was used instead of MK, these values decreased by 2.6% and 1.1% to 3.04 and 5.19, respectively. In the MK75ESP25 mixture, where 25% ESP was used, the WA and AP values decreased by 5.4% and 2.5% to 2.95 and 5.12, respectively. With the introduction of fiber into the mixture, the AP and WA values continued to trend downward. The increased fiber volume decreased both the WA and AP values in the GP mortars. These results were attributed to the fibers filling the voids in the concrete and, thereby, disconnecting the interconnected voids. While Niyasom and Tangboriboon [49] stated that WA values decreased with increasing ESP, Teare et al. [50] used ESP with 30% FA at different rates instead of cement. They reported that the WA values of the samples with 5%, 10%, and 15% ESP decreased by 3.7%, 6.2%, and 10.0%, respectively, compared to the control mixture. Zaid et al. [51] corroborated the above results by assuming that the addition of ESP reduced the WA value of the concrete and that the fibers and nano-silica used in conjunction with ESP strengthened the bond between the matrix and the fibers, thereby reducing the connections between the pores.

3.3. Flexural Strength

The flexural strengths (FSs) of the geopolymer samples are listed in Figure 6. While the control mixture, in which no ESP was used, showed the lowest FS value, increasing amounts of ESP improved the FSs of the MK-based GP mortars. Additionally, the MK75ESP25 mixture, which utilized 25% ESP, achieved the highest FS value among the samples without fibers. In the MK75ESP25 mixture with the highest ESP content (25%), the FS increased by 37.1% compared to the control, reaching a value of 4.8 MPa. With the inclusion of PP fibers in the mixture, the FS values of the samples continued to increase. While the highest value of 5.9 MPa was obtained from the MK75ESP25%0.1PP mixture in which 0.1% PP was used, the highest FS value of 6.9 MPa was obtained from the MK75ESP25%0.2PP mixture in which 0.2% PP, 75% MK, and 25% ESP were used. By increasing the fiber ratio from 0.1% to 0.2%, improvements ranging from 77.1% to 97.1% were obtained in FS values compared to the control mixture. The FS value of 3.5 MPa in the control mixture reached 4.8 MPa in MK75ESP25, where the ESP ratio was increased to 25%. When 0.1% and 0.2% PP fiber were added to the mixtures where MK was used at 75% and ESP at 25%, the FS values became 5.9 MPa and 6.9 MPa, respectively. Chen et al. [52] examined the properties of GP mortars produced by using MK and GGBS at different ratios, and they reported that improvements of up to 54.4% were obtained in FS by replacing MK with GGBS. They attributed the increases in FS values with the addition of GGBS to the fact that GGBS is rich in calcium. Canfield et al. [53] and Temuujin et al. [52] stated that the calcium content in FA components plays an active role in filling the voids in the GP internal structure by causing aluminosilicate dissolution in GP samples. Another study examining the effects of fibers used at different rates on MK-based composites [53] reported that increasing fiber usage improved the FS of GP composites. It was stated that the FS of GP composites increased by 1.9 times, 2.5 times, and 2.6 times, respectively, using bamboo fiber at 1, 3, and 5% by volume. Mashri et al. [54] reported that using ESP rich in CaO and silica fume (SF) rich in SiO2 in GP mortar production resulted in forming C-S-H gels due to alkali activation. Amin et al. [55] reported that ESP can be used as a substitute for cement in cement mortars up to 10%.

3.4. Compressive Strength

The compressive strengths (CSs) of the GP mixtures produced within the scope of the study are shown in Figure 7. It is observed that increasing amounts of ESP, as with FS, positively affect the CS values of the samples. While the CS in the control mixture was 37.5 MPa, this value increased to 47.8 MPa in MK85ESP15, where ESP was 15%, and to 56.5 MPa in MK75ESP25, where ESP was 25%. With the introduction of PP fibers to the GP mortars, improvements were observed in CS values, as for FS. In the MK100ESP0%0.1PP, MK85ESP15%0.1PP, and MK75ESP25%0.1PP mixtures, where 0% ESP, 15% ESP, and 25% ESP were used together with 0.1% PP fiber by volume, the CS values were determined as 48.6 MPa, 57.1 MPa, and 68.6 MPa, respectively. The increasing trend observed in CS values continued with the increase in fiber volume from 0.1% to 0.2%. The CS values of the A6-A8 mixtures in which PP fibers were used at 0.2% by volume varied between 62.3 MPa and 65.8 MPa. The PP fibers filled some of the voids in the internal structure of the GP mortars, causing an increase in the CS values of the samples. While Ahamed et al. [56] stated that a 25% change in CS was obtained by increasing eggshell ash (ESA) from 25 g to 75 g, Yuan et al. [29] reported that in their studies in which FA was replaced with ESP at different rates, the CS values in mixtures in which ESP was used at rates of 10% and 20% increased significantly. The researchers attributed the obtained results to the fact that ESP acts as a filler, expanding the fullness of the matrix and accelerating geopolymerization due to curing at 70 °C. It was also noted that the curing of ESP with heat positively affected the CS values of GP concretes. Shin et al. [57] stated that the CS value increased by 30% with ESP in 10% glass-fiber-reinforced composites. Moradikhou et al. [58] stated that PP fiber in MK-based GP concretes had a partially adverse effect on CS, while Ziada et al. [59] indicated that fiber in MK-based mortars increased CS. Similarly, Zhong et al. [60] noted that using fiber-filled voids in the GP prevented crack propagation, which improved CS.

3.5. Microstructure Analysis

The internal structure photographs of the selected control, MK75ESP25, MK75ESP25%0.1PP, and MK75ESP25%0.2PP mixtures are shown in Figure 8. It is observed that the internal structures of GP mortars produced entirely using MK are more porous; however, with the increasing use of ESP, these pores are filled with ESP, resulting in a finer grain structure. By using the finer ESP in GP mortars, a more compact structure is achieved, and the interface transition area is strengthened, resulting in concretes with higher strength [61,62]. It is known that the geopolymerization reaction is accelerated by the heat curing used in this study, resulting in a more complete internal structure of the concrete [63]. With the introduction of PP fibers to GP mortars, another option has been added to fill the pores in the internal structure in addition to ESP.

4. Conclusions

This study investigated the potential of using ESP, a biological waste, as a more environmentally friendly and sustainable alternative in the production of MK-based GP mortars. Additionally, the effect of incorporating PP fibers at two different dosages on the properties of GP mortars was examined. The findings are summarized as follows:
  • Workability decreased when using ESP instead of MK in GP mortars.
  • By increasing the amount of ESP, the water absorption and apparent porosity values of GP mortars decreased.
  • The use of ESP positively affected the mechanical behavior of GP mortars. In the mixture using 25% ESP, the flexural and compressive strengths increased by 37.1% and 50.7%, respectively, compared to the control.
  • The use of PP fiber decreased the workability of GP mortars, similarly to ESP. In addition, as the PP fiber dosage increased, the mortars’ apparent porosity and water absorption values decreased.
  • Increasing amounts of PP fiber usage increased both the flexural and compressive strengths of the mortars. It was observed that the flexural strengths were more sharply affected by the use of fibers, while the highest flexural strength was obtained with 6.9 MPa from the mixture in which 0.2% PP fiber was used by volume.
  • Microstructure analysis demonstrated a dense microstructure and strong bonding between components, highlighting the positive influence of ESP on the overall performance of GP mortars.
  • The use of eggshell powder in metakaolin-based geopolymer mortars stands out as a promising alternative due to the high calcium content of eggshells, as it is sustainable and cost-effective. In addition to waste utilization, the reaction mechanisms within the geopolymer matrix change when eggshells are used instead of metakaolin. With the increased calcium ions, the formation of calcium–sodium–aluminosilicate–hydrate (C,N)-A-S-H) gels is facilitated in addition to traditional sodium–aluminosilicate–hydrate (N-A-S-H) gels, depending on the activator content and curing conditions. A more dense microstructure and improved strength can be achieved with these hybrid gels formed within the geopolymer mortar.
  • These results enhance the comprehension of ESP’s potential as an environmentally friendly alternative to GP mortars, offer perspectives on material enhancement, and show better mechanical and durability characteristics. Future studies can investigate the usability of ESP in GP mortar production by using various fibers, different fiber dosages, and alternative binders.

Funding

This research received no external funding.

Data Availability Statement

Data will be made available upon request.

Conflicts of Interest

The author declare no conflict of interest.

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Figure 1. Appearances of MK, ESP, and PP fiber.
Figure 1. Appearances of MK, ESP, and PP fiber.
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Figure 2. SEM images of MK and ESP.
Figure 2. SEM images of MK and ESP.
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Figure 3. The spreading diameter test results.
Figure 3. The spreading diameter test results.
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Figure 4. WA values of the tested specimens.
Figure 4. WA values of the tested specimens.
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Figure 5. AP values of the tested specimens.
Figure 5. AP values of the tested specimens.
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Figure 6. FS test results of the tested specimens.
Figure 6. FS test results of the tested specimens.
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Figure 7. CS test results of the tested specimens.
Figure 7. CS test results of the tested specimens.
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Figure 8. SEM images of selected mixes.
Figure 8. SEM images of selected mixes.
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Table 1. The physical and chemical properties of MK and ESP.
Table 1. The physical and chemical properties of MK and ESP.
Chemical PropertiesMKESP
SiO263.510.08
Al2O330.370.03
Fe2O30.570.04
CaO0.2753.4
MgO0.160.21
Na2O0.340.17
K2O1.070.02
SO3-0.59
P2O5-0.75
Loss in ignition1.9843.5
Physical properties
Specific gravity (g/cm3)2.542.15
Specific surface area (cm2/g)11762960
Table 2. Properties of PP fibers.
Table 2. Properties of PP fibers.
PP FiberCharacteristic Features
Density (g/cm3)0.91
Length (mm)27
Diameter (mm)0.95
Tensile stress (MPa)530
Modulus of elasticity (GPa)7.2
Melting point (°C)160
Aspect ratio (l/d)28
Table 3. Mix proportions of geopolymer mortars.
Table 3. Mix proportions of geopolymer mortars.
MixesMix IDMK (g)ESP (g)Sand (g)Na2SiO3 (g)NaOH (g)Water (g)Fiber (%)
MK100ESP0Control45001350265.2106100-
MK85ESP15A1382.567.51350265.2106100-
MK75ESP25A2337.5112.51350265.2106100-
MK100ESP0%0.1PPA345001350265.21061000.1
MK85ESP15%0.1PPA4382.567.51350265.21061000.1
MK75ESP25%0.1PPA5337.5112.51350265.21061000.1
MK100ESP0%0.2PPA645001350265.21061000.2
MK85ESP15%0.2PPA7382.567.51350265.21061000.2
MK75ESP25%0.2PPA8337.5112.51350265.21061000.2
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Yavuz, D. Enhancing Metakaolin-Based Geopolymer Mortar with Eggshell Powder and Fibers for Improved Sustainability. Buildings 2025, 15, 2526. https://doi.org/10.3390/buildings15142526

AMA Style

Yavuz D. Enhancing Metakaolin-Based Geopolymer Mortar with Eggshell Powder and Fibers for Improved Sustainability. Buildings. 2025; 15(14):2526. https://doi.org/10.3390/buildings15142526

Chicago/Turabian Style

Yavuz, Demet. 2025. "Enhancing Metakaolin-Based Geopolymer Mortar with Eggshell Powder and Fibers for Improved Sustainability" Buildings 15, no. 14: 2526. https://doi.org/10.3390/buildings15142526

APA Style

Yavuz, D. (2025). Enhancing Metakaolin-Based Geopolymer Mortar with Eggshell Powder and Fibers for Improved Sustainability. Buildings, 15(14), 2526. https://doi.org/10.3390/buildings15142526

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