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Experimental study of mortar incorporating nano-magnetite on engineering performance and radiation shielding

  • Kittipong Kunchariyakun , Suthatip Sinyoung EMAIL logo , Kenneth J. D. MacKenzie , Vithit Pungkun , Pakkamai Raknarong , Musofpar Teh , Afham Jekabaso and Narumol Sittichan
Published/Copyright: February 7, 2025
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Nanotechnology Reviews
From the journal Nanotechnology Reviews Volume 14 Issue 1

Abstract

Here, this study reports the effect of nano-magnetite (nano-Fe3O4) on the γ and neutron-radiation shielding properties of mortar using 1–10 wt% additions of nano-Fe3O4. The results indicate that nano-Fe3O4 additions enhance the radiation-shielding properties of the mortar as a result of pore filling and nucleation effects. The mortar incorporating nano-Fe3O4 exhibited relatively high compressive strength values at 28 and 90 days compared to the control mixture (NFC0). A 5 wt% addition of nano-Fe3O4 provided the best physical (1,847 ± 19.1 kg m−3), compressive strength (216.79 ± 6.19 ksc at 28 days), and radiation shielding properties, increasing the photon linear attenuation coefficient to 0.155 cm−1 from 0.144 cm−1 in the material without nano-Fe3O4. This 5 wt% addition of nano-Fe3O4 also increased fast neutron removal cross-section (ΣR) of neutrons from 0.1109 cm−1 in the control sample to 0.1192 cm−1. These results indicate that the addition of nano-Fe3O4 to radiation-shielding mortar can potentially attenuate gamma rays rather than neutrons and lead to the development of materials for shielding radiation from radioactive storage facilities, thereby reducing the impact of this hazardous waste on humans and the environment.

Keywords: nano-magnetite; radiation shielding; mortar; compressive strength; microstructure

1 Introduction

Nowadays, nuclear materials are widely used in various applications such as medical diagnostics, nuclear research, nuclear reactors, and high-energy particle accelerators. All these activities eventually involve the need to store radioactive waste and protect the living from the natural radioelements [1,2,3], ideally in ways that decrease the effect of nuclear radiation. For this purpose, a number of shielding materials have been investigated, for example, building materials [4,5], polymers [6], and glass [7]. Cementitious materials, which can also include the incorporation of waste materials, have proved to be extremely popular for this application because of their ease and flexible construction method [8,9,10,11], their relative cheapness, and their ability to provide a high shielding capacity for nuclear radiation. Typically, high-density concrete (approximately 2,600–4,500 kg m−3) is specified for radiation shielding because of its excellent gamma-ray attenuation and the fact that the presence of hydrogenous materials, heavy metal elements, and other neutron absorbers in its matrix [12] will improve its ability to shield against neutrons.

From the previous literature [13,14,15,16,17,18,19], radiation shielding concrete (RSC) is a useful material by virtue of its good shielding ability, high durability, low cost, and good versatility, providing it with structural functionality that outperforms design standards [18]. More than 60% of light water reactor nuclear power plants in the United States are constructed using RSC [18]. In addition, radiation-shielding concrete is used as biological shielding in nuclear power plants, particle accelerators, medical units, and radioactive waste storage facilities [19]. In the world’s oldest nuclear industry (in the UK), about 4.9 million tons of radioactive waste is forecast to be produced by 2125 [20]. Therefore, there will be an ongoing necessity for the development of radiation shielding material to reduce the impact of nuclear radiation on living organisms and the environment.

With the advent of nanotechnology, extensive research has been carried out in the past decade into the applications of nanomaterials in various fields, including cementitious materials. The effect on the properties of cementitious materials of various nanomaterials such as nano-silica [21,22,23], carbon nanotubes [24], nano-titanium [25,26], nano-aluminum [27], and nano-Fe2O3 [28,29] has been reported. Of these nanomaterials, nano-silica had the most beneficial effect on cementitious materials due to its pozzolanic properties [30], but more recently, nano-magnetite (nano-Fe3O4) has been of interest as a nano-additive. Amin et al. [31] showed that a small addition of nano-Fe3O4 (up to 0.3%) can enhance the mechanical properties of cement and refine its pore structure. Sikora et al. [32] reported that cementitious composites containing nano-Fe3O4 showed an improvement in the compressive strength of up to 20%, while Bragança et al. [33] examined the effect of chloride and sulfate conditions on concrete containing 1% nano-Fe3O4 and concluded that the addition of nano-Fe3O4 produced a more durable cement matrix even in such highly aggressive environments. An improvement in the thermal resistance of cementitious materials containing nano-Fe3O4 at temperatures up to 600°C has also been reported [19].

An examination of the literature suggests that the addition of nano-Fe3O4 to cementitious materials is likely to result in a reduction in the porosity of the cement, leading to a higher relative density. This effect could be the key to the development of high-density concrete for gamma-ray attenuation [34]. Horszczaruk et al. [35] noted that the gamma-ray attenuation coefficient of cement pastes increased with increasing density caused by the incorporation of nano-Fe3O4. Florez et al. [36] also reported that the addition of nano-Fe3O4 in the cement paste enhanced both the compressive strength and the gamma-ray attenuation coefficient. However, the literature on the effect of cementitious materials containing nano-Fe3O4 on neutron attenuation is limited. In the present investigation, the effect of adding various percentages (1–10 wt%) of nano-Fe3O4 to mortar for radiation shielding applications was determined by studying the physical and mechanical properties as well as the microstructures of the materials and their efficiency in shielding both gamma-rays and neutrons.

2 Methodology

2.1 Materials and mix proportions

The starting materials in this study were ordinary Portland cement (OPC), river sand, water, and nano-magnetite (nano-Fe3O4). The specific gravity of the OPC was 3.13, and its chemical composition is presented in Table 1. The river sand had a fineness modulus of 2.58 and a specific gravity of 2.65. The nano-Fe3O4 (carbon nanotube materials store, CAS No. 1317-61-9) had a purity of 96.42% (Table 1) with a particle size of 50–100 nm (Figure 1a) and was characterized by Brunauer–Emmett–Teller (BET) (Micromeritics – ASAP2460), transmission electron microscopy (TEM) (JEM 2010), X-ray fluorescence (XRF) (Philips PW2400 XRF spectrometer), and X-Ray diffraction analysis (XRD) (Rigaku Miniflex 600 with Cu Kα radiation, λ = 1.5406 Å, 40 kV and 40 mA). The BET surface area of the nano-Fe3O4 was 12.763 m2 g−1, with a total pore volume of 0.0454 cm3 g−1 and an average pore diameter of 142.283 Å. The TEM micrograph (Figure 1a) shows the particles to be predominantly spherical, while the XRD of this phase (Figure 1b) contains the reflections of crystalline magnetite (ICDD database no. 01-088-0866).

Table 1

Chemical composition of the starting materials OPC, sand, and nano-Fe3O4

Compounds Concentration (%)
OPC Nano-Fe3O4 Sand
CaO 70.1 0.04 —
SiO2 15.2 0.49 96.21
Fe2O3 3.29 — 0.04
Fe3O4 — 96.42 —
Al2O3 3.33 0.01 6.21
MgO 1.89 0.97 —
Na2O — 0.18 0.56
P2O5 0.03 0.01 —
SO3 4.39 0.45 —
Cl 0.02 0.02 —
TiO2 0.21 0.12 0.05
MnO 0.03 0.73 —
ZnO 0.01 0.04 —
K2O 1.30 — 0.54
SrO 0.07 — —
H2O — — —
Figure 1 Characteristics of the nano-Fe3O4: (a) TEM micrograph and (b) XRD diffractogram.
Figure 1

Characteristics of the nano-Fe3O4: (a) TEM micrograph and (b) XRD diffractogram.

2.2 Experimental program

2.2.1 Sample preparation

The samples, containing OPC, river, sand, and nano-Fe3O4, were weighed and dry-mixed in a Hobart mixer for 1 min. The compositions of the samples containing 1, 3, 5, 7, and 10% nano-Fe3O4 by weight of OPC (designated NFC1, NFC3, NFC5, NFC7, and NFC10, respectively) and a control sample without nano-Fe3O4 (NFC0) are shown in Table 1. The preparation process of the samples is illustrated in Figure 2. Water was added to these dry mixtures before mixing again for 1.5 min. The slurry was then poured into 5 × 5 × 5 cm3 molds for the measurements of dry density, water absorption, and compressive strength according to ASTM C109 [37]. In addition, 30 × 30 cm2 molds of thicknesses ranging from 2 to 8 cm were prepared for tests of radiation transmission. After casting, the samples remained in the molds overnight before demolding and curing for 7, 28, and 90 days for compressive strength determinations using a compression testing machine, 28 days for measurements of the dry density and water absorption, and 90 days for the radiation transmission tests.

Figure 2 Samples preparation process.
Figure 2

Samples preparation process.

2.2.2 Radiation transmission tests

The representative samples chosen for these attenuation measurements were samples NFC0, NFC5, and NFC10. Prior to testing, the cured samples were dried in an electric oven at 105°C. A 0.662 MeV Cs137 gamma-ray source with 0.662 MeV was used, with a NaI (TI) scintillation detector and a multi-channel analyzer. The neutron cross-section measurements were made using a 241 Am–Be neutron-sealed source and a BF3 detector. Figure 3 shows the schematic diagram for the gamma-ray attenuation and neutron cross-section measurements.

Figure 3 Schematic diagrams of (a) the gamma-ray attenuation measurement and (b) the neutron cross-section measurement.
Figure 3

Schematic diagrams of (a) the gamma-ray attenuation measurement and (b) the neutron cross-section measurement.

The transmitted radiation intensity I was calculated by the Beer–Lambert law,

(1) I =   I 0 e − μ x ,

where I is the radiation intensity passing through the samples of different thicknesses (compared to the source intensity I 0), x is the sample thickness (cm), and μ is the linear attenuation coefficient for gamma rays. The equation for the fast removal cross-section for neutrons (ΣR) (cm−1) is also applied from equation (1), which changes from μ to ΣR.

Then, the total mass attenuation coefficients (μ m ) were calculated by

(2) μ m =   μ / ρ ,

where ρ is the sample density.

The radiation shielding potential of a material can also be reported as the half-value layer (HVL) and tenth-value layer (TVL), which refers to the thickness of the samples that reduces the radiation intensity to half or one-tenth of its original intensity. The HVL and TVL values can be expressed as

(3) HVL = ln 2 / μ ,

(4) TVL = ln 10 / μ .

The mean free path (mfp), which is the average distance between two successive interactions of photons, can be calculated by

(5) mfp =   1 / μ .

2.2.3 Microstructure analysis

The microstructures of the samples were investigated by XRD (Rigaku Miniflex 600 with Cu Kα radiation, λ = 1.5406 Å, 40 kV, and 40 mA), Fourier transform infrared spectroscopy (Bruker Tensor 27 FTIR spectrometer), and scanning electron microscopy (JEOL-JSM-6400, 10 kV). The samples of NFC0, NFC5, and NFC10 were also selected to represent the behavior of this investigation. The SEM analysis was carried out with the morphology changed by adding nano-Fe3O4 and was prepared by broken samples from compressive strength testing, which were soaked in acetone to remove any remaining water and then gold-coated. The samples (broken compressive strength test samples) for XRD and FTIR analyses were prepared by grinding and soaking the samples in acetone. The FTIR was carried out on the functional groups that had changed due to the addition of nano-Fe3O4. The crystalline phases that had changed under curing times (7–90 days) and the nano-Fe3O4 contents were observed by XRD. The XRD diffraction patterns were obtained with a step size of 0.02° in the range 10°–60° 2θ at a scan rate of 3° min−1. The FTIR samples were packed in a circle sheet and scanned with an attenuated total reflection (ATR) method in the range 400–4,000 cm−1 with a resolution of 4 cm−1.

3 Results

3.1 Compressive strength

The compressive strength measurements of the samples after 7, 28, and 90 days (Figure 4) show that the strength increased with increasing nano-Fe3O4 content up to 5% by weight (sample NFC5), but then continuously declined at all curing times with further additions of nano-Fe3O4. The nano-Fe3O4 acted as a filler and nucleating agent, resulting in the formation of denser and more compact microstructures [32,38,39]. However, the reduction in the compressive strength in the samples containing more than the optimum 5% by weight of nano-Fe3O4 may be due to two reasons:

  1. The presence of the additional nanoparticles decreases the available space for the growth of crystalline calcium hydroxide (portlandite) crystals, thereby decreasing the ratio of the crystals to the strengthening gel. This would lead to an increase in both the shrinkage and creep in the cement paste, which would become more porous [38].

  2. Another possible explanation might be the agglomeration of the nano-Fe3O4, decreasing its ability to actively participate in the hydration process [32].

Figure 4 Compressive strengths of the magnetite/mortar samples and the control sample at 7, 28, and 90 days.
Figure 4

Compressive strengths of the magnetite/mortar samples and the control sample at 7, 28, and 90 days.

An interesting feature of this study is the relatively high compressive strengths of samples NFC7 and NFC10 compared to the control sample NFC0. These results are attributed to the beneficial effect of high nano-Fe3O4 contents on strength development in the samples. It should also be noted that the optimum nano-Fe3O4 content of the present study (5%) is consistent with a previous literature report [40]. In addition, at this nano-Fe3O4 content (5%), a relatively high strength development from 28 to 90 days (approximately 11%) was shown, compared to the NFC0 sample (5%). This was possibly due to the nano-Fe3O4 reacting with the remaining Ca(OH)2, resulting in nucleating and facilitating the C–S–H or other hydrate phase formations [33].

3.2 Dry density and water absorption

The 28-day dry density values of the present samples (Figure 5, solid bars) behave similarly to their compressive strengths (Figure 4), increasing with increasing nano-Fe3O4 contents up to 5%, but decreasing at higher nano-Fe3O4 contents. The relatively low dry density of the mortar containing nano-Fe3O4 of more than 5% was due to the loose porous structure in the matrix caused by agglomeration or the amount of nano-Fe3O4. The dry density values were 1,733, 1,729, 1,794, 1,847, 1,771, and 1,758 kg m−3 for NFC0–NFC10, respectively. The values also exhibited that the addition of nano-Fe3O4 tends to gain high dry density, compared to samples without nano-Fe3O4. The relatively high density of NFC came from the refinement pore structure in the mortar matrix [31] and the high density of the Fe3O4 nanoparticles [38].

Figure 5 Dry density and water absorption results at 28 days.
Figure 5

Dry density and water absorption results at 28 days.

The water absorption of the samples containing nano-Fe3O4 (Figure 5, broken line) indicates that the addition of nano-Fe3O4 produces a less porous, denser structure of the mortar matrix. Previous studies [40,41] have similarly shown that nanoparticles can occupy the voids and pores in a cement matrix, leading to improved particle packing and reduced water absorption. The loss of absorption water values from the control sample (NFC0) and the samples containing nano-Fe3O4, calculated from the water absorption values, are 23, 26, 37, 28, and 29% for NFC1, NFC3, NFC5, NFC7, and NFC10, respectively.

3.3 Microstructure

The microstructure analyses were carried out on samples NFC0, NFC5, and NFC10. The XRD diffractograms patterns of all the 7-day samples (Figure 6a) contain the reflections of quartz (ICDD database no. 01-070-7344), calcite (ICDD database no. 01-083-0577), portlandite (Ca(OH)2, ICDD database no. 00-044-1481), calcium silicate hydrate (C–S–H, ICDD database no. 00-33-0306), and calcium silicate (ICDD database no. 00-027-1064). These peaks also occur in the 28 and 90-day samples (Figure 6b and c). However, the portlandite peaks at ≈18° and 34° 2θ in the samples cured for 28 days are of slightly higher relative intensity (Figure 6b); portlandite is known to be one of the products of the hydration process, especially the reaction of the calcium silicates (C2S and C3S) with water [42,43]. Thus, the portlandite is probably related to the matrix C–S–H and thus to the development of 28-day compressive strength. Interestingly, the intensity of the portlandite peak at 18° 2θ in the 90-day samples containing nano-Fe3O4 decreases (Figure 6c), possibly due to the formation of further hydration products by the reaction of the portlandite with nano-Fe3O4 at longer curing times.

Figure 6 XRD patterns of selected magnetite/mortar samples and the control sample at (a) 7 days, (b) 28 days, and (c) 90 days. Key: Q = Quartz, C = calcite, P = Portlandite, S = calcium silicate hydrate, and CS = calcium silicate.
Figure 6

XRD patterns of selected magnetite/mortar samples and the control sample at (a) 7 days, (b) 28 days, and (c) 90 days. Key: Q = Quartz, C = calcite, P = Portlandite, S = calcium silicate hydrate, and CS = calcium silicate.

To confirm the reaction of portlandite with nano-Fe3O4, the crystalline size of portlandite at ≈34° 2θ was used, according to the Scherrer equation, as shown in equation (6). At this peak, the portlandite was not found at all in the samples of 7 days. The growth of portlandite crystalline at 28 days was calculated as 41.34, 37.74, and 30.14 nm for NFC0, NFC5, and NFC10, respectively. The decrease in the crystalline size of portlandite during hydration is primarily caused by its ongoing dissolution, reprecipitation, interaction with pozzolanic materials, and strain effects [42]. These processes lead to smaller, less ordered crystallites, which are reflected in the XRD pattern as broader peaks. In this work, the crystalline size of portlandite obviously decreased with the nano-Fe3O4 ratios. This means that the nano-Fe3O4 could react with portlandite or Ca(OH)2 to produce more hydration products. The crystalline sizes continued decreasing to 37.74, 34.72, and 28.94 nm for NFC0, NFC5, and NFC10, respectively, when curing times were prolonged (90 days). This finding related to the development of compressive strength from early to late curing times (Figure 4)

(6) D =   K λ β cos θ ,

where D is the crystallite size, K is the shape factor (∼0.9), λ is the wavelength of the X-ray, β is the full width at half maximum (FWHM), and θ is the Bragg angle.

The FTIR spectra of the 28-day NFC0, NFC5, and NFC10 samples are shown in Figure 7. For the purpose of this study, changes in the wavelength range 800–1,200 cm−1 were selected to monitor the behavior of the mixtures containing nano-Fe3O4 compared with the control sample (NFC0). The peak at 969 cm−1 in the control is related to the polymerization of SiO4 units during the hydration of cement [44]. The addition of nano-Fe3O4 shifts this peak to 1,032 and 990 cm−1 in samples NFC5 and NFC10, respectively (Figure 7). Previous workers have reported that the shifts in these peaks during cement hydration are indicators of the degree of polymerization of these silicate units [45,46,47], with a higher wavelength number corresponding to a higher degree of polymerization. Thus, the higher SiO4 wavelengths in samples NFC5 and NFC10 compared with the control sample NFC0 indicate a greater degree of polymerization associated with the formation of C–S–H. This result is in agreement with the observed enhancement of compressive strengths in mixtures containing nano-Fe3O4.

Figure 7 FTIR spectra of the 28-day samples and the control sample.
Figure 7

FTIR spectra of the 28-day samples and the control sample.

The SEM micrographs of the 28-day samples NFC5, NFC10, and the control sample NFC0 are shown in Figure 8. These reveal the presence of C–S–H on the surface of all the samples, including those containing nano-Fe3O4. In addition, sample NFC10 (Figure 8c) is also seen to contain surface nanoparticles. At higher concentrations, the high specific surface energy of these nanoparticles can cause them to agglomerate, leading to a slight improvement in the hydration process [28,32]. This observation of surface nanoparticle agglomeration suggests an explanation for the observed reduction of the compressive strengths in the samples containing >5% nano-Fe3O4.

Figure 8 SEM micrographs of the 28-day samples. (a) control sample NFC0, (b) sample NFC5, (c) sample NFC10, and (d) EDS mapping of NFC5.
Figure 8

SEM micrographs of the 28-day samples. (a) control sample NFC0, (b) sample NFC5, (c) sample NFC10, and (d) EDS mapping of NFC5.

The chemical analysis by SEM-EDS, as shown in Table 2, represents the weight fraction of C–S–H (red point in Figure 8a) as 30.69% Ca and 11.84% Si. According to the stoichiometric ratio of C–S–H, the Ca/Si ratio ranged from 1.2 to 2.3, with a mean value of 1.7–1.8 [48,49]. In this work, the Ca/Si ratio was calculated as 1.81, which was in line with the literature. From EDS mapping of NFC5 samples (Figure 8d), the Fe was dispersed on the surface with a weight fraction of 4.10%. This value is related to the nano-Fe3O4 ratio used in the mixture of NFC5.

Table 2

Chemical analysis by SEM-EDS

Element Weight fraction (%)
Red point in CT (Figure 7a) Mapping in Figure 8
C 10.05 12.08
O 45.55 42.33
Mg 0.25 0.80
Al 2.01 2.10
Si 11.84 11.07
Ca 30.69 26.99
Fe — 4.10
K — 0.53

3.4 Gamma-ray and neutron transmission

Figures 9 and 10 show the relationships between −ln(I/I 0) and the sample thickness for gamma-ray and neutron transmission, respectively. The slopes of each graph with R 2 > 0.99 indicate the linear attenuation coefficient (μ) of photons (Figure 9) and the fast removal cross-section (ΣR) of neutrons (Figure 10). The linear attenuation coefficient values (μ) of the gamma-rays are 0.1442, 0.1549, and 0.1507 cm−1 for NFC0, NFC5, and NFC10, respectively. Hassan et al. [50] noted that the gamma-ray shielding property of a material depends on the photon energy and the atomic number as well as the dry density of the material. For cementitious materials, gamma-ray transmission can be reduced by increasing the dry density of the cementitious material [5,12,51]. In the present work, the dry densities decreased in the order NFC5 > NFC10 > NFC0, which corresponds to the linear attenuation coefficient value (μ). Based on these values of the linear attenuation coefficients, the smallest thickness of the half-value layer HVL and tenth-value layer TVL (the sample thickness that reduces the radiation intensity to half or one-tenth of its original value, respectively) is 4.475 cm and 14.865 cm, and the mfp is 6.456 cm; these optimum values of the shielding properties are displayed by sample NFC5 (Table 3). The dense structure of sample NFC5 explains its enhanced ability to attenuate the radiation energy [51]. As further confirmation of these experimental gamma-ray results, theoretical values of μ, μ m , HVL, TVL, and mfp were determined using Phy-X/PSD software [52] (Table 3). These calculations show good agreement between the experimental and theoretical results, with an estimated error of 5.6, 6.5, and 8.5% for samples NFC0, NFC5, and NFC10, respectively, i.e., all within an error of <10% [4,53]. Under various energies, the behaviors of the samples were also computed using Phy-X/PSD software, as shown in Table S1. All the samples showed that the values of μ decreased with increasing energy, which was in line with a previous study on RSC [54].

Figure 9 Relationships between −ln(I/I 0) and sample thickness for gamma-ray transmission.
Figure 9

Relationships between −ln(I/I 0) and sample thickness for gamma-ray transmission.

Figure 10 Relationships between −ln(I/I 0) and sample thickness for neutron transmission.
Figure 10

Relationships between −ln(I/I 0) and sample thickness for neutron transmission.

Table 3

Experimental and theoretical radiation transmission results

Parameters NFC0 NFC5 NFC10
Gamma transmission
Experimental
 μ (cm−1) 0.144 0.155 0.151
 μ m (cm2 g−1) 0.083 0.086 0.086
 HVL (cm) 4.807 4.475 4.600
 TVL (cm) 15.968 14.865 15.279
 mfp (cm) 6.935 6.456 6.636
Calculated
 μ (cm−1) 0.136 0.145 0.138
 μ m (cm2 g−1) 0.079 0.079 0.079
 HVL (cm) 5.081 4.771 5.051
 TVL (cm) 16.879 15.848 16.660
 mfp (cm) 7.331 6.883 7.235
Neutron transmission
 ΣR (cm−1) 0.1109 0.1192 0.1119
 ΣRm (cm2 g−1) 0.064 0.065 0.064
 HVL (cm) 6.250 5.815 6.194
 TVL (cm) 20.763 19.317 20.577
 mfp (cm) 9.017 8.389 8.937

The trend in the values of the fast removal cross-sections (ΣR) is similar to the linear attenuation coefficients, being 0.1109, 0.1192, and 0.1119 cm−1 for samples NFC0, NFC5, and NFC10, respectively. Sample NFC exhibited the highest fast removal cross-section value, but this is only slightly higher than NFC0. Cementitious materials are typically able to absorb neutrons because of their hydrogen content (approximately 1% of their unit weight) [12]. Their neutron attenuation can be improved by the addition of materials with a high neutron capture cross-section such as those containing boron, iron, or iron hydroxide [5,55]. In the present study, the addition of nano-Fe3O4 increased the number of iron atoms, but also resulted in the loss of H2O (Table 4). Consequently, the addition of nano-Fe3O4 would have a smaller effect on neutron attenuation. However, the overall results indicate that the addition of 5% nano-Fe3O4 is capable of producing a radiation shielding mortar.

Table 4

Chemical composition of selected magnetite/mortar samples and the control sample NFC0

Compounds Concentration (%)
NFC0 NFC5 NFC10
CaO 15.47 15.30 15.14
SiO2 59.59 58.94 58.31
Fe2O3 0.75 0.74 0.73
Fe3O4 — 1.06 2.09
Al2O3 4.51 4.46 4.41
MgO 0.42 0.42 0.43
Na2O 0.34 0.34 0.34
P2O5 0.01 0.01 0.01
SO3 0.97 0.96 0.96
Cl — — —
TiO2 0.08 0.08 0.08
MnO 0.01 0.01 0.02
ZnO — — —
K2O 0.61 0.61 0.60
SrO 0.02 0.02 0.02
H2O 17.23 17.05 16.86

3.5 Comparison of the efficiency of cementitious materials containing nanomaterials

Table 5 compares the radiation transmission results (optimum density, μ and ΣR values) of this study with the literature. All the literature indicates that gamma-ray attenuation by cementitious materials is enhanced by the presence of nanomaterials, especially in high-density concrete. This occurs by pore filling and the nucleation effects of the nanomaterials which decrease the porosity and increase the density, thereby attenuating gamma-ray shielding. Consistent with the results of the present study, the literature shows that the presence of nanomaterials has no effect on neutron attenuation (although nano-silica exhibits excellent properties in cementitious materials). Thus, the general conclusion from the literature, as well as from this study, is that nanomaterials have an excellent potential for gamma-radiation shielding cementitious materials. However, mortar or concrete for shielding applications against both gamma rays and neutrons should preferably contain more neutron absorbers [12], in addition to an optimized content of suitable nanomaterials. The latter may be based either on calculation or on experiment, but should take into account the reported negative effect of nanomaterials on neutron shielding [56]. In addition, previous research also reported that the size effect of materials became insignificant at high photon energies [57,58]. This should be further investigated in the future.

Table 5

Comparison of the radiation transmission results of this study with the literature

Nanomaterial Matrix Density (g cm−3) μ (cm−1) ΣR (cm−1) Ref.
5% nano-Fe3O4 Mortar 1.847 0.155 0.1192 This study
10% nano-Fe3O4 Cement paste 1.690 0.137 — [35]
50% nano-Fe3O4 Cement paste ≈1.900 0.088 — [36]
25% nano-Fe2O3 Mortar 2.314 0.150 — [59]
2% nano-Fe2O3 Cement paste — ≈0.173 — [29]
2% nano-Fe2O3 High-density concrete 3.793 0.5568 — [60]
1.5% nano-ZnO + 3% nano-SiO2 High-density concrete 3.020 0.349 — [61]
8% nano-TiO2 Fiber-reinforced concrete — ≈0.193 — [62]
Control High-density concrete 3.613 0.197* 0.013** [56]
9% nano-TiO2 3.649 0.229* 0.003**
9% nano-Fe3O4 3.649 0.223* 0.014**
9% nano-SiO2 3.649 0.209* 0.013**

Notes: *Source is 60Co, 1.332 MEV, **calculated by NCNR software at 8 MeV.

4 Conclusion

In this study, various amounts of nano-Fe3O4 were added to mortar for the production of radiation-shielding concrete. The physical, mechanical, microstructural, and radiation shielding properties of the resulting materials were determined with the following conclusions:

  1. The addition of nano-Fe3O4 increased the compressive strength and dry density and decreased the water absorption by the mortar, compared to the mortar without nano-Fe3O4.

  2. The optimum amount of added nano-Fe3O4 producing the best physical and mechanical properties of the mortar was 5% by weight of OPC, providing 216.79 ± 6.19 ksc at 28 days for compressive strength, 1,847 ± 19.1 kg m−3 for dry density, and 8% for water absorption.

  3. The FTIR spectra showed that the silicate unit peak of the reference sample NFC0 at 969 cm−1 shifted to 1,032 and 990 cm−1 in the samples containing 5 and 10% nano-Fe3O4 (samples NFC5 and NFC10, respectively) due to the high degree of polymerization of the SiO4 during the hydration of the OPC. This finding agreed with the XRD analysis, which exhibited the size of portlandite crystalline at 28 days calculated as 41.34, 37.74, and 30.14 nm for NFC0, NFC5, and NFC10, respectively. A smaller crystalline size refers to the dissolution and reprecipitation of portlandite crystalline to other hydration products, such as C–S–H.

  4. Nano-Fe3O4 contents of >5% resulted in the agglomeration of the nanoparticles on the sample surface, which is related to compressive strength loss.

  5. Mortars containing nano-Fe3O4 exhibited the potential for gamma-ray attenuation due to their greater structural density than in the control sample without nano-Fe3O4. By contrast, the presence of nano-Fe3O4 has less effect on neutron attenuation due to the influence of nano-Fe3O4 on the loss of H2O from the samples.

  6. The optimum values of HVL, TVL, and mfp for gamma-ray transmission by the samples were 4.475, 14.865, and 6.456 cm, respectively. The corresponding values for neutron transmission were 5.815, 19.317, and 8.389 cm−1, respectively. These optimum values were for sample NFC5 (containing 5% by weight of OPC).

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Acknowledgments

The authors acknowledge the instruments and laboratory support provided by the Ionizing Radiation Metrology Section, Regulatory Technical Support Division, Office of Atoms for Peace, Ministry of Higher Education, Science, Research and Innovation, Thailand. Also, this research was supported by the National Science, Research and Innovation Fund (NSRF) and Prince of Songkla University (Grant No. ENG6601060S).

  1. Funding information: The instruments and laboratory support were provided by Ionizing Radiation Metrology Section, Regulatory Technical Support Division, Office of Atoms for Peace, Ministry of Higher Education, Science, Research and Innovation, Thailand. Also, this research was supported by National Science, Research and Innovation Fund (NSRF) and Prince of Songkla University (Grant No. ENG6601060S).

  2. Author contributions: All authors have accepted responsibility for the entire content of this manuscript and approved its submission.

  3. Conflict of interest: The authors state no conflict of interest.

  4. Data availability statement: All data generated or analyzed during this study are included in this published article.

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Received: 2024-03-24
Revised: 2024-10-15
Accepted: 2024-12-10
Published Online: 2025-02-07

© 2025 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/ntrev-2024-0135
Keywords for this article
nano-magnetite; radiation shielding; mortar; compressive strength; microstructure
Creative Commons
BY 4.0

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  70. Retraction
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