Journal of Cleaner Production 446 (2024) 141355

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Journal of Cleaner Production

journal homepage: www.elsevier.com/locate/jclepro

A novel type of mineral-impregnated fiber reinforcements based on

alkaline-resistant glass fiber and magnesium oxychloride cement for
enhanced sustainability in construction
Jitong Zhao , Julius Scheel , Marco Liebscher *, Thomas Köberle , Viktor Mechtcherine
Technische Universität Dresden, Institute of Construction Materials, 01062, Dresden, Germany

A R T I C L E I N F O A B S T R A C T

Handling Editor: Panos Seferlis The present study addresses an innovative methodology for the design and creation of mineral-impregnated
fiber-reinforcement structures utilizing magnesium oxychloride (MOC) cement and commercial alkaline-
Keywords: resistant glass fiber (AR-GF) rovings. The approach of custom-built material design and manufacturing equip­
Glass-fiber composite ment makes a high-quality and stable impregnation process possible, ensuring efficient industrial manufacturing
Mineral impregnation
and great flexibility in field applications. Particular fresh mineral-impregnated glass fibers (MGFs) are air-cured
Magnesium oxychloride cement
at ambient temperature and evaluated over the course of 28 days. The MGF composites exhibit a considerable
Reinforcement
Automated production initial strength after the 1st day, with further improvement with subsequent curing periods, particularly until the
first 7 days. The remarkable flexural and tensile performance achieved by the MGF prototypes at both 1-day and
28-day curing periods is in the same range as currently available fiber-reinforced polymers (FRP). Analysis using
mercury intrusion porosimetry (MIP), environmental scanning electron microscope (ESEM) and micro-computed
tomography (μCT) validate a more reacted and densified matrix microstructure and enhanced fiber-matrix
interphase due to prolonged curing. The proposed reinforcement type leverages a sustainable impregnation
medium and digital production, contributing to carbon-neutral, lightweight and fire-safe construction.

1. Introduction The replacement of such organic matrices with inorganic ones rep­
resents a promising technique to overcome the aforementioned draw­
Textile-reinforced concrete (TRC) is a composite material based on a backs in previous years. In recent years mineral-impregnated carbon
fine-grained cementitious matrix and high-performance, continuous fiber (MCF) composites have been introduced to the family of reinforced
multifilament yarns made of glass, carbon, polymers, or other materials structures, in particular for scenarios where organic matrix composites
(Tlaiji et al., 2020). Numerous research projects, both in repair and in are inappropriate (Li et al., 2023; Mechtcherine et al., 2020b; Zhao et al.,
new construction, have been able to prove that delicate, efficient, and 2023d). MCFs consist of mineral matrices reinforced with unidirectional
environmentally friendly components in complicated geometries can be or multidirectional continuous carbon fiber (CF) bundles. A series of
realized by utilizing TRC (Mechtcherine, 2013). However, pilot studies has been conducted in the literature on the development of
state-of-the-art organic impregnation matrices for textile reinforcements mineral impregnation techniques rich in amorphous silica (Guo et al.,
have several drawbacks, including vulnerability at elevated tempera­ 2022; Nadiv et al., 2017; Signorini et al., 2018, 2019) and hydraulic
tures, relatively high cost, lack of vapor permeability, less compatibility cement (Cohen and Peled, 2012; Peled et al., 2006) and open interesting
with cementitious substrates, and irreversibility after installation (Bisby scenarios for the replacement by sustainable binders featuring high
et al., 2005). Holz and Curbach (2020), Silva et al. (2014), and pozzolanic reactivity (Rambo et al., 2015; Strauss Rambo et al., 2016) or
Schneider et al. (2019) and Zhao et al. (2023d) recorded a considerable geopolymerisation by means of aluminosilicate precursors (He et al.,
loss in the bond strength between the polymer-coated carbon yarns and 2010; Hung et al., 2011; Lyon et al., 1997; Pernica et al., 2010; W. Wang
the cement/geopolymer (GP) based concrete substrate when exposed to et al., 2023). For efficient, reproducible production and a completely
temperatures exceeding the glass transition temperature (Tg) of the homogenous fiber-matrix distribution, the geometric particle size of the
polymer. mineral impregnation agents is specifically required to approach the

* Corresponding author.
E-mail address: [email protected] (M. Liebscher).

https://doi.org/10.1016/j.jclepro.2024.141355
Received 9 November 2023; Received in revised form 12 February 2024; Accepted 18 February 2024
Available online 19 February 2024
0959-6526/© 2024 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-
nc-nd/4.0/).
J. Zhao et al. Journal of Cleaner Production 446 (2024) 141355

fiber diameter applied (Zhao et al., 2023b). Considering its economic highly scalable automated process established in prior studies by the
viability and technical flexibility, Zhao et al. (2021a) employing GP authors (Liebscher et al., 2022). Thereafter the resulting composites
impregnation technology enables a considerable processing window were characterized with regard to their fiber-matrix morphology, pore
conducive to efficient industrial manufacturing in the fresh state, while structure, and mechanical performance to investigate the relationship
facilitating rapid setting and strength gain via targeted heating. In recent between the matrix microstructure and composite behavior. The syn­
studies, the unique design of the impregnation suspensions based on ergetic utilization of commercial and eco-friendly materials and
ultrafine cement and silica, conducted by Schneider et al. (2019) and state-of-the-art automation for streamlined production lay the ground­
polycondensating GP, as described in Zhao et al. (2023e), allows MCFs work for large-scale industrial deployment and sustainable construction
to achieve comparable mechanical properties to polymeric systems and practices.
significantly enhanced bond strength and compatibility up to 500 ◦ C and
200 ◦ C when incorporated into concrete substrates. Additionally, owing 2. Experimental program
to the very high geometrical flexibility in the fresh status, the feasibility
to accommodate MCFs into concrete 3D printing and potential appli­ 2.1. Materials
cations for digital processability have been demonstrated by Mechtch­
erine et al. (2020a). Furthermore, based on the exceptional electrical To manufacture the MGF, a commercially available AR-GF heavy
conductivity of CF, the bar or grid structure of MCF possesses satisfac­ tow with tradename NEG-AR2400S-920, provided by Nippon Electric
tory conductivity and is envisaged to confer smart features as multi­ Glass Group®, Japan was used. According to the supplier (NEG glass
functional building materials, e.g., efficient self-heating in fiber), the tow, consisting of 1600 individual filaments, possessed a
manufacturing (Junger et al., 2022), and thermoelectric fineness of 2400 tex and an average filament diameter of 27 μm.
generator-enabled MCF grids (Zhao et al., 2023a) and Joule heater de­ The molar ratios and weights of the MOC cement impregnation
vice exploiting MCF-based GP concrete (Karalis et al., 2024). suspension are given in Table 1. Molar ratios of MgO/MgCl2 = 7 and
However, the majority of mineral impregnation matrices available H2O/MgCl2 = 15 were obtained by using industrial highly reactive
are by far highly alkaline media and therefore only compatible with CFs. magnesium oxide (MgO) and magnesium chloride (MgCl2⋅6H2O). Spe­
This poses significant environmental challenges related to economically cifically, the Austrian firm Styromag®‘s product OK10, calcined
sustainable waste management and recycling techniques. Furthermore, magnesia burnt at 800 ◦ C, and Magnesol S1–S3-Schuppen (purity:
as a consequence of their energy-intensive production, CFs are subject to 47.4% of MgCl2), supplied by Schüssler Novachem®, Germany, were
considerably higher levels of energy expended in production, when selected as primary binder components. As seen in Fig. 1, the MgO
compared to other synthetic fibers. In contrast, glass fibers (GFs) or powder consists of fine sheet-like particles, which appear to have
basalt fibers (BFs) can be substantially and easily recycled via re-melting agglomerated into larger groups. The particle-size distribution of MgO is
processes but require a pH-neutral or slightly alkaline embedding determined using a Laser Diffraction Particle Size Analyzer LS 237 from
environment. Beckmann Coulter, USA. The particle diameters of the 10%, 50% and
In this regard, magnesium oxychloride (MOC) cement, also known as 90% quantiles were d10 = 1.34 μm, d50 = 16.71 μm, and d90 = 74.26 μm,
Sorel’s cement (Lauermannová et al., 2021), can deliver lower alkalinity respectively. More than 50% of the particles had sizes smaller than the
ranges (pH of 10–11) while offering advantages of fast setting, fire­ GF filament diameter, which was around 27 μm, as marked by the red
proofing, wear resistance, high strength, and excellent bonding ability to line. To ensure adequate penetration of the MOC cement slurry into the
numerous fillers (Li et al., 2020). MOC cement is a non-hydraulic cement dense GF bundle, large particle sizes, approximately smaller or matching
made by combining magnesium oxide (MgO) generated through the filament diameter, are often desired in the formulation design, as
magnesite calcination with a concentrated solution of magnesium discussed in prior studies (Schneider et al., 2019; Zhao et al., 2023a).
chloride (MgCl2) (Sglavo et al., 2011). MgO binders consume signifi­ The mineralogical composition of the MgO obtained by the technical
cantly less energy in the manufacturing process and can absorb CO2 data of the supplier (“Styromag GmbH,” 2023) is given in Table 2,
from the atmosphere to form a range of carbonates and hydroxycar­ expressing periclase MgO as the main mineral phase with small quan­
bonates, in this way making them an eco-friendly and “carbon-neutral” tities of aluminum oxide (Al2O3), quartz (SiO2), quicklime (CaO) and
cement type (Walling and Provis, 2016). MgCl2 can be obtained from wüstite (FeO). The content of active MgO in the applied product was
low-cost, natural sources, e.g., from seawater and saline lakes (Maier, quantitatively determined using the hydration method in accordance
2023). By virtue of these obvious features, MOC cement has been with the Chinese standard WB/T 1019–2002 (2002), indicating a
applied conventionally in the manufacture of industrial floor materials remaining weight mass of 75.4% due to the formation of Mg(OH)2 and
(Li et al., 2003; Li and Chau, 2007), grinding wheels (Nehdi and Khan, representing a high-quality class “QM-85”.
2001; Xu et al., 2016), a variety of panels with specific functions, e.g., Mixing of the MOC cement suspensions, mixing was conducted using
decoration, fire protection, sound and thermal insulations (Mar­ an IKA T50 digital ULTRATURRAX high-speed disperser at 2000 rpm for
avelaki-Kalaitzaki and Moraitou, 1999; Plekhanova et al., 2007), the 2 min and then at 4000 rpm for another 5 min to ensure complete
novelty of bio-material (Nabiyouni et al.), and solid­ dispersion of the MgO particles. Air bubbles in the suspension were
ification/stabilization agents (Jianli et al., 2010). Since the major removed using a vibrating table for 3 min. A flow cup with a volume of
drawback of MOC cement is its limited durability with respect to per­ 100 ml and a diameter of 5 mm for the nozzle opening was used to
manent water contact, considerable research efforts have been under­ determine the flowability of the resulting suspension in accordance with
taken in recent years toward its hydrophobization and stabilization (Li EN ISO 2431 (2019), which showed a good flow time of 35 s in the range
et al., 2020; Walling and Provis, 2016). of values reported in previous studies (Schneider et al., 2019; Zhao et al.,
In the study at hand, the advantages of alkaline-resistant GFs (AR- 2021a). This demonstrated a high degree of penetration of the MOC
GFs) and MOC cement matrices are combined to develop a novel type of cement suspension. Furthermore, an initial setting time of 220 min (3.7
mineral-impregnated GF (MGF) reinforcements. The production utiliz­
ing MgO and GFs is less energy-intensive than the previously investi­
Table 1
gated cement and carbon fibers. Initially, a MOC cement impregnation
Compositions and properties of mineral-based impregnation suspensions for 1 L.
suspension has been purposefully designed and thoroughly character­
ized regarding physicochemical and mechanical properties during Mixture constituent Density [g/cm3] Mass [g/L]

aging. For the fabrication of the proposed model composite reinforce­ Magnesium oxide (MgO) 3.58 800.77
ment, a commercially available AR-GF heavy tow was used and then Magnesium chloride (MgCl2) 1.57 496.59
Water 1 395.42
impregnated with the developed MOC cement suspension following a

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J. Zhao et al. Journal of Cleaner Production 446 (2024) 141355

Fig. 1. Micrographs of (a) MgO, Styromag OK10 and (b) its particle size distribution curve of Styromag OK10 as measured by laser granulometry.

et al., 2018; Nanni, 2005). The ready-made prototype possesses a fiber

Table 2 volume fraction of approximately 13%, which is identical for each
Mineralogical compositions of Styromag OK10 obtained from the manufacturer.
curing parameter. However, the obtained value is much lower than that
Oxide composition (Styromag OK10) MgO SiO2 CaO FeO Al2O3 of classical GFRPs, primarily varying from 50% to 75% (Burgoyne et al.,
[wt%] 86 2.7 5.3 4.4 1.4 2007), due to inherent particle morphology characteristics of mineral
powders (Zhao et al., 2023b). Therefore, further experimental and nu­
merical studies on mixture design and manufacturing optimization are
h) and a final setting time of 270 min (4.5 h) was measured by Vicat’s needed to identify the optimal fiber volume fractions suitable for various
apparatus according to EN 14016–2 (2004), which ensures a certain practical applications.
breadth of the processing window during continuous impregnation for
efficient industry production (Supporting information - Fig. S1).
2.3. Mechanical characterization of the impregnation matrix
2.2. Preparation of MGF composites
Three-point bending and compressive tests were conducted using a
Zwick Roell Z1445 machine at a loading rate of 1 mm/min, with
The continuous impregnation of the AR-GF roving with the MOC
maximum load cell capacities of 1 kN and 10 kN, respectively. Prismatic
cement suspension was performed using an automated, inline pultrusion
samples, each measuring 10 × 10 × 60 mm3 in volume, were used for
process, integrated with a five-roller-Foulard and a filament winding
the flexural strength tests with a span of 30 mm. Halves of the remaining
system. The Foulard system enhanced impregnation effectiveness
bending samples were used for the compressive test. Reported values
through multiple yarn deflection, with each roller having a diameter of
represent the average of at least five measurements from both bending
4.2 cm. The GF heavy tow was drawn at a production speed of 100 m/h
and compressive tests.
to ensure consistent stress for proper filament alignment and thereafter
shaped by two funnel-like nozzles with an inner opening diameter of 4.5
mm. Freshly pultruded MGF elements with 1.2 m lengths were contin­ 2.4. Mechanical characterization of MGF
uously assembled side by side on a large hexagonal, motor-driven wheel,
facilitated by an engine-controlled, linear guide unit. Further informa­ The flexural properties and thus impregnation quality of MGF were
tion and details on the equipment employed can be found in the previous evaluated through three-point bending tests using a displacement-
studies (Liebscher et al., 2022; Mechtcherine et al., 2020c; Zhao et al., controlled Zwick-Roell testing machine (model Z1445) with a span of
2023c). 24 h after the preparation process, the MGFs produced were 100 mm and a loading rate of 5 mm/min. At ages of 1 day, 7 days, and 28
removed from the wheel and cut to the appropriate length for testing, days, at least five composites were tested, and the average value was
followed by storage in a standard climate of 20 ◦ C and relative humidity reported for each. Flexural strength was determined using individual
(RH) of 65% until testing at the age of 1, 7, and 28 days. A photo with a measurements of the height and width of the cross-section for each
corresponding μCT image of the produced MGF is given as well in Fig. 2. composite specimen.
At 28 days, the as-produced MGF composite attains an excellent The tensile stress-strain behavior of the MGF composite was assessed
density of 1.72 g/cm3, expressing a comparable or even lower value in through uniaxial tension tests following ISO 10406-1 (2008) at 28 days,
comparison with GFRPs (typically from 1.25 to 2.10 g/cm3) and 78% with a servo-hydraulic Instron testing machine model EU 20 with a
lower density than steel rebar (typically 7.90 g/cm3) (Mugahed Amran displacement-controlled loading rate of 1 mm/min, as described in

Fig. 2. Schematic drawing of the inline production of MGF-based AR-GF and MOC cement.

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J. Zhao et al. Journal of Cleaner Production 446 (2024) 141355

(Zhao et al., 2021). Each specimen had a total length of 600 mm, with reported in past studies (Guo et al., 2021; Huang et al., 2022).
end anchorage lengths of 100 mm on each side. The MGF yarn was The representative ESEM micrographs of MOC cement impregnation
embedded into aluminum tubes (length: 100 mm, outer diameter: 12 matrices after 1, 7, and 28 days of curing are given in Fig. 4. The sample
mm, inner diameter: 8.5 mm) at its ends and then clamped into the microstructures are composed of heterogeneous phases of different
machine for loading. Deformations of the specimens were measured morphology, compactness, and porosity, largely dependent on the
using an electro-optical video extensometer Rudolph XR200 with a curing age. After one day of curing, samples exhibited a rough fracture
precision of ±0.02 mm and a gauge length of 100 mm, positioned cen­ surface and poorly connected microstructure accompanied by a signif­
trally on the samples. Black and white striped target marks were affixed icant presence of irregular particles (Fig. 4a and b) which are likely
to each sample before testing. At least five specimens were tested unreacted particles from the MgO raw material (Dung and Unluer,
following a hardening period of 24 h. 2018). In the course of the dissolution of these particles, pore spaces
would be created. Within the confined region and pore space, the growth
2.5. Morphological and chemical characterization of needle-like crystal phases with a size of ~1–1.5 μm, probably to be Mg
(OH)2 (Yang et al., 2021), is evident with rising the curing age. This
The matrix structure and filament-matrix distribution within the phenomenon leads to reduced porosity in the matrix and, as a result,
entire cross-section of MGF were examined using an environmental improved compactness that contributes to the development of me­
scanning electron microscope (ESEM) Quanta 250 FEG from FEI, Eind­ chanical strength, as displayed in Fig. 4e and f, for the counterparts
hoven, Netherlands. This was equipped with an Energy-dispersive X-ray cured after 28 days.
analysis (EDX)-mapping system QUANTAX 400 from Bruker in the
United States. Three-dimensional (3D) imaging of the inner structure 3.1. Mechanical characterization of impregnation matrices
and failure behavior was achieved using a micro-computed tomography
(μCT) scanner, specifically the CT-XPRESS model from ProCon X-Ray, The mechanical properties of the MOC cement matrices during aging
Germany. This equipment features a highly productive 65 W X-ray tube from 1 day to 28 days were measured, the results of which are given in
and a high-resolution flat panel detector. Porosity evaluations of both Fig. 5. With increasing aging period, both their compressive strength
the MOC cement matrices and resulting MGFs were conducted using and flexural strength gradually increase, reaching excellent levels of 87
mercury intrusion porosimetry (MIP). The measurements were per­ MPa and 27 MPa, respectively, ascribed to the advanced degree of
formed on a Porotec® Porosimeter PASCAL 140/440, Germany, with chemical reaction (Mi et al., 2023) and, simultaneously, the matrix
specific parameters including a mercury surface tension of 0.48 N/m, a densification, as determined by MIP; see Fig. 3. Specifically, the 1
contact angle of 140◦ , and testing pressure ranging from 0 to 400.71 day-compressive and flexural strengths are 49% and 47% of those
MPa. respective values at 28 days.

3. Results and discussion 3.2. Characterization of MGF composites

Fig. 3 presents the evolution of pore structures in the produced MOC Fig. 6 illustrates a backscatter SEM image and an EDX-mapping
cement-impregnating matrices, revealing a significant presence of nano- image of a polished cross-section of the impregnated yarn. Due to the
scaled pores across a wide range, distinguishing them from previously application of the same material composition and processing device, all
developed impregnation suspensions (Zhao et al., 2020). It should be specimens possess the same impregnation quality and the fiber-matrix
noted that the measured pore sizes in the MIP analysis varied between 3 distribution over the composite cross-section. Hence, the images are
nm and 100 μm, of which the further categorization as micropores representative of specimens produced subject to the other two curing
(<0.1 μm), mesopores (0.1–10 μm), and macropores (>10 μm) can be ages. All filaments are homogeneously distributed within the impreg­
made as described in (Rouquerol et al., 1994). The cumulative pore nating MOC cement matrix and keep a small, certain distance from each
volume decreased considerably until 7 days and varied slightly there­ other, as shown in Fig. 6. Only a few accumulations of the impregnation
after, consistent with findings from other studies (Li et al., 2023). This matrix without embedded filaments were observable. This can be
observation suggests that employing air curing with extended durations further confirmed by the images of EDX-mapping with primarily Si el­
is advantageous to form a denser composite microstructure. Notably, ements within the multifilament yarn cross-section. These features
extending the curing period to 28 days results in a gradual increase in demonstrate the remarkable penetration ability of the tailor-made, low-
mesopores, associated with reductions in both micro- and macropores. viscosity MOC cement suspension into the dense AR-GF bundle. This
This phenomenon can be linked to the physicochemical densification high-quality and uniform impregnation behavior, characterized by
process, facilitated by gradual filling through the formation of more 5 consistent fiber saturation and less void formation, ensures the repro­
Mg(OH)2•MgCl2•8H2O (phase 5) products, as described in (Mi et al., ducibility of processing conditions in industrial settings. Additionally,
2023). These features are in good agreement with the observations the uniform fiber-matrix distribution facilitates efficient shear-stress

Fig. 3. Pore size distributions obtained from MIP for the MOC cement impregnation matrices.

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J. Zhao et al. Journal of Cleaner Production 446 (2024) 141355

Fig. 4. Typical ESEM micrographs showing the fracture surfaces of MOC cement matrices at (a,b) 1 day, (c,d) 7 days and (e,f) 28 days.

crystals of reaction products and minerals from the impregnation matrix

tightly adhere to the GF surface. Li et al. (Shuiping et al., 2006) deter­
mined the growth of Phase 5 (5 Mg(OH)2 ⋅ MgCl2 ⋅ 8H2O) crystals on GF
surfaces in the development of MOC cement composites. In proximity to
the 1-day-cured counterparts, the least amount of MOC cement matrix
attached to the fiber surface is attained with huge areas of bare filament
surfaces and a lack of strong bonding with the fiber surface. However,
the extension of the curing ages to 28 days results in a higher amount of
matrix precipitations on the filament surface, signifying enhanced
physical-chemical interaction between the GF and the constituents of
the mineral matrix, which is related to an improved stress transfer with
the MGF; see Fig. 7e and f. It is worth noting the formation of extensively
less reacted microstructure at the fiber-matrix interface when cured at 1
day, as seen in the fiber channel in Fig. 7g. Conversely, the prolonged
curing to 28 days leads to a considerably more densified and homoge­
nous MOC cement microstructure with higher matrix strength in the
interfacial zone, also supported by MIP results, as shown in Fig. 11.
Fig. 5. Development of mechanical properties of (a) compressive strength and
(b) flexural strength of the MOC cement impregnation matrix. Figs. 8 and 9 present the average flexural strength and the corre­
sponding flexural stress-deflection curves of the derived MGFs obtained
from bending tests after different curing ages. The MGF produced
transfer mechanisms between the individual filaments. As such, the
already possesses an excellent flexural strength of 190 MPa on the first
composite demonstrates outstanding mechanical properties, including
day, which delivers the highest flexibility in subsequent industrial
high flexural and tensile performance (cf. Figs. 8 and 12), making it
manufacturing and field applications. The extension of the aging period
suitable for various construction applications.
contributes up to 7 days to further strength gains due to the progression
Insights into the fracture morphology and fiber-matrix interactions
of the matrix reaction and densification, given in MIP analysis and in
were acquired by splitting produced MGFs along the fiber direction for
(Chau and Li, 2008; Hu et al., 2016). Beyond 7 days, the flexural
differently aged samples; see Fig. 7. In all composite variants, contin­
strength remains almost unchanged thereafter taking into account the
uous fiber embedment without any distinct gaps is seen, expressing good
error bars. The failure mode of all MGFs inspected under bending in­
physical interaction among the components. Similar to unreinforced
dicates an initially non-linear elastic response with a slightly decreasing
MOC cement samples, the composites yield increased reaction products
slope until reaching the maximum flexural stress. This is followed by
and a reduction in non-reacted or partially reacted MgO residues with
several sudden declines in stress levels, which can be attributed to sus­
higher age.; cf. Fig. 4. In the interfacial area, it can be noticed that
tained crack-bridging behavior and debonding mechanisms of GF as well

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J. Zhao et al. Journal of Cleaner Production 446 (2024) 141355

Fig. 6. Microscopic images showing the cross-section of MGF cured at 28 days at (a) lower magnification and (b) higher magnification (EDX mapping image: Green
circles indicate the positioning of single filaments). (For interpretation of the references to colour in this figure legend, the reader is referred to the Web version of
this article.)

Fig. 7. ESEM images of the fracture surface of split MGFs parallel to the fiber direction at (a,b) 1 day, (c,d) 7 days and (e,f) 28 days and corresponding fiber channel
at (g) 1 day and (h) 28 days.

as to fiber breakage. It should be noted that some premature local fail­ concentrations in specific interfacial areas, thereby reducing
ures, taking place prior to the ultimate peak stress, and a lower load-bearing capacity.
ascending slope are visible in the insufficiently cured MGFs at 1 day. Fig. 9b discloses the representative failure modes of MGFs produced
These failures can be attributed to the lesser effectiveness of stress graphically, similar to conventional GFRP (P. Wang et al., 2023). The
transfer between the GF and matrix and higher porosity leading to stress failure of MGF is dominated by fiber kinking and matrix cracking on the

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J. Zhao et al. Journal of Cleaner Production 446 (2024) 141355

range of 0.01–1 μm in their structure while reducing the number of

micropores. Since all composites were manufactured with the same
device and materials, differences with respect to the impregnation
quality were deemed negligible. A comparison among the porosities of
MGF with an increasing aging period discloses a clear decreasing ten­
dency in cumulative pore volume, macropores, and micropores and a
gradual increase in mesopores, similar to their unreinforced counter­
parts. The lower porosity of the specimens cured over 28 days validates
their superior mechanical performance; see Fig. 8.
In the investigation of the tensile properties of MGF prototypes at 28
days, the ability of this novel reinforcement material to withstand ten­
sion was assessed. Tensile strengths were calculated by dividing the
maximum tensile forces by the total filament cross-sectional areas, while
Young’s modulus E was obtained within the linear elastic region of stress
levels. The MGFs achieved show a distinguished tensile strength of 1096
MPa and Young’s modulus of 70 GPa falling within the same range as
conventional FRP, but slightly reduced to the pristine GF roving, as seen
in Table 3. Such achieved tensile strength falls within the same range as
conventional GFRP reinforcements, typically ranging from 483 to 1600
MPa, and surpasses that of steel rebar, which normally ranges from 483
to 690 MPa (Firmo et al., 2015; Nanni, 2005; Van Den Einde et al.,
2003). Note, fiber tensile strengths depend highly on the testing pa­
rameters, such as free length and testing speed. The schematic repre­
Fig. 8. Average flexural strengths for MGFs obtained from the yarn sentation of the typical tensile stress-strain curve is depicted in Fig. 12,
bending tests. signifying a linearly increasing trend and failure upon reaching the ul­
timate stress, without an intermediate yielding point in brittle material
compression side as well as interlaminar shear failure, i.e., layer sepa­ behavior. As observed by ESEM, the embedment of all filaments into the
ration, across the entire composite. Only a limited number of GFs un­ MOC cement matrix ensures sufficient shear force transfer capacity from
derlie tensile stresses, breaking on the tension side with some matrix the outer to the inner filaments under tensile loading; cf. Fig. 6.
cracks. These features can be well observed in the μCT slices of Therefore, the failure of the achieved MGF yarn is primarily governed by
post-bending damaged MGF specimens; see Fig. 10. It can also be the breakage of the filaments, rather than by fiber slippage.
noticed that the MGF counterparts subjected to prolonged curing pe­
riods until 28 days exhibit a noticeable radial distribution of oval-shaped 4. Summary
cracks, indicative of a heightened propensity towards brittle failure
mechanisms. This phenomenon is attributed to the augmented The integration of inorganic impregnation binders with continuous
compactness and strength of the matrix, resulting from extended curing rovings represents a groundbreaking approach to produce temperature-
durations. Conversely, in younger counterparts, pronounced delamina­ resistant, high-performance, lightweight reinforcement systems. This
tion failures manifest primarily at the yarn center, attributable to the study aims to introduce a novel mineral-impregnated fiber-reinforce­
diminished interfacial bond strength between the fiber and matrix. ment system for the building industry, leveraging MOC cement and
These observations underscore the structural integrity and failure modes commercial AR-GF rovings. The tailor-made, low-viscosity impregna­
of the composite material under investigation. tion agent affords a sufficient processing window of several hours for
The aforementioned aspects of the porosity of MOC cement matrices continuous industrial manufacturing and high flexibility in prospective
can be well correlated with the pore sizes of the corresponding MGF on-site applications and thorough wetting of fibers. Engineered with a
composites, as displayed in Fig. 11. In general, the porosity of the specialized pultrusion inline process, the continuous impregnation of
mineral-impregnated composite is considerably influenced not only by AR-GFs was implemented automatically. This approach facilitated
the chemical reaction in the matrix but also by the penetrability of the exceptional filament-matrix distribution, ensuring robust stress transfer
mineral particles during processing (Nadiv et al., 2017; Schneider et al., between each filament and resulting in outstanding mechanical prop­
2019; Zhao et al., 2023b) and the fiber-matrix interaction (Zhao et al., erties both immediately and after 28 days.
2020). Hence, slightly higher cumulative pore volumes are attained for The cost and scalability of the proposed production methodology
the MGF composites as compared to the unreinforced MOC cement depend significantly on its adaptability to varying production volumes
samples. More precisely, the number of mesopores increases within the and needs. The custom-built equipment for MGF is essentially derived

Fig. 9. (a) Flexural stress-deflection curves and (b) schematic drawing of the failure mode of the fiber composite under bending according to (P. Wang et al., 2023).

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J. Zhao et al. Journal of Cleaner Production 446 (2024) 141355

Fig. 10. μCT images of the tested MGFs (a–c) at 1 day and (d–f) at 28 days (F: loading direction).

Fig. 11. Pore size distributions obtained from MIP for the MGF composites.

Table 3
Average tensile properties of MOC cement-based MGF at 28 days; standard de­
viations are given in parentheses.
Yarn type Tensile strength Failure strain Young’s modulus
[MPa] [%] [GPa]

MGF 1096 (78) 1.20 (0.18) 70 (19)

AR-GF 1500a 2.00a 74a
roving
a
Data obtained from the manufacturer (NEG glass fiber).

from the pultrusion common to classical FRPs, making it highly

economical and reproducible (Volk et al., 2022). Scaling up production
is fundamentally feasible by adapting industry-scale FRP pultrusion line,
with tailored parameters for specific mineral materials, as described in
(Mechtcherine et al., 2020b). Investment costs may cover research,
Fig. 12. (a) Graphic representation of a typical tensile stress-strain curve for design, manufacturing, and installation, along with ongoing expenses.
MGF and (b) failed specimens after the tensile test. From the production side, the cost of pultruded products remains the
main driver for increasing line speeds and developing mineral slurries,

8
J. Zhao et al. Journal of Cleaner Production 446 (2024) 141355

while the need for recyclability puts the focus on the renewable matrix and also acknowledge with thanks the support of Mrs. Annett Willo­
and fiber option, e.g., MOC cement and GF. Lower cost and higher mitzer for carrying out the laser granulometry and MIP.
sustainability are expected with mineral matrices compared to poly­
meric systems. Nevertheless, a thorough cost-benefit analysis is needed Appendix A. Supplementary data
for assessing scalability and optimal investment in future studies.
For the environmental impact, MOC cement stands out for its low Supplementary data to this article can be found online at https://doi.
carbon footprint in production and carbon sequestration compared to org/10.1016/j.jclepro.2024.141355.
Portland cement. Additionally, MOC cement offers superior durability
and chemical resistance, thereby extending the lifespan of structures and References
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