Construction and Building Materials: Yuan Jing, Chunwei Zhang, Guangyi Lin, Yuanyuan Niu, Meng Zhao

Construction and Building Materials 440 (2024) 137516
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Construction and Building Materials

journal homepage: www.elsevier.com/locate/conbuildmat
Studies on the mechanical properties of rubber concrete reinforced with

high-temperature stirred pretreated waste rubber particles
Yuan Jing a, Chunwei Zhang a,c,*, Guangyi Lin b,**, Yuanyuan Niu c , Meng Zhao b
a
College of Civil Engineering, Qingdao University of Technology, Qingdao 266000, PR China
b
College of Electromechanical Engineering, Qingdao University of Science and Technology, Qingdao 266061, PR China
c
Multidisciplinary Center for Infrastructure Engineering, Shenyang University of Technology, Shenyang 110870, PR China
A R T I C L E I N F O A B S T R A C T
Keywords: Using waste rubber particles to replace fine aggregates in the production of rubber concrete not only promotes
Waste rubber granules the recycling of waste rubber but also reduces the consumption of natural sand. The difference in bonding in-
Rubber concrete terfaces between waste rubber particles and the concrete matrix leads to a loss of concrete strength, which has
Pretreatment
prompted many researchers to investigate surface pretreatment methods for waste rubber particles. However,
Mechanical properties
these studies have been limited by low production efficiency, inconspicuous strength enhancement, and the
generation of chemical waste. This study proposes a new method of pretreating waste rubber particles through
high-temperature mixing, with temperature (100◦ C, 150◦ C, 200◦ C, 250◦ C, 300◦ C) and mixing time (15 minutes,
30 minutes, 45 minutes) as variables. The treated waste rubber particles were then subjected to thermal gravi-
metric analysis (TGA), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM),
energy dispersive X-ray (EDS), and water contact angle (WCA) tests.The results show that, compared to untreated
waste rubber particles, the waste rubber particles after high-temperature stirring pretreatment form a hard oxide
film on the surface under high-temperature oxidation, which enhances the elastic modulus of the particles. At the
same time, surface small molecular organic compounds and loose impurities are removed under the effects of
stirring and friction, greatly improving the surface cleanliness.The mechanical properties of rubber concrete
prepared with high-temperature stirred pretreated waste rubber particles show an initial increase followed by a
decrease with the rise of temperature.In comparison, rubber concrete prepared with pretreated waste rubber
particles (Stirred for 30 minutes at 250◦ C) shows a 38.58 % increase in cubic compressive strength, a 67.79 %
increase in shear strength, a 44.45 % increase in axial compressive strength, and a 38.06 % increase in static
compressive elastic modulus after 28 days of curing, compared to rubber concrete prepared with untreated waste
rubber particles.
1. Introduction natural river sand is also one of the environmental issues of concern.
River sand has a long regeneration cycle and slow natural renewal, and
The problem of "black pollution" caused by used tires is becoming over-exploitation affects the flooding capacity of rivers, causing floods
more and more serious. It is reported that about 1 billion used tires are [4]. Substituting waste tire particles for fine aggregates not only pro-
produced in the world every year [1]. In China, the annual generation of motes the recycling of waste tires but also reduces the consumption of
used tires grows at a rate of 8 %-10 %, of which only about 20 % is natural river sand [5].Simultaneously, adding rubber particles enhances
recycled [2]. The main components of used tires are natural rubber, the wear resistance, chloride ion resistance, impact resistance, heat
synthetic rubber, carbon black, additives, etc., which are difficult to resistance, freeze-thaw resistance, and vibration and noise reduction
degrade under natural conditions, and are prone to causing fires, performance of concrete [6,7]. For example, BS Thomas et al. [8]. use
contaminating the soil, breeding mosquitoes and rodents, and causing waste rubber particles to replace fine aggregates to prepare rubber
the spread of diseases and pestilence [3]; the decreasing amount of concrete, and the results show that the incorporation of waste rubber
* Corresponding author at: College of Civil Engineering, Qingdao University of Technology, Qingdao 266000, PR China.
** Corresponding author.
E-mail addresses: zhangchunwei@sut.edu.cn (C. Zhang), gylin666@163.com, qkgryjy@163.com (G. Lin).
https://doi.org/10.1016/j.conbuildmat.2024.137516
Received 13 May 2024; Received in revised form 24 June 2024; Accepted 16 July 2024
Available online 18 July 2024
0950-0618/© 2024 Elsevier Ltd. All rights are reserved, including those for text and data mining, AI training, and similar technologies.
Y. Jing et al. Construction and Building Materials 440 (2024) 137516
particles can improve the wear resistance of concrete. AA Gheni et al. waste rubber particles, and enhances the bonding interface and me-
[9]. use different amounts of waste rubber particles mixed into concrete, chanical properties of waste rubber particles with concrete base. Najim
improving the concrete’s chloride ion penetration resistance. LJ Li et al. and Hal et al. [24] pretreat waste rubber particles using the mortar
[10] analyze the effects of rubber particle size, rubber content, and pre-coating method, and the compressive strength of rubberized con-
strain rate on the dynamic compressive strength and toughness of crete increases by 37 %. Onuaguluchi et al.[25] use cement pre-coating
RMRAC. The test results show that adding rubber particles enhances the overlay, and silica fume pre-coating, and the compressive strength of
strain rate effect of concrete and has good impact resistance. I Marie’s rubberized concrete increases by 42 % and 49 %, respectively. They
[11] research shows that using 10 % waste rubber particles by volume to conclude that the pre-coating method of pretreating waste rubber par-
replace fine aggregates can reduce the thermal conductivity of concrete. ticles makes the waste rubber particles encapsulated with a layer of hard
A Richardson et al. [12]use waste rubber particles with a particle size of shell, which increases the modulus of elasticity of the material, and the
less than 0.5 mm mixed into concrete, improving the freeze-thaw surface covered with mortar, cement, and silica fume enhances the
resistance of rubber concrete. B Zhang et al. [13]. prepare rubber con- interfacial bonding and mechanical properties of the rubber and the
crete with good vibration damping capacity and sound insulation concrete base material. A.Kashani et al. [26] use 30 % NaOH to pretreat
performance. the waste rubber particles, and the compressive strength of the
However, the weakening effect of waste rubber particles on the rubberized concrete increases by 40 %. They conclude that NaOH pre-
strength of concrete is very serious, which is a key problem restricting treatment of waste rubber particles removes oily impurities such as
the application of rubber concrete [14–16]. Studies show that when stearic acid on the surface of waste rubber particles, improves the sur-
rubber particles with a volume content of less than 10 % replace fine face cleanliness and hydrophilicity of waste rubber particles, and en-
aggregates, the strength loss is about 25 %. If the rubber particles’ hances the interfacial bonding and mechanical properties of rubber and
content does not exceed 20 %, the strength loss is about 30 %[17–19]. concrete-based materials.Alireza [20] and A. Kashani [26] et al. use
When the rubber content exceeds 20 %, its strength is significantly sulfuric acid to pretreat waste rubber particles, and the compressive
reduced [20,21]. strength of rubber concrete is increased by 56 % and 53 %, respectively.
To minimize the loss of strength caused by the replacement of fine They conclude that the use of sulfuric acid to pretreat waste rubber
aggregates with waste rubber particles, researchers tried a large number particles removes impurities on the surface of the waste rubber particles.
of pretreatment methods, as shown in Table 1. These pretreatment At the same time, due to the corrosive effect of sulfuric acid, the surface
methods can be broadly categorized into physical method pretreatment of the waste rubber particles becomes rough, which increases the fric-
(water cleaning, pre-coating, etc.) [22–27], chemical method pretreat- tion and occlusion between the waste rubber particles and the concrete
ment [26,28–34] (acid solution, alkali solution, potassium permanga- base material. B. Huang [32] and R.X. Liu [33] use a silane coupling
nate solution, silane coupling agent pretreatment, etc.), and other agent to pretreat the waste rubber particles, and the compressive
pretreatment (ultraviolet light pretreatment, latex pretreatment, etc., strength of rubber concrete is increased by 24 % and 14 %, respectively.
and two-phase method pretreatment) [35–38] methods. Bowland et al.[35] use latex to pretreat waste rubber particles, and the
Youssf et al. [22] pretreat waste rubber particles using water strength of rubber concrete is increased by 31 %. They believe that the
washing and the compressive strength of rubberized concrete increases latex coating of waste rubber particles enhances the bonding interface
by 15 %. Mohammadi et al. [23] pretreat waste rubber particles using between the waste rubber particles and the concrete base material.
the water immersion method and the compressive strength of rubber- Ossola et al.[36] use ultraviolet irradiation to irradiate the waste rubber
ized concrete increases by 22 %. They conclude that the method of water particles, and the strength of rubber concrete is increased by 15 %. They
washing or water immersion pretreating waste rubber particles cleans believe that the strength of rubber concrete is enhanced, attributing it to
the surface of waste rubber particles, enhances the hydrophilicity of the fact that UV radiation contains the appropriate level of energy to
break chemical bonds in rubber, which is highly susceptible to the
generation of free radicals and cross-linking of polymer chains, thus
Table 1 generating new hydrophilic functional groups on the surface of the
Effect of pretreatment methods on the strength of rubberized concrete. rubber and strengthening the bonding interface between the waste
references Pre-processing methods 28-day compressive rubber particles and the concrete base material. Chou [37] et al. use a
strength improvement certain proportion of nitrogen and oxygen at 250℃ to pretreat waste
rate (%) rubber particles, and the strength of the prepared rubber concrete is
Youssf et al.[22] water washing 15 % enhanced by 153 %. They conclude that hydrophilic sulfur-oxygen
Mohammadi et al. Soak in water for 24 h 22 % functional groups are formed on the surface of the rubber after partial
[23]
oxidation, which enhances the intermolecular forces between the rubber
Najim，Hal et al. Pre-coated mortar 37 %
[24] and the hydrated calcium silicate (C-S-H). G. Li et al. [38] use latex and a
Onuaguluchi et al. Limestone powder pre-coating 19 % silane coupling agent for the two-stage method of treating waste rubber
[25] particles, and the strength of the prepared rubber concrete is enhanced
A Kashani et al.[26] Cement pre-applied covering, 42 %、49 % by 24 %. They conclude that the combination of latex and a silane
silica fume pre-applied covering
Liang He et al.[27] potassium 48.7 %
coupling agent can enhance the bonding interface between rubber and
permanganate+NaHSO3 cementitious.
Alireza et al.[28] sulfuric acid 56 % In summary, physical pretreatment methods such as water treatment
A Kashani et al.[26] sulfuric acid 53 % and soaking do not significantly enhance the mechanical properties of
Guo et al.[29] 15 %NaOH 23.4 %
rubber concrete. Most chemical pretreatment methods involve soaking
KhurramShahzad 4 %NaOH 19.86 %
et al.[30] in solutions of acids, alkalis, silane coupling agents, etc., resulting in
Yang Li et al.[31] 10 %，20 %，30 %NaOH 11.6 %，13.9 %，4 % chemical waste liquids that are difficult to handle. Other pretreatment
A Kashani et al.[26] 30 %NaOH 40 % methods, such as two-stage processes, are complex and often generate
B. Huang et al.[32] Silane coupling agent 24 % wastewater, making industrial application difficult. These issues greatly
R.X. Liu et al.[33] Silane coupling agent 14 %
H. Su, J et al.[34] Silane coupling agent 7%
limit their scope of application.
Bowland et al.[35] latex 31 % Although researchers reduce the strength loss of concrete caused by
Ossola et al.[36] ultraviolet radiation 15 % the incorporation of rubber particles to a certain extent by pretreating
Chou et al.[37] Partial oxidation at 250℃ 153 % waste rubber particles through different methods, the problems of
G. Li et al.[38] Latex + Silane coupling agent 24 %
chemical wastewater, productivity, and low strength enhancement
2
caused by the pretreatment of waste rubber particles by these methods used the volumetric flask method to measure the apparent density of the
become the key constraints to their industrialized application in the waste rubber particles. The test numbers and mix ratios are shown in
construction industry. In this paper, a novel rubber pretreatment Table 2.
method is introduced to heat treat waste rubber particles under high-
temperature conditions (within the interval of 100℃-300℃) in 2.3. Specimen preparation
conjunction with high-speed stirring. In this study, it is assumed that the
surface oxidation of waste rubber particles can be promoted under high- 2.3.1. Pre-treatment specimen of waste rubber granules
temperature stirring, which strengthens the surface hardness of waste First, weigh a certain mass of waste rubber particles. Pour the par-
rubber particles and improves the elastic modulus of waste rubber ticles into the stirring tank at temperatures of 100℃, 150℃, 200℃,
particles; a part of small molecule compound impurities on the surface of 250℃, and 300℃ (air atmosphere). For each set of temperatures, set the
waste rubber particles volatilizes under the action of high-temperature stirring time to 15 minutes, 30 minutes, and 45 minutes at a speed of
stirring, and a part of loose impurities is removed by the friction and 700 rpm. Then, take out the material, cool and let it static for 24 hours,
extrusion between waste rubber particles during the process of stirring. and sieve the 20-mesh rubber powder for use.As shown in Fig. 1, the
At the same time, the rubber hydrocarbon shows a viscous flow state microscope images depict the morphology of untreated waste rubber
under high-temperature stirring, which covers some of the impurities on particles and waste rubber particles obtained after stirring at 100℃-
the surface of the waste rubber particles, improves the surface cleanli- 300℃ for 30 minutes. From the images, it can be seen that the
ness of the waste rubber particles, and enhances the interface between morphology of the waste rubber particles changes after high-
the waste rubber particles and the concrete base. The study is carried out temperature stirring pretreatment. With the increase in temperature,
using microscopic characterization such as thermo gravimetric Analysis there are noticeable viscous flow streaks on the surface of the waste
(TGA) detection, Fourier infrared spectroscopy (FT-IR) detection, scan- rubber particles. Notably, waste rubber particles stirred at 250◦ C for
ning electron microscopy (SEM) detection, energy dispersive X-ray 30 minutes will agglomerate into lumps, which need to be crushed and
(EDS) detection, water contact angle (WCA)detection, etc., and the screened before use.Waste rubber particles stirred at 300◦ C for 30 mi-
waste rubber particles are pre-treated using different temperatures and nutes do not agglomerate into lumps but remain granular and exhibit a
different stirring times to study the effects of temperature and stirring certain carbonized morphology.
time on the surface and molecular structure of rubber particles and to
verify the effects of different pretreatment methods on the properties of 2.3.2. Concrete specimens
rubber concrete in terms of workability, macroscopic mechanical Prepared by no premixing process, pre-weigh coarse aggregate, fine
properties, and microscopic observations. This high-temperature stir- aggregate, waste rubber particles, cement, water, and water reducer are
ring pretreatment of waste rubber particles is a simple process with injected into the mixer and mixed for 6 minutes. Then, they are loaded
controllable stability and no wastewater generation, which has a certain into the mold in three layers, vibrated on a vibrating table, smoothed,
reference value for the industrial application of rubber concrete in the and placed in a curing box at a temperature of 20±2℃ and 92 % relative
construction industry. humidity for 7 and 28 days, and left to be tested.
2. Materials and programs 2.4. Test methods
2.1. Test raw materials Thermogravimetric Analysis (TGA): Using the Mettler TGA2 instru-
ment (Mettler Toledo, Switzerland), the quantitative analysis of the
The benchmark concrete is designed according to a C40 ratio. The components of waste rubber particles is performed in the temperature
cement used in the tests is P.O42.5 ordinary Portland cement, with a range of 70◦ C to 650◦ C with the intermittent introduction of N2 and O2.
bulk density of 3100 kg/m3, a fineness of 360 m2/kg, an initial setting The test is divided into two stages: In the first stage, N2 is injected as a
time of 200 minutes, and a final setting time of 255 minutes. The coarse protective gas, the temperature is heated from 70◦ C to 300◦ C at a
aggregate consists of continuously graded crushed stone sized 5–16 mm, heating rate of 10 K/min, and held at 300◦ C for 10 minutes; then heated
with a bulk density of 2726 kg/m3. The fine aggregate is sand with a from 300◦ C to 550◦ C at a heating rate of 20 K/min, and held at 550◦ C for
fineness modulus of 2.7, a bulk density of 2688 kg/m3, and a silt content 15 minutes. The first stage ends with the completion of the pyrolysis of
of approximately 0.2 %. The water reducer is a light yellow powder with organics in the waste rubber particles. In the second stage, the temper-
a moisture content less than 4 %, a bulk density of 625 kg/m3, and a pH ature is first reduced to 300◦ C at a cooling rate of 30 K/min, and O2 is
value (20◦ C, 10 % aqueous solution) of 9.0, provided by Shandong injected. The temperature is then heated from 300◦ C to 650◦ C at a
InnoStar New Material Co., Ltd. The rubber particles are 20-mesh, heating rate of 20 K/min, completing the pyrolysis of carbon black,
provided by Guangrao Changguan Recycled Resources Co., Ltd., with leaving the remaining part as ash.Fourier Transform Infrared Spectros-
a bulk density of 1100 kg/m3. copy (FT-IR): Using the Vector70 Fourier Transform Infrared Spec-
trometer (Bruker, Germany), the pre-treated waste rubber particles are
2.2. Test fit ratio characterized by grinding and mixing evenly with KBr at a ratio of 100:1
and then making pellets for sample preparation.Water Contact Angle
According to the research of this paper, the concrete benchmark Test: Using the G-1 type εrma goniometer contact angle measuring in-
concrete ratio design is based on the Chinese national standard "building strument (Kyowa, Japan), deionized water is dripped onto the surface of
concrete ratio design specification" (GB 50007–2011) in the relevant the waste rubber particles and tested after 1 minute.Scanning Electron
provisions of the design of strength class LC40. The researchers con- Microscopy (SEM): Using the JSM-7500 F scanning electron microscope
ducted a large number of experiments to determine the concrete mix (JEOL, Japan) to observe the microstructure of the waste rubber particle
ratio after replacing 20 % of the fine aggregates with rubber particles in materials.Energy Dispersive X-ray Spectroscopy (EDS) Analysis: Using
the same volume. This study examines the effect of waste rubber par- the JSM-7500 F scanning electron microscope combined with an energy
ticles at different temperatures (100℃, 150℃, 200℃, 250℃, 300℃) dispersive X-ray spectrometer (Bruker, Germany), the elements con-
and different stirring times (15 min, 30 min, 45 min). A total of 16 tained in the sample are determined based on the different wavelengths
groups of tests were conducted. The waste rubber particles were pre- of characteristic X-rays of different elements.
treated with high-temperature stirring at different temperatures and The slump and air content of concrete mixtures are tested according
stirring times, while the untreated waste rubber particles were used as a to the Chinese national standard "Standard Test Method for Performance
baseline control group. To accurately calculate the concrete mix ratio, of Ordinary Concrete Mixtures" (GB/T 50080–2016). Slump test: A
3
Table 2
Concrete test mix ratios.
Samples Pre-processing Apparent density of waste rubber Waste rubber Sand Stone Cement Water Water reducing agent
methods granules (kg/m3) granules (kg) (kg) (kg) (kg) (kg) (kg)
0 No processed 1100 55 537.6 1173 420 168 3.7

1–1 100℃/15 min 1100.2 55.01 537.6 1173 420 168 3.7
1–2 100℃/30 min 1100.7 55.035 537.6 1173 420 168 3.7
1–3 100℃/45 min 1100.9 55.045 537.6 1173 420 168 3.7
2–1 150℃/15 min 1102.1 55.105 537.6 1173 420 168 3.7
2–2 150℃/30 min 1105.4 55.27 537.6 1173 420 168 3.7
2–3 150℃/45 min 1106.8 55.34 537.6 1173 420 168 3.7
3–1 200℃/15 min 1109.3 55.465 537.6 1173 420 168 3.7
3–2 200℃/30 min 1111 55.55 537.6 1173 420 168 3.7
3–3 200℃/45 min 1112.4 55.62 537.6 1173 420 168 3.7
4–1 250℃/15 min 1116.1 55.805 537.6 1173 420 168 3.7
4–2 250℃/30 min 1118.2 55.91 537.6 1173 420 168 3.7
4–3 250℃/45 min 1120.9 56.045 537.6 1173 420 168 3.7
5–1 300℃/15 min 1123.2 56.16 537.6 1173 420 168 3.7
5–2 300℃/30 min 1130.2 56.51 537.6 1173 420 168 3.7
5–3 300℃/45 min 1145.7 57.285 537.6 1173 420 168 3.7
Fig. 1. Microscope photograph of waste rubber particles（a.No processed;b.100℃stirring 30 min；c.150℃stirring 30 min；d.200℃stirring 30 min；e.250℃stir-
ring 30 min;f.300℃stirring 30 min）.
slump cone with upper, lower, and height dimensions of 100 mm, machine (Tianjin Meitesi, China) according to the following step-
200 mm, and 300 mm, respectively, is used. The concrete to be tested is s:①Remove the specimen from the curing room and clean its surfa-
filled into the slump cone in three layers, with each layer being com- ce.②Place the specimen on the lower platen of the testing machine with
pacted by tapping the sides to ensure it is dense and free of voids. After the bearing surface perpendicular to the molded top surface.③Control
filling, the slump cone is lifted, allowing the concrete to slump naturally the loading rate at 0.5 MPa/s, applying load continuously and uni-
due to its own weight. The slump value is obtained by subtracting the formly.④When the specimen starts to deform rapidly near failure, stop
height of the highest point of the slumped concrete from the height of adjusting the machine throttle until failure, and record the load；
the cone.Air content test: A CA-3 direct-reading concrete air content Splitting Tensile Strength Test:Specimens are
tester is used, following these steps:①Wipe the inner surfaces of the 150 mm×150 mm×150 mm cubes. The splitting tensile strength is
measuring bowl and cover with a wet cloth, then fill the concrete tested using the YA-300 microcomputer-controlled fully automatic
mixture into the bowl in three layers, compacting each layer with a pressure testing machine (Tianjin Meitesi, China) according to the
tamping rod until smooth and bubble-free.②Place a small piece of following steps:①Remove the specimen from the curing room and clean
plastic film on the surface of the concrete opposite the operation valve its surface. Draw parallel lines on the top and bottom surfaces to
hole, clean the flange, cover the measuring bowl, and tighten the clamp. determine the splitting plane.②Place the specimen in the center of the
Open the exhaust valve.③Close the operation valve, introduce com- lower platen of the testing machine, with the splitting bearing surface
pressed air through the intake valve until the pressure gauge reads 1 and splitting plane perpendicular to the molded top surface. Place arc-
Kgf/cm2.④Tighten the operation valve, open the water inlet valve to shaped pads and strips between the upper and lower platens and the
add a small amount of water, then close the water inlet valve and specimen, aligning them with the centerline of the molded top surfa-
exhaust valve to ensure a sealed and leak-free system.⑤Open the ce.③Control the loading rate at 0.5 MPa/s, applying load continuously
operation valve, allowing the compressed air in the pressure chamber to and uniformly.④When the specimen starts to deform rapidly near fail-
enter the measuring bowl. Once the pressure gauge stabilizes, read the ure, stop adjusting the machine throttle until failure, and record the
value.Testing the compressive strength of concrete cubes, the splitting load；Axial Compressive Strength Test:Specimens are
tensile strength, axial compressive strength, and static compressive 150 mm×150 mm×300 mm prisms. The axial compressive strength is
elastic modulus is carried out in accordance with the Chinese National tested using the WAW31000 microcomputer-controlled electro-hy-
Standard "Standard for Test Method of Mechanical Properties on Ordi- draulic servo universal testing machine according to the following
nary Concrete" (GB/T 50081–2019). Cube Compressive Strength Test: steps:①Remove the specimen from the curing room and clean its sur-
Specimens are 150 mm×150 mm×150 mm cubes. The compressive face. Measure the width of the specimen at the middle section (accurate
strength of concrete cubes is tested using the WAW31000 to 1 mm) and calculate the load-bearing area, denoted as A, in
microcomputer-controlled electro-hydraulic servo universal testing mm2.②Place the prism specimen on the lower platen of the pressure
4
testing machine, ensuring geometric alignment.③Control the loading

rate at 0.5 MPa/s, applying load continuously and uniformly.④When
the specimen starts to deform rapidly near failure, stop adjusting the
machine throttle until failure, and record the maximum load, denoted as
F, in N.⑤Calculate the axial compressive strength (fcp) = F/A；The
static compressive modulus of elasticity: The specimen is a prism with
dimensions 150 mm×150 mm×300 mm, and the test is conducted using
a WAW31000 computer-controlled electro-hydraulic servo universal
testing machine. The test procedure is as follows: ①Take the specimen
out of the curing room and clean its surface. Calculate the compressive
area of the specimen, denoted as A, with units in mm2. Install the
deformation measuring instrument on the specimen, with a gauge length
(L) of 150 mm.②Align the specimen axis with the centerline of the lower
platen and start the testing machine.③Load the specimen to the initial
load value F0 corresponding to a reference stress of 0.5 MPa, maintain
this constant load for 60 s, and record the deformation readings Ɛ0 at
each measurement point within the following 30 s. Immediately and
continuously apply load uniformly until the load value Fa corresponding
to one-third of the axial compressive strength fcp is reached. Maintain
this constant load for 60 seconds, and record the deformation readings
Ɛa at each measurement point within the following 30 s. The loading
Fig. 2. TGA of untreated waste rubber pellets.
rate is 0.5 MPa/s, ensuring that the difference between the values on the
left and right sides is less than 20 % of their average value.④Unload at
the same rate as the loading rate to a reference stress of 0.5 MPa, for 15 min, with no mass-loss step appearing, and the remaining mate-
maintain this constant load for 60 s, and perform three preloads using rial is ash[39].
the same loading and unloading rates with 60 s of constant load each According to the same test method, the heat weight loss analysis of
time. Record the values of F0、Fa、Ɛ0and Ɛa during the last pre- 15 groups of waste rubber particles pretreated by high-temperature
load.⑤The formula for calculating the static elastic modulus under stirring at different temperatures and different times is being carried
compression（Ec） is as follows: out, as shown in Fig. 3. The trend of heat loss analysis of waste rubber
pellets pretreated by high-temperature stirring is the same, and three
Fa − F0 L mass loss steps appear, but there is a large difference in the mass loss of
Ec = ×
A εa − ε0 each step, indicating that the content of small molecular organics and
rubber hydrocarbons in the waste rubber pellets pretreated by high-
3. Analysis of results temperature stirring has changed.
According to the data obtained in Fig. 3, the changes in small
3.1. Analysis of pretreatment waste rubber properties molecule organic matter and total organic matter of waste rubber pellets
are statistically analyzed, as shown in Fig. 4. Compared with untreated
3.1.1. Composition analysis of pretreated waste rubber waste rubber particles, the content of small molecule organic matter in
To test for compositional changes in pretreated waste rubber pellets, waste rubber particles prepared by stirring for 15 min at 100℃ (sample
we determine the small molecule organic matter, rubber hydrocarbon 1–1) decreases sharply by 49.29 %, after which the content of small
（Rubber hydrocarbons are high molecular compounds formed by the molecule organic matter in waste rubber particles shows a slow decrease
polymerization of olefinic hydrocarbons and are the main components with the increase of temperature and the prolongation of stirring time.
in rubber. The rubber hydrocarbons in natural rubber are cis-1,4-poly- This is because most of the small molecules of organic matter (oil or
isoprene.）, and carbon black content of the waste rubber pellets using volatile impurities) at 100℃ stirring for 15 minutes have been volatil-
TGA. ized, the remaining organic matter is mostly difficult to decompose
In Fig. 2, the heat weight loss analysis of untreated waste rubber rubber hydrocarbon. The volatilization of these small-molecule organic
pellets (sample 0) shows that a two-stage test is carried out under two compounds under the effect of high temperature enhances the cleanli-
gas atmospheres, N2 and O2. The organic matter in the waste rubber ness of the waste rubber surface, which is favorable to the interfacial
pellets can be pyrolyzed under the N2 atmosphere, while the carbon bonding between the waste rubber particles and the concrete-based
black needs to be pyrolyzed under the O2 atmosphere to determine its materials [40].
mass loss. In the first stage, N2 is injected as a protective gas to prevent The total organic content shows a decreasing trend with the increase
the organic matter in the waste rubber pellets from burning at high in temperature, which can be divided into two stages. In the temperature
temperatures. The temperature is heated from 70℃ to 300℃ with a range from 100◦ C to 250◦ C, the waste rubber particles prepared (from
heating rate of 10 K/min, and the temperature is held at 300℃ for sample 1–1 to sample 4–2) exhibit a slow rate of total organic content
10 min. A mass-loss step appears with a mass loss of 16.4572 %, indi- loss. The lowest total organic content is observed at a temperature of
cating the mass loss of volatile small-molecule organics, generally oil 250◦ C for waste rubber particles stirred for 45 minutes (sample 4–3),
substances, and volatile impurities. The temperature is then heated from with a 9.8 % decrease compared to untreated waste rubber particles
300℃ to 550℃ at a rate of 20 K / min, and insulation is maintained at (sample 0). In the temperature range from 250◦ C to 300◦ C, the waste
550℃ for 15 min, resulting in a quality loss step of 53.3177 %, indi- rubber particles prepared (from sample 4–3 to sample 5–3) show a faster
cating the quality loss of organic matter, generally rubber hydrocarbon. rate of total organic content loss. At 300◦ C, the waste rubber particles
This marks the end of the first stage, completing the pyrolysis of organic stirred for 45 minutes (sample 5–3) exhibit a 13.92 % decrease in total
matter in waste rubber particles. In the second stage, the temperature is organic content compared to those stirred at 250◦ C for 45 minutes
first reduced to 300℃ with a cooling rate of 30 K/min. O2 is injected, (sample 4–3), and a 22.38 % decrease compared to untreated waste
and the temperature is heated from 30℃ to 650℃ with a heating rate of rubber particles (sample 0). This is due to the gradual thermal oxidation
20 K/min. A mass-loss step appears with a mass loss of 24.5153 %, decomposition of rubber hydrocarbons within the waste rubber particles
indicating a mass loss of carbon black. The temperature is held at 650℃ as the temperature increases, leading to mass loss. Below 300◦ C, the
5
Fig. 3. TGA of pretreated waste rubber pellets.
6
Fig. 4. Content of small molecule organic matter and total organic matter in waste rubber pellets.
thermal decomposition rate is slower because the thermal decomposi- to the enhanced cleavage of C-H bonds after high-temperature treatment
tion of rubber hydrocarbons in an air atmosphere proceeds at a slower [44]. When magnifying the C-O stretching vibration peak region, as
speed, resulting in a relatively stable oxidation and decomposition re- presented in Fig. 5(c), a smoothing of peaks occurs for both untreated
action within the waste rubber particles. When the temperature reaches waste rubber particles (sample 0) and those treated at 100◦ C with stir-
300◦ C, a vigorous oxidation reaction occurs within the waste rubber ring (samples 1–1, 1–2, 1–3), with no significant characteristic peak
particles, accompanied by the observation of intense black smoke upon developing. At 150◦ C, with 15 minutes of stirring pretreatment, Sample
material discharge, leading to a rapid loss of rubber hydrocarbon mass. 2–1 reveals the emergence of a vibration peak, which subsequently
In the temperature range from 100◦ C to 250◦ C, the stirring time has little becomes stronger as temperature increases; at 250◦ C with 30 minutes of
effect on the total organic content of the waste rubber particles, showing stirring pretreatment (Sample 4–2), the vibrational peak reaches its
a fluctuating trend. At 300◦ C, with the prolongation of stirring time, the highest intensity. Samples treated at 300◦ C (samples 5–1, 5–2, 5–3) once
total organic content within the waste rubber particles decreases, as the again show a smoothing of this peak, with no significant development
stirring action further promotes the oxidation and thermal decomposi- evident. The observed trend arises because the surfaces of untreated
tion of rubber hydrocarbons on the surface of waste rubber particles, waste rubber particles and those treated at 100◦ C without oxidization
consistent with the trends observed in the changes in C-O stretching fail to form C-O bonds; from 150◦ C with stirring pretreatment, surface
vibration peaks obtained from subsequent (FT-IR) spectroscopy analysis oxidation of the waste rubber particles gradually intensifies, enhancing
and observations from scanning electron microscope images of the waste the oxidative reaction as temperature and stirring time increase. At
rubber particles. During the oxidation reaction, rubber hydrocarbons 300◦ C, a vigorous surface oxidation results in thermolysis of the oxide
cover the surface of the waste rubber particles with a hard oxide film, film, aligned with trends seen in earlier thermogravimetric analysis of
increasing the elastic modulus of the waste rubber particles to some organic content changes and subsequent surface SEM images and EDS
extent, thereby reducing the strength loss of the rubber concrete. tests showing oxygen content data. Amplifying the C-C stretch vibration
peak region, as illustrated in Fig. 5(d), reveals that the amplitude of the
3.1.2. Fourier transform infrared (FT-IR) spectral analysis vibration peaks for both untreated and high-temperature stirred pre-
To further characterize the chemical reactions occurring during the treated waste rubber particles remains consistent, demonstrating that
loss of organic materials from waste rubber particles under high- the high dissociation energy of C-C bonds prevents significant damage
temperature stirring, Fourier-transform infrared (FT-IR) spectroscopy within the temperature range studied (100◦ C-300◦ C)[45].
analyses were conducted on waste rubber particles pretreated at
different temperatures and stirring times. As depicted in Fig. 5(a), both 3.1.3. Scanning electron microscopy（SEM） analysis
untreated waste rubber powder and high-temperature stirred pretreated To directly observe the morphological changes that occur in the
waste rubber powder exhibit three distinct vibration peaks: a C-H waste rubber particles pretreated by high-temperature agitation, we
stretching vibration peak at 2960 cm− 1[41], a C-O stretching vibration carry out SEM microscopic observation. Fig. 6 shows the SEM images of
peak at 1030 cm− 1[42], and a C-C stretching vibration peak at unpretreated waste rubber particles and waste rubber particles pre-
1440 cm− 1[43]. Upon magnifying the C-H stretch vibrational peak re- treated at different temperatures and for different times, with 100 µm
gion, as shown in Fig. 5(b), it is observed that the untreated waste rubber and 10 µm micrographs selected, and the blue boxes are labeled as the
particles (sample 0) feature a prominent peak, whereas the peak position of magnified observation and the position of subsequent EDS
weakens for particles pretreated at high temperatures, indicating a detection scans.
degradation of C-H bonds due to their low dissociation energy, leading The micrograph of the surface of untreated waste rubber particles
7
Fig. 5. FT-IR of waste rubber particles.
shows that the surface of the waste rubber particles has an uneven and smoother surface. This is because, with prolonged stirring time under
rough appearance and is adhered with many loose particles. This is due the same temperature condition, the waste rubber particles experience
to the stripping of tire fillers (e.g., carbon black, silica, zinc oxide, sufficient friction and extrusion, fully utilizing the cleaning effect.
magnesium oxide, oil attachments, etc.) due to mechanical forces during Fig. 6 (2− 1, 2− 2, 2− 3) displays the surface micrographs of waste
the crushing process of the waste rubber pellets, and these tiny fillers rubber particles pretreated with stirring at 150℃ for 15 minutes,
attach to the surface of the waste rubber pellets[46]. These tiny at- 30 minutes, and 45 minutes. The figures demonstrate that the surface
tachments attached to the surface are defined as impurities in this study. roughness of the waste rubber particles further improves, with only
These loose impurities are detrimental to the bonding of the waste minimal loose impurities remaining. This is due to the further volatili-
rubber particles to the concrete interface and, at the same time, intro- zation of small organic molecules and the increase in temperature,
duce a large amount of gas, increasing the gas content of the concrete which reduces the adhesion between impurities and waste rubber par-
mix, which is one of the reasons for the quality loss of rubberized con- ticles and promotes the removal of loose impurities. It is worth noting
crete[47]. that stirring at 150℃ for 45 minutes (Fig. 6 (2− 3)) shows an occurrence
Fig. 6 (1− 1, 1− 2, 1− 3) shows the surface micrographs of waste where impurities are covered by rubber. This is because, under this
rubber particles pretreated with stirring for 15 minutes, 30 minutes, and condition, the waste rubber particles experience intensified friction,
45 minutes at 100℃. The figures indicate that the surface roughness of resulting in the viscous flow of rubber hydrocarbon on the surface of the
the waste rubber particles improves and the impurities adhered to the waste rubber particles. This viscous flow covers smaller impurities on
surface are reduced. This phenomenon occurs due to the volatilization of the waste rubber particles’ surface.
small molecule organic matter on the surface of the waste rubber par- Fig. 6 (3− 1, 3− 2, 3− 3) presents the surface micrographs of waste
ticles at this temperature. Additionally, under the action of stirring, the rubber particles pretreated with stirring at 150℃ for 15 minutes,
waste rubber particles in the stirring tank undergo friction and extru- 30 minutes, and 45 minutes. The figures display significant improve-
sion, effectively removing loose impurities from the particles’ surface. ment in the surface smoothness of the waste rubber particles, with only a
As the stirring time extends, the surface smoothness of the waste rubber very small number of loose impurities remaining on the surface. When
particles further improves. For instance, waste rubber particles prepared observed at a 10um scale, it can be seen that some impurities on the
by stirring for 45 minutes at 100℃ (Fig. 6 (1− 3)) exhibit a partially waste rubber particles’ surface are encapsulated. This occurs due to the
8
Fig. 6. SEM of waste rubber particles（0.No processed；1–1.100 ℃ stirring 15 min; 1–2.100 ℃ stirring 30 min; 1–3.100 ℃ stirring 45 min; 2–1.150 ℃ stirring
15 min; 2–2.150 ℃ stirring 30 min; 2–3.150 ℃ stirring 45 min; 3–1.200 ℃ stirring 15 min; 3–2.200 ℃ stirring 30 min; 3–3.200℃ stirring 45 min; 4–1.250℃ stirring
15 min; 4–2.250℃ stirring 30 min; 4–3.250℃ stirring 45 min; 5–1.300℃ stirring 15 min; 5–2.300℃ stirring 30 min; 5–3.300℃ stirring 45 min).
enhanced viscous flow of rubber hydrocarbon on the surface of the waste flow-like streaks left behind by the cooling of the waste rubber particles
rubber particles under this temperature condition. The increased viscous can be observed in the 10um electron micrographs of stirring for
flow encapsulates more unshed impurities. It should be noted that the 30 minutes at 200℃ (Fig. 6 (3− 2)) and stirring for 45 minutes at 200℃
viscous flow becomes more apparent with extended stirring time. The (Fig. 6 (3− 3)).
9
Fig. 6 (4− 1, 4− 2, 4− 3) exhibits micrographs of the surface of pre- content of 2.9 %, with the elevation of the temperature, the surface
treated waste rubber particles stirred at 250℃ for 15 minutes, impurity content shows a trend of first decreasing and then increasing,
30 minutes, and 45 minutes. The figures demonstrate that the surface of this is because in the 100 ℃ − 250 ℃ temperature interval with the
the waste rubber particles becomes very smooth, with almost no loose elevation of the temperature and stirring time, on the one hand, the
impurities present. This occurs because, under this temperature condi- waste rubber particles surface impurities by the particles of the friction
tion, the rubber hydrocarbon on the waste rubber particles’ surface between each other, extrusion effect to remove, on the other hand,
experiences strong viscous flow. Additionally, the rubber hydrocarbon presents the On the one hand, the impurities on the surface of waste
undergoes oxidation through its reaction with oxygen in the air, rubber particles are removed by the friction and extrusion between the
resulting in the formation of an oxidized film on the waste rubber par- particles, and on the other hand, the rubber hydrocarbons with mobility
ticles’ surface. This phenomenon is confirmed through the trend of the cover the impurities on the surface of waste rubber particles. Under the
C-O stretch vibration peaks in the FTIR spectra and the oxygen content condition of 300℃, the oxidized film of the rubber hydrocarbon
observed in the subsequent EDS test. The clean surface optimizes the encapsulating the impurities was destroyed, and the impurities were re-
bonding interface between the waste rubber particles and the concrete exposed, which is consistent with the phenomenon observed in the
base. Furthermore, the formation of the oxide film increases the elastic aforementioned SEM image (Fig. 6).
modulus of the waste rubber particles themselves, contributing to the Untreated waste rubber particles (sample 0), with an oxygen content
strength enhancement of rubber concrete. It should be noted that, under of 3.2 %, with the increase in temperature oxygen content showed a
this temperature condition, the surface of the waste rubber particles tendency to increase and then decrease, the highest value of the oxygen
undergoes minor changes with extended stirring time. For example, content appeared at 250 ℃, stirring 30 min (sample 4–2) prepared
waste rubber particles prepared under the temperature condition of rubber particles, amounting to 17.1 %, which is 5.3 times higher than
250℃ and stirred for 45 minutes (Fig. 6 (4− 3)) show a rougher surface the oxygen content of untreated waste rubber particles (sample 0). This
at some points, exposing certain impurities. This is due to the gradual is because under the effect of temperature and stirring, the mobile
start of pyrolysis of the oxidized film formed from the oxidation of rubber hydrocarbon and oxygen in the air undergo oxidation reaction,
rubber hydrocarbons, which aligns with the trend observed in the total C-O bond formation [54],The oxygen content of waste rubber particles
organic matter in previous heat loss analyses, the trend of C-O stretching prepared by stirring for 15 min under 300℃ temperature conditions
vibration peak in FT-IR spectra, and the trend of oxygen elements (sample 5–1) has undergone a sharp decrease, and the surface oxide film
observed in subsequent EDS tests. is destroyed, which is due to the fact that the oxide film is violently
Fig. 6 (5− 1, 5− 2, 5− 3) reveals micrographs of the surface of waste oxidized and pyrolyzed under this temperature condition[55], which is
rubber particles pretreated by stirring for 15 minutes, 30 minutes, and consistent with the results in Fig. 5 the convergence of the change in the
45 minutes under the temperature condition of 300℃. The figures show peak C-O bond value of the telescopic vibration peak measured by FTIR
that the surface of the waste rubber particles appears rough with cracks spectroscopy and the phenomenon observed in the SEM image of Fig. 6.
accompanied by loose impurities. This occurs because, at a temperature
of 300℃, the rubber hydrocarbon on the waste rubber particles’ surface 3.1.5. Water contact angle（WCA） test
undergoes intense oxidation, leading to the pyrolysis of surface organic To test the change of hydrophilicity of high-temperature pretreated
matter. As a result, impurities covered by the rubber hydrocarbon oxide waste rubber particles, researchers test the water contact angle of waste
film become exposed again. With prolonged stirring time, this phe- rubber particles, as shown in Fig. 9. As can be seen from the figure, the
nomenon becomes more evident. water contact angle of untreated waste rubber particles is 65◦ , and the
water contact angle of waste rubber particles pretreated by high-
3.1.4. Energy dispersive X-ray （EDS）analysis temperature stirring floats between 58◦ and 62◦ , indicating that the
To further analyze the elemental changes on the surface of high- hydrophilicity of the pretreated waste rubber particles is slightly
temperature stirred pretreated waste rubber pellets, EDS analysis is improved. This improvement may be because the high-temperature
performed, as shown in Fig. 7. The scanning point position is the blue stirring of the pretreated waste rubber particles removes the oily sur-
box in the electron microscope diagram in Fig. 6. From the figure, it can face material and increases the hydrophilicity.
be seen that the main elements on the surface of waste rubber particles
are carbon, oxygen, sulfur, zinc, magnesium, silicon, calcium, and iron. 3.1.6. Mechanistic analysis
Carbon mainly comes from the small molecules of organic matter in the Based on the above tests, the oxidation mechanism of waste rubber
rubber, carbon black, rubber hydrocarbons, etc[48]. The main source of particles under the action of high-temperature stirring is analyzed, as
oxygen is the oxygen adsorbed on the surface of the waste rubber par- shown in Fig. 10. Under the action of unapplied temperature, the waste
ticles or the oxidized film formed by high-temperature stirring pre- rubber particles in the stirring tank are attached with loose impurities
treatment[49]. The element of sulfur is mainly derived from sulfur as a and mixed with the surrounding oxygenated air, and then under the
vulcanizing agent for rubber[50]. The elements zinc, magnesium, and action of high-temperature stirring, the waste rubber particles are
calcium are mainly derived from rubber vulcanizing agents. Zinc, extruded and rubbed against each other, and some of the impurities are
magnesium, and calcium mainly come from rubber additives such as removed, and with the increase of the temperature and the extension of
zinc oxide, magnesium oxide, calcium oxide, etc[51]. Silicon mainly the stirring time, the surface of the rubber hydrocarbons gradually be-
originates from the rubber filler silicon dioxide[52]. Iron mainly comes comes viscous, and begins to wrap the surface of the impurities that are
from the tire wire cord and other ferrous skeleton materials produced in not removed, and at the same time under the action of the temperature
the crushing process of the powder[53]. Among them, zinc oxide and and the stirring, the rubber hydrocarbons oxidize with the air. At the
magnesium oxide are small in particle size, which can be easily adsorbed same time, under the effect of temperature and stirring, the rubber hy-
on the surface of waste rubber particles, causing a serious impact on the drocarbon and oxygen in the air undergo an oxidation reaction and
bonding interface between waste rubber particles and concrete matrix. gradually form an oxide film.
Here, we define these two elements as surface impurities of waste rubber The essence of the rubber molecular chain of the side chain is
particles. affected by the surface oxidation of scrap rubber pellets. It involves the
According to the data obtained in Fig. 7, the statistical analysis of the breakage of cross-linking bonds and the formation of new cross-linking,
oxygen element in the surface elements of waste rubber particles, and leading to the surface hardening of the oxidized waste rubber pellets.
surface impurities (zinc oxide and magnesium oxide) of waste rubber The surface oxidation of scrap rubber granules is a free radical chain
particles, as shown in Fig. 8. As can be seen from the figure, the un- reaction, with its primary product being hydroperoxide. The oxidation
treated waste rubber particles (sample 0), have a surface impurity reaction process of rubber hydrocarbons is as follows: using RH to
10
Fig. 7. EDS analysis of waste rubber pellets.
11
Fig. 8. Impurities and oxygen content in waste rubber pellets.
Fig. 9. WCA test of waste rubber particles.
represent the rubber hydrocarbon molecule, the oxidation process oc- hydrocarbon molecular chain undergoes cross-linking, while the
curs in three stages. remaining oxide forms an oxide film (as observed in the SEM electron
In the initiation stage, the high temperature reduces the dissociation micrograph in Fig. 6). The chemical equations are as follows:
energy of the C-H bond on the rubber hydrocarbon, leading to C-H bond First stage: RH→R*
breaking (as shown by the change in the C-H stretching vibration peak Second stage:R*+O2→RO2；RO2+RH→ROOH+R*；ROOH→RO*
measured in the Fourier infrared spectroscopy). In the oxidation stage, a +ROO*
complex di-peroxide is generated (as seen from the change in the oxygen Third stage:2 R*→R-R；R*+ROO*→ROOR；2ROO*→non-free
content observed in the EDS, Fig. 8), while the decomposition reaction radical product
of ROOH generates free radicals. In the final stage, part of the rubber The formation of the oxide film and the improvement of the surface
12
Fig. 10. Mechanism of oxidized film formation of waste rubber particles.
cleanliness of the rubber particles optimize the interface bonding be- 3.2. Analysis of rubberized concrete performance
tween the rubber particles and the concrete base material, as shown in
Fig. 11. The impurities on the surface of untreated waste rubber particles 3.2.1. Working performance analysis
are in direct contact with the concrete base material, and these loose Collapse degree and air content are commonly used indicators for
impurities greatly affect the rubber particle-concrete base material evaluating the working performance of concrete, and the larger the
bonding interface, resulting in the loss of rubberized concrete collapse degree, the better the concrete mix fluidity and ease and har-
compressive strength. After high-temperature stirring treatment of mony. High air content, on the one hand, can improve the concrete mix
waste rubber particles, the surface impurities are encapsulated, and at fluidity, but too many holes in the concrete will lead to the appearance
the same time, an oxide film is formed, which improves the elastic of honeycomb-pockmarked concrete, which affects the strength of the
modulus of the waste rubber particles, optimizes the bonding interface concrete. Fig. 12 shows the data of concrete mix collapse (Fig. 12(a))
between the waste rubber particles and the concrete base material, and and air content (Fig. 12(b))[56].
improves the compressive strength of rubber concrete. From the figure, it can be seen that the collapse of rubber concrete
mixes prepared from untreated waste rubber particles (sample 0) is
56 mm, and the collapse of rubber concrete mixes prepared from high-
temperature stirring of pre-treated waste rubber is lower than this
Fig. 11. Mechanism of interfacial bonding between waste rubber particles and concrete base material.
13
Fig. 12. Rubber coagulum collapse and gas content (a. collapse; b. gas content).
value, of which the lowest values of the collapse occur in the stirring at 32.24 MPa and 41.16 MPa, respectively, which are 61.44 % and
250℃ for 30 min and 45 min (samples 4–2,4–3), and the collapse is 38.58 % higher than those of rubber concrete prepared from untreated
42 mm, compared to the collapse of concrete mixes prepared from un- waste rubber particles (sample 0), respectively. This is because the
treated waste rubber particles. The collapse is 42 mm, which is 25 % surface of waste rubber particles prepared by stirring for 30 min at 250
lower than that of the concrete mix prepared with untreated waste ℃ is smooth and free of impurities, which enhances the interfacial
rubber particles, indicating that the rubberized concrete mix prepared bonding of waste rubber particles with the concrete base material, and at
with high-temperature stirring pretreated waste rubber particles has the same time, a layer of hard oxidized film is formed on the surface of
deteriorated fluidity. waste rubber particles under the action of high-temperature stirring,
The collapse degree of rubberized concrete prepared by High- which strengthens the stiffness of waste rubber particles and improves
temperature stirred pretreatment of waste rubber particles shows a the compressive strength of rubberized concrete. In the 100 ℃ - 200 ℃
trend of decreasing and then increasing, which is consistent with the temperature range, the cubic compressive strength of rubber concrete
trend of air content. This is because the rubber concrete mix collapse and prepared by stirring treatment of waste rubber particles is higher than
air content are generally positively correlated[57]. Air content and that of the untreated waste rubber particles prepared rubber concrete,
waste rubber particles’ surface smoothness, untreated waste rubber but lower than the 250 ℃ conditions of stirring treatment of waste
particles’ surface roughness, easy to attach a large amount of air, these rubber particles prepared rubber concrete cubic compressive strength.
gases wrapped on the surface of the rubber particles to reduce the This is because the surface of the waste rubber particles in this tem-
mutual friction between the mortar, and therefore the collapse is large, perature range under the conditions of the oxidation film is not fully
the high-temperature stirring of pre-treated rubber particles prepared by formed and the presence of impurities on the surface affects the inter-
the waste rubber particles’ surface smoothness, the adsorption force of facial bond between the waste rubber particles and the concrete base
air is weak, the gas content is weak, and the air content is weak, and the material. The cubic compressive strength of rubber concrete prepared by
flowability of the rubber concrete mix becomes poorer. The surface of stirring waste rubber particles at 300℃ is lower than that prepared by
waste rubber particles prepared by high-temperature stirring pretreat- stirring waste rubber particles at 250℃. This is because the oxide film on
ment is smooth, with weak adsorption to air and low gas content, so the the surface of the waste rubber particles is destroyed at this temperature,
degree of collapse is reduced, and the trend is consistent with the phe- and the impurities on the surface of the waste rubber particles are re-
nomenon of surface smoothness change observed in the aforementioned exposed, resulting in poorer interfacial bonding between the surface of
electron microscope diagram of waste rubber particles. the waste rubber particles and the concrete substrate material. It is
noteworthy that under the same temperature conditions, the mechanical
3.2.2. Analysis of mechanical properties properties of rubber concrete prepared from waste rubber particles with
To further investigate the effect of high-temperature stirring pre- different stirring times vary. For example, using waste rubber particles
treatment of waste rubber particles on the mechanical properties of pre-treated at 250℃ with stirring times of 15 minutes, 30 minutes, and
rubber concrete, we test the cubic compressive strength, split flexural 45 minutes, the mechanical performance of the rubber concrete pre-
strength, axial compressive strength, and static compressive modulus of pared from these three groups shows an upward trend. This is because
elasticity of rubber concrete, as shown in Fig. 13. the longer the stirring time, the more noticeably the surface smoothness
As shown in Fig. 13(a) for the cubic compressive strength of rubber of the waste rubber particles improves, further enhancing the interface
concrete at 7 and 28 days of curing, it can be seen from the figure that bonding performance between the waste rubber particles and the con-
compared with the rubber concrete prepared from untreated waste crete materials.
rubber particles (sample 0), with the temperature elevation of the cubic As shown in Fig. 13(b) for the rubber concrete curing 7 days and 28
compressive strength of the rubber concrete prepared from treated days splitting tensile strength, it can be seen from the figure that,
waste rubber particles shows a trend of increasing first and then compared with the untreated waste rubber particles prepared rubber
decreasing. Among them, the 7-day and 28-day cubic compressive concrete (sample 0), with the temperature increase and stirring time
strengths of rubber concrete prepared from treated waste rubber parti- prolongation of the rubber concrete prepared by the treatment of waste
cles with 30-min stirring at 250℃ (sample 4–2) are the highest, reaching rubber particles, splitting tensile strength shows the trend of first
14
Fig. 13. Mechanical properties of rubberized concrete (a. cubic compressive strength; b. split tensile strength; c. axial compressive strength; d. static compressive
modulus of elasticity).
increasing and then decreasing. This trend is consistent with the trend of and 36.07 MPa, which are 85.61 % and 44.45 % higher than those of
the compressive strength of cubes at high temperatures, mainly with the rubber concrete prepared from untreated waste rubber particles (sample
high-temperature stirring pretreatment of waste rubber particles’ sur- 0), respectively.
face cleanliness and oxide film formation. The split flexural strength of Fig. 13(d) shows the static compressive modulus of elasticity of
rubber concrete prepared from waste rubber particles stirred for 30 min rubber concrete cured for 7 and 28 days, the modulus of elasticity is one
at 250℃ (sample 4–2) reaches 3.31 MPa and 4.95 MPa at 7 and 28 days, of the important mechanical parameters of concrete, characterizing the
which is 59.9 % and 67.79 % higher than that of rubber concrete pre- relationship between the stresses sustained and the strains generated
pared from untreated waste rubber particles (sample 0), respectively. under the concrete load, similar to the trend of the compressive strength
Fig. 13 (c) shows the axial compressive strength of rubber concrete of the cube, compared to the rubber concrete prepared from untreated
maintained for 7 days and 28 days, similar to the trend of cubic waste rubber particles (sample 0), and with the elevation of the tem-
compressive strength, compared with the rubber concrete prepared from perature and the prolongation of the stirring time of the treated Rubber
untreated waste rubber particles (sample 0), with the elevation of the concrete prepared from waste rubber particles static compressive
temperature and stirring time prolongation of rubber concrete prepared modulus of elasticity shows a trend of increasing and then decreasing,
from treated waste rubber particles cleavage flexural strength shows a mainly associated with high temperature stirring pretreatment of waste
trend of first increasing and then decreasing, mainly associated with rubber particles surface cleanliness and oxide film formation. The static
high temperature stirring pretreatment of waste rubber particles surface compressive modulus of elasticity of rubber concrete prepared from
cleanliness and oxide film formation. The 7-day and 28-day axial treated waste rubber particles (sample 4–2) with stirring for 30 min at
compressive strengths of rubber concrete prepared from waste rubber 250℃ reaches 30.76 MPa and 38.12 MPa at 7 and 28 days, which in-
particles with 30-min stirring at 250℃ (sample 4–2) reach 27.49 MPa creases by 61.8 % and 38.06 %, respectively, compared with that of
15
Fig. 14. Scanning electron microscope image of the bond between concrete matrix and rubber particles（0.No processed；1–1.100 ℃ stirring 15 min; 1–2.100 ℃
stirring 30 min; 1–3.100 ℃ stirring 45 min; 2–1.150 ℃ stirring 15 min; 2–2.150 ℃ stirring 30 min; 2–3.150 ℃ stirring 45 min; 3–1.200 ℃ stirring 15 min; 3–2.200
℃ stirring 30 min; 3–3.200℃ stirring 45 min; 4–1.250℃ stirring 15 min; 4–2.250℃ stirring 30 min; 4–3.250℃ stirring 45 min; 5–1.300℃ stirring 15 min;
5–2.300℃ stirring 30 min; 5–3.300℃ stirring 45 min).
rubber concrete prepared from untreated waste rubber particles (sample and the data from Fig. 8 showing the content of surface impurities
0). (where zinc and magnesium contents first decrease then increase within
150◦ C-300◦ C) and changes in oxygen content (where oxygen content
3.2.3. SEM Analysis first increases then decreases within the same temperature range). The
To directly observe the interfacial bonding between the waste rubber cleaner the surface of waste rubber particles and the lower the impurity
particles and the concrete matrix, scanning electron microscopy (SEM) content, the more complete the formation of the oxide film, which re-
analysis is carried out on the rubber concrete particles at the rubber sults in better interfacial bonding between the waste rubber particles
concrete fracture, which is taken from the debris at the fracture site of and concrete base materials.
the cubic compression test as shown in Fig. 14.
From Fig. 14, it can be clearly observed that there are very noticeable 4. Conclusion
gaps in the transition zone between the rubber particles of the rubber
concrete prepared with untreated waste rubber particles (Fig. 14(0)) and This study aims to improve the interfacial bonding properties and
the concrete matrix, indicating extremely poor interfacial bonding. This mechanical properties of rubber-concrete by pretreating waste rubber
is because the surface of untreated waste rubber particles is covered with particles with high-temperature stirring. The changes in rubber micro-
a large amount of impurities, which seriously affects the interface morphology and chemical components at different temperatures and
bonding between the rubber particles and the concrete materials. This is stirring times are investigated and compared, and the oxidation reaction
observed in the phenomenon shown in the electron microscope image in mechanism of waste rubber particles under the action of high temper-
Fig. 6(a large amount of loose impurities distributed on the surface of ature is discussed. Using waste rubber particles to replace fine aggregate
untreated waste rubber particles) and confirmed by the impurity with 20 % content volume to prepare rubberized concrete, evaluating
element content in Fig. 8 (Zn and Mg content reaching 2.9 %).Under the working performance of rubberized concrete mix, mechanical
temperature conditions of 100 ℃ (Fig. 14 (1− 1, 1− 2, 1− 3)), processed properties of rubberized concrete, verifies the effectiveness of the pre-
waste rubber particles prepared rubber-concrete interface still exhibit treatment method of waste rubber particles, the main conclusions are as
larger gaps. At 150 ℃ temperature conditions (Fig. 14 (2− 1, 2− 2, follows:
2− 3)), treated waste rubber particles prepared rubber-concrete inter- 1. After high-temperature stirred pretreatment, some of the small
face has been improved, but there are still gaps. When the temperature molecule organic matter on the surface of waste rubber particles vola-
reaches 200 ℃ (Fig. 14 (3− 1, 3− 2, 3− 3)), the treated waste rubber tilizes, some of the loose impurities are removed by friction and extru-
particles prepared rubber-concrete interface has greatly improved, with sion, and some of the impurities are covered by viscous fluid rubber
no obvious gap between the rubber particles and the concrete matrix. At hydrocarbon, the surface cleanliness of the waste rubber particles is
250 ℃ temperature conditions (Fig. 14 (4− 1, 4− 2, 4− 3)), the treated greatly improved, and the rubber hydrocarbon on the surface of the
waste rubber particles prepared rubber-concrete interface is very close, rubber particles undergoes an oxidation reaction to form a hard oxidized
due to the surface cleanliness of the waste rubber particles treated at this film.
temperature, and the formation of a high degree of hardness oxide film. 2. In the temperature range of 100 ℃ - 300 ℃, the surface cleanliness
This is the reason for the improved mechanical properties of the rubber- of waste rubber particles shows a trend of improvement and then
concrete prepared using waste rubber particles treated at this temper- deterioration. Among them, 250 ℃, stirring for 30 minutes conditions
ature. However, when the temperature reaches 300 ℃ (Fig. 14 (5− 1, prepared under the conditions of waste rubber particles smooth surface
5− 2, 5− 3)), the treated waste rubber particles prepared rubber-concrete without impurities, the oxidation film is fully formed.
bond interface deteriorates. This is because, at this temperature, the 3. High-temperature stirring pretreatment of waste rubber particles
surface oxide film of the waste rubber particles undergoes pyrolysis, prepared by the rubber concrete mix performance is slightly worse than
leading to the disappearance of the oxide film and poor surface the untreated waste rubber particles prepared by the rubber concrete
cleanliness. mix, with the temperature and stirring time extending, the caving degree
Based on the above phenomena, conclusions can be drawn by and gas content are first reduced and then improve the trend.
combining the observations from Fig. 6 on the surface morphology of 4. The mechanical properties of rubber concrete prepared from waste
waste rubber particles prepared under different temperatures and pre- rubber particles pretreated with high-temperature stirring initially
treatment durations (where surface cleanliness improves between increased and then decreased with the rise in temperature. Compared to
150◦ C-250◦ C with increased temperature, but deteriorates at 300◦ C), rubber concrete made with untreated waste rubber particles, the rubber
16
concrete prepared from pretreated waste rubber particles (stirred at [8] B.S. Thomas, S. Kumar, P. Mehra, R.C. Gupta, M. Joseph, L.J. Csetenyi, Abrasion
resistance of sustainable green concrete containing waste tire rubber particles,
250℃ for 30 minutes) exhibited the best mechanical performance.
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Ethical approval Buildings 12 (11) (2022) 1975.
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strength concrete containing recycled rubber, Constr. Build. Mater. 227 (2019)
This work was supported by the Key Research and Development Plan 116660.
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other people or organizations that can inappropriately influence our Constr. Build. Mater. 171 (2018) 467–473.
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Contents lists available at ScienceDirect

Construction and Building Materials

Studies on the mechanical properties of rubber concrete reinforced with

2. Materials and programs 2.4. Test methods

0 No processed 1100 55 537.6 1173 420 168 3.7

testing machine, ensuring geometric alignment.③Control the loading

Fig. 3. TGA of pretreated waste rubber pellets.

Fig. 5. FT-IR of waste rubber particles.

Fig. 7. EDS analysis of waste rubber pellets.

Fig. 8. Impurities and oxygen content in waste rubber pellets.

Fig. 9. WCA test of waste rubber particles.

Fig. 10. Mechanism of oxidized film formation of waste rubber particles.

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