Journal of Hazardous Materials xxx (xxxx) xxx

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Journal of Hazardous Materials

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

Research Paper

Heavy-ion irradiation effects on uranium-contaminated soil for

nuclear waste
Guilin Wei a, Wenhong Han b, Xiaoyan Shu b, c, *, Fen Luo b, c, Hexi Tang d, Shunzhang Chen e,
Lan Wang f, Yi Xie f, g, Xirui Lu a, b, c, **
a
State Key Laboratory of Environmental Friendly Energy Materials, Southwest University of Science and Technology, Mianyang Sichuan 621010, PR China
b
Fundamental Science on Nuclear Wastes and Environmental Safety Laboratory, Southwest University of Science and Technology, Mianyang 621010, PR China
c
Collaborative Innovation Center of Nuclear Wastes and Environmental Safety, Southwest University of Science and Technology, Mianyang 621010, PR China
d
Sichuan Radiation Detection & Protection Institute of Nuclear Industry; Chengdu 610052, PR China
e
Institute of Nuclear Science and Technology, Sichuan University, Chengdu 610064, PR China
f
University of Science and Technology of China, Hefei 230026, PR China
g
Institute of Plasma Physics, Chinese Academy of Sciences, Hefei 230031, PR China

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

Keywords: In the field of radioactive waste immobilization, the investigation of irradiation stability is of considerable
Contaminated soil importance. In this study, uranium-contaminated soil samples were irradiated by 1.5 MeV Xe20+ ions with flu­
Uranium ences ranging from 1 × 1012 to 1 × 1015 ions/cm2. Xe20+ heavy-ion radiation was used to simulate the self-
Irradiation effects
irradiation of actinide nuclides. The uranium-contaminated soil samples were sintered via microwaves. Graz­
Chemical durability
ing incidence X-ray diffraction results showed that irradiation can cause crystallization of the sample. After
Microwave
irradiation, the Vickers hardness of the samples decreased slightly. Comparative analysis showed that the sample
had good radiation resistance, and the leaching rate (28 d) of the sample increased slightly after irradiation, but
the overall performance was stable. Our investigation reveals the corresponding mechanism of uranium-
contaminated soil irradiation of 1.5 MeV Xe20+ ions.

1. Introduction In situ vitrification (ISV) has been effectively used to transform

In the past several decades, the application of nuclear technology in
national defense has inevitably caused radionuclide pollution to the soil
around nuclear test sites (Zhu and Shaw, 2000; Willey and Chris, 2007;
Liu et al., 2020a, 2021). In complex soil systems, the bioavailability and
mobility of soil radioisotopes can directly or indirectly affect the
geochemical, biological, and hydrological processes, and ultimately
affect the ecological quality and human health (Zhang et al., 2002). In
particular, uranium-contaminated soil is highly radioactive and
threatens the ecological environment and human health (Zhang et al.,
2019). Therefore, it is urgent to dispose of these radioactive contami­
nated soils. The method of immobilization can inhibit radionuclide
movement, thus protecting the surrounding environment (Chen et al.,
2019; Liu et al., 2020b, 2017; Wang et al., 2020).
radioactive contaminated soil into a vitrified matrix since it was
developed by the Pacific Northwest Laboratory (PNL) in 1980 (Buelt and
Farnsworth, 1991; FitzPatrick et al., 1984; Brouns and Timmerman,
1982; Marques et al., 2011; Jacobs et al., 1988). This method has the
advantages of a lack of excavation, minimal disturbance to the
contaminated site (He et al., 2015); however, it is also characterized by
the disadvantages of high power and time consumption (Dragun, 1991),
and difficulty in guaranteeing the uniformity of the matrix (Dixon et al.,
2015). Phytoremediation is often used to treat radioactive contaminated
soil. Entrya et al. (1999) showed that the use of arbuscular mycorrhizal
fungi or intercropping with grasses may be a feasible and relatively low-
cost strategy for the remediation and recovery of radionuclide-
contaminated sites. The Joule heating method and microwave sinter­
ing have also been used to stabilize radioactive contaminated soil.

* Corresponding author at: Fundamental Science on Nuclear Wastes and Environmental Safety Laboratory, Southwest University of Science and Technology,
Mianyang 621010, PR China.
** Corresponding author at: State Key Laboratory of Environmental Friendly Energy Materials, Southwest University of Science and Technology, Mianyang Sichuan
621010, PR China.
E-mail addresses: shuxiaoyanmvp116@163.com (X. Shu), luxiruimvp116@163.com (X. Lu).

https://doi.org/10.1016/j.jhazmat.2020.124273
Received 5 August 2020; Received in revised form 9 October 2020; Accepted 10 October 2020
Available online 24 October 2020
0304-3894/© 2020 Elsevier B.V. All rights reserved.

Please cite this article as: Guilin Wei, Journal of Hazardous Materials, https://doi.org/10.1016/j.jhazmat.2020.124273
G. Wei et al.
Compared with the Joule heating method, microwave sintering has the
advantages of fast heating and a short sintering time (Demirskyi et al.,
2013; Wilson and Kunz, 2010). Microwaves have been used to immo­
bilize radioactive contaminated soil in our previous work, and the re­
sults showed that this sintering method also has the advantage of
improving the stability of the radioactive contaminated soil (Zhang
et al., 2017; Zhang et al., 2016). In our previous work (Chen et al., 2019;
Shu et al., 2020), microwave sintering was used to immobilize uranium-
contaminated soil, and the immobilization mechanism was investigated.
However, as an important parameter of the radioactive waste solidified
matrix, the radiation stability of the sintered matrix is not clear. Thus,
obtaining the corresponding irradiation mechanism of uranium-
contaminated soil after microwave sintering is significant.
In this work, uranium-contaminated soils were first sintered via
microwaves. To understand the effect of irradiation on the matrix, 1.5
MeV Xe20+ ions were used to irradiate three types of sintered samples for
comparison. Grazing incidence X-ray diffraction (GIXRD) was employed
to characterize the phase evolution as a function of irradiation fluence. A
Vickers hardness test was used to evaluate the mechanical properties of
the samples before and after irradiation. The heavy-ion irradiation-
induced elemental distribution of uranium was investigated. Finally, the
influence of irradiation on the stability of the sample was revealed by a
leaching test.
2. Experimental details
2.1. Preparation of the original samples
Saline-alkali soil was selected as the cured substrate, which was
collected in Gansu Province, China. The elemental composition patterns
are shown in Table 1. To remove moisture and volatile matter, the
saline-alkali soil was pretreated for 6 h at 600 ℃. AR-grade
UO2(NO3)2⋅6 H2O was purchased to simulate uranium waste.
UO2(NO3)20.6 H2O is decomposed into UO3 and finally transformed to
U3O8 when heated, and the main valence states are + 3 and + 4, which is
more similar to the real uranium-contaminated soil (Kulyukhin et al.,
2009; Rudel and Florian, 2017). The uranium contents were 0, 500, and
50,000 μg/g, and each mixed sample weighed 20 g; the details are given
in Table 2. The simulated uranium-contaminated soil samples were
sintered at 1300 ℃ via a microwave sintering furnace. After sintering for
30 min, the samples were naturally cooled to approximately 25 ℃. The
sample preparation process is shown in Fig. 1.
2.2. Irradiation experiment
At the Institute of Modern Physics, Chinese Academy of Sciences,
heavy-ion irradiation experiments were conducted using a 320 kV
multi-discipline research platform for highly charged ions. The sliced
sample (8 mm × 8 mm × 1 mm) was irradiated on the target of a vac­
uum chamber with fluences ranging from 1 × 1012 to 1 × 1015 ions/cm2
with a flux of 5 × 1011 ions/(cm2 s). The 1.5 MeV Xe20+ ions were
implanted vertically on the sample surface. A schematic of the 320 kV
high-voltage platform and high vacuum terminal is shown in Fig. 2.
2.3. Characterizations
Under Cu Kα radiation (λ = 1.5406 Å), the phase of the sintered
Table 1
Elemental composition of saline-alkali soil.
Soil SiO2 Al2O3 Fe2O3 CaO MgO K2O Na2O TiO2
Saline- 60.44 14.27 11.27 5.41 2.95 2.44 1.56 0.73
alkali
soil (wt
%)
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Journal of Hazardous Materials xxx (xxxx) xxx
Table 2
Experimental design of uranium-contaminated saline-alkali soil.
Soil Uranium element (μg/ Soil content Uranium content
g) (g) (g)
Saline-alkali 0 20.0000 0.0000
soil 500 19.9882 0.0118
50,000 18.8207 1.1793
samples was obtained using GIXRD (X′ Pert PRO, Netherlands). At a
scanning speed of 2◦ /min, the data were collected in the 2θ range of
5–80◦ . Irradiation samples were carefully polished to obtain a flat
indentation face. The Vickers hardness was tested using a Vickers
hardness tester (TMVS-1S, China). The microstructure and elemental
distribution of the samples were characterized by scanning electron
microscopy (SEM; Ultra 55, Germany). The chemical stability of the
samples was tested by the MCC-1 method. The sintered samples before
and after irradiation were placed in deionized water at ambient tem­
perature (25 ℃). The normalized leaching rate (LRi, g/(m2⋅d)) of ura­
nium was calculated by the following equation (Xie et al., 2017; ASTM,
2010):
Ci ⋅V
LRi =
A⋅fi ⋅T
where Ci is the tested result of the concentration of element i which was
analyzed using an inductively coupled plasma mass spectrometer (ICP-
Mass, Agilent 7700x, Agilent, USA), V (m3) represents the volume of the
leachate, A (m2) represents the area of the sample surface, fi (wt%) is the
mass fraction of element i, and T (d) represents the leaching day.
3. Results and discussion
3.1. Phase evolution and structural analysis
The uranium-contaminated soil samples were firstly obtained, and
the results are shown in Fig. 3(a). All three samples sintered at 1300 ℃
showed no continuous or discrete sharp peaks, which was characteristic
of an amorphous glass structure (Sidek et al., 2009). This phenomenon
indicated that all the uranium was immobilized in the glass structure via
microwave sintering. However, under the irradiation condition, the
crystallization of the sample was clear. Fig. 3(b) shows the sample with
50,000 μg/g of uranium-contamination irradiated with 1.5 MeV Xe20+
ions at a fluence of 1 × 1012–1 × 1015 ions/cm2. The pure sintered
sample irradiated at a fluence of 1 × 1012 ions/cm2 maintained a glassy
phase. With increasing irradiation fluence, a slightly crystallization of
quartz (PDF#46–1045) was noted under fluences of 1 × 1013 and
1 × 1014 ions/cm2. The crystallization behavior was clearer for the
sample irradiated at a fluence of 1 × 1015 ions/cm2. For the samples
with 500 μg/g of uranium-contaminated irradiated with 1.5 MeV Xe20+
ions to a fluence of 1 × 1012–1 × 1015 ions/cm2 (Fig. 3(c)), the same
phenomenon was observed for the sample without uranium contami­
nation. However, the crystallization of quartz was not obvious for the
samples without uranium contamination. For the sintered sample, no
crystallization phenomenon was observed (Fig. 3(d)). Combined with
the results, the irradiated samples with a greater amount of uranium was
more inclined to be damaged under irradiation with 1.5 MeV Xe20+ ions.
After irradiation, the structure of the glass sample was affected, which
might have caused the crystallization of quartz (Kilymis and Delaye,
2014; Delaye et al., 2011).
3.2. Vickers hardness analysis
To investigate the irradiation effect on the three types of samples,
namely the blank sample and two uranium-contaminated samples (500
and 50,000 μg/g), the Vickers hardness results are shown in Fig. 4. All
samples were tested six times to obtain the average value. The three
G. Wei et al.
Fig. 1. Sample fabrication process.
Fig. 2. Schematic of the 320 kV high-voltage platform and high vacuum terminal.
types of samples presented the same change trend, in which the hardness
decreased as the fluence increased. For the blank sample, the Vickers
hardness decreased from 6.56 GPa to 6.51 GPa. The Vickers hardness
results of uranium-contaminated samples (500 and 50,000 μg/g)
decreased from 6.61 GPa and 6.88–6.57 GPa and 6.80 GPa, respec­
tively. In addition, it can be conducted form Fig. 4 that the slight vari­
ation resulted from the heavy-ion irradiation fluences. Under the sample
irradiation fluence, the samples with higher uranium contamination
showed higher Vickers hardness results. For the sample without irradi­
ation, the Vickers hardness of the blank sample was 6.56 GPa, while that
of the uranium-contaminated sample (50,000 μg/g) was 6.88 GPa. Even
under the highest irradiation fluence (1 × 1015 ions/cm2), the Vickers
hardness values of the samples with uranium contamination were higher
than that of the blank sample, and the higher the uranium contamina­
tion, the higher the Vickers hardness. Therefore, it can be concluded that
the doped uranium is beneficial to Vickers hardness improvement. Shu
et al. (2017) reported that with an enhanced waste doping content, the
Vickers hardness shows a clear increase. Moreover, all the Vickers
hardness values in this study were higher than those reported in the
literature; for example, the Vickers hardness of Na-Ca(Pb, Al)-Si glasses
is approximately 2.70–6.30 GPa (Yamane and Mackenzie, 1974) and
that of soda glass is approximately 5.30 GPa as reported by Marsh
(1964) and 5.67 GPa as reported by Yoshioka and Yoshioka (1995).
3
Journal of Hazardous Materials xxx (xxxx) xxx
3.3. Microstructure analysis by SEM-EDS
To investigate the effect on uranium immobilization at the highest
irradiation fluence (1 × 1015 ions/cm2), the SEM-EDS results of the
sample with the highest uranium contamination (50,000 μg/g) are
shown in Fig. 5. Fig. 5(a) shows that the surface of the sample was
smooth without any pores or cracks. Fig. 5(b–e) presents the elemental
distributions of Al, Si, O, and U, respectively. All the detected elements
were distributed uniformly, thereby indicating that the uranium waste
was immobilized in the irradiated sample. This is consistent with the
GIXRD result, which showed that no uranium-related phase could be
detected in this sample. Combined with the GIXRD results of other
samples, there was no clear uranium-related phase, and it could be
concluded that the uranium waste was immobilized in the sintered
samples.
3.4. Chemical stability of sintered samples
Considering the importance of chemical stability, the leaching
behavior of uranium was characterized by the MCC-1 method. The LRU
of the sample contaminated with 50,000 μg/g of uranium was investi­
gated. After 28 d, the LRU of the sample without irradiation was
3.20 × 10− 5 g/(m2 d). For the sample irradiated with 1.5 MeV Xe20+
ions at a fluence of 1 × 1015 ions/cm2, on the 28th d, the LRU was
5.10 × 10− 5 g/(m2 d). After irradiation, the LRU was higher than that of
the sample without irradiation. Aloy et al. (2004) used borosilicate
G. Wei et al. Journal of Hazardous Materials xxx (xxxx) xxx

Fig. 3. GIXRD patterns of sintered samples: (a) samples contaminated with different contents of uranium without irradiation and (b) 50,000 μg/g; (c) 500 μg/g; (d)
0 μg/g samples irradiated with 1.5 MeV Xe20+ ions at a fluence of 1 × 1012–1 × 1015 ions/cm2.

glasses to immobilize uranium waste, and the leaching rate of uranium

(28 d) was investigated by the MCC method. Xie et al. (2020) deter­
mined the leaching rate of uranium in uranium-rich glass ceramics. All
the details are listed in Table 3. Compared with the reported literatures,
the LRU for the unirradiated and irradiated samples presented adequate
results. In short, the matrix (before and after irradiation) sintered via
microwave showed considerable chemical durability.

3.5. Discussion

It is essential to understand the effect of irradiation on the hardness

of glass samples. Yang et al. (2013) investigated the effect of electron
irradiation on the hardness of borosilicate glass and found that the
hardness of the irradiated glass decreased by approximately 4.0%. In the
study conducted by Abbas et al. (2000), the hardness of alumino-
borosilicate glass decreased by approximately 20.0% after irradiation
by 2.1 MeV Kr3+ ions. Weber and Matzke (1986) conducted irradiation
experiments on simulated waste glass with α particle and found that the
hardness of the glass decreased by approximately 15.0% after irradia­
tion. In this work, the hardness of the blank glass sample declined by
approximately 0.8% at the highest fluence (1 × 1015 ions/cm2). The
Fig. 4. Vickers hardness results of the blank sample (0 μg/g) and uranium-
hardness of the uranium-contaminated glass samples (500 and
contaminated samples (500 and 50,000 μg/g) irradiated with 1.5 MeV Xe20+
ions at a fluence of 1 × 1012–1 × 1015 ions/cm2.
50,000 μg/g) decreased by approximately 0.6% and 1.2%, respectively.
The sintered samples prepared in this work had good irradiation sta­
bility, and the decrease in hardness was lower than that reported in the
literatures (Yang et al., 2013; Abbas et al., 2000; Weber and Matzke,

4
G. Wei et al. Journal of Hazardous Materials xxx (xxxx) xxx

Fig. 5. SEM-EDS results of uranium-contaminated samples (50,000 μg/g) irradiated with 1.5 MeV Xe20+ ions at a fluence of 1 × 1015 ions/cm2: (a) SEM and
elemental distributions of (b) Al, (c) Si, (d) O, and (e) U.

Table 3
Comparison of the leaching rate among reported studies.
Materials Uranium waste content Sintering temperature (℃) Leaching time (d) LRU g/ (m2 d)

Borosilicate glasses (Aloy et al., 2004) 10.9–13.3 wt% 1300–1350 28 0.03–0.18

Glass-ceramics (Xie et al., 2020) 9.6–23.9 wt% 1550 21 1.06 × 10− 4–6.70 × 10− 5
This study 50,000 μg/g 1300 28 3.20 × 10− 5 (unirradiated)
5.10 × 10− 5 (irradiated)

reason for the increase in LRU after irradiation compared with that of the
Table 4
unirradiated sample. Moreover, the quartz phase detected in the GIXRD
Comparison of reduced hardness among reported studies.
results might have been affected by the change in the microstructure
Material Irradiation Fluence Reduction (%) Ref. after irradiation, and the schematic is shown in Fig. 6. For the sintered
type
matrix with lower uranium content, there was less uranium waste
Borosilicate 0.5 MeV He 109 Gy 4.0 Yang et al., immobilized in the glass structure, and its stability was high. For the
glass ions 2013
sample that immobilized higher uranium content, the glass structure
1.2 MeV 14.0
electrons was unstable, and it was more vulnerable to radiation damage (Lu et al.,
Alumino- 2.1 MeV 4.36 × 1015 Approximately Abbas 2019). This could also explain the decrease in the Vickers hardness and
borosilicate Kr3+ ions ions/cm2 20.0 et al., the increase in the leaching rate. After irradiation, the leaching rate of
glasses 2000 uranium increased slightly but was sufficiently low compared with those
Simulated α particles / 15.0 Weber and
in other studies (Table 3), which indicates that microwaves are suitable
waste glass Matzke,
1986 for immobilizing uranium-contaminated soil.
Glass without 0.5 MeV 1 × 1015 0.8 This study
uranium Xe20+ ions ions/cm2
3.6. Practical implications of this study
Glass with 0.6
500 μg/g
uranium The phase, morphology, mechanical prosperity, and leaching resis­
Glass with 1.2 tance of uranium-contaminated soil samples under simulated self-
50,000 μg/g irradiation were studied using 1.5 MeV Xe20+ heavy-ion irradiation.
uranium
The results showed that the uranium-contaminated soil sintered by
microwaves had good irradiation stability. Simultaneously, the feasi­
1986). All the details are listed in Table 4. The formation of bubbles after bility of microwave sintering for uranium-contaminated soil treatment
irradiation is considered a possible reason for the decrease in glass was verified. However, before determining its practical significance,
hardness (Abbas et al., 2000; Weber and Matzke, 1986). However, no considerable research still needs to be conducted. Based on the current
clear bubbles were observed from the SEM results in this work. After research results, future work can focus on the comprehensive radiation
irradiation, the change in the microstructure of the glass sample also stability (including α irradiation and neutron irradiation). Considering
influenced the hardness value (Yuan et al., 2017). Delaye et al. (2011) the complexity of soil types and nuclide contamination in real nuclear
and Kilymis and Delaye (2014) simulated the irradiation effect of bo­ test sites, the radiation stability of other soil (gray desert soil, aeolian
rosilicate glass using the molecular dynamics method, and explained the sandy soil, etc.) and contaminated nuclides (137Cs, 90Sr, etc.) after mi­
micro-mechanism of hardness decline. The fracture of the network body crowave treatment should also be studied in order to obtain compre­
related to silicon in the borosilicate glass network is considered the hensive information before practical application.
reason for the decrease in hardness. Uranium waste was immobilized in
the glass structures. After the irradiation process, part of the glass 4. Conclusions
structure was broken under the effect of Xe20+ ions, which was also the
The roles of heavy-ion irradiation with fluences ranging from

5
G. Wei et al.
Fig. 6. Schematic diagram of the effect of irradiation on the glass microstructure.
1 × 1012–1 × 1015 ions/cm2 in sintered uranium-contaminated soil
samples (0, 500, and 50,000 μg/g) were investigated via GIXRD, Vickers
hardness, and SEM-EDX, and the chemical stability was determined by
the MCC-1 method. The GIXRD results showed that heavy-ion irradia­
tion can cause the crystallization of quartz in the glass phase. The higher
uranium content might enhance the crystallization. The Vickers hard­
ness decreased (0.6–1.2%) as the heavy-ion irradiation fluences
increased. At the highest irradiation fluence, uranium was distributed
uniformly in the sintered sample. After 28 d of leaching experiments, the
matrix presented reliable chemical stability and the LRU increased
slightly after heavy-ion irradiation, which might have been affected by
the change in the microstructure after irradiation. Based on the analyses
above, microwaves are suitable to disposal of uranium contaminated soil
to obtain a stability waste matrix.
CRediT authorship contribution statement
Guilin Wei: Writing - original draft, Writing - review & editing,
Methodology, Investigation, Formal analysis. Wenhong Han: Formal
analysis, Investigation, Writing - review & editing. Xiaoyan Shu:
Investigation, Writing - review & editing. Fen Luo: Methodology,
Writing - review & editing. Hexi Tang: Data curation. Shunzhang
Chen: Investigation. Lan Wang: Data curation. Yi Xie: Investigation.
Xirui Lu: Conceptualization, Funding acquisition, Data curation,
Writing - review & editing.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgments
The authors appreciate the experimental support provided by the
320 kV platform of the Institute of Modern Physics, Chinese Academy of
Sciences and the financial support provided by the National Natural
Science Foundation of China (No. 21677118) and the Project of State
Key Laboratory of Environment-Friendly Energy Materials, Southwest
University of Science and Technology (No. 18fksy0213).
6
Journal of Hazardous Materials xxx (xxxx) xxx
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