J Radioanal Nucl Chem (2015) 304:859–865
DOI 10.1007/s10967-014-3850-2
Illite-supported nanoscale zero-valent iron for removal of
from aqueous solution: characterization, reactivity
and mechanism
Chen Jing • Yilian Li • Ruiping Cui •
Jiali Xu
Received: 16 October 2014 / Published online: 21 December 2014
Ó Akadémiai Kiadó, Budapest, Hungary 2014
Abstract In this work, illite was used to support zero-
valent iron nanoparticles to remove 238U in aqueous solu-
tions. Compared to nZVI, I-nZVI shows high stability and
removal efficiency. Removal process of U on I-nZVI can
be concluded into four stages in illite dominated zone, Fe0
released zone, ferrous dominated zone and reaction equi-
librium zone. The study shows that illite is a good dis-
persant and stabilizer which decreases the aggregation of
nZVI and improves the activity of Fe0. Removal capacity
of U on I-nZVI achieves 1.79 lg/mg. I-nZVI is an efficient
and promising remediation material for waste-soluble
uranium compounds.
Keywords Uranium
Zero-valent iron
Illite

Nanoscale
Characterization
Introduction
Uranium is an actinide element naturally existing in rocks
and soils [1–3]. Since ancient times, uranium has been used
as a colorant in ceramic glazes and glassmaking industry
[4]. Nowadays uranium is a major contaminant in soils,
sediments, and groundwater through anthropogenic activ-
ities such as mining operations, ore processing, coal com-
bustion and nuclear fuel processing [5]. The main oxidation
states of uranium in natural water systems are U(IV) and
U(VI). U(IV) is low solubility and always appears in
reducing aquatic environment such as uranium ore [6].
Dissolved U(VI) mainly occurs as uranyl ions (UO22?)
C. Jing
Y. Li (&)
R. Cui
J. Xu
School of Environmental Studies, China University of
Geosciences, Wuhan 430074, China
e-mail: yl.li@cug.cn
238
U
which is most toxic and radioactivity heavy metal [7]. In
the United States, a national survey about radionuclide
concentrations in community water supplies shows that
uranium is present in drinking-water sources in circum-
stances [8]. The majority intake of uranium to human can
be through drinking-water [9]. In 2004, the World Health
Organization (WHO) has regulated the maximum concen-
tration level of uranium in drinking water, 15 ng/mL [10].
Recently, zero-valent iron nanoparticles (nZVI) have
been widely studied for the remediation of groundwater
and other environmental matrices [11–13]. The advantages
of nZVI facilitate remediation of hazardous wastes con-
tamination that the small particle size and large surface
area per unit mass of nanoparticles [12, 14–16]. Nanoscale
zero-valent iron has the potential for efficient and cost
effective remediation of contaminated solutions [13, 17–
19]. However, the frequent aggregation of nZVI reduces its
efficiency [20, 21]. Technologies have been improved
using porous materials as mechanical supports to enhance
the dispersibility of nZVI particles [22–24]. Recently,
nZVI supported by natural clays such as zeolite [25, 26],
kaolinite [23, 27], and bentonite [22, 28, 29] has been
employed to increase the durability and mechanical
strength of nZVI and investigated for the removal of var-
ious heavy metals such as Pb2?, Cu2?, Co2?, and Cr6? ions
from aqueous solutions [22, 23, 27, 28, 30]. Illite is a
stable, high load-carrying capacity, low-cost clay mineral,
and a good adsorbent to remove heavy metals in solution
[31–33]. It can decrease the aggregation, improve the
activity and carrying capacity of nZVI to use illite as a
support material to load nZVI. Illite [34–36] and Fe [37,
38] have been always found in uranium deposits. It has the
possibility for uranium ore formation while using I-nZVI as
Permeable Reactive Barriers in remediation of uranium. It
is of great value to do the present study which has quite an
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important reference for the treatment of uranium-contained
water.
The basic objectives of this paper are: (1) synthesized
and characterized I-nZVI by X-ray diffraction (XRD) and
scanning electron microscopy (SEM) to determine its
chemical constituents and crystal structure; (2) removal of
U by various materials (illite, nZVI and I-nZVI) were
performed to demonstrate the advantages of I-nZVI; (3)
removal process of U on I-nZVI was investigated under
experimental conditions; and (4) FTIR spectra for I-nZVI
samples during the reaction were scanned to analyze the
mechanisms of U removal on I-nZVI.
Materials and methods
Materials
The sample of illite was obtained from Hebei Province, the
north of China. After drying at 80 °C overnight, illite
sample was ground and sieved through a 200 mesh screen
prior to use in experiments. Iron(III) chloride hexahydrate
(FeCl3
6H2O) and sodium borohydride (NaBH4) were
purchased from Sinopharm Chemical Reagent Co.
(Shanghai, China). U stock solution was prepared by dis-
solving uranyl nitrate hexahydrate (UO2(NO3)2
6H2O) in
TKA-GenPure purified water (Thermo Fisher Scientific.,
Pittsburgh, PA). All the chemicals used in the experiments
were purchased in analytical purity grade and used without
further purification. The TKA-GenPure purified water was
used in all the experiments.
Synthesis of nZVI and I-nZVI
The nZVI/I-nZVI were prepared by the conventional
liquid-phase sodium borohydride reduction of ferric iron
(Fe3?) with/without illite as a support material. The I-nZVI
materials were synthesized as the Fe:illite mass ratio 1:1.
Illite (2.00 g) was prepared in a three-necked open flask,
and a solution of FeCl3
6H2O (9.66 g) in ethanol–water
(50 mL, 4:1 v/v) was added. The mixture was vigorous
stirred for 30 min to insure illite in a homogeneous dis-
tribution. Subsequently, a previously prepared NaBH4
solution (3.54 g of NaBH4 in 100 mL) was carefully added
into the mixture. The resulting mixture continued stirring
for 30 min. The prepared materials were separated from the
liquid phase through a vacuum filtration. The entire process
was carried out under a N2 atmosphere to avoid the oxi-
dation of zero valent ion nanoparticles. The black solid
products were vacuum dried at 65 °C overnight. The nZVI
and I-nZVI samples were stored in sealed brown bottles
under dry conditions.
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Batch experiments
Experiments were carried out under ambient conditions by
batch technique. Uranium removal procedures were
undertaken in a scale of 2 mg I-nZVI with 20 mL U
aqueous solution in 50 mL centrifugal tube. Reaction
mixtures were placed on a rotary shaker at 25 °C and
mixed at 250 rpm for 3 h. Then the mixture was filtered
through a 0.22 lm mixed cellulose ester membrane (to
remove the bulk of suspended particulates) and analyzed
by Inductively Coupled Plasma Mass Spectrometry (ICP-
MS) for concentration of 238U and total iron. The control
experiments were conducted in parallel. All the experi-
ments were carried out in triplicate. The relative errors of
the data were about 5 %.
Characterization
The concentration of total 238U and Fe in solution were
determined using an ELAN DRC-II (PE SCIEX., Waltham,
MA) ICP-MS. Surface topography was recorded by means of
SEM with scanning microscope type SU8010 (Hitachi.,
Tokyo, Japan), operating at an accelerating voltage of 10 kV
and electron beam current of about 15 lA. Prior to the
measurements, samples were coated with thin gold layers.
The XRD pattern of the sample was obtained using a D8
advance diffractometer (Bruker., Karlsruhe, Germany)
equipped with a LynxEye detector using Ni-filtered Cu Ka
radiation (l = 0.15406 nm). The diffractometer was oper-
ated at a tube voltage of 40 kV and a current of 40 mA. XRD
spectra were acquired between 2h angles of 5°–70°. The N2-
BET surface area were detected by micromeritics ASAP
2020 Chemisorption Surface Area Analyzer (Micromeritics
Instrument Corp., Norcross, GA). The FTIR spectra of
I-nZVI samples were obtained using a FTIR (Nicolet 6700,
Thermo Corp., USA). Samples for determination were pre-
pared by mixing 1 % (w/w) specimens with 100 mg of KBr
powder and pressing the mixture into a sheer slice. Following
this the average over 9 scan was collected for each mea-
surement with a resolution of 2/cm. All samples had been
dried under vacuum at 60 °C for 12 h before testing.
Results and discussion
Characterization
The SEM images show the morphology and distribution of
illite, nZVI and I-nZVI (Fig. 1). Figure 1a displays the
surface of illite is plate-like crystals stacked in the layer
structure. This plate-like surfaces provide load space for
nZVI and make illite a good support material. Morphology
of synthesized nZVI is shown in Fig. 1b. The picture of
J Radioanal Nucl Chem (2015) 304:859–865 861

Fig. 1 SEM scanning images of samples. a Illite; b nZVI; c, d I-nZVI

nZVI reveals the aggregation of nZVI as a coral formation

which could cause less reduction activity and mobility of
nZVI. Figure 1c, d represent synthesized I-nZVI in dif-
ferent scales. These two photos show that iron nanoparti-
cles disperse evenly on the surface and edges of illite.
Those pictures clearly demonstrate the aggregation of
nZVI is eliminated and provide a good example of nZVI
loaded on the surface of illite. It’s the main purpose of this
study that Fe0 nanoparticles immobilize on illite to
decrease the aggregation of Fe0 nanoparticles and increase
its mechanical strength.
The XRD patterns of illite, nZVI and I-nZVI samples
are shown in Fig. 2. As shown in Fig. 2a, the main peaks at
2h of 8.91°, 20.94° and 26.72° are the characteristic dif-
fraction peaks for natural illite [39]. The other peaks
marked by Q are impurities corresponding to quartz. The
XRD pattern of I-nZVI sample is shown in Fig. 2b. The Fig. 2 XRD patterns of samples. a Illite; b I-nZVI; c pure nZVI.
positions of characteristic diffraction peaks of illite are I Illite, Q quartz, F ferrous oxide
unchanged which indicate that the synthesized material
(I-nZVI) keeps the crystal structure of illite. Moreover, the and ferrous oxide (Fe3O4/c-Fe2O3) crystalline phases on
characteristic peak at 2h of 44.9° confirms the existence of nZVI. The two main characteristic peaks suggest that some
Fe0 (a-Fe0) in the I-nZVI sample. XRD pattern of nZVI irons of nZVI are oxidized quickly after synthesis. Ferrous
sample is shown in Fig. 2c. The apparent peaks at 2h of oxidation are found on nZVI rather than I-nZVI, it suggests
44.9° and 35.8° indicate the presence of both Fe0 (a-Fe0) that the load of nZVI on illite offers the stability of Fe0.

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BET-N2 surface area
Surface area of illite, nZVI and I-nZVI were detected by
BET-N2 method. The nitrogen adsorption–desorption iso-
therms are shown in Fig. 3. The increase in nitrogen
adsorption capacity at even higher relative pressure for
illite was quite small, indicating the end of the capillary
condensation and narrow pore size distribution for this
sample. Type IV isotherms could be found for nZVI and
I-nZVI samples with typical hysteresis loops in the meso-
pore range (2–50 nm). Along with the increase of relative
pressures, steady increases in adsorption capacity were
caused by the monolayer/multilayer adsorptions of nitro-
gen molecules on the mesopores or macropores [40]. In
samples of nZVI and I-nZVI, closure could be found in
relative pressure range of 0.4–0.8, which can be ascribed to
the capillary condensation of nitrogen molecules in mes-
opores with relatively uniform dimensions.
The specific surface areas (SSA) of illite, nZVI and
I-nZVI were obtained from the nitrogen adsorption iso-
therms. When nZVI was loaded on to illite, a mean specific
surface area of 9.46 m2/g was obtained, which is twice
lager than illite alone (4.72 m2/g). Despite the nZVI SSA
(44.96 m2/g) being lager than that of I-nZVI (9.46 m2/g),
the reaction activity of nZVI is much lower than I-nZVI
due to more pronounced oxidation and aggregation of Fe0
on nZVI.
The removal of U by various materials
Three absorbents (illite, nZVI and I-nZVI) were used to
remove uranium from aqueous solution. Initial content of U
from 4.20 9 10-7 to 8.40 9 10-7mol/L were used to
investigate removal capacity of three materials. Removal
Fig. 3 N2 adsorption–desorption isotherms at 77 K of illite, nZVI
and I-nZVI
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Fig. 4 Removal of U by illite, nZVI and I-nZVI as a function of initial
concentration of U. T = 298 K, m/V = 0.1 g/L, C[U(initial)] =
4.2 9 10-7–8.4 9 10-7mol/L
percentage of uranium are shown in Fig. 4. The results
show that removal rates of U on illite are from 11.9 to
17.1 % with average removal percentage of 14.7 %. These
indicate that illite has the absorbability to uranium. With U
initial concentration below 5.88 9 10-7mol/L, the removal
efficiency of nZVI and I-nZVI are very close which the
average removal percentages are 92.5 and 97.1 %,
respectively. With initial concentration of U higher than
5.88 9 10-7mol/L, the removal efficiency of U from
aqueous solutions by I-nZVI are much higher than nZVI.
Removal efficiencies of I-nZVI and nZVI are both high and
regular in low uranium concentration. As the concentration
of uranium increased, removal rates of I-nZVI reduced
regularly and slightly. On the contrary, removal percent-
ages of nZVI went down irregularly and quickly. The
results showed that the reducibility of I-nZVI are much
higher than nZVI which suggested less Fe0 oxidized as
I-nZVI than nZVI. And these conclusions are consistent
with XRD results. The results indicate that the removal
capacity of U and stability of I-nZVI are much higher than
nZVI. As shown in Fig. 4, I-nZVI provided considerable
reaction activity from a high concentration of
8.40 9 10-7mol/L U solution compared to either illite or
nZVI. Consequently, illite increased the reactivity of nZVI
even though I-nZVI has a lower content of Fe0 than nZVI
in a same reaction solid content. As a support material,
illite could stabilize Fe0 from being oxidized and increase
its reactivity.
Removal process of U on I-nZVI
As shown in Fig. 5a, the removal of U on I-ZVI was
studied as a function of contact time. The curve of removal
percentage varied with time can be divided into four zones:
J Radioanal Nucl Chem (2015) 304:859–865
ZONE 1: The removal rate of U in aqueous solution
achieves 16.5 % once I-nZVI used and then decreases to
4.1 % in the later 8 min. ZONE 2: In the later 50 min, the
removal rate of U on I-nZVI grows back to 16.5 % slowly.
ZONE 3: From 50 to 120 min, the removal percentage
raises to a maximum as a removal rate of 91.3 %. And
ZONE 4: removal of U on I-nZVI comes to an equilibrium
and stays constant at 92.6 %.
In order to better explain the mechanism of U removal on
I-nZVI, removal of U on illite and nZVI were also studied by
time. Sorption of U on illite as a function of contact time can
be seen in Fig. 5c. Sorption of U on illite is very fast that it
obtains a maximum in the first 20 s of contact and then
decreases. The fast uranium removal rate at the beginning is
attributed to the rapid diffusion of U from the solution to the
external surfaces of illite. Desorption of uranium due to
re-equilibration after the sorption saturation. This variation
Fig. 5 Uptake of U according to contact time. a Removal in
percentage of U varying on I-nZVI; b total iron and ferrous iron
concentration in solution varying on I-nZVI removal of U; c sorption
863
consistent with the I-nZVI removal performance of U in
ZONE 1. With increasing time, Fe0 of I-nZVI dissolved into
aqueous solutions so as uranium on Fe0. The results indicate
that the removal of U on I-nZVI in ZONE 1 is dominated by
support material (illite) which is a sorption process. At
ZONE 2, the removal percentage of U on I-nZVI increased
slowly like a buffers zone. At the same time, ferrous iron
release into aqueous solution and then the concentration of
total iron raises to a maximum as shown in Fig. 5b. The
removal percentage of U in solution on nZVI is shown in
Fig. 5d. The removal curve of U on nZVI is exactly the same
to the removal performance on I-nZVI. This phenomenon
indicates that the removal of U on I-nZVI in ZONE 3 are
dominated by Fe0 which is a reduction process.
The removal mechanism of U on I-nZVI varied with
time can be concluded as four stages: STAGE 1: Illite
Dominated Zone, the removal of U in aqueous solution is
in percentage of U varying on illite; d removal percentage of U on
nZVI varying by time. T = 298 K, m/V = 0.1 g/L, C[U(initial)]
= 8.4 9 10-7mol/L
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dominated by a sorption process on support material
(illite); STAGE 2: Fe0 released Zone, Fe0 of I-nZVI dis-
solve into aqueous solution and U(VI) begin to reduce;
STAGE 3: Ferrous Dominated Zone, U(VI) in aqueous and
on I-nZVI are reduced to U(IV) by ferrous; STAGE 4:
Reaction Equilibrium Zone, removal of U on I-nZVI reach
an equilibrium. The results suggest that the removal of U
on I-nZVI is a combination effect of support material
(illite) and supported material (nZVI) which illite function
first and nZVI function mainly.
Mechanisms of removal
FTIR spectra for I-nZVI samples were scanned in range of
4000–400 cm-1 (Fig. 6) where Fig. 6a–d refer to I-nZVI
before reaction, 3 min (STAGE 1), 50 min (STAGE 2) and
80 min (STAGE 3) during the reaction of U removal,
respectively. Compared to the FTIR spectra of I-nZVI
before reaction (Fig. 6a), changes are observed in adsorp-
tion peaks from I-nZVI after first 3 min reaction in Fig. 6b.
For instance, the characteristic absorption peaks of I-nZVI
at 881, 726, 582 and 515 cm-1, corresponding to Al–O–Si,
Al–O, Si–O–Al and Si–O vibration, are significantly
reduced [41, 42]. The strong band at 1078 cm-1 assign to
Si–O–R stretching vibration are also reduced, which is due
to cation R on illite of I-nZVI replaced by UO22? in
aqueous solution [43]. The broad band near 3406 cm-1
attributed to R–OH stretching vibration disappear, which is
caused by U adsorbed on illite of I-nZVI and formed
complexes such as R–OUO2? [44]. In Fig. 6c (STAGE 2)
and Fig. 6d (STAGE 3), the adsorption peaks at 1629 cm-1
Fig. 6 FTIR spectrum of I-nZVI during the reaction of U removal.
a I-nZVI before reaction; b I-nZVI after 3 min reaction (STAGE 1);
c I-nZVI after 50 min reaction (STAGE 2); d I-nZVI after 80 min
reaction (STAGE 3). T = 298 K, m/V = 0.1 g/L, C[U(initial)] = 8.4 9
10-7mol/L
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J Radioanal Nucl Chem (2015) 304:859–865
corresponding to Fe–O stretch are enhanced, which
because of the oxidize of Fe0 on illite. And the band at
463 cm-1 assigned to Fe2O3 and Fe3O4 are reduced, which
is due to iron and ferrous iron release into aqueous. It can
be concluded that UO22? is primarily reduced to U(IV) and
precipitated on the iron surface [12, 13]. U(VI) was
removed from solution via sorption with reduction form
U(IV) [17]. Consistent with the results obtained from
contact time, these results demonstrate that removal of U
on I-nZVI is a combination effect of sorption and reduc-
tion. And in STAGE 1, illite and Fe0 sorption play a lead
role at first and then is the reduction by iron species in
STAGE 2 and STAGE 3.
Conclusions
This work demonstrate that 238U can be effectively removed
from aqueous solution by illite supported zero-valent iron
nanoparticles (I-nZVI). The results obtained from SEM and
XRD indicate that nZVI loaded onto illite is well dispersed,
and it decreases the aggregation of Fe0. Removal capacity of
U on I-nZVI and stability of I-nZVI are much higher than
nZVI. Removal process of U on I-nZVI can be conclude into
four stages in illite dominated zone, Fe0 released zone, fer-
rous dominated zone and reaction equilibrium zone. The
removal of U on I-nZVI is a combination effect of illite and
nZVI. And the removal efficiency of U in solution is attrib-
uted to the sorption and reductive precipitation of U(VI) in
aqueous. FTIR results suggest that in the removal of U on
I-nZVI, illite and Fe0 sorption play a lead role at first and then
is the U(VI) reduction by iron species. It has been shown that
illite has the potential to act as a dispersant and stabilizer
during the synthesis of I-nZVI, which decreases the aggre-
gation and improves the activity of nZVI. As illite is a stable,
high load-carrying capacity, low-cost clay mineral, and a
useful support material for nZVI; I-nZVI is an efficient and
promising remediation material for waster-soluble uranium
compounds.
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