Preparation of self-supporting flexible NiFe2O4 fibers and their

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adsorption performance for Pb(II)

Zitao Guoa, Zetao Liua, Ailin Yanga, Long jianga, Shuying Shia,*,Hao denga, Pengfei Gaoa,b

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a School of Materials and Chemistry, Southwest University of Science and Technology, Mianyang

621010, P. R. China

b State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese

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Academy of Sciences, Lanzhou 730000, P. R. China

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*Corresponding author: Shuying Shi

Tel.: +86-0816-2419201 er
E-mail address: [email protected]; [email protected]

Abstract:
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Compared to commonly used direct electrospinning and surface loading, we developed an

original and simple method to fabricate flexible NiFe2O4 magnetic fibers, and applied to Pb(II)

adsorption for the first time. The spinning solution was synthesized by sol-gel method with iron
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sources, nickel sources and citric acid, the iron and nickel ions in the spinning solutions were

coordinated to carboxyl group in mono-dentate fashion. The spinning solution prepared by this
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method had good spinnability. After that, fluffy and flexible NiFe2O4 fibers were prepared by

electrospinning and heat treatment. The saturation magnetization of the prepared NiFe2O4 fibers

was 18.2 emu/g, and the specific surface area of the fibers was 13.443 m2/g. The adsorption
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experiments showed that the maximum adsorption capacity of NiFe2O4 fibers for Pb(II) calculated

from Langmuir model was 49.53 mg/g. Due to the self-supporting and non-agglomeration

advantages of the fiber structure in aqueous solution, the maximum adsorption capacity of Pb(II)
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adsorbed by NiFe2O4 fibers prepared in this work was higher than those of most reported NiFe2O4

adsorbents among the NiFe2O4 adsorbents. Flexible magnetic fibers provided a new solution for
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simultaneously improving the adsorption capacity of pollutant and achieving rapid magnetic

separation, becoming another effective strategy for expanding the application prospects of magnetic

adsorbents.

This preprint research paper has not been peer reviewed. Electronic copy available at: https://ssrn.com/abstract=4982008
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Keywords: Flexible fiber; Self supporting; sol-gel method; Magnetic separation; NiFe2O4; Pb(II)
adsorption.

1. Introduction

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Water is the source of life, and the treatment and reuse of wastewater is a global issue. In the

past century, the world population has increased fourfold, and the demand for water by humans has

increased sevenfold [1]. According to the World Water Council's assessment, approximately 3.9

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billion people will live in water scarce environments by 2030 [2]. However, heavy metal pollution

has exacerbated the global water scarcity situation. Water contaminated with heavy metals has

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characteristics such as inability to degrade, difficulty in metabolism, enrichment, and high pollution

levels, making it impossible to achieve self-purification. How to improve water quality and reduce
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the impact of heavy metal pollution on humans and ecosystems has become an urgent problem to

be solve. Pb(II) is one of the most dangerous heavy metal pollutants [3-5], and is a very important

raw material in industrial production such as battery manufacturing, metal electroplating, cosmetics,
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ceramic industry, and dyes [6]. Research had shown that long-term exposure or ingestion of lead

can cause headaches, diarrhea, and dysfunction of the kidneys, liver, brain, and central nervous

system [7]. In addition, Pb2+ has good solubility in water and is prone to complex with acidic free
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radical ions (such as CO32-, SO42-) and sink into sediment during wastewater treatment, which has

a serious negative impact on sewage treatment [8]. Therefore, it is urgent to solve the problem of
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Pb(II) pollution in the water environment.

Adsorption method is one of the economical, effective, and highly selective methods for

removing heavy metals [9]. After desorption, the adsorbent can be recycled. The functionality of
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adsorbents can also be flexibly designed to improve their performance and pollutant selectivity [10-

12]. Li et al. synthesized Prussian blue (PB)-based nanocubes as a Cs(I) adsorbent [13]. Huang et
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al. fabricated K2W4O13 nanowires to removal Pb2+ from water [14]. Wang et al. synthesized flower-

like WS2 microcrystals for the removal of Au (III), Ag (I) and Pd (II) [15]. Rahmanifar et al.

obtained a Schiff base containing intermediate product (PEIMB) by reacting 1- (2-aminoethyl)

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piperazine with methyl terephthalate, and then obtained a new Schiff base adsorbent (MCS-PEIMB)

by reacting with chitosan and Fe3O4, the maximum adsorption capacity of MCS-PEIMB for Pb (II)

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 was 142.86 mg/g [16]. Although these complex nanostructure materials have large specific surface

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areas, they tend to agglomerate in aqueous solutions, which then impair the actual area of adsorption;

resulting in the decline of adsorption performance. Moreover, they are difficult to separate from the

aqueous solutions, which may cause secondary contamination. As for fiber adsorbents, they not

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only have the advantage of low-dimensional materials with large specific surface areas, but also

exhibit fiber morphological advantages. They are entangled, self-supported without agglomeration,

and easily separated [17]. The magnetic fiber adsorbents have magnetic properties, which further

simplify the separation process [18].

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NiFe2O4 fibers were a popular kind of magnetic adsorbent. The most commonly used methods

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were direct electrospinning and surface loading. Direct electrospinning was the process of blending

prepared NiFe2O4 nanoparticles into the spinning solution to obtain composite materials through

electrospinning. For example Durga et al. synthesized NiFe2O4 nanoparticles through the
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autocombustion method and integrated them as fillers within the PVDF matrix. The mat containing

5 wt% of NiFe2O4 registering a maximum saturation magnetization of 4.6 emu/cm3 [19]. Xicheng
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et al. used a similar method to add NiFe2O4 nanoparticles as a filler to PAN spinning solution and

obtained NiFe2O4@ slit modified hollow carbon fiber by electrospinning [20]. Surface loading was

the process of first preparing nanofibers and then loading NiFe2O4 onto the fiber surface, which
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involves integrating NiFe2O4 onto the nanofibers. Such as, Wanxi et al. prepared biomass-based

carbon fibers using cotton fiber, hemp fiber, and bamboo fiber as carbon sources. Then, precise
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loading of NiFe2O4 nanoparticles on biomass-based carbon fibers to prepare NiFe2O4/carbonized

cotton fibers [21]. Sun et al. reported the synthesis of a Fe2O3 nanorod/NiFe2O4 nanoparticle

composite on the cotton fiber cloth of expired shirts (Fe2O3-NiFe2O4/CF) for enhanced HER
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performance [22]. Whether using NiFe2O4 as a filler for direct electrospinning or loading it onto

fibers, there are issues with limited NiFe2O4 content and uneven loading.

Durga et al. used iron nitrate and nickel nitrate dissolved in DMF as spinning solutions to
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produce NiFe2O4 fibers by electrospinning. Then the NiFe2O4 fibers were employed as fillers in

appropriate amounts (3, 6 and 9 wt %) to fabricate P(VDF-HFP)/ NiFe2O4 fiber composite films
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[23]. Yongqian et al. reported the synthesis of FeNi/NiFe2O4/NiO/C nanofibers via electrospinning

technique using Ni(acac)2, Fe(acac)3, and DMF/ PAN solution as precursor [24]. However, this

method required P(VDF-HFP) and PAN to assist in fiber formation.

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 For the first time, we developed a simple sol-gel method to prepare the spinnable precursor

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solution, and used electrospinning technology to prepare pure NiFe2O4 fibers. Iron nitrate and nickel

acetate were used as iron and nickel sources, while citric acid was used as a chelating agent, the iron

and nickel ions in the spinning solution were coordinated to carboxyl group in mono-dentate fashion.

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The prepared NiFe2O4 fibers were fluffy and flexible and were used as an adsorbent for removing

heavy metal ion Pb (II) in water. The flexible magnetic fibers provided an original alternative to

simultaneously improve the Pb(II) adsorption capacity and achieve rapid magnetic separation. This

indicated that NiFe2O4 fibers were a quite potential candidate as a heavy metal adsorbent for

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wastewater treatment, which became another effective strategy to expand the application prospects

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of magnetic adsorbents.

2. Experimental procedure er
2.1. Materials
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Iron (III) nitrate nonahydrate (Fe(NO3)3·9H2O, ≥ 98.5%, Tianjin Kermel), citric acid

(C6H8O7·H2O, CA, ≥ 99.5%, Tianjin Kermel), ammonia solution (NH3·H2O, wt.%(NH3) 25~28%,

Tianjin Kermel), nickel acetate(Ni(CH3COO)2·6H2O, ≥ 99.0%, Tianjin Damao), anhydrous ethanol

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(CH3CH2OH, ≥ 99.7%, Tianjin Fuyu), polyethylene oxide (PEO, Mw~1,000,000, Aladdin),

deionized water (resistivity no lower than 18.2 MΩcm).

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2.2. Preparation of NiFe2O4 fibers

Generally, the spinning solution of NiFe2O4 precursor fibers was prepared by sol-gel method.
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Iron hydroxide precipitation was prepared first by dissolving iron nitrate in deionized water and

then dropwise adding ammonia solution. The newly prepared iron hydroxide precipitation after
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centrifuged and cleaned, and CA (keep the molar ratio of Fe3+: CA at 2:3) were dispersed in

deionized water and continuously stirred until the solution became transparent. Concentrated the

solution and then dilute it with a mixture of water and ethanol. Next, added nickel acetate
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(maintaining a molar ratio of Ni2+: Fe3+: CA of 1:2:3) and dissolved it in the solution. Finally, PEO

was dissolved in the solution at 1% solution mass to prepare the spinning solution.

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 The electrospinning technology was used to prepare precursor fibers at a temperature of 25–

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35 °C and humidity of 20–40%. The electrospinning process was optimized with the voltage of 12

kV, the injection rate of 1.2 mL/h, and the distance of 15cm between needle and collector.

The precursor fibers were heat-treated to 550 °C at a heating rate of 2 °C/min to obtain nickel

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ferrite fibers.

2.3. Physicochemical measurements

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Fourier-transformation infrared spectrum (FT-IR) was measured using KBr pellet method on

an RT-DLATGS spectrometer (ALPHA-T, Bruker). The phase compositions of different fibers

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were characterized by X-ray diffraction (XRD, D8 advance, Bruker) diffractometer with Cu Kα

radiation (λ = 1.540598 Å). The surface morphologies and microstructures of the fibers were
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observed using a scanning electron microscope (SEM, S-4800, Hitachi). Hysteresis measurements

were tested using a Lake Shore 7410 Vibrating Sample Magnetometer (VSM). The Brunauer-

Emmett-Teller (BET) surface areas of the fibers were tested using specific surface area instrument
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(JW-BK112, JWGB Sci & Tech). The surface chemical compositions of the fibers were detected by

X-ray photoelectron spectroscopy (XPS, ESCALAB 250 ThermoFisher SCIENTIFIC, Germany).

The concentrations of Pb(II) in the samples were determined by atomic absorption spectrometer
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(AAS, SP-3520AA).
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2.4. Batch adsorption experiments

Pb(II) solutions with different concentrations were prepared by Pb(NO3)2. The initial pH values
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of the Pb(II) solutions were adjusted to 5.0±0.2 with HCl (0.1 M) and NaOH (0.1 M). All beakers

containing Pb (II) solutions were oscillated at 150 rpm on the thermostatic vibrator.

Batch experiments were carried out to obtain adsorption isotherms of Pb(II) on NiFe2O4 fibers.
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Typically, 20 mg NiFe2O4 fibers were infiltrated into 40 mL of Pb (II) solutions with different initial

concentrations (in the range of 10-100 mg/L) and kept shaken at 300K for 4h. 100 mg NiFe2O4

fibers were soaked into 200 mL Pb (II) solution (50 mg/L), and the adsorption capacities of the
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fibers at different adsorption time to obtain adsorption kinetics. After adsorption, the adsorbent was

easily separated and collected from the aqueous solution by placing a magnet outside the beaker.

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 The adsorption capacities were calculated by Eq. (1):

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(𝐶0−𝐶𝑡)
𝑞=
𝑚
𝑉 (1)

where C0 is the initial concentrations of heavy metal ions, Ct (mg/L) is the concentrations of heavy

metal ions at time t (min), V (mL) is the solution volume and m (mg) is the mass of fiber adsorbents.

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The pseudo-first-order (PFO) and pseudo-second-order models (PSO) models were described

as Eqs. (2) and (3), respectively:

𝑞𝑡 = 𝑞𝑒(1−𝑒−K1𝑡) (2)

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𝑞2𝑒 K 𝑡
𝑞𝑡 = 1 + 𝑞 2K (3)
𝑒 2𝑡

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where 𝑞𝑒 and 𝑞𝑡 (mg/g) are the adsorption capacities at equilibrium and at time t (min),

respectively; K1 (min − 1) and K2 (g·mg − 1·min − 1) are the PFO and PSO model rate constants,

respectively. er
The Langmuir and Freundlich models were described as Eqs. (4) and (5), respectively:
QmKL𝐶𝑒
𝑞𝑒 = 1 + KL𝐶𝑒 (4)
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where Qm is a theoretical limit of adsorption capacity (mg/g) and KL (L/mg) is Langmuir

constant related to the rate of adsorption.

1
𝑞𝑒 = Kf𝐶𝑒 n (5)
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where Kf and n are the Freundlich constants, representing the capacity and intensity of the

adsorption, respectively.
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3. Results and discussion

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3.1 Formation of NiFe2O4 fibers

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Fig. 1 FT-IR spectra of the citric acid and precursor fibers at room temperature (a) and the
precursor fibers heat-treated at different temperatures (b)

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Fig. 1(a) was the infrared spectrum of citric acid and precursor fibers, the bands at 1717 cm-1,

1614 cm-1, and 1385 cm-1 corresponded to the stretching vibration of -C=O in -COOH, the
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asymmetric and symmetric stretching vibrations stretching of -COO [25]. Compared with citric acid,

the carbonyl stretching vibration band at 1717 cm-1 in the precursor fibers was significantly

weakened, and obvious carboxylate asymmetric and symmetric stretching vibration appeared at
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1614 cm-1 and 1385 cm-1, which indicated that most of the citric acid chelated with iron and nickel

ions in the formation of the spinning solutions, while the spinning solutions still contained a small
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amount of unreacted citric acid.

The frequency separation (Δν) between the asymmetric and symmetric stretching vibrations of

carboxyl group can indicate the coordination mode of the carboxyl group with the metal ion [26].
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The frequency separation (Δν) between the asymmetric and symmetric stretching vibrations of

carboxyl group in precursor fibers was 229 cm-1, which was larger than the Δν value of free RCOO

(the Δν value of sodium citrate RCOO is 196 cm-1). This indicated that the iron and nickel ions in
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the spinning solutions were coordinated to carboxyl group in mono-dentate fashion [27]. The

spinning solution prepared by this sol gel method had good spinnability, and the prepared NiFe2O4
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fibers were fluffy and would not be pulverized during heat treatment.

Fig. 1(b) showed the infrared spectra of the precursor fibers heat-treated at different

temperatures. With the increase of heat treatment temperature, the infrared vibration peaks of

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 organics gradually weakened, and then disappeared, indicated organics in the fibers gradually

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decomposed. The infrared peaks in the range of 500 -600 cm−1 were attributed to the metal–oxygen

bond (Me-O) stretching vibration peaks [28]. The vibration peaks of Ni-O/Fe-O appeared in the

composite material at 581 cm−1, which also confirmed that the as-prepared fibers contain NiFe2O4.

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Fig. 2 XRD pattern of the precursor fibers heat-treated at 550 ℃

Fig. 2 showed the XRD pattern of the precursor fibers heat-treated at 550 ℃, it could be

observed that the sample exhibited significant peaks at 30.31°, 35.70°, 43.38°, 53.81°, 57.39° and
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63.02°. The characteristic peaks could be indexed to the crystal surfaces of NiFe2O4 (220), (311),

(400), (422), (511), (440), which was in agreement with the standard spectrum of the spinel phase
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NiFe2O4 (JCPDS No. 54-0964) [29]. This confirmed the successful synthesis of NiFe2O4 fibers.
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Fig. 3 XPS spectra of NiFe2O4 fibers (a), XPS high-resolution spectra of NiFe2O4 fibers: O 1s (b),

Fe 2p (c), Ni 2p (d) for NiFe2O4 fibers

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The surface element composition and valence state distribution of NiFe2O4 fibers were
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obtained by XPS analysis. Fig. 3(a) exhibited the XPS full spectrum of NiFe2O4 fiber, indicating

the presence of distinct characteristic peaks of Ni, Fe, C, and O elements in the sample. In order to

better analyze the surface elemental valence states of the fibers, Gaussian fitting was used to separate
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the characteristic peaks of Ni, Fe, and O elements in the samples. Fig. 3(b) showed the XPS high-

resolution spectra of O ls, where the peak at 529.82 eV corresponded to a typical M-O bond, the
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peak at 531.00 eV belonged to surface defects such as hydroxyl groups and adsorbed oxygen, and

the peak at 531.85 eV was a typical peak for physical or chemical adsorption of water [30].

Fig. 3(c) was the XPS high-resolution spectra of Ni 2p. It could be observed from the figure
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that the Ni 2p spectrum consists of four peaks located at 854.77, 872.38, 861.33 and 878.96 eV,

respectively. These four peaks corresponded to the Ni 2p3/2, Ni 2p1/2, and their two satellite peaks.

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 The metal atoms inside spinel oxide occupy the tetrahedral and octahedral voids composed of

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oxygen atoms. Generally speaking, compared with metal atoms occupying tetrahedral vacancies,

the same type of metal atoms occupying octahedral vacancies exhibit lower binding energies [31,32].

Based on this theoretical, peak fitting was performed on the Ni 2p3/2 and Ni 2p1/2 peaks. For the

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Ni 2p3/2, the peaks located at 854.66 and 856.00 eV corresponded to Ni2+ occupying octahedral and

tetrahedral vacancies, respectively. For the Ni 2p1/2, the peaks located at 872.10 and 873.76 eV

correspond to Ni2+ occupying octahedral and tetrahedral vacancies, respectively. Fig. 3(d) showed

the XPS high-resolution spectra of Fe 2p, four peaks of Fe 2p were located at 710.59, 724.03, 719.13,

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and 733.38 eV, which corresponds to Fe 2p3/2 and Fe 2p1/2, as well as their satellite peaks,

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respectively. Similarly, peak fitting was performed on the spin orbit peaks, with each spin orbit peak

consisting of three peaks. Specifically, the Fe 2p3/2 peak can be divided into peaks located at 710.17

and 712.22, 715.54 eV, corresponding to Fe2+, Fe3+ in octahedral vacancies, and Fe3+ in tetrahedral
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vacancies. Similarly, the Fe 2p1/2 peaks could be divided into three peaks: 723.67 eV (Fe2+), 726.40

eV (Fe3+ in octahedral vacancies), and 730.02 eV (Fe3+ in tetrahedral vacancies) [33]. In summary,
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it was found through peak fitting that Fe element exists in two valence states, Fe2+/Fe3+, within the

prepared NiFe2O4 fibers.

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Fig. 4 Digital photos of the precursor fibers (a), digital photos and SEM images of the NiFe2O4
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fibers (b, c, d).

Fig. 4(a, b) presented digital photo of precursor fibers and NiFe2O4 fibers. The fibers had
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excellent flexibility and could be folded and curled at will without damaging the one-dimensional

fiber structure. Fig. 4(c, d) exhibited SEM images of the NiFe2O4 fibers. It can be seen that NiFe2O4

fibers were composed of nanocrystals, had perfect one-dimensional morphologies and high aspect
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ratios, and would not be pulverized during heat treatment. The fibers entangled with one another

and were self-supported, therefore, they did not agglomerate in aqueous solutions. The non-

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 aggregation and magnetic separation of adsorbents in water are important properties that are

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beneficial for the practical use of adsorbent materials.

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Fig. 5 Hysteresis loops of the NiFe2O4 fibers heat-treated at 550 ℃ (a), N2 adsorption-

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desorption isotherms (b) and the corresponding pore size distributions of NiFe2O4 fibers heat-
treated at 550 ℃ (c).

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Fig. 5(a) showed the hysteresis loops of the NiFe2O4 fibers heat-treated at 550 ℃. When

subjected to a magnetic field strength of 5000 Oe, the sample exhibited a maximum saturation
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magnetization intensity of 18.2 emu/g, making it very easy to magnetic separation. The NiFe2O4

fibers were ferromagnetic and had a coercive force of 190 Oe. The fiber morphology has self-

supporting properties such that it does not agglomerate even with weak remanence and is easily

redispersed in water. These findings highlight the potential applications of NiFe2O4 fibers and their
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significance in addressing adsorption recovery and reuse.

The N2 adsorption-desorption isotherms and pore size distributions of NiFe2O4 fibers were
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displayed in Figs. 5(b, c). The isotherms of fibers showed type-Ⅳ characteristics isotherm with H2

hysteresis loops, which indicated the mesoporous structure of NiFe2O4 fibers in nature and the ink-
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bottle shape of pores [34], and the mesoporous size distribution showed a peak centered at the mean

value of 4.08 nm, indicating a uniform mesopore. The BET surface area and total pore volume are

calculated to be 13.443 m2/g and 0.074 cm3/g, respectively.

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3.2 Bath adsorption

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 ed
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Fig. 6 Adsorption kinetics and model fitting of Pb(II) on NiFe2O4 fibers (a), adsorption isotherm

and model fitting of Pb(II) on NiFe2O4 fibers (b).

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Table 1 Adsorption kinetic model fitting parameters.
Pseudo-first-order (PFO) Pseudo-second-order (PSO)
k1 qe (mg/g) R2 k2 qe (mg/g) R2
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0.0608 57.7324 0.9218 0.0015 62.6208 0.9673

Adsorption kinetics is the functional relationship between the adsorption capacity of NiFe2O4
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fibers for Pb (II) and contact time [35]. Adsorption kinetics was studied to analyze the adsorption

equilibrium and adsorption behavior. As shown in Fig.6(a), the initial concentration (C0) of Pb(II)
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was 100 PPm, the rapid adsorption process occurred in the first 1 h.Then the adsorption rate

gradually slowed down as the decrease of adsorption sites, and reached equilibrium state in 3 h.

Two models, pseudo-first-order models (PFO) and pseudo-second-order models (PSO) were used
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to analyze the experimental data in order to understand the adsorption behavior. The corresponding

kinetic parameters were listed in Table 1. According to kinetic parameters of PFO and PSO, the
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adsorption equilibrium capacities (qe) of NiFe2O4 fibers were 57.7324 and 62.6208 mg/g,

respectively. Compared with the PFO model, the PSO model had a higher correlation coefficient

(R2), this indicated that the PSO model could better describe the adsorption of Pb(II) on NiFe2O4
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fibers.

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 ed
Table 2 Adsorption isotherm model fitting parameters.
Langmuir Freundlich

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Qm (mg/g) KL R2 Kf n R2
49.5314 0.0046 0.9781 7.9602 2.2331 0.8197

The adsorption isotherms were drawn based on the equilibrium adsorption capacities of Pb(II)

on the NiFe2O4 fibers at different initial concentrations [36]. Adsorption isotherm data of Pb(II)

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adsorbed on NiFe2O4 fibers were shown in Fig. 6(b), and the nonlinear regression fitting was carried

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out according to the Langmuir and Freundlich models, respectively. The fitted parameters of these

two models were given in Table 2. Langmuir model was more suitable to describe Pb(II) dsorption

on NiFe2O4 fibers due to the higher correlation coefficients (R2 > 0.97). The results suggested that
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the Pb(II) was monolayer adsorbed on the NiFe2O4 fibers surface. The maximum adsorption

capacity (Qm) was 49.53 mg/g. The n value of Freundlich model indicated the difficulty of Pb(II)
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adsorption on NiFe2O4 fibers. The results implied that NiFe2O4 fibers could easily adsorb Pb(II)

since the n values were much higher than 2 [37].

The Qm of Pb(II) adsorbed by NiFe2O4 fibers was higher than those of most reported NiFe2O4

adsorbents in the literatures (Table 3). This indicated that the fiber adsorbents did not agglomerate
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in the aqueous solutions, therefore, they could give full play to their adsorption active sites, and

improve their adsorption capacities for Pb(II).

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Table 3 Comparative study of maximum adsorption capacities (Qm) of Pb(II) using various NiFe2O4
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adsorbents.

SBET Ms pH Qm
Adsorbent Ref.
(m2/g) (emu/g) value (mg/g)
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NiFe2O4 16.452 8.8411 6.0 20.75 [38]

Ni0.9Ca0.1Fe2O4 22.525 12.3514 6.0 24.25 [38]

Ni0.9Mg0.1Fe2O4 3.8766 6.0 24.12 [38]

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Ni0.975Ca0.025Fe2O4 13.4049 6.0 24.12 [38]

Ni0.975Mg0.025Fe2O4 9.9302 6.0 23.75 [38]

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 GONF 41.34 5.5 25.00 [39]

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NiFe2O4 NPs 5.0 19.2150 [40]

MnO2/NiFe2O4 164.9 15.7 6.0 85.78 [41]

NiFe2O4 fibers 13.443 18.2 6.0 49.53 This work

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Conclusion

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We developed an original and simple method to fabricate flexible NiFe2O4 magnetic fibers.

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The spinning solution was synthesized by sol-gel method with iron sources, nickel sources and citric

acid, the iron and nickel ions in the spinning solutions were coordinated to carboxyl group in mono-

dentate fashion. The spinning solution prepared by this sol gel method had good spinnability, and
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the prepared NiFe2O4 fibers through electrospinning were fluffy, could be curled and folded at will

without destroying the fiber structure and would not be pulverized during heat treatment. The
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saturation magnetization of the prepared NiFe2O4 fibers was18.2 emu/g, and the specific surface

area of the fibers was 13.443 m2/g. The adsorption experiments showed that the maximum

adsorption capacity of NiFe2O4 fibers for Pb(II) calculated from Langmuir model was 49.53 mg/g.

Among the NiFe2O4 adsorbents, the maximum adsorption capacity of Pb(II) adsorbed by NiFe2O4
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fibers was higher than those of most reported NiFe2O4 adsorbents. Since the fiber adsorbents were

self-supporting in aqueous solutions, they did not agglomerate, and therefore, have no hinderance
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on adsorption performance. The flexible magnetic fibers provided an original alternative to

simultaneously improve the Pb(II) adsorption capacity and achieve rapid magnetic separation.
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Further modification of the fibers could increase the adsorption capacity and maintain rapid

magnetic separation. This indicated that Fe3O4 fibers were a quite potential candidate as a heavy

metal adsorbent or adsorbent core for wastewater treatment, which became another effective
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strategy to expand the application prospects of magnetic adsorbents.

Acknowledgments
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This work was supported by the Natural Science Foundation of Southwest University of Science

This preprint research paper has not been peer reviewed. Electronic copy available at: https://ssrn.com/abstract=4982008
 and Technology (No. 21zx7134 and No. 20zx7139), the Natural Science Foundation of Sichuan Province

ed
(2023NSFSC1114), the National Natural Science Foundation of China (No. 22106127), the Open project

of the State Key Laboratory of Solid Lubrication (LSL-2316).

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This preprint research paper has not been peer reviewed. Electronic copy available at: https://ssrn.com/abstract=4982008
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This preprint research paper has not been peer reviewed. Electronic copy available at: https://ssrn.com/abstract=4982008