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Phase Components, Microstructures, and Magnetic Properties of Liquid-Phase-Sintered Li ZN Fe O / Y Fe O Ferrite Nanocomposites
Phase Components, Microstructures, and Magnetic Properties of Liquid-Phase-Sintered Li ZN Fe O / Y Fe O Ferrite Nanocomposites
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1
State Key Laboratory of Electronic Thin Films and Integrated Devices, School of Electronic Science and Engineering, University of
Electronic Science and Technology of China, Chengdu 610054, People’s Republic of China
2
Institute of Electronic and Information Engineering of UESTC in Guangdong, Dongguan 523808, People’s Republic of China
3
School of Materials and Energy, University of Electronic Science and Technology of China, Chengdu 610054, People’s Republic of
China
https://doi.org/10.1007/s10854-023-10656-8
1250 Page 2 of 9 J Mater Sci: Mater Electron (2023) 34:1250
performances compared to their bulk counterparts narrow magnetic resonance frequency and negative
[2, 7, 14–16]. These modifications are mainly deter- permeability properties, which is conducive to
mined by quantum effects and increasing specific improving the low-frequency electromagnetic prop-
surface area [16, 17]. Factually, sintering tempera- erties of the composite materials [31, 32]. H3BO3-
tures of ferrites can also be lowered by using nano- - Bi2O3 - SiO2 - ZnO (BBSZ) glass powders have
sized precursors as raw materials [18]. been added to achieve ferrite–glass nanocomposites,
Nano-sized spinel ferrites have attracted current considering that BBSZ glass has low soften temper-
interests due to their impressive physical properties atures and good liquidity [33, 34]. Thereafter, LiZn/
viz., particle size dependent magnetization, low YIG-BBSZ ferrite-glass nanocomposites have been
coercivity, large resistivity [2, 16, 19], etc. The most realized though a low-temperature liquid phase sin-
widely used spinel ferrites are Ni-, Zn-, Mn-, and Li- tering process. We have investigated phase compo-
ferrites [19]. Compared to other types of spinel fer- nents, microstructures, and magnetic properties
rites, Li-ferrites possess higher Curie temperature based on the composite materials using systematical
and are less sensitive to stress [20]. Zn substitution is characterization methods and have been discussed in
generally adopted for Li-ferrites due to its effective- detail.
ness in adjusting magnetization moment, lowering
magnetocrystalline anisotropy constant, improving
grain growth and densification [6, 20]. So far, nano- 2 Materials and methods
sized LiZn ferrites have been mainly synthesized for
electromagnetic shielding or microwave absorbers Li0.4Zn0.2Fe2.4O4–Y3Fe5O12–BBSZ three-phase com-
[21, 22]. Various synthesis methods have been posites were prepared on the basis of LiZn ferrite,
reported in the preparation of LiZn ferrite nanopar- YIG ferrite, and BBSZ glass powders in the following.
ticles, like chemical route [23, 24], sol–gel method Here, LiZn ferrite powders were synthesized by a
[19–22], solution combustion [7], etc. Sol–gel sol–gel combustion method, as similarly described in
approaches have attracted much attention due to its the literature [20, 22, 35]. First, lithium nitrate
well-known inherent advantages to generate glass, [LiNO3], zinc nitrate [Zn(NO3)26H2O], iron nitrate
glass–ceramic and ceramic powders [19, 20, 25]. [Fe(NO3)39H2O], and citric acid [C6H8O7H2O] with
However, low magnetic loss and dielectric loss of a molar ratio of 2:1:12:15 were dissolved in de-ionized
LiZn ferrites restrain them from being widely used as water (500 mL). Ammonia was slowly added to the
microwave absorbers [26]. solution to adjust the pH value to 7. During this
One alternative way to improve the electromag- process, the solution was continuously stirred using a
netic properties of LiZn ferrites is to form composites magnetic agitator. Thereafter, the solution was
with dielectric materials, such as carbon nanotubes poured into a beaker, heated to 80 °C and stirred
[21] and polymers [22]. The other way is to fabricate vigorously for 4 h to form a sol. Dried gel was
LiZn ferrites hollow microspheres by self-reactive achieved after the sol was oven-dried for 24 h at
quenching technology, which enhances the micro- 110 °C. When ignited at any point, the dried gel
wave absorption properties in low frequencies [27]. burned in a self-propagating combustive manner
Moreover, ferrite–glass composite is supposed to until all gels were burned completely out to form
possess competitive microwave absorption ability loose LiZn ferrite powders. As described elsewhere
compared with ferrite–polymer composites espe- [36–39], YIG ferrite powders were synthesized using
cially in low frequency range [28]. the sol–gel combustion method starting with yttrium
In this work, ferrite–glass nanocomposites have nitrate [Y(NO3)36H2O], iron nitrate [Fe(NO3)39H2O],
been motivated to prepare based on a ceramic route. and citric acid [C6H8O7H2O] with a molar ratio of
Herein, nano-sized LiZn ferrites with a composition 3:5:8 dissolved in de-ionized water (500 mL).
of Li0.4Zn0.2Fe2.4O4 prepared by sol–gel combustion Ammonia was added to adjust the pH value to 3. The
method have been chosen because they possess high following fabrication process to obtain YIG ferrite
saturation magnetization, high thermal stability, and powders was the same with that of LiZn ferrite
low density [20, 29, 30]. Meanwhile, yttrium iron powders. For the BBSZ glass powders, they were
garnet (Y3Fe5O12, YIG) has also been selected to form prepared as described elsewhere [33, 34]. Then the
spinel-garnet ferrite composites, as YIG possesses powders of LiZn ferrite ? 2 wt. % BBSZ glass, YIG
J Mater Sci: Mater Electron (2023) 34:1250 Page 3 of 9 1250
ferrite ? 2 wt. % BBSZ glass, and LiZn ferrite ? YIG average crystallite size is 28.6 ± 0.5 nm via calcula-
ferrite (the mass ratio of LiZn ferrite and YIG ferrite tion using the Scherrer formula [40] from the main
was 1:1) ? 2 wt. % BBSZ glass were wet-milled (iron peaks of the XRD pattern. The lattice parameter is
balls with 10 mm and 6 mm in diameter) for 6 h, 8.372 Å. Granular particles were obtained according
respectively. The dried compounds were then mixed to the TEM image (see Fig. 1b). Pure spinel structure
with a 10 wt% polyvinyl binder, sieved through a was observed in the selected area electron diffraction
mesh of 100 lm and pressed at 9 MPa to form tor- (SAED) pattern as shown in Fig. 1c, which was con-
oidal samples ([18 mm). Finally, LiZn ferrite-BBSZ sistent with the XRD analysis results. The XRD pat-
glass, YIG ferrite-BBSZ glass, and LiZn/YIG-BBSZ tern of the YIG nanoparticles is shown in Fig. 1d. The
glass composite samples were sintered in air at main phase of YIG was observed as well as a small
975 °C for 4 h, respectively. The corresponding amount of perovskite (YFeO3) and hematite (a-Fe2O3)
samples are termed as LiZn-BBSZ, YIG-BBSZ, and phases, which might be due to the fact that the sol–
LiZn/YIG-BBSZ, respectively. gel combustion process lacks the necessary heat
The ferrite phases were investigated at room tem- treatment to obtain a pure YIG phase [36, 39]. The
perature used a Philip X’Pert Pro X-ray diffraction lattice parameter of YIG in the nanoparticles is
with Cu Ja radiation (k = 1.5406 Å). Ultra-fine 12.376 Å. TEM and HR-TEM images (see Figs. 1e and
powders of the LiZn/YIG ferrite nanocomposites 1f) indicate that mainly YIG phase is identified in the
were prepared for the XRD measurements by grind- obtained nanoparticles, in agreement with the XRD
ing the samples in an agate mortar. TEM was carried results.
out on a Tecnai G2 F20 S-TWIN at 200 kV. Before Figure 2 shows the XRD patterns of the LiZn-BBSZ,
imaging, the LiZn ferrite and YIG ferrite powders YIG-BBSZ, and LiZn/YIG-BBSZ, respectively. As can
prepared by the sol–gel combustion method were be seen, only spinel LiZn ferrite phase was observed
dispersed in ethanol, and then the suspensions were in the LiZn-BBSZ. Based on calculation from the XRD
treated by ultrasound for * 5 min. The microstruc- data, the lattice parameter of LiZn ferrite in the LiZn-
tures of the samples of LiZn-BBSZ, YIG-BBSZ, and BBSZ is 8.364 Å. For the YIG-BBSZ, main YIG ferrite
LiZn/YIG-BBSZ were characterized by a field emis- phase with a handful of YFeO3 was detected.
sion scanning electron microscopy (FE-SEM, JEOL Accordingly, the lattice parameter of YIG ferrite in
JSM-7600F). The magnetic hysteresis loops of liquid- the YIG-BBSZ is 12.367 Å. As for the LiZn/YIG-
phase-sintered samples were measured using a BHV- BBSZ, a clear signature of phase separation of LiZn
525 vibrating sample magnetometer (VSM) in mag- ferrite and YIG ferrite is present while the diffraction
netic fields ranging from ? 5000 Oe to -5000 Oe at peaks are consistent with the standard powder
room temperature. Part of the sintered toroids were diffraction patterns of Li0.435Zn0.195Fe2.37O4 (JCPDS
crashed and shaped to small spheres having a No. 37-1471) and Y3Fe5O12 (JCPDS No. 43-0507). The
diameter of * 1.0 mm for the measurement of fer- lattice parameters of LiZn ferrite and YIG ferrite in
romagnetic resonance (FMR) linewidth (DH) in a the LiZn/YIG-BBSZ are 8.363 Å and 12.368 Å,
TE106 cavity at 9.5–9.6 GHz by applying a perturba- respectively. The lattice parameter of LiZn ferrite in
tion method. the LiZn-BBSZ is very close to that in the LiZn/YIG-
BBSZ but is lower than that of the LiZn ferrite
nanoparticles. Similarly, the lattice parameter of YIG
3 Results and discussion ferrite in the YIG-BBSZ or in the LiZn/YIG-BBSZ is
almost the same but both of them are lower than that
To check the nanocrystalline structures and mor- of the YIG ferrite nanoparticles or the standard
phologies of the LiZn ferrite and YIG synthesized by Y3Fe5O12 (JCPDS No. 43-0507). These behaviors may
the sol–gel combustion method, XRD and TEM be associated with oxygen deficit caused by the ball
analysis were performed as results shown in Fig. 1. milling procedure. Moreover, a small amount of
The XRD pattern of the LiZn ferrite nanoparticles is YFeO3 is also presented in the ferrite composites as
shown in Fig. 1a. The corresponding XRD diffraction similarly observed in the LiZn/YIG-BBSZ.
peaks could be indexed to (111), (220), (311), (222), Figure 3 shows the SEM images of the LiZn-BBSZ,
(400), (422), (511), and (440) reflections, indicating YIG-BBSZ, and LiZn/YIG-BBSZ, respectively. As
that only the spinel structure is presented. The shown in Fig. 3a, a compact microstructure with an
1250 Page 4 of 9 J Mater Sci: Mater Electron (2023) 34:1250
Fig. 1 a XRD pattern of the LiZn ferrite nanoparticles prepared by prepared by sol–gel combustion method. e TEM image of the YIG
sol–gel combustion method. b TEM image of the LiZn ferrite ferrite nanoparticles. f High resolution-transmission electron
nanoparticles. c Selected area electron diffraction (SAED) pattern microscopy (HR-TEM) image of the YIG ferrite nanoparticles
of the LiZn ferrite obtained from the area shown in the green box obtained from the area shown in the red box of e (Color
of b. d XRD pattern of the nanoparticles of Y3Fe5O12 (YIG) figure online)
Fig. 3 SEM image of the cross section of a LiZn-BBSZ, b, YIG-BBSZ, and c LiZn/YIG-BBSZ
Fig. 6 FMR spectrum with fitted line for a LiZn-BBSZ, b YIG-BBSZ, and c LiZn/YIG-BBSZ. d FMR linewidth (DH) values obtained
from the experimental data
magnetization, a is lattice constant and D is grain Figure 6a-c show the ferromagnetic resonance
size. Hc is inversely proportional to the grain size and (FMR) spectra with fitted curves for the LiZn-BBSZ,
saturation magnetization. A smaller grain size gives YIG-BBSZ, and LiZn/YIG-BBSZ, respectively. All the
rise to a higher Hc owing to pinning of domain walls fitting curves match well with the FMR spectra. The
caused by grain boundaries which requires a higher FMR linewidth (DH) calculated from the experimen-
energy for switching [41]. Moreover, coercivity is also tal data is shown in Fig. 6d. Among all types of
related to porosity as reported by Goldman [42]. samples, the LiZn/YIG-BBSZ possesses the largest
Porosity can also increase Hc but its effect on Hc is DH (* 1018.4 Oe), about 285% of that of the LiZn-
smaller than the grain size. Saturation magnetization BBSZ (* 356.9 Oe) and * 454% of that of the YIG-
of the LiZn-BBSZ, YIG-BBSZ, and LiZn/YIG-BBSZ BBSZ (* 224.4 Oe). The sharp enhancement of
is * 75.1 emu/g, * 21.6 emu/g, and * 46.4 emu/ DH for the ferrite composites is mainly owing to the
g, respectively. Depending on crystal structure and increase in both intrinsic and extrinsic damping as
molecular magnetic moment, saturation magnetiza- similarly reported in BaM/YIG ferrite nanocompos-
tion of the LiZn-BBSZ is much higher than that of the ites [43], or other nanocomposites [44]. Specifically,
YIG-BBSZ. Besides, YIG ferrites act as magnetic the polydispersity and the dynamic magnetic inho-
dilution centers in the LiZn/YIG-BBSZ. This is why mogeneity in the LiZn/YIG-BBSZ could effectively
the saturation magnetization of the LiZn/YIG-BBSZ broaden the FMR linewidth. The YIG-BBSZ exhibited
is lower than that of the LiZn-BBSZ.
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