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Sun et al. Soft Sci. 2025, 5, 35 https://dx.doi.org/10.20517/ss.2025.21 Page 3 of 16

EXPERIMENTAL
Chemicals and reagents
Ferrous sulfate (FeSO ·7H O), zinc chloride (ZnCl ), thioacetamide (C H NS), sodium hydroxide (NaOH),
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glycerol (C H O ) and hydrazine hydrate (N H ·H O) were purchased from Sinopharm Chemical Reagent
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Co., Ltd., cobalt (II) chloride hexahydrate (CoCl ·6H O), nickel (II) chloride hexahydrate (NiCl ·6H O),
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were got from Shanghai Aladdin Biochemical Technology Co., Ltd., Indium (III) chloride tetrahydrate
(InCl ·4H O) was got from Shanghai Macklin Biochemical Technology Co., Ltd.
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Preparation of FeCoNi microspheres
The FeCoNi microspheres were synthesized at room temperature. Firstly, 1.668 g FeSO ·7H O, 1.142 g
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CoCl ·6H O, and 0.285 g NiCl ·6H O were all dissolved in 100 mL H O with stirring 3 min (solution A).
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After that, 5 g NaOH and 18 mL N H ·H O were dissolved in 10 mL H O (solution B). Then, solution B was
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slowly added drop by drop to solution A. After reacting 24 h, the final FeCoNi microspheres were
magnetically separated and further washed with H O and EtOH several times, and dried under vacuum in
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an oven at 60 °C overnight.
Preparation of FeCoNi@ZnIn S microspheres
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The original FeCoNi@ZnIn S microspheres were synthesized by oil bath method. Firstly, 0.027 g ZnCl ,
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0.117 g InCl ·4H O and 0.060 g C H NS were dissolved in 80 mL H O and 20 mL glycerol with vigorous
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stirring for 30 min, after which 0.2 g FeCoNi microspheres powders were poured into the above mixture to
be ultrasonicated for 10 min. Then, the mixture was heated at 80 °C for 2 h, cooled down to room
temperature and then washed with H O and EtoH for several times. Finally, the original FeCoNi@ZnIn S
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2 4
microspheres were dried at 60 °C overnight. The original FeCoNi@ZnIn S microspheres were denoted as
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FCNZ. ZnIn S can also be prepared by using the above procedures without the addition of FeCoNi.
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To obtain the final FeCoNi@ZnIn S -500, FeCoNi@ZnIn S -600 and FeCoNi@ZnIn S -700 microspheres,
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the FeCoNi@ZnIn S powders were annealed in H /Ar at 500, 600, and 700 °C for 5 h. The FeCoNi@ZnIn S
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-500, FeCoNi@ZnIn S -600 and FeCoNi@ZnIn S -700 microspheres were denoted as FCNZ-500, FCNZ-600
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and FCNZ-700. ZnIn S was annealed under the identical conditions to obtain the ZnIn S -500, ZnIn S -600,
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and ZnIn S -700.
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Characterization and measurement
The crystal structure of the samples was analyzed by X-ray diffraction (XRD, Brucker, D8 ADVANCED).
The morphology of the samples was observed using field emission scanning electron microscope (FESEM,
HITACHI, S4800). The JEOL JEM-2100F transmission electron microscope (TEM) was used to analyze the
material morphology. The XPS spectra in this study were obtained using a Thermo Scientific ESCALAB
250Xi. The hysteresis loops were analyzed using a superconducting quantum interference device
magnetometer [MPMS(SQUID) VSM]. The mixtures of ZnIn S , FeCoNi, ZnIn S -500, ZnIn S -600, ZnIn S
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2 4
2 4
2 4
-700, FCNZ, FCNZ-500, FCNZ-600, and FCNZ-700 composites with 60 wt% paraffin were measured by
using the Agilent N5230C vector network analyzer over the range of 2-18 GHz. Detailed information can be
found in the Supplementary Materials.
RESULT AND DISCUSSION
Structural and morphology analysis
The synthesis process and morphological evolution of FCNZ-500, FCNZ-600 and FCNZ-700 microspheres
are depicted in Figure 1A. Firstly, metal salt ions (Fe , Co , and Ni ) were combined with OH , and
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2+
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2+
subsequently ferromagnetic FeCoNi powders were synthesized in the presence of hydrazine hydrate
(N H ·H O). Next, it was ultrasonically dispersed in a mixed solution of glycerol and water containing Zn ,
2+
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