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. 2024 Jul 2;17(13):3260.
doi: 10.3390/ma17133260.

The Effect of Silanized Halloysite Nanotubes on the Structure of Polyethylene-Based Composite

Affiliations

The Effect of Silanized Halloysite Nanotubes on the Structure of Polyethylene-Based Composite

Martina Wieczorek et al. Materials (Basel). .

Abstract

Chemical modification of the surface of halloysite nanotubes (HNT) by alkalization (with sodium hydroxide (NaOH)) and grafting with silanes (bis(trimethylsilyl)amine (HMDS)) was carried out. The efficiency of the alkalization and grafting process was evaluated by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and the nitrogen adsorption method were used. XRD and FTIR analysis confirmed the formation of bonds of trimethylsilyl groups to the HNT surface which changed the nature of the surface from hydrophilic to hydrophobic. In addition, it was noted that grafting with silanes decreases by 7.2% the specific surface area of the halloysite compared to the alkalized material. High-density polyethylene (HDPE) composites with halloysite (HNT), alkalized halloysite (alk-HNT), and HMDS-modified halloysite (m-HNT) were processed in the molten state in a Brabender mixer chamber. On SEM/EDS micrographs of HDPE composites with silanized HNT, a change in surface characteristics from smooth to ductile was observed. Higher melting point values based on differential scanning calorimetry (DSC) analysis of HDPE composites with 5%wt silanized halloysite in comparison with HNT and alk-HNT of, respectively, 2.2% and 1.4% were found, which indicates a slight beneficial influence of the filler on the quality of ordering of the crystalline phase of the matrix.

Keywords: halloysite; high–density polyethylene; silanization; structure properties.

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Conflict of interest statement

The authors declare no conflicts of interest.

Figures

Figure 1
Figure 1
Scheme of possible hydrophobic surface modification of the HNTs through hexamethyl–disilazane (HMDS) grafting.
Figure 2
Figure 2
XRD patterns of HNTs before and after alkali treatment and HMDS modification.
Figure 3
Figure 3
IR–spectra of HNTs surfaces before and after modification.
Figure 4
Figure 4
SEM microphotographs of (AC) raw halloysite, (DF) alkalized halloysite, (GI) HMDS–modified halloysite.
Figure 5
Figure 5
FTIR spectrum of HDPE/5HNT, HDPE/5alk–HNT, HDPE/5m–HNT composites.
Figure 6
Figure 6
SEM microphotographs of the prepared composites: (A,B) HDPE/5HNT, (C,D) HDPE/5alk–HNT, (E,F) HDPE/5m–HNT.
Figure 6
Figure 6
SEM microphotographs of the prepared composites: (A,B) HDPE/5HNT, (C,D) HDPE/5alk–HNT, (E,F) HDPE/5m–HNT.
Figure 7
Figure 7
EDS maps: (A) HDPE/5HNT, (B) HDPE/5alk–HNT, (C) HDPE/5m–HNT.
Figure 8
Figure 8
Elemental EDS mapping of composites with 5 wt% raw halloysite, alkalized halloysite, and HMDS–modified halloysite.
Figure 9
Figure 9
DSC curves of HDPE and HDPE/5HNT, HDPE/5alk–HNT, HDPE/5m–HNT composites.

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