Effect of Surface Organic Functional Modification of ZrB2 Nanosize Multiphase Ceramics on the Thermal Properties of Its Composites†

doi:10.7503/cjcu20150145

Abstract

Abstract:

In order to enhance the thermal properties of the epoxy resin, zirconium diboride(ZrB₂) powders were chosen as reinforcement to add to the epoxy resin matrix to prepare composites by the in-situ polymerization due to its high melting point, good thermal conductivity and good heat resistance. The nano-alumina(Al₂O₃) was introduced in to form ZrB₂-Al₂O₃ multiphase ceramics through the high energy ball milling and by surface organic modification of nano-Al₂O₃ to achieve improved dispersibility of ZrB₂ particles in epoxy resin. The multiphase ceramic particles were modified by γ-aminopropyltriethoxysilane, γ-glycidoxypropyltri-methoxysilane and γ-methacryloxypropyltrimethoxysilane, respectively. The modified multiphase particles were characterized by scanning electron microscopy(SEM), Fourier transform infrared spectroscopy(FTIR) and X-ray photoelectron spectroscopy(XPS). The microstructure and thermal properties of composites filled with modified particles were analyzed using transmission electron microscopy(TEM), dynamic thermomechanical analysis(DMA) and thermo gravimetric analysis(TGA). The results show that the quality of multiphase particles is good after modification. The three organic coupling agent molecules are all combined to the surfaces of multiphase particles by the covalent bonds. The multiphase particles modified with organic coupling agents disperse well in epoxy resin matrix and the effect of γ-glycidoxypropyltrimethoxysilane is the best. The Composites filled with modified particles present higher thermal properties compared to unmodified composites.

Key words: ZrB2-Al2O3 multiphase ceramics, Surface organic modification, Epoxy resin, Thermal property

CLC Number:

O633.13

TrendMD:

HE Yannan, YU Zhiqiang. Effect of Surface Organic Functional Modification of ZrB₂ Nanosize Multiphase Ceramics on the Thermal Properties of Its Composites^†[J]. Chem. J. Chinese Universities, 2015, 36(9): 1846.

Figures/Tables 10

Fig.1 FTIR spectra of ZrB2-Al2O3 multiphase particlesa. Unmodified; b. modified with γ-aminopropyltriethoxysilane; c. modified with γ-glycidoxypropyltrimethoxysilane; d. modified with γ-methacryloxypropyltrimethoxysilane.

Fig.2 XPS spectra of ZrB2-Al2O3 multiphase particles(A) Unmodified; (B) modified with γ-aminopropyltriethoxysilane; (C) modified with γ-glycidoxypropyltrimethoxysilane;(D) modified with γ-methacryloxypropyltrimethoxysilane.

Table 1 Binding energy(EB) of elements on the surface of different particles

ZrB₂-Al₂O₃ Multiphase particle	E_B(O₁_s)/eV	E_B(S $i 2 p 3$ )/eV	E_B(Al₂_p)/eV
Unmodified	534.0	103.0	76.0
Modified with γ-aminopropyltriethoxysilane	528.0	97.0	71.0
Modified with γ-glycidoxypropyltrimethoxysilane	531.0	101.0	74.0
Modified with γ-methacryloxypropyltrimethoxysilane	533.0	103.0	75.0

Table 1 Binding energy(EB) of elements on the surface of different particles

ZrB₂-Al₂O₃ Multiphase particle	E_B(O₁_s)/eV	E_B(S $i 2 p 3$ )/eV	E_B(Al₂_p)/eV
Unmodified	534.0	103.0	76.0
Modified with γ-aminopropyltriethoxysilane	528.0	97.0	71.0
Modified with γ-glycidoxypropyltrimethoxysilane	531.0	101.0	74.0
Modified with γ-methacryloxypropyltrimethoxysilane	533.0	103.0	75.0

Fig.3 TEM image(A) and EDS spectrum(B) of unmodified ZrB2-Al2O3 multiphase particles

Fig.4 TEM image(A) and EDS spectrum(B) of surface modified ZrB2-Al2O3 multiphase particles

Scheme 1 Surface modification mechanism diagram of multiphase particles with coupling agents γ-glycidoxypropyltrimethoxysilane

Fig.5 TEM images of composites filled with ZrB2-Al2O3 multiphase particles unmodified(A), modified with γ-aminopropyltriethoxysilane(B), γ-glycidoxypropyltrimethoxysilane(C) and γ-methacryloxypropyltrimethoxysilane(D)

Fig.6 DMA curves of epoxy resin and composites modified by γ-glycidoxypropyltrimethoxy-silanea. Epoxy resin; b. 5% ZrB2-Al2O3; c. 5% modified ZrB2-Al2O3; d. 10% modified ZrB2-Al2O3; e. 15% modified ZrB2-Al2O3.

Fig.7 TGA curves of epoxy resin and composites modified by γ-glycidoxypropyltrimethoxy-silanea. Epoxy resin; b. 5% ZrB2-Al2O3; c. 5% modified ZrB2-Al2O3; d. 10% modified ZrB2-Al2O3; e. 15% modified ZrB2-Al2O3.

Table 2 TGA results of epoxy resin and composites

Filler	T_i/℃	T_e/℃	T_max/℃
Epoxy resin	318.6	392.1	367.8
5% ZrB₂-Al₂O₃	337.6	394.6	375.4
5% Modified ZrB₂-Al₂O₃	367.6	403.9	392.7
10% Modified ZrB₂-Al₂O₃	341.6	399.1	381.1
15% Modified ZrB₂-Al₂O₃	325.2	396.6	375.2

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Effect of Surface Organic Functional Modification of ZrB₂ Nanosize Multiphase Ceramics on the Thermal Properties of Its Composites^†

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