Fabrication of transparent methacrylate zirconium siloxane hybrid materials using sol–gel synthesized oligosiloxane resin

Bae, Jun-Young; Yang, SeungCheol; Jin, Jung Ho; Jung, Kyung‐Won; Kim, Joon-Soo; Bae, Byung Seong

doi:10.1007/s10971-010-2363-x

Cited by 35 publications

(29 citation statements)

References 28 publications

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“…The Si–OH band (3230‐3560 cm −1 ) of oligosiloxane was almost disappeared because of sol‐gel condensation, and the new formed broad band (1030‐1140 cm −1 ) of oligosiloxane further confirmed the formation of the Si–O–Si bond. On the other hand, the Si–OCH 3 band (2840 cm −1 ) in MPTMS and VTMS did not disappear representing presence of residual Si–OCH 3 group, which was consistent with the results of the 29 Si NMR spectrum …”

Section: Resultssupporting

confidence: 89%

“…In addition, a narrow peak appeared at −31 ppm, and as the ZrO 2 content increased to 10 wt%, this peak and D 1 (−35 to −38 ppm) signal moved to high field at −37 and −39 ppm, respectively. This effect of field shift is attributed to the formation of Si–O–Zr heterometallic bond . A covalent bond was formed by cohydrolysis reaction between zirconium propoxide and unreacted alkoxy group, and this strong interaction was beneficial to increase compatibility between the polymer matrix and the inorganic nanoparticles.…”

Section: Resultsmentioning

confidence: 99%

“…The RI of silicone can be adjusted by changing the monomer type and their ratio. Similarly, the metal alkoxide can also participate in the polycondensation process of the monomers to synthesize a hybrid resin with heterometallic bond at a molecular level . As the Ti and Zr contents increased, the RI of the resins increased from 1.57 to 1.62 and 1.53 to 1.58, respectively.…”

Section: Introductionmentioning

confidence: 99%

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Preparation of ZrO₂/silicone hybrid materials for LED encapsulation via in situ sol‐gel reaction

Huang

Feng

Sun

et al. 2019

Polymers for Advanced Techs

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Organic silicones have been used as encapsulant materials for light‐emitting diodes (LEDs) for many years, while their performances need to be improved in order to satisfy the requirements of high‐power LEDs. A ZrO2/silicone hybrid resin (ZHR) was synthesized for LEDs encapsulation by in situ sol‐gel reactions. The oligosiloxane was synthesized as polymeric matrix by nonaqueous sol‐gel condensation using diphenylsilanediol (DPSD), vinyltrimethoxysilane (VTMS), and 3‐methacryloxy propyl trimethoxysilane (MPTMS) as monomers. Then zirconium propoxide was added into this polymeric matrix to be hydrolyzed to obtain the hybrid resin with a uniform dispersion of ZrO2 nanoparticles. The Si–O–Zr covalent bond was detected and benefited for excellent dispersibility of the ZrO2 nanoparticles and the well compatibility between organic and inorganic phases. The cured ZHR with 5 wt% ZrO2 content showed high light transmittance (greater than 80% in visible light range), high refractive index (=1.56), and high thermal stability (no yellowing at 150°C for 240 hours). The luminous flux of the LED chip with ZHR encapsulant was 10% higher than that of the pure silicone resin, suggesting that ZHR has great application potential in the field of LED packaging.

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Section: Resultssupporting

confidence: 89%

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Preparation of ZrO₂/silicone hybrid materials for LED encapsulation via in situ sol‐gel reaction

Huang

Feng

Sun

et al. 2019

Polymers for Advanced Techs

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“…Mahmood et al used a sol‐gel technique to synthesize epoxidized natural rubber/zirconia hybrid films, varying the amount of zirconium(IV) n ‐propoxide added in an attempt to improve the thermal stability and glass transition temperature ( T g ) of the product . Bae et al used the sol‐gel reaction between 3‐(trimethoxysilyl)propylmethacrylate, diphenylsilanediol and zirconium n ‐propoxide chelated with methacrylic acid to synthesize a methacrylate zirconium siloxane resin, and then spin‐coated and photo‐polymerized the product to fabricate a highly transparent methacrylate zirconium siloxane hybrimer coating film . Du and colleagues used a non‐hydrolytic sol‐gel process with zirconium oxychloride (ZrOCl 2 .8H 2 O) and silicic acid, used as ZrO 2 and SiO 2 precursors, respectively, to prepare a poly(methylmethacrylate)/silica/zirconia nanocomposite that gave excellent optical transmittance and was very thermally stable …”

Section: Introductionmentioning

confidence: 99%

Synthesis of a liquid zirconium hybrid resin and the ability of the resin to accelerate the curing of a transparent silicone-modified cycloaliphatic epoxy nanocomposite

et al. 2015

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A liquid zirconium hybrid resin (Zr–QR) was synthesized through sol‐gel reactions of zirconium butoxide with silanol‐terminated polydimethylsiloxane (DMS‐S12) and γ‐glycidoxypropyltrimethoxysilane (Z‐6040). The sol‐gel reactions were monitored using Fourier transform infrared (FTIR) spectroscopy and proton nuclear magnetic resonance spectroscopy. The Zr–QR morphology was investigated using field emission transmission electron microscopy. The Zr–QR had a well‐ordered morphology and the dimensions were less than 5 nm. These properties were achieved because DMS‐S12 was used to separate the zirconium clusters and Z‐6040 was used to stabilize the Zr–QR. The acceleration of the curing reaction between silicone‐modified cycloaliphatic epoxy (SEP) and methylhexahydrophthalic anhydride (MHHPA) caused by the Zr–QR was investigated. Differential scanning calorimetry and FTIR spectroscopy investigations showed that the Zr–QR first reacted with MHHPA, producing chelating ligands and carboxylic acid. Unlike in the conventional method (adding acetic acid to cause non‐reactive chelating ligands to form), the carboxylic acid produced effectively accelerated the curing reaction between the SEP and MHHPA. The chelating ligand produced from the Zr–QR and MHHPA suppressed the gelation of the Zr–QR itself during the nanocomposite (SEP–Zr–QR) curing process. The cured SEP–Zr–QR nanocomposite exhibited excellent optical transmittance at visible wavelengths.© 2015 Society of Chemical Industry

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“…34 ZrO 2 nanoparticles were also formed with other chelating reagents, such as acetylacetone, 2,2 -bipyridine and 3,4-diaminobenzoic acid. 19,20,23 The degree of corrosion protection depends on the type of chelating agent used. 20,35 The hybrid silane coatings based on TEOS, MAPTMS, ZTP and MAA are amorphous and do not contain ZrO 2 particles seen by SEM, AFM and TEM techniques.…”

mentioning

confidence: 99%

Electrochemical and Salt Spray Testing of Hybrid Coatings Based on Si and Zr Deposited on Aluminum and Its Alloys

Rodič

Milošev

2015

J. Electrochem. Soc.

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Hybrid coatings based on Si and Zr were assessed for their protection of aluminum and its alloys 2024-T3 and 7075-T6 against corrosion in 0.5 M NaCl. Coatings were prepared from sol synthesized from mixtures of tetraethyl orthosilicate and 3-methacryloxypropyl trimethoxysilane to which various concentrations of zirconium tetrapropoxide and methacrylic acid were added. Short-and long-term electrochemical behavior was assessed. The degree of protection was dependent on the sol composition, ageing time and curing temperature. A coating containing Zr/Si ratio of 0.41, aged for 48 h and cured at 100 • C exhibited the best combination of resistance towards general and localized corrosion. Electrochemical parameters obtained under polarization (corrosion current density of 4.4 nA/cm 2 and stability up to 7 V), and under open circuit conditions (impedance in the few tens of Mohm cm 2 after one week immersion) prove that the protection was high. At other conditions, such as higher Zr/Si ratios, shorter ageing time or curing at room temperature, protection was excellent early after immersion but then lessened rapidly. Coatings prepared under optimal conditions provided a high degree of protection over 500 hours salt spray testing, especially on aluminum metal. These coatings have the potential to provide good protection in chloride environments. While aluminum has good corrosion resistance in seawater, its high-strength alloys in the 2xxx (Al-Cu-Mg) and 7xxx series (Al-ZnMg) are normally not recommended for use under these conditions. 1,2Since there is an ongoing need for light-weight, high-strength materials, the possibility of using alloys other than those of the series 5xxx (Al-Mg-Mn) and 6xxx (Al-Mg-Si) normally recommended for sea-coast applications has to be considered. 2,3Aluminum and its alloys are highly susceptible to oxidation, resulting in the passivation of the surface by a 0.01 to 10 μm thick oxide layer when exposed to air. This naturally formed oxide protects aluminum under atmospheric conditions.2 Passivation of the alloys is, however, less effective. Due to the presence of unevenly distributed intermetallic particles (IMPs), the passive film is, overall, thinner and less uniform. IMPs such as Al 2 CuMg, Al-Cu-Mn-Fe, Al 2 Cu, Al 3 Fe, MgSi 2 , MgZn 2 , create local galvanic cells that promote corrosion on the surface. [4][5][6] Al 2 O 3 is a good insulator but, when containing IMPs, is a semiconductor that allows limited passage of electrons.2 High concentrations of chloride ions allows localized breakdown of the aluminum oxide film, most commonly observed as pitting, crevice or galvanic corrosion.Al alloys have been protected for decades using chromate conversion coatings. In the last decade these coatings have been widely prohibited within 7 and outside 8 the EU due to the fact that hexavalent chromium is a toxic, carcinogenic and environmentally hazardous compound.9-11 Other environmentally hazardous compounds, such as volatile organic compounds (VOCs) used, for example, in the painting industry, have ...

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Fabrication of transparent methacrylate zirconium siloxane hybrid materials using sol–gel synthesized oligosiloxane resin

Cited by 35 publications

References 28 publications

Preparation of ZrO₂/silicone hybrid materials for LED encapsulation via in situ sol‐gel reaction

Preparation of ZrO₂/silicone hybrid materials for LED encapsulation via in situ sol‐gel reaction

Synthesis of a liquid zirconium hybrid resin and the ability of the resin to accelerate the curing of a transparent silicone-modified cycloaliphatic epoxy nanocomposite

Electrochemical and Salt Spray Testing of Hybrid Coatings Based on Si and Zr Deposited on Aluminum and Its Alloys

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Fabrication of transparent methacrylate zirconium siloxane hybrid materials using sol–gel synthesized oligosiloxane resin

Cited by 35 publications

References 28 publications

Preparation of ZrO2/silicone hybrid materials for LED encapsulation via in situ sol‐gel reaction

Preparation of ZrO2/silicone hybrid materials for LED encapsulation via in situ sol‐gel reaction

Synthesis of a liquid zirconium hybrid resin and the ability of the resin to accelerate the curing of a transparent silicone-modified cycloaliphatic epoxy nanocomposite

Electrochemical and Salt Spray Testing of Hybrid Coatings Based on Si and Zr Deposited on Aluminum and Its Alloys

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Preparation of ZrO₂/silicone hybrid materials for LED encapsulation via in situ sol‐gel reaction

Preparation of ZrO₂/silicone hybrid materials for LED encapsulation via in situ sol‐gel reaction