• Korean Journal of Materials Research
• /
• v.19 no.4
• /
• pp.220-223
• /
• 2009

Lithium dihydrogen phosphate ($LiH_2PO_4$) powder was purchased from Aldrich Chemical Co. From the scanning electron microscope (SEM) observation, these polycrystals have dimensions in the range of $25-250{\mu}m$. The electrical conductivity was measured at a measuring frequency of 1 kHz on heating polycrystalline lithium dihydrogen phosphate ($LiH_2PO_4$) from room temperature to 493 K. Two anomalies appeared at 451 K ($T_{p1}$) and 469 K ($T_{p2}$). The electrical conductivity reached the magnitude of the superprotonic phases: $3{\times}10^{-2}{\Omega}^{-1}cm^{-1}$ at 451 K ($T_{p1}$) and $1.2{\times}10{\Omega}^{-1}cm^{-1}$ at 469 K ($T_{p2}$). It is uncertain whether the superprotonic phase transformations are due to polymorphic transitions in the bulk, surface transitions, or chemical reactions (thermal decomposition) at the surface. Considering several previous thermal studies (differential scanning calorimetry and thermogravimetry), our experimental results seem to be related to the last case: chemical reactions (thermal decomposition) at the surface with the progressive solid-state polymerization.

• Polymer(Korea)
• /
• v.35 no.6
• /
• pp.599-604
• /
• 2011

The PET-PEN copolymers have been synthesized and the effect of their morphology on the physical properties of polyester flexible substrate was investigated. It was found that the block sequence of synthesized copolymer was varied depending upon DMT/NDC ratio in polymerization. Higher PET-PEN and PEN block sequence in polyester copolymer resulted in the increase of glass transition temperature and it caused the enhancement of dimensional stability as a polyester flexible substrate. The highest coefficient of thermal expansion(CTE) was obtained when DMT/NDC ratio is 50/50. Synthesized PET-PEN copolymer seems to be acceptable as a flexible substrate since it shows that their optical transmittance at 550 nm is over 80% and thermal weight loss at $280^{\circ}C$ for 1 hr is less than 0.4 wt%.

• Journal of the Korean Ceramic Society
• /
• v.34 no.2
• /
• pp.216-224
• /
• 1997

Porous silica ceramics were prepared(with HCI catalyst) using H2O/TEOS molar ratios of 2.6~59.0, with the EtOH/TEOS ratio fixed. After preparing 9 kinds of sol, the followings were investigated; measurement of the gelation time, thermal analyses by TG/DTA, property analyses of the intermediates by FT-IR and X-ray diffractometry with dried samples, analyses of SiO2 polymer by FT-IR, the investigation of specific sur-face area and pore size distribution by N2-adsorption isotherm, and structural change of SiO2 polymer and pore morphology by TEM observation, with samples heat-treated to 50$0^{\circ}C$. In the concentrations of in-vestigated compositions and catalyst, gelation time showed a minimum at ca. 11 moles of water per one mole of TEOS, the highest degree of polymerization at ca. 8-18 moles, and the largest specific surface area at ca. 11 moles, which means that the polymerization proceeded fastest at ca. 11 moles of water. In con-clusion, the more water used, the faster the polymerization reaction up to ca. 11 moles, but more than ca. 11 moles of water caused retardation of gelation and resultant reduction of specific surface area.

• Journal of the Korean Chemical Society
• /
• v.60 no.3
• /
• pp.181-186
• /
• 2016

The hydrophilic ophthalmic lens with addition of 2-hydroxyethyl acrylate (HEA), 2-hydroxyethyl methacrylate (HEMA), hydroxypropyl methacrylate (HPMA) and Ag nanoparticles were manufactured. And also, the cross-linker ethylene glycol dimethacrylate (EGDMA) and the initiator azobisisobutyronitrile (AIBN) were used for polymerization. The polymerization of the hydrogel lens material was conducted through thermal polymerization in 100 ℃ for 1h. The optical and physical characteristics of hydrogel lens were evaluated by measuring water content, refractive index and optical transmittance. The water content of sample containing HEA, HEMA and HPMA was in the average of 82.12%, 37.06% and 21.57%, respectively. And also, refractive index of the sample containing HEA, HEMA and HPMA was in the average of 1.3540, 1.4330 and 1.4649, respectively. In case of the optical properties of the sample, the results showed that the near-UV transmittance was 82.67%, 80.32% and 79.83%, and the visible transmittance was 89.72%, 88.24% and 86.89%, respectively. And also, optical transmittance of the sample containing Ag nanoparticles showed that the near-UV transmittance of 10.59% and visible transmittance of 43.74% were obtained. From the results, the molecular length influenced on the water content and refractive index of the polymerized material.

• Elastomers and Composites
• /
• v.39 no.3
• /
• pp.217-227
• /
• 2004

A new thermotropic liquid crystalline polymer(TLCP) containing a triad aromatic ester type mesogenic unit and butylene terephthalate unit(BT) in the main chain was synthesized by polycondensation reaction. The TLCP synthesized showed nematic mesophasic behavior and its transition temperature from solid to mesophase was $260^{\circ}C$. The TLCP/PBT blends were prepared by in-situ polymerization in PBT solution and characterized by differential scanning calorimeter(DSC), thermogavimetric analyzer(TGA), scanning electron microscope(SEM), x-ray diffractometer(XRD), and dynamic mechanical thermal analyze, (DMTA). The blends showed well dispersed TLCP phases with domain sizes $0.05{\sim}0.2{\mu}m$ in the PBT matrix. As the increasing TLCP content from 5 to 20 wt%, ${\Delta}Hm$ values of pure PBT in the blend were increased because TLCP acts as a nucleating agent in the PBT matrix. The mechanical properties of the blends depended on the TLCP contents because the TLCP acted effectively as a reinforcing material in the PBT matrix. The blends showed good interfacial adhesion between the TLCP phase and PBT matrix.The blends prepared by in-situ polymerization showed higher mechanical properties and well dispersed TLCP domains than those of the blends prepared by melt blending.

• Polymer(Korea)
• /
• v.28 no.2
• /
• pp.143-148
• /
• 2004

${\alpha}$,$\omega$-Hydrogen polyorganosiloxane(HPMDMS) prepolymer was prepared from equilibrium polymerization ofoctamethylcyclotetrasiloxane, 1,3,5-trimethylcyclotrisiloxane, 1,3,5,7-tetravinyl-1,3,5,7-tetramethyl-cyclotetrasiloxane, and 1,1,3,3-tetramethyl disiloxane as an end-blocker in the presence of tetramethylammonium siloxanolate as a catalyst. Polyorganosiloxane modified with dimethylacrylamide(APMDMS) was prepared by hydrosilylation of HPMDMS with dimethylacrylamide in the presence of Pt catalyst, and followed by coordination of metal oxide (APMDMS-MO), such as NiO and FeO, to the amide moieties of the resulting polymer. The chemical structures of HPMDMS and APMDMS were confirmed by FT-IR and $^1$H-NMR analysis. Liquid silicone rubber containing metal oxide composite (LSRMO) was prepared by compounding APMDMS-MO, ${\alpha}$,$\omega$-vinylpolydimethylsiloxane, and a catalyst in a high speed dissolver. The thermal conductivity of LSRMO composite was determined to be 0.29 W/mK, and the volume resistivity exhibited a lower value than that of LSR composite. The mechanical and thermal properties of LSRMO and LSR composite were measured by UTM and TGA.

• Membrane Journal
• /
• v.19 no.2
• /
• pp.96-103
• /
• 2009

A series of organic-inorganic composite membranes from poly(vinyl chloride) (PVC) graft copolymer electrolyte and heteropolyacid (HPA) were prepared for proton conducting membranes. First, poly(vinyl chloride)-g-poly(styrene sulfonic acid) (PVC-g-PSSA) was synthesized by atom transfer radical polymerization (ATRP) using direct initiation of the secondary chlorines of PVC. HPA nanoparticles were then incorporated into the PVC-g-PSSA graft copolymer though the hydrogen bonding interactions, as confirmed by FT-IR spectroscopy. The proton conductivity of the composite membranes increased from 0.049 to 0.068 S/cm at room temperature with HPA contents up to 0.3 weight traction of HPA, presumably due to both the intrinsic conductivity of HPA particles and the enhanced acidity of the sulfonic acid of the graft copolymer. The water uptake decreased from 130 to 84% with the increase of HPA contents up to 0.45 of HPA weight traction, resulting from the decrease in number of water absorption sites due to hydrogen bonding interaction between the HPA particles and the polymer matrix. Thermal gravimetric analysis (TGA) demonstrated the enhancement of thermal stabilities of the composite membranes with increasing concentration of HPA.

• Polymer(Korea)
• /
• v.35 no.1
• /
• pp.52-59
• /
• 2011

L-PLA or D-PLA was synthesized in bulk at $140^{\circ}C$ by ring opening polymerization(ROP) of L-lactide or D-lactide as a monomer using tin(II) octoate and lauryl alcohol as a catalyst and an initiator with changing the amounts of catalyst(0.25~1.0 wt%) and initiator(0.l~0.5 wt%). And stereocomplex-PLA was prepared by L-PLA/D-PLA having a wide range of molecular weight(30000~90000 g/mol) and L-PLA/D-PLA blends having different mixing ratio ($X_D$). The melting temperature. thermal degradation temperature and thermal stability of stereocomplex-PLA were higher than those of homopolymers(L-PLA, D-PLA). We supposed that these improvements arose from a strong interaction between L-PLA and D-PLA. The improved mechanical properties and changes in morphology of LPLA/D-PLA blends were compared to those of homopolymers(L-PLA, D-PLA).

• Polymer(Korea)
• /
• v.28 no.5
• /
• pp.404-411
• /
• 2004

The microcapsules containing triphenyl phosphate (TPP), a flame retardant, were prepared by phase-inversion emulsification technique using the epoxy resin (Novolac type) with excellent physical properties and network structure. This microencapsulation process was adopted for the protection of TPP evaporation and wetting of polymer composite during the polymer blend processing. The TPP, epoxy resin and mixed surfactants were emulsified to oil in water (O/W) by the phase inversion technology and then conducted on the crosslinking of epoxy resin by in-situ polymerization. The capsule size and size distribution of TPP capsules was controlled by mixed surfactant ratio, concentration and TPP contents, The formation and thermal property of TPP capsules were measured by differential scanning calorimetry and thermogravimetric analysis. The morphology and size of TPP capsules were also investigated by scanning and transmission electron microscopies. As the surfactant concentration increased, the TPP capsules were more spherical and mono-dispersed at the same weight ratio of mixed surfactants (F127: SDBS).

• Macromolecular Research
• /
• v.17 no.10
• /
• pp.739-745
• /
• 2009

N,N'-(bicyclo[2,2,2]oct-7-ene-tetracarboxylic)-bis-L-amino acids 3a-g were synthesized by the condensation reaction of bicyclo[2,2,2]oct-7-ene-2,3,5,6-tetracarboxylic dianhydride 1 with two equimolars of Lalanine 2a, L-valine 2b, L-leucine 2c, L-isoleucine 2d, L-phenyl alanine 2e, L-2-aminobutyric acid 2f and L-histidine 2g in an acetic acid solution. Seven new poly(amide-imide)s PAIs 5a-g were synthesized through the direct polycondensation reaction of seven chiral N,N'-(bicyclo[2,2,2]oct-7-ene-tetracarboxylic)-bis-L-amino acids 3a-g with bis(3-amino phenyl) phenyl phosphine oxide 4 by two different methods: direct polycondensation in a medium consisting of N-methyl-2-pyrrolidone (NMP)/triphenyl phosphite (TPP)/calcium chloride ($CaCl_2$/pyridine (py), and direct polycondensation in a tosyl chloride (TsCl)/pyridine (py)/N,N-dimethylformamide (DMF) system. The polymerization reaction produced a series of flame-retardant and thermally stable poly(amide-imide)s 5a-g with high yield. The resulted polymers were fully characterized by FTIR, $^1H$ NMR spectroscopy, elemental analyses, inherent viscosity, specific rotation and solubility tests. Data obtained by thermal analysis (TGA and DTG) revealed that the good thermal stability of these polymers. These polymers can be potentially utilized in flame retardant thermoplastic materials.