• Macromolecular Research
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• 제14권5호
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• pp.504-509
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• 2006

Poly(vinyl phosphate-b-styrene) (PVPP-b-PS) block copolymers were synthesized successfully from poly(vinyl alcohol-b-styrene) (PVA-b-PS) by reaction with phosphorus oxychloride and subsequent hydrolysis. The obtained block copolymers were slightly crosslinked, and were characterized by various analytical techniques. The total phosphorus content and the ratio of the differently bound phosphorus were obtained by both solid-state $^{31}P$ NMR and pH titration, but the results differed slightly. Characterization by energy dispersion X-ray analysis (EDS) or Rutherford back scattering (RBS), on the other hand, determined the total phosphorus contents, but the results were quite different from those by solid-state $^{31}P$ NMR.

• Bulletin of the Korean Chemical Society
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• 제34권11호
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• pp.3253-3256
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• 2013

Lithium is a highly attractive material for high-energy-concentration batteries, since it has low weight and high potential. Rechargeable lithium-ion batteries (LIBs), which have the extremely high gravimetric and volumetric energy densities, are currently the most preferable power sources for future electric vehicles and various portable electronic devices. In order to improve the efficiency and lifetime, new electrode compounds for lithium intercalation or insertion have been investigated for rechargeable batteries. Solid-state nuclear magnetic resonance (NMR) is a very useful tool to investigate the structural changes in electrode materials in actual working lithium-ion batteries. To detect the in-situ microstructural changes of electrode and electrolyte materials, $^7Li-^{19}F$ double-resonance solid-state NMR probe with a static solenoidal coil for a 600-MHz narrow-bore magnet was designed, constructed, and tested successfully.

• 한국자기공명학회논문지
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• 제17권2호
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• pp.81-85
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• 2013

Various fluorine-containing materials are used in electronic devices like LCD display panels and Li-ion batteries. The structural conformation of fluorine in fluorinated materials is an important contributing factor that influences the chemical and physical properties. The conformation can be changed by heat and stress during manufacture or use. Understanding the conformational changes is critical for understanding the performance and durability of electronic devices. Solid-state NMR spectroscopy could be widely used for the analysis of various fluorine-containing materials for electronic devices. However, conventional CPMAS probes cannot be used for in-situ analysis of fluorine-containing electronic devices like LCD panels and Li-ion batteries. In this paper, we show the design, construction, and optimization of a $^{19}F-^{13}C$ double-resonance solid-state NMR probe for a 400MHz wide-bore magnet with a flat square coil for in-situ analysis of fluorine-containing electronic devices without observing fluorine background signals. This custom-built probe does not show any fluorine background signals, and can have higher efficiency for lossy samples.

• 한국자기공명학회논문지
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• 제10권1호
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• pp.74-88
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• 2006

Since the first commercial NMR spectrometer came out in 1953 from Varian, much of the hardware development has been improved and matured through commercial equipments. Many of magnetic resonance laboratories however still build and use home-built spectrometers, which are satisfactory even with the consideration of educational purpose only. The home-built NMR spectrometer could be further advantageous and could be often an only option for investigating new ideas with demanding experimental conditions or new hardware support. A solid state NMR spectrometer was designed with extra interest in stochastic experiment and built for an 8.93 T superconducting magnet from Oxford instrument. Super-heterodyned system was implemented for the transmitter and receiver parts. Intermediate frequency (IF) for the heterodyne system was chosen to 70 MHz for the first and the second channels, with additional 120 MHz for the third channel for maximum NMR frequency capability. We will show overall schematics, and discuss the designs with detailed diagrams, then demonstrate the applicability of home-built spectrometer with stochastic-excitation in solid state NMR and in applications to quadrupolar nuclear Spins.

• 한국고분자학회지:고분자과학과기술
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• 제4권4호
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• pp.287-304
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• 1993

• 한국자기공명학회논문지
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• 제5권1호
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• pp.19-28
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• 2001

Miscibility and morphology in blends of bisphenol-A type polycarbonate and poly (ester-ether) elastomer with different compositions are studied by solid-state NMR spectroscopy. $^{13}$ C Solid-state NMR of CP/MAS/TOSS/DD, CP/MAS/DD, inversion recovery CP/MAS/DD, and 2D rotor driven spin diffusion techniques are used to identify the miscibility, morphology, and transesterification in blends. The blends of PC /BT elastomer with 15% to 42% of soft segment seem to be single phase miscible mixing and those of PC/PBT and PC/PBT elastomer with 62% of soft segment are cocontinuous two phase immiscible mixing. No significant transesterification reactions are observed in blends with different compositions.

• Elastomers and Composites
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• 제43권4호
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• pp.281-287
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• 2008

고체상태 $^{13}C$ NMR을 이용하여 폴리부타디엔 고무(BR) 가황체의 정성 및 정량분석을 행하였다. TBBS로 촉진된 기존의 충진 BR 가황체에서는 올레핀성 이중결합에의 부가반응과 이중결합 옆의 $\alpha$ 위치에서의 치환반응이 동시에 일어났다. 또한 반응 초기에는 이중결합 옆의 $\alpha$ 위치에서의 치환반응은 이중결합에의 부가반응보다 빠르게 진행되었다. 한편 과가류(overcure) 시간 동안 이중결합-부가 폴리설파이드 구조는 5각형 및 6각형 고리 구조로 변형되는 것으로 추정되었다. 이러한 사슬 변형은 과가류 시간에 발생하는 화학적 가교 밀도와 상관되었다.

• 한국자기공명학회논문지
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• 제21권1호
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• pp.1-6
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• 2017

Enhancements in NMR sensitivity have been the main driving force to extend the boundaries of NMR applications. Recently, techniques to shift the thermally populated nuclear spin states are employed to gain high NMR signals. Here, we introduce a technique called photochemically induced dynamic nuclear polarization (photo-CIDNP) and discuss its progresses in enhancing the solution-state NMR sensitivity.

• Bulletin of the Korean Chemical Society
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• 제32권10호
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• pp.3644-3649
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• 2011

Multinuclear solid-state nuclear magnetic resonance (NMR) experiments were performed to investigate the local structure changes of nanoporous silica during hydrothermal treatment and surface modification with 3-aminopropyltriethoxysilane (3-APTES). The nanoporous silica was prepared by sol-gel polymerization using inexpensive sodium silicate as a silica precursor. Using $^1H$ magic angle spinning (MAS) NMR spectra, the hydroxyl groups, which play an important role in surface reactions, were probed. Various silicon sites such as $Q^2$, $Q^3$, $Q^4$, $T^2$, and $T^3$ were identified with $^{29}Si$ cross polarization (CP) MAS NMR spectra and quantified with $^{29}Si$ MAS NMR spectra. The results indicated that about 25% of the silica surface was modified. $^1H$ and $^{29}Si$ NMR data proved that the hydrothermal treatment induced dehydration and dehyroxylation. The $^{13}C$ CP MAS and $^1H$ MAS NMR spectra of 3-APTES attached on the surface of nanoporous silica revealed that the amines of the 3-aminopropyl groups were in the chemical state of ${NH_3}^+$ rather than $NH_2$.

• Bulletin of the Korean Chemical Society
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• 제20권8호
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• pp.921-924
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• 1999

Hydrogels were prepared from poly( Υ-glutamic acid) (PGA) solution by g-irradiation of 90 kGy and 170 kGy. The hydrogels were more cross-linked with a higher dosage g-irradiation and completely hydrolyzed at 85℃ within 4 hours resulting in homogeneous solution. NMR techniques were employed to clarify chemical bond formation and scission involved during γ-irradiation and hydrolysis. Characterization of these samples was carried out by taking both liquid state and solid state NMR spectra of PGA and hydrolyzed hydrogels and comparison of these spectra with the solid state NMR spectra of hydrogels. Our results indicate that complicated chemical bond formation and scission have occurred during hydrolysis and γ-irradiation. The samples prepared with higher dosage of γ-irradiation showed more diverse chemical bond formation and scission.