Pattern formation of polyimide by using photosensitive polybenzoxazole as a top layer

A versatile method for positive-type patterning of polyimide (PI) based on a two-layer photosensitive poly(benzoxazole) (PSPBO) and poly(amic acid) (PAA) film has been developed to provide a promising material in the field of microelectronics. This patterning system consisted of a pristine PAA thick bottom-layer and a poly(o-hydroxy amide) (PHA) thin top layer with 9,9-bis[4-(tert-butoxycarbonyl-methyloxy)phenyl]fluorene (TBMPF) as a dissolution inhibitor, and (5-propylsulfonyloxyimino-5H-thiophene-2-ylidene)-(2-methylphenyl)-acetonitrile (PTMA) as a photoacid generator (PAG). The PHA and PAA were prepared from 4,4′-(hexafluoroisopropylidene)-bis(o-aminophenol) and 4,4′-oxybis(benzoic acid) derivatives, and 3,3′,4,4′-biphenyltetracarboxylic dianhydride and 4,4′-oxydianiline, respectively, in N,N-dimethylacetamide. This two-layer system based on PHA (150-nm thickness) and PAA (1.5-μm thickness) showed high sensitivity of 35 mJ/cm² and high contrast of 10.3 when exposed to a 365 nm line (i-line), post-baked at 100 °C for 2 min, and developed in a 2.38 wt.% tetramethylammonium hydroxide aqueous solution/5 wt.% iso-propanol at 25 °C. A clear positive image of a 4-μm line-and-space pattern was printed on a film which was exposed to 100 mJ/cm² of i-line by a contact-printing mode and fully converted to the corresponding PBO/PI pattern upon heating at 350 °C, confirmed by FT-IR spectroscopy. This two-layer system could be applied to the patterning of various PAAs.     

Electrochemical properties of thin TiO2 electrode on Li1 + xAlxGe2 − x(PO4)3 solid electrolyte

A fabrication of all-solid-state thin-film rechargeable lithium ion batteries by sol-gel method is expected to achieve both the simplification and cost reduction for fabrication process. TiO₂ thin film electrode was prepared by PVP (polyvinylpyrrolidone) sol-gel method combined with spin-coating on Li_1 + xAl_xGe_2 − x(PO₄)₃ (LAGP) solid electrolyte which has wide electrochemical window. The thin film was composed of anatase TiO₂ that is the most active phase for Li insertion and extraction and contacted well with LAGP substrate. In the cyclic voltammogram, a redox couple was observed at 1.8 V vs. Li/Li⁺ assigned to Li insertion/extraction into/from anatase TiO₂, indicating that the thin film worked as electrode for lithium battery. The charge and discharge test in various charge and discharge rates revealed that the discharge process (delithiation) is thought to be faster than charge process (lithiation). It is attested that the sol-gel process, which derives both simplification and cost reduction for fabrication process, can be applied to thin film battery using LAGP solid electrolyte.     

NMR studies of a ternary complex reagent of lithium ester enolate, chiral diether, and lithium diisopropylamide in an asymmetric Michael reaction

A ternary complex reagent of lithium ester enolate-chiral diether-lithium diisopropylamide was formed in an equimolar mixture of these reagents in toluene based on low-temperature NMR spectroscopy. The use of [⁶Li,¹⁵N]-lithium diisopropylamide as a lithiodeprotonation and complexing reagent produced two sets of doublet peaks in ⁶Li NMR of a 1:1:1 mixture of lithium enolate-chiral diether-lithium diisopropylamide, indicating the formation of a ternary complex reagent.     

Theoretical study on quantum dynamics of bose system interacting with photon field

We investigate the quantum dynamics of two‐boson and two‐level systems interacting with a one‐mode photon field. The time evolution of the population for each state is calculated in terms of the Jaynes–Cummings model. We find the collapses and revivals of the order parameter for the Bose–Einstein condensation. © 2001 John Wiley & Sons, Inc. Int J Quantum Chem 84: 401–408, 2001     

Synthesis of 7‐acetyloxy‐3,7‐dimethy1‐7,8‐dihydro‐6H‐isochromene‐6,8‐dione and its analogues

7‐Alkanoyloxy‐3,7‐dimefhyl‐7,8‐dihydro‐6H‐isochromene‐6,8‐diones 12‐15 were synthesized in 69‐16% yields from the reaction of 2,4‐dihydroxy‐3‐methyl‐6‐(2‐oxopropyl)benzaldehyde 11 with p‐toluenesulfonic acid in various carboxylic acids such as acetic acid, propionic acid, butyric acid and heptanoic acid followed by oxidation with lead tetraacetate. On the other hand, (±)‐daldinin A 5 (oleate) was not obtained using oleic acid as a medium. In the cases of heptanoic acid and oleic acid, esters 16 and 17 were produced in 23 and 9% yields, respectively. 6,8‐Dihydroxy‐3,7‐dimethyl‐2‐benzopyrylium p‐toluenesulfonate 31 is considered as the intermediate for the production of 12‐15. Overall yields of isochromenes 12‐15 were 26‐6% starting from 2‐methylresorcinol for seven steps.     

Electric Field Gradients of B in TiO2

We observed the electric quadrupole interaction of ¹²B implanted in the interstitial site of TiO₂ using β-NMR method. The electric field gradients including the direction of the principal axes were determined. The direction agreed well with the theoretical calculation.     

Proton response of high sensitivity CR-39 copolymer

We studied the track response for the copolymer of CR-39 monomer with N-isopropylacrylamide (NIPAAm) as well as etching properties. It was found that copoly (CR-39/NIPAAm/Naugard 445) composed in wieght ratio of 99/1/0.01 is highly sensitive to low LET particles in the region below 10 keV/μm of LET and able to record normally incident particles of LET down to 1.5 keV/μm, recording protons up to the energy of 27 MeV. These results were compared with the responses for two types of CR-39 detectors containing a small quantity of antioxidant. The threshold energy proton registration is discussed.     

Layered silicate‐polyamide‐6 nanocomposites: Influence of silicate species on morphology and properties

The effect of two different species of layered silicates on the morphology, mechanical properties, and methanol vapor barrier properties of polyamide‐6 (PA6) nanocomposites was examined using identical experimental conditions for both species. The layered silicate species used were natural montmorillonite (MMT) and synthetic expandable fluoro‐mica (FM), the chemical compositions of which were Na_0.43(Al_1.56Mg_0.31Fe²⁺ _0.09)(Si_3.95Al_0.05)O₁₀(OH)₂ and Na_0.66Mg_2.68(Si_3.98Al_0.02)O₁₀F₂, respectively. The layered silicates were modified with a dodecylammonium salt (DDA) using an ion‐exchange method. The resulting organically modified layered silicates were melt‐kneaded with PA6 in a twin‐screw kneader at 260 °C. By quantitative analysis of the silicate layers dispersed in the PA6, the number‐average aspect ratio was estimated to be 76 for DDAMMT‐PA6 and 85 for DDAFM‐PA6. This confirmed that the primary particle size of the initial silicate did affect the aspect ratio. The rigidity and gas barrier properties of the nanocomposites appeared to depend upon the morphology of the nanocomposite. On the other hand, the elongation at break of the nanocomposites decreased as the amount of silicate increased. This reduction in ductility was ascribed to the difference in morphology of the nanocomposites, that is, distribution of silicate nanolayers in the polymer matrix. The homogeneity of the particle fraction of exfoliated nanolayers was clearly an important factor affecting the properties of the nanocomposites. © 2009 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 47: 583–595, 2009