Table of Content

23 March 2008, Volume 26 Issue 2

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Synthesis of Spiropyran with BOC Protective Function and Research of Photochromism

GU Ling-yan, ZHANG Qing, SHENG Qiao-rong, XUE Min-zhao, LIU Yan-gang

2008, 26(2):  81-87.  DOI: 10.7517/j.issn.1674-0475.2008.02.81

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Two indolinebenzopyran derivatives, 5-Amino-N-(tert-butyloxycarbon-yl)-1,3,3-trimethyl-6′-nitro-spiro(indole-2,2′-[2H-1]benzopyran) (BOCSPI) and 5-Amino-N-(tert-butyloxycarbonyl)-1,3,3-trimethyl-6′-nitro-8′-methoxy-spiro(indole-2,2′-[2H-1]benzopyran) (BOCSPII), were synthesized and characterized. BOCSPI and BOCSPII were doped in polymethylmethacrylate (PMMA) host films with different concentration respectively. The photochromic properties of the two compounds in solution and film were investigated. It has been found that both the rate of photo-colorization from the closed form(SP) to open form(MC) and the rate of thermal isomerization between the closed form(SP) to the open form(MC) decreased remarkably with the increase of the concentration of spiopyran derivatives in PMMA film. The existence of 8′-methoxy group in BOCSPII made the opened form MC more stable at room temperature.

Studies on Synthesis of Sulfonium Salts and Their Properties as Photo-acid Generator

WANG Mei-li, WANG Wen-guang, HAN Yuan-li, PU Jia-ling

2008, 26(2):  88-93.  DOI: 10.7517/j.issn.1674-0475.2008.02.88

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Two kinds of sulfonium salts as Photo-acid Generator have been successfully synthesized. Their structures were confirmed by ¹1HNMR and MS. Some physical performances have also been measured. Further, their photo-decomposition and acid-forming performance in acetonitrile under irradiation at 405 and 365 nm were evaluated by the method ascertained in our laboratory. It is found that two sulfonium salts have high thermo-decomposition temperature and good dissolution in some organic solvents. When exposed at 405 nm, the quantum yields of decomposition of 4-(9-phenyl-anthracenyl)phenyl sulfonium salt of methyl trifluoromethanesulfonate (PAGS1) and 4-(4′-(N, N-diethyl)-1′-styrenyl)phenyl sulfonium salt of methyl trifluoromethanesulfonate (PAGS2) were 10% and 15% respectively; their quantum yields of acid-forming were 8.1% and 13% respectively. However, when exposed by 365 nm, their quantum yields of decomposition and acid forming were very low. Finally, it is concluded that both PAGS1 and PAGS2 are sensitive to light at 405 nm and applicable to be used as PAG in Purple Laser CTP technology.

The Influence of Metallic Stearates on the Photographic Properties of Photothermographic Material Based on Silver Tolyltriazole

LIANG Hai-yan, LI Jin-pei, LIU Hua

2008, 26(2):  94-103.  DOI: 10.7517/j.issn.1674-0475.2008.02.94

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The influence of metallic stearates on the photographic properties of photothermographic (PTG) material based on silver tolyltriazole(AgTTA) was reported. The results showed that the stearates can accelerate the development of PTG material. The addition of NiSt₂ greatly increased the maximum density and the sensitivity together with a slight fog increase. However the addition of BaSt₂ and CaSt₂ did not make such great increase in the maximum density and the sensitivity, together with a slight fog decrease. The development processes were discussed by studying the effect of component and content on pH, [Ag⁺] and the photographic properties.

The Preparation of Ag Loaded Nanotube Titanic Acid Catalyst

MA Xin-qi, FENG Cai-xia, GUI Li-li, YAO-Li, NIU Yu-qi, GUO Xin-yong

2008, 26(2):  104-108.  DOI: 10.7517/j.issn.1674-0475.2008.02.104

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The Ag loaded nanotube titanic acid was prepared by the photo-reduction method. The photograph of TEM showed that Ag particles deposited on the surface of the nanotube titanic acid. Results of XPS and XRD indicated that the Ag⁺ was reduced to metal. The results of photodegradation of methylene blue showed that the photocatalytic activity of Ag loaded nanotube titanic acid was higher than that of the nanotube titanic acid.

Study on the Interaction of Transition Ions with a Open-Chain Crown Ether Schiff Base

YU Tian-zhi, DING Xian-sheng, ZHAO Yu-ling, QIAN long, FAN Duo-wang

2008, 26(2):  109-115.  DOI: 10.7517/j.issn.1674-0475.2008.02.109

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A ligand containing open-chain crown ether Schiff base, N, N’-bis(salicylidene)-3,6-dioxa-1, 8-diaminooctane (H₂L), was synthesized. Its fluorescent properties in various organic solvents and the presence of transition metallic ions (Zn²⁺, Cd²⁺, Cu²⁺ and Ni²⁺) were investigated in detail. The effects of different solvents and the transition metallic ions on the fluorescent spectra of the ligand were discussed. The results show that solvents and prescence of transition metallic ions have great influence on the fluorescent property of the ligand. The weaker the solvent polarity is, the stronger the fluorescent intensity changes, and the fluorescence peak is blue-shifted. The prescence of Zn²⁺ and Cd²⁺ can enhance the fluorescent intensity of the ligand, but the prescence of Cu²⁺ and Ni²⁺ can quench its fluorescence. The effect of pH on the interaction of transition ions with the ligand was investigated, and the optimal pH value is 7—8.

Preparation of Water-Soluble Negative Photoresist

SHAN Ying-min, CAO Rui-jun, GAO Ying, LIU Yi

2008, 26(2):  116-124.  DOI: 10.7517/j.issn.1674-0475.2008.02.116

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A formula for preparing the photoresist is developed. The main compositions of the formula are P(AM-DAAM), PVP and 4,4′-diazido-2,2′-stilbenedisulfonate sodium salt(DAS). The influence on the light sensitivity by components of the formula is studied. According to the orthogonality method, the results are that: the light sensitivity turns out to be best when the ratio of AM/DAAM of the copolymer by weight is 1:1, the ratio of P(AM-DAAM)/PVP by weight is 1:2, the amount of DAS is 1/2 to the total amount of P(AM-DAAM) and PVP by weight; the amount of the coupling agent is 1/60 to the total amount of P(AM-DAAM) and PVP by weight; the amount of the surface active agent is 1/40 to the total amount of P(AM-DAAM) and PVP by weight. With this formula, the light sensitivity of the photoresist is 58.4 mJ·cm^-2. And a clear pattern can be obtained. With this formula, the light sensitivity of the photoresist can reach the industry requirements. And the photoresist acts as good as the products from abroad.

Influence of Triton X-100 on the Performance of Dye-Sensitized Solar Cell

ZHANG Yuan, CAI Ning, ZHAO Ying, ZHAO Da-wei, LIU Guang-lu, JI Wei-wei, YANG Rui-xia

2008, 26(2):  125-130.  DOI: 10.7517/j.issn.1674-0475.2008.02.125

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In the fabrication of TiO₂ film electrodes for dye-sensitized solar cells using screen-printing technique, the composition of TiO₂ slurry plays an important role in film microstructure and J-V curve of the solar cells. One of anhydrous TiO₂ slurry was used to prepare anode film by screen-printing technique in this paper, and it was applied in dye-sensitized solar cells. Experimental results show that the addition of Triton X-100 can influence the morphology of TiO₂ film obviously as well as the performance of solar cell. It could be concluded that deficient or excessive addition of Triton X-100 would result in the decrease of open circuit voltage, short circuit current, fill factor and conversion efficiency. Good performance of solar cell can be obtained at the Triton X-100 amount of 0.8 mL in 3 g P25.

Decomposition of Hydrogen Sulfide to Produce Hydrogen under Ultraviolet Light

XU Hong, BAI Xue-feng

2008, 26(2):  131-137.  DOI: 10.7517/j.issn.1674-0475.2008.02.131

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The direct photodecomposition of hydrogen sulfide to produce hydrogen under ultraviolet light is studied in the sodium solution illuminated by the 10 W low-pressure mercury-lamp (λ= 253.7 nm) as illuminant. The effects of the reaction conditions on the hydrogen production from hydrogen sulfide, such as the form of sulfide ions, the concentration of sodium solution, the pH value of the reaction solution and the rate of hydrogen sulfide are investigated. The results show that direct decomposition of hydrogen sulfide under ultraviolet light could occur without catalyst. The highest hydrogen production rate is 3.0 mL/W·h when the sodium solution is 0.6 mol/L and the successive hydrogen sulfide rate is 25 mL/h.

Preparation of Three Types of Titanium Dioxides with Different Crystallite and the Photoreactivity

LIU Song-cui, LÜ Kang-le, DENG Ke-jian, TANG Hong-mei, LI Xiao-fang

2008, 26(2):  138-147.  DOI: 10.7517/j.issn.1674-0475.2008.02.138

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Anatase (AT) nanoplates, club-shaped rutile (RT) and prism-shaped brookite (BT) TiO₂ were prepared on a large scale through hydrothermal treatment of Ti(SO₄)₂ or TiCl₄ at certain pH. The mean particle size of the prepared AT was about 10 nm, the smallest one among the three types of TiO₂, compared with 30—50 nm of BT and 50—70 nm of BT. The maximum responsive wavelength of AT, BT and RT was to about 375, 385 and 415 nm, respectively, and AT shows the strongest absorption in the range of UV light. The photooxidation activity evaluated from the photocatalytic degradation of X3B, an anionic organic dye, revealed that the relative photoreactivity of the TiO₂ samples was as follows: AT>RT>BT, which is consistant with the adsorption ability of the catalysts. The reasons that caused the differences in photoreactivity among the three types TiO₂ were also discussed.

Progress of the Study on Nanoimprint Resists

HUO Yong-en, JIA Yue, WANG Li-yuan

2008, 26(2):  148-156.  DOI: 10.7517/j.issn.1674-0475.2008.02.148

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Nanoimprint is one of the most promising next generation nanolithography technologies. Based on the mechanical embossing principle, nanoimprint technique can achieve pattern resolutions beyond the limitations set by the light diffraction or beam scatterings in other conventional techniques. This article introduces the basic princeples of nanoimprint technology and reviews the recent progress in the study of nanoimprint resists. Main factors affecting the performance of resists, including Tg temperature/thermal stability, viscosity/average molecular weight, etch resistance, etc, are discussed. The common resist materials for thermal nanoimprint and ultroviolet nanoimprint are introduced respectively, main parts of the resists including polymethacrylate, organic silicon modified polyacrylate, hybrane, polydimethylsilane, compounds with vinyl ether group, epoxy resin, etc. The advantages and disadvantages of the resist systems are also presented. The main problems existing in nanoimprint resists are introduced. The advantages and problems of nanoimprint technique are summed up in this article.

Surface Plasmon Resonance (SPR)——The Principle of a New Method for Chemical Detection

WU Shi-kang, WANG Peng-fei

2008, 26(2):  157-168.  DOI: 10.7517/j.issn.1674-0475.2008.02.157

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Recently, the phenomenon of surface plasmon resonance (SPR) has attracted more and more extensive attention due to its special application in the field of metallic nano-materials and to be used as a sensitive reporter for the detection of different chemical and bio-chemical species.In this paper, the mechanism for the formation of SPR was introduced in details. And some problems concerned how to use this type of reporter for detection were also discussed systematically.

Study on the Preparation of Bisdodecylphenyliodonium Hexafluoroantimonate

LIU An-chang, XIAO Qing, WEN Yu-ping, TAN Zhen-you, LIU Fang

2008, 26(2):  169-173.  DOI: 10.7517/j.issn.1674-0475.2008.02.169

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Bisdodecylphenyliodonium hexafluoroantimonate salt was prepared via reaction of dodecyl benzene with KIO₃ and H₂SO₄ in the presence of Ac₂O to give the corresponding iodonium hydrogen sulfate, which was converted to the compound, via anion exchange with KSbF₆. The structure of bisdodecylphenyliodonium hexafluoroantimonate salt was identified by UV, IR and H-NMR.