1993 Volume 10 Issue 1

STM AND ECSTM TIP FABRICATION AND ITS EFFECTS ON THE IMAGES
Zhang Bailin , Wang Erkang
1993, 10(1): 1-6
[Abstract](307) [FullText HTML] [PDF 577KB](0)
Abstract:
This article reviews the fabrication of STM and ECSTM tips and their characterizations.And the influence of the tip on STM and ECSTM images is evaluated.
BULK GRAFT COPOLYMERIZATION OF PVC WITH 2-OXAZOLINE-TERMINATED POLY (PROPYLENE OXIDE)
Liu Junhan , Pan Enli
1993, 10(1): 7-11
[Abstract](479) [FullText HTML] [PDF 537KB](0)
Abstract:
The mechanical graft copolymerization of PVC with the 2-oxazoline-terminated poly (propylene oxide) by heating process of the bulk polymers has been studied. The occurrence of graft reaction was verified by solvent extract, IR, GPC, DSC and SEM analysis. It was found that the graft eopolymerization of PVC with reactive polyether could take place in absence of any catalysts under certain temperature.
STUDIES ON SYNTHESIS OF A/B RING ANALOGUES OF CASTASTERONE Ⅱ. STEREOSELECTIVE SYNTHESIS OF 2β,3β-DIHYDROXY-6-CHOLESTERONE
Gao Bi , Wang Zhicai , Zheng Qihuang , Xu Zhiwen
1993, 10(1): 12-15
[Abstract](432) [FullText HTML] [PDF 271KB](0)
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2β, 3β-Dihydroxy-6-cholesterone, a structural analogue in A/B rings of castasterone was stereoselectively synthesized from cholesterol via nitration, reduction; elimination and oxidation reactions. The key step in the synthesis is the introduction of 2β, 3β-dihydroxy groups by oxidation with I2-AgOAe-H2O.
WATER-SOLUBLE AND AMPHIPHILIC POLYMERS 16. SYNTHESIS AND CHARACTERIZATION OF POLYSTYRENE/POLYACRYLAMIDE BLOCK POLYMERS
Fang Tianru , Xu Zhengyan , Xu Suxian
1993, 10(1): 16-20
[Abstract](248) [FullText HTML] [PDF 372KB](0)
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A polyazoester initiator was used to synthesize polystyrene/polyaerylamide (PSt/PAM) block polymers by its consecutive decomposition in styrene(St) and aerylamide(AM). The polymerization behavior of AM in 1,4-dioxane initiated by an azo group-containing styrene prepolymer (prePSt) was investigated, and the factors influencing the conversion of the second monomer and the content of the homopolystyrene were discussed. The PSt/PAM block polymers were characterized by elemental analysis, solubility, IR, DSC, TGand pyrolysis-gas chromatography.
OPTICAL PROPERTIES OF 2,2-BIS(4-METHACRYLOYLOXYPHENYL)PROPANESTYRENE COPOLYMER
Yang Bai , Yang Fan , Lin Dehou , Li Yingjun , Shen Jiacong
1993, 10(1): 21-24
[Abstract](287) [FullText HTML] [PDF 276KB](0)
Abstract:
Transparent resins were synthesized from title methacryloyloxyphenyl propane (abbr. bisvinyl-A) homopolymer and its copolymer with styrene. The homopolymer of bisvinyl-A is light(d420 1.19),has high surface hardness (pencil hardness 6H),heat resistance (Tg 155℃) and superior optical properties (nD20 1.578,transparency 90~91%). But it is too fragile. The property of bisvinyl-A and styrene copolyrner was dependent on the content of bisvinyl-A. Copolymer containing 70% bisvinyl-A has the most absorption of UV-light (with complete absorbtion at<370nm). The copolymer with 5%~10% bisvinyl-A shows an excellent water absorbing resistance,acid and alkali resistance,impact resistance and high refractive index (nD 1.588).
SPHERULITIC GROWTH RATES AND MORPHOLOGY IN MALEIC ANHYDRIDE-g-POLYPROPYLENE
Liu Jingjiang
1993, 10(1): 25-29
[Abstract](331) [FullText HTML] [PDF 715KB](0)
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The isothermal radial growth rates of spherulites and the morphology of maleic anhydride-g-polypropylene have been determined by means of polarizing microscope. Chain segments of maleic anhydride and polypropylene in the graft copolymer are partly compatible. A change in the growth region is observed at 132℃ and interpreted as a Region Ⅲ→Region Ⅱ transition, according to the kinetic theory of compatible polymer blend crystallization. The equilibrium melting temperature (Tmo) of the graft copolymer was measured as 200℃, lower than that of ipp.
MECHANISM OF SULFUR POISONING ON SUPPORTED NOBLE METAL CATALYST Pd(Pt)/Al2O3
Xiao Tiancun , An Lidun , Ma Jun
1993, 10(1): 30-33
[Abstract](322) [FullText HTML] [PDF 285KB](1)
Abstract:
With the aid of CO and pyridine as probe molecules, infrared spectrophotorneter was employed to characterize the industrial catalyst Pd(Pt)/Al2O3 used for eliminating H2 from feed CO2 in urea synthesis. It is concluded that the factor which directly causes the deactivation of the catalyst comes from S2- and S22-, and the last factor resulting in the deactivation are S(Ⅵ) species:SO42- and Al2O3-SO3-H2O compounds.
MASS SPECTROMETRIC STUDY ON ORGANICPHORSPHORUS COMPOUNDS Ⅹ. EI MASS SPECTROMETRIC STUDY ON 1,2-DIPHENYL-3,3-DIALKYL-1,4,2-DIAZAPHOSPHOLIDIN-5-ONE-2-OXIDE
Qiu Fenghe , Song Fengrui , Liu Shuying , Feng Kesheng , Chen Ruyu
1993, 10(1): 34-38
[Abstract](408) [FullText HTML] [PDF 302KB](0)
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The EI mass spectra of 13 phorsphorus-containing compounds were reported. The EI spectra of these compounds are characterized by cycle opening cleavage and rearrangement under electron impact conditions. Some rearrangement processes were reported in detail. The substituent effects on fragmentation mechanism of molecular ions were also discussed.
EPOXY-TERMINATED PHENOLPHTHALEIN POLYARYL-ETHERKETONE: SYNTHESIS AND CHARACTERIZATION
Chen Tianlu , Xia Ping , Guo Qipeng , Li Binyao
1993, 10(1): 39-42
[Abstract](344) [FullText HTML] [PDF 294KB](0)
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Epoxy-terminated phenolphthalein polyaryletherketones (E-PEK) of Mn=1000~8000 were synthesized by reaction of epichhlorohydrin with PEK oligomer having-OK terminal groups prepared by condensation of phenolphthalein (PPH) with 4,4'-dichlorobenzophenone (DCBP) at molar ratios of PPH to DCBP from 1:0.5 to 1:0.9. The E-PEKs were characterized by IR and 1H NMR spectra,initial glass transtion temperature (Tgi); the melting viscosity and solubility of E-PEK samples were also measured. The E-PEKs were cured with 4, 4'-diaminodiphenylether (DDE) and the glass transition temperatures of the fully erosslinked E-PEK/DDE (Tg∞) were found to be in relation with the initial molecular weight of the oligomer. The Tg∞ values for all samples closslinked were in the range of 183~215℃.
AN NMR METHOD FOR PHASE DIAGRAM DETERMINATION Ⅰ. THE PrCl3-CH3CONH2-D2O SYSTEM
Yang Xujie , Liu Jinsong , Zhang Xuexian , Lu Lude , Wang Xin , Bryan C. Sanctuary
1993, 10(1): 43-46
[Abstract](463) [FullText HTML] [PDF 299KB](0)
Abstract:
The NMR technique has been satisfactorily applied to determine the isothermal phase diagram of PrCl3-CH3CONH2-D2O system. Based on the values of chemical shifts and integral areas, the chemical compositions of both the liquid and the solid phases have been obtained.
EFFECT OF TRANSITION METAL-CONTAINING ORGANIC COMPLEX ADDITIVE ON THE PROPERTIES OF POLYIMIDE GAS SEPARATION MEMBRANES
Wu Yonglie , Liu Jingzhi , Zheng Jinghe , Yang Jinrong , Yang Fu , Ding Mengxian
1993, 10(1): 47-50
[Abstract](280) [FullText HTML] [PDF 767KB](0)
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Polyirnide gas separation membranes were preparated using metal-containing organic complex with big substituting group as additive. The effects of tranaition metal salts, organic ligand and metal complex on the permeability of polyimide homogenous membranes and asymmetric membranes for separation of hydrogen and nitrogen were studied. It was showed that MnCl2, Co(NO3)2, Cr(Ac)3 enhanced the separation coefficient and lowered the permeability of the membrane; organic ligand additive enhanced the permeability and lowered separation coefficient; when metallorganic complex was used, the gas permeability was enbanced without decline of separation coefficient.
GRAFT COPOLYMERIZATION OF METHYL METHACRYLATE ONTO ALGINIC ACID USING KPS-U AS INITIATION SYSTEM
Wu Gongsheng , Hou Shizheng , Chen Yougiang
1993, 10(1): 51-53
[Abstract](519) [FullText HTML] [PDF 243KB](0)
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Potassium persulfate-urea (KPS-U) appeared an effective initiation system for the graft copolymerization of methyl methacrylate (MMA) onto alginic acid. Infrared spectral analysis has been adopted to prove the structure of the reaction product. The better grafting efficiency (G%) and graft efficiency (E%) were obtained at[KPS]=4.0×10-3mol/L,[MMA]=4.0×10-1mol/L,[KPS]:[U]=1,alginic acid of 2.0g/100mL,at 50℃ in 5h.
SYNTHESIS AND PROPERTY OF SILICA-BOUND BENZO CROWN ETHERS
Lu Xueran , Lin Shengzai , Chen Yuanyin
1993, 10(1): 54-57
[Abstract](311) [FullText HTML] [PDF 296KB](0)
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3- and 4-allyl-1,2-bis (β-hydroxyethoxy) benzene were synthesized from ethylene chlorohydrin and 3-or 4-allyleatechol, respectively. Reacting 3-aUyl-1,2-bis (hydroxyethoxy) benzene with diethylene glycol ditosylate or reacting 4-allyl-1, 2-(hydroxyethoxy) benzene with 1, 2-bis (hydroethoxy) benzene ditosylate, two benzo crown ethers, 3'-propenyl-2, 3-benzo-1,4, 7, 10, 13, 16-hexaoxa-cyclooctadec-2-ene and 4'-propenyl-2, 3, 11, 12-dibenzo-1,4,7, 10, 13, 16-hexaoxa-cy-clooctadeca-2,11-diene,were obtained. The benzo crown ethers were subjected to hydrosilylation with trichlorosilane,followed by immobilization on silica, to give the title silica-bound benzo crown ethers.The silica-bound benzo crown ethers could coordinate with platinum. The both platinum complexes were found to be an effective catalyst for hydrosilylation of olefins with triethoxysflane.
CASTING SOLUTIONS FROM CELLULOSE DERIVATIVES FOR REVERSE OSMOSIS MEMBRANE
Yang Kexuan , He Wenjie , Mao Runsheng , Wu Fenglian , Huang Jicai , Qi Qinghui
1993, 10(1): 58-61
[Abstract](349) [FullText HTML] [PDF 308KB](0)
Abstract:
Casting Solutions from cellulose acetate, cyanoethyl acetyl cellulose, hydroxypropyl acetyl cellulose and titanium cellulose acetate have been studied with IR and viscosity methods. McAllister equation and Huggins equation are used to describe the viscosity behavior of acetone-additive solutions and cellulose derivative-acetone-additive solutions, respectively. Phosphoric acid, formamide, npropanol and glycerine were used as additives. It is found that additives used showed a certain effect on the interaction among macromolecules of cellulose derivatives and on their morphological structures.
STUDY ON PORPHYRIN COMPOUNDS ⅩⅩⅢ. SYNTHESIS AND PHOTOSENSITIVITY OF PORPHYRIN-CHOLESTEROL ESTER
Ke Hanzhong , Xia Suzhen , Zhou Xiang , Huang Suqiu , Li Lezhen , Xu Jingya , Yang Jun
1993, 10(1): 62-65
[Abstract](310) [FullText HTML] [PDF 254KB](0)
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Six cholesterol-porphyrins have been synthesized. The photoradiative effect on cancer and the interaction of compounds 5 and 9 with red cells have been examined. The results shown that to some degree, they showed a destructive effect on Ehrlich ascitogenous cells and Mouse ascitic breast carcionma cells directly,but very little photo-hemolytic action.
FORMATION OF RESINOUS SUBSTANCE FROM POLYVINYL ALCOHOL AND Cr(Ⅲ)
Cheng Chuanxuan , Su Yingeao
1993, 10(1): 66-70
[Abstract](394) [FullText HTML] [PDF 406KB](1)
Abstract:
A greyish blue resinous substance was separated by adding Cr3+ to a basic aqueous solution of 5% PVA at 12 ≤pH ≤13. The formation of the resinous substance has been studied by XPS,ESR, IR and electrophoretie techniques. It is considered that at the experimental conditions deprotonation of some hydroxyl groups in the PVA may afford a ligand L- which may form coordinate with Cr3+ through partial ionic bond. Thus,it results in a cross-linking between Cr3+ and deprotonated hydroxyl groups of PVA. The product is paramagnetic. This phenomena may be applied to treating Cr3+ containing waste for chromium recovery by dissolving the complex in hydrochloric acid.
CATALYTIC ESTER INTERCHANGE OF 1,1'-BISNAPHTHOL-4,4'-DIACETATE AND DI(2-ETHYLHEXYL)CARBONATE
Ping Xuezhen , Qiu Xingyu
1993, 10(1): 71-73
[Abstract](233) [FullText HTML] [PDF 215KB](0)
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The ester interchange of 1,1'-bisnaphthol-4,4'-diacetate and di (2-ethylhexyl) carbonate using various metal compounds as catalysts has been investigated. The relative reactivity of the catalysts was compared from the kinetic data measured by determining the amount of 2-ethylhexyl acetate released during the reaction. GC/MS analysis showed that the poly (1,1'-bisnaphthol carbonate), 2-ethylhexyl acetate, heptanone,octene and acetic acid (acetic anhydride) were formed during the ester interchange.
GAS PERMEABILITIES OF DIALKYL FUMARATE COPOLYMERS
Song Zhengzhe , Wen Jiumian , Xu Jiping
1993, 10(1): 74-76
[Abstract](200) [FullText HTML] [PDF 215KB](0)
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Several kinds of dialkyl fumarate copolymers were synthesized by radical copolymerization in the presence of AIBN. The permeabilities for oxygen and nitrogen of the copolymer membranes were determined. Effects of the copolymer composition on the gas permeability of the membrane were examined.
GAS PERMEATION OF MOISTENED POLYVINYLACETAL MEMBRANES
Yi Ying , Yu Xianda , Wu Heping , Wang Anlai , Cao Suqin , Liu Huansui , Li Caiyun
1993, 10(1): 77-79
[Abstract](358) [FullText HTML] [PDF 227KB](0)
Abstract:
The permeabilities of O2,N2 and CO2 were measured at 293K and 303K for the moistened membranes made of polyvinyl alcohol(PVA),polyvinyl aoetal (PVAL),polyvinyl butylral(PVB) and polyvinyl octylral (PVO). The apparatus for measuring the gas permeability of water-moistened membrane is described. It was observed that the permeability coefficients of O2 and N2 for the moistened PVA membrane are several hundred times as much as that for anhydrous PVA membrane, with slight increase in the permselectivity of O2 to N2. The permeabilities,diffusion and solubility coefficients of O2, N2 and CO2 and permselectivities of O2 to N2 and of CO2 to O2 in the moistened polyvinyl acetals membranes increase with the increase of the alkyl chain.
CONTINUOUS DETERMINATION OF ARSENIC AND TIN BY HYDRIDE GENERATION-SPECTROPHOTOMETRY TECHNIQUE
Wang Bingwu , Chen Yao , Niu Jianjun
1993, 10(1): 80-82
[Abstract](226) [FullText HTML] [PDF 251KB](0)
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For continuous determination of arsenic and tin a new method consisted of the hydride generation-silver sol spectrophotometry has been proposed. The separation of As and Sn was achieved in the form of AsH3 and SnH4 in 3.0 mol/L HCI and in a medium of pH 5.5, respectively from the same solution. With a hydride separator which eliminates the interference of other covalent hydrides, the method is characterized by high sensitivity, selectivity and applicability. Satisfactory results were obtained in analysing pure lead,ferrotungsten alloy,ore, and sediments.
INFLUENCE OF THE STRUCTURE OF CuCr/γ-Al2O3 ON THE GASEOUS CATALYTIC HYDROGENATION OF FURFURAL TO FURFURYL ALCOHOL
Yin Hengbo , Wu Jing , Zhao Bingqian
1993, 10(1): 83-85
[Abstract](420) [FullText HTML] [PDF 235KB](0)
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The influence of the structure of the CuCr/γ-Al2O3 catalyst on gas phase hydrogenation of furfural to furfuryl alcohol at atmosphere pressure has been studied by XRD, XPS spectra and TPR technique. It is found that Cu and Cr appeared widely distributed in the surface of γ-Al2O3 support and converted into CuCrO4 when their contents in the catalyst were high. This very CuCrO4 increases the hydrogenation activity and selectivity of the catalyst.
THE EFFECTS OF POLYMETHACRYLATES ON β-PHASE CRYSTALLIZATION IN HIGHLY ORIENTED PVF2 FILMS
Chen Ye , Yang Decai
1993, 10(1): 86-88
[Abstract](351) [FullText HTML] [PDF 470KB](0)
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Fourier transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM) have been used to study the effect of polymcthaerylates (PMAs),including PMMA,PEMA,PBMA,on the crystalline structure of highly oriented films of poly(vinylidene fluoride) (PVF2). The melt-drawn films of PVF2 consist of highly oriented lamellar structure. Addition of PMAs (in 20% by weight) in PVF2 resulted in the formation of shish-kabab structure and β-phase in order of PMMA >PEMA >PBMA. The results are discussed in terms of the hydrogen bonding between PVF2 and PMAs.
REGENERATION OF CATALYST USED FOR RESIDUAL OIL CRACKING
Li Rongsheng , Zhang Wuyang , Gao Chuanfu , Wei Quan
1993, 10(1): 89-91
[Abstract](333) [FullText HTML] [PDF 216KB](0)
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The hydrochloric acid has been used to reactivate the Ni, Fe-deposited fluid cracking catalyst. The results show that the HCl treatment can partly remove the nickel and the iron deposited on the catalyst and regenerate its activity, increasing the gasoline yield and decreasing the carbon deposit.The hydrothermal stability of the catalyst is not affected by the HCl treatment.
DETERMINATION OF TRACE RARE EARTH IN HIGH PURE METALLIC PRASEODYMIUM BY INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETRY
Yuan Fu , Qi Wendi
1993, 10(1): 92-94
[Abstract](222) [FullText HTML] [PDF 240KB](0)
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A spectrophotometric method for the direct simultaneous determination of five trace rare earth in high pure metallic praseodymium is described. The ethanol sample solution was introduced into the plasma for desolvation. The effect of matrix concentration on detection limits,and the calculation and correction of spectral interferences in ICP-AES have been investigated. For the sample solution containing 5 mg/mL of Pr,the limits of determination were 0.002% for La,Nd and Sm,0.003 for Ceand 0.0005% for Y. The accuracies of the determinations were satisfactory and the relative standard deviations were in the range of 1.2~6.2%.
ON THE SINGLE CRYSTAL IN MF/PVA COMPOSITES
Zhang Guanghua , Zhang Xinghua
1993, 10(1): 95-97
[Abstract](626) [FullText HTML] [PDF 515KB](0)
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The structure of melamine formaldehyde resin/poly(vinyl alcohol) (MF/PVA) composites has been studied with transmission electron microscopy,electron diffraction and X-ray diffraction techniques. The single crystals found in MF/PVA(90/10) composite are monoclinie with a=0.51nm,b=1.69rim,c=0.53nm and β=59.5°.
SYNTHESIS OF 2,4,6-TRIIMIDO-N,N',N〃-TRI(2-NITRO-BENZOFUROXAN)-1,3,5-TRIAZINE
Wang Naixing , Chen Boren , Ou Yuxiang
1993, 10(1): 98-100
[Abstract](218) [FullText HTML] [PDF 210KB](0)
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The title compound was synthesised from cyanurie chloride and 3, 5-dichloroaniline followed by nitration,azidation and denitrogenation. The compound is a yellowish crystal with desity of 1.93 g/cm3,soluble in DMF,DMSO,decomposed at 316℃ (by DTA). It is an excellent high energy density material.
NEAR RESONANT ABSORPTIVE NONLINEARITY OF EOSIN FILM
Kang Yin , Zhang Shuqing , Zhang Jianguo , Wong Zhaoheng , Feng Jiazhang
1993, 10(1): 101-103
[Abstract](921) [FullText HTML] [PDF 333KB](1)
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The experimental results are reported on the near resonant absorptive nonlinearity, low power continuous wave degenerate four wave mixing and compensation of distorted image by optical phase conjugation in organic polymeric matrix film of eosin.
SYNTHESIS OF 1-PHENYLACETYL-4-AROYLTHIOSEMICAR-BAZIDES AND THEIR CYCLIZATION
Feng Xiaoming , Chen Rong , Zhang Ziyi
1993, 10(1): 104-106
[Abstract](243) [FullText HTML] [PDF 246KB](0)
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A series of 1-phenylaeetyl-4-aroylthiosemicarbazides (1) were synthesized by the reaction of phenylacetylhydrazine with aroyl isothiocyanates. Some of 3-benzyl-4-aroyl-1,2, 4-triazoline-5-thione (2) were obtained in good yields through the cyclization of 1 in 1mol/LK2CO3 solution. The structures of all compounds prepared were characterized by elemental analysis,IR,1H NMR and MS.The preliminary experiments showed that compounds 1 and 2 possess some inhibiting activity on B. substilis.
SYNTHFESIS AND ELECTRONIC ABSORPTION SPECTRA OF STYRYL DYE CONTAINING PRYLIUM END GROUP
Yao Zuguang , Zhu Zhenghua
1993, 10(1): 107-109
[Abstract](206) [FullText HTML] [PDF 175KB](0)
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The synthesis of some new styryl dyes containing pyrylium end group is described. The structure of the compound was confirmed by elemental analysis, IR spectra and 1H NMR spectroscopy.The electronic absorption spectra of the dyes in red and near infrared region is reported.
STUDIES ON SOLID STATE REACTIONS OF COORDINATION COMPOUNDS LV. INVESTIGATION OF SOLID STATE REACTIONS OF PHENANTHROLINE WITH METAL CHLORIDES(M=Fe,Co,Ni,Cu)
Jia Dianzeng , Li Changxiong , Xin Xinquan
1993, 10(1): 110-112
[Abstract](401) [FullText HTML] [PDF 252KB](0)
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Solid state reactions of metal chlorides (M=Fe, Co, Ni, Cu) with Phenanthroline at room temperature have been studied. A two-step addition reaction was observed. The intermediates M(Phen)2Cl2·nH2O(M=Co,Ni,Cu) were confirmed by experimental results. Effects of molecular structure of the reactants and the stability of the complexes formed were also discussed.
PRELIMINARY INVESTIGATION OF ACETYLENE BLACK AS NEGATIVE ELECTRODE FOR LITHIUM BATTERY
Yang Hanxi , Lei Ming , Li Shengxian , Ai Xinping
1993, 10(1): 113-115
[Abstract](436) [FullText HTML] [PDF 202KB](0)
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The carbon electrode made from acetylene black showed a high discharge/charge capacity, long cycling life, low working voltage and safety for lithium ion battery. The discharge/charge characteristics of the lithium battery with carbon negative electrode has been briefly discussed.
PREPARATION OF ROOM TEMPERATURE SnO2-α-Fe2O3 GAS SENSOR
Li Wenfan , Liu Xiuying
1993, 10(1): 116-117
[Abstract](252) [FullText HTML] [PDF 127KB](1)
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A room temperature gas sensor has been prepared from SnO2-α-Fe2O3 without doping of noble metals. The sensor has a large specific surface area and higher sensitivity for H2, coal gas and LPG, but insensitive to CO and CH4. Its response time is about 25 seconds, recovery time is about 21 seconds, and energy consumption of 0.1 W.
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