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    15 January 2017, Volume 46 Issue 1
    Influence of Microwave-assisted Hydrothermal Conditions on Crystal Structure Properties of SAPO-11 from Diethylamine Template
    ZHAO Ying;YANG Wei-jia;YANG Kai-xu;XU Zheng;CAO Jian-xin;LIU Fei
    2017, 46(1):  1-7. 
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    Effect of various reaction temperature and time on crystal structure properties of SAPO-11 synthesized from diethylamine template via microwave-assisted hydrothermal route was investigated in this paper. These obtained products were characterized by XRD, FT-IR, SEM, BET and NH3-TPD techniques to investigate their crystalline phase, skeletal structure, morphology, pore structure and surface acidity. The results indicate that different hydrothermal conditions pose significant impact on the structure properties of the synthesized products. Only SiO2 phase but no SAPO-11 crystalline phase existed in the product synthesized when the reaction temperature below 180 ℃, and the SAPO-11 with rather small specific surface area and inhomogeneity in crystal size was also obtained when the reaction temperature higher than 200 ℃. A small amount of AlPO4-5 and CFSAPO-1 ( C ) miscellaneous crystal phases are derived from SAPO-11 crystal when the reaction time over 1 h. The product with pure SAPO-11 phase and spherical crystalline grains was eventually and successfully synthesized at 200℃ for 1 h via microwave-assisted hydrothermal route, and the SAPO-11 possessed distinct physicochemical properties with the weak acid on the surface, high specific surface area of 199. 4 m2·g-1, pore volume of 0. 15 cm3 ·g-1 and average pore diameter of 2. 92 nm.
    Systhesis and Performance of SnSb Anode Materials Modified by Carbon Aerogels
    LUO Da-wei;CHEN Jia-ming;LI Shi-wei;CHEN Yu-qi;LI Zhi-jun;LI Xue
    2017, 46(1):  8-12. 
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    Carbon aerogels were synthesized by supercritical drying method, then a carbon aerogels/SnSb composite was successfully prepared from carbon aerogels modification of SnSb by a simple chemical reduction method. Both the structure and the morphology of the SnSb and CA/SnSb powders were characterized by X-ray diffraction and SEM. The samples were used as active anode materials for lithium-ion batteries, and their cycle performance was examined by constant current charge-discharge cycling. The results show that carbon aerogels exhibited nano porous three-dimensional network structure, and CA/SnSb is obtained when the SnSb was modified by carbon aerogels. The feature of CA/SnSb was carbon aerogels and SnSb particles mutually staggered distribution, and carbon aerogels particles were contained in the network backbone, then reunion of CA/SnSb was greatly improved. The first discharge capacity of CA/SnSb is measured as 1120. 2 mAh·g-1 and a large reversible capacity of 557. 3 mAh· g-1 is observed after 50 cycles, which is far higher than that of SnSb without modification by carbon aerogels. The capacity retention of CA/SnSb was improved due to the improving of reunion and alleviating volume expansion during the charge-discharge process by addition of carbon aerogels.
    Influence of Cooling Rate on the Minority Carrier Lifetime of Multicrystalline Silicon Grown with Metallurgical Grade Silicon Feedback by Directional Solidification
    LIU Zhi-hui;LUO Yu-feng;GONG Hong-yong;RAO Sen-lin;ZHANG Fa-yun;HU Yun
    2017, 46(1):  13-17. 
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    According to multicrystalline silicon ( mc-Si ) ingots cast by one-step directional solidification growth with the pre-purification metallurgical grade silicon feedback, the effect of cooling rate on the minority carrier lifetime of mc-Si ingots can be known. In the study, using a lower cooling rate during growth process of mc-Si ingots, a higher lifetime on the mc-Si ingots can be obtained. But when the cooling rate is low to a certain degree, the minority carrier lifetime of mc-Si ingots reduces. The cause of the phenomenon is analyzed by measuring the curvature radius and the crystal structure of the grown mc-Si ingot. This phenomenon can be used to guide the production applications of metallurgical route with one-step directional solidification growth of mc-Si ingots.
    Preparation of Nesquehonite Whisker Using Magnesium Sulfate as Material
    ZHAO Bin;JIA Zhi-dan;SHAO Duo-duo;CAO Ji-lin
    2017, 46(1):  18-25. 
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    The nesquehonite whisker was prepared with MgSO4 ·7H2 O and Na2 CO3 as raw materials in this paper. The effect of concentration of magnesium sulfate, raw material ratio, reaction time and temperature on the products was investigated. Samples were analyzed and characterized in this work. The results indicate that the optimum conditions to synthesize the nesquehonite whisker with well crystallization are under 50℃ for 40 min with 1 . 2 mol/L magnesium sulfate and raw material ratio of 1∶1. 2. Under this condition, conversion of magnesium ions can reach 82. 35;. The nesquehonite will transform into basic magnesium carbonate with the increase of reaction time, temperature and concentration of Na2 CO3 . Meanwhile, the condition for preparation of the nesquehonite whisker by bloedite and the process design of mother liquor circulation were studied.
    Structure Modeling of Dimethylsulfoxide Intercalating into Kaolinite
    ZHOU Yi;CHENG Hong-fei;DU Bei-bei;ZHANG Shuai;LIU Qin-fu
    2017, 46(1):  26-32. 
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    Kaolinite/DMSO intercalation complex was prepared with kaolin in Xuanhua, Zhangjiakou. X-ray diffraction ( XRD) , Fourier transform infrared spectracopy ( FT-IR) , Thermogravimetric-differential thermal analysis ( TG-DTA) were used to characterize the complex. Of which, XRD and FT-IR show that DMSO has already insert into interlayer of kaolinite, and the interlayer spacing expands from 0. 718 nm to 1. 130 nm. TG-DTA shows thermal transformation of complex goes through three phases de-intercalation of DMSO ( about 199 ℃) , dehydroxylation ( about 522 ℃) , recrystallization of kaolinite ( 997 ℃) . Moreover, the existing form of DMSO in the kaolinite layers has been surmised according to the characterization results, the structural modeling is constructed in terms of molecular dynamics simulation, and the kaolinite/DMSO intercalating mechanism is discussed.
    Growth of CdSe Crystal by Modified Horizontal Seed Vapor Phase Method
    ZHANG Chun-li;WU Hai-xin;NI You-bao;HUANG Chang-bao;WANG Zhen-you;CHEN Shi-jing
    2017, 46(1):  33-37. 
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    The CdSe single crystal with ?15 mm × 35 mm size was grown by the modified double-temperature zones horizontal vapor phase method with seed aided technique. The grown CdSe single-crystalline ingot is compact and integrated , and its surface is smooth. The obtained CdSe crystal samples were characterized by X-Ray diffractionmeter( XRD) , energy dispersive spectrometer( EDS) , and fourier infrared spectrometer. The XRD spectrum of CdSe is agreement with the standard diffraction peaks. The rocking curves of CdSe single crystal sample possess high intensity and good symmetry,and the full width at half maximum(FWHM) of the rocking curves is 0. 5°. The stoichiometry ratio was tested by EDS to be Cd∶Se=1∶0 . 977 , close to the ideal ratio of 1∶1 . The infrared transmission is beyond 65; in the region from 2. 5 to 20 μm, and the absorption coefficient α is less than 0. 1 cm-1 . The above results show that the as-grown CdSe crystal has good quality.
    Synthesis and Spectral Properties of BaWO4∶Eu3+Phosphors for White Light Emitting Diodes
    YU Hai-hui;ZHAO Ming-yue;QU Lian-jun;KONG Li
    2017, 46(1):  38-42. 
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    The powders WO3!·0. 34H2O were successfully prepared by hydrothermal method,and the red phosphors BaWO4 ∶ Eu3+ were synthesis by high-temperature solid state reaction and hydrothermal method. The results show that the phosphors for both of these two methods have the same excitation and emition spectrum. The excition and emittion spectrum are f → f of Eu3+, with the excitation spectra at 416 nm, 464 nm, 535 nm, and the higher one is 464 nm and the emittion spectra at 578 nm, 592 nm, 612 nm, 703 nm,and the higher one is 612 nm. The result show that the better doped concentration is 20 at;. The typical phosphors can match blue LED to develop the red emittion and to make up the defects of low color rendering index.
    Synthesis and Magnetic Purification Research of CNOs by Chemical Vapor Deposition Method
    ZHANG Min;ZHANG Wei-ke;JIAO Chen;YANG Hong-Yan;CHUA Hui-tong;ZHANG Yu-jun
    2017, 46(1):  43-49. 
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    Carbon nano onions ( CNOs ) were high selectively synthesized through chemical vapor deposition method using Ni-Fe metal as catalysts. As harvested CNOs contains metal core inside and hollowed CNOs. Amorphous is formed with the broken of carbon shells through the normal acid wash -burning technology. The magnetic properties of CNOs were analysised and magnetic separating technology was proposed. The results show that CNOs with metal core inside can be separated from the hollowed CNOs efficiently using this method and the purification rate reaches up to 95;.
    Preparation and Lithium Storage Properties of CoO/NiO/CoNi Composites
    LIU Huan;WANG Xin-lu;WANG Jin-xian;YU Wen-sheng;YANG Ying;ZHANG Hong-bo;DONG Xiang-ting
    2017, 46(1):  50-54. 
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    Al76 Ni13. 4 Co14. 6 decagonal quasicrystals was used as a precursor alloy and transformed into the unique CoO/NiO/CoNi three dimension structure by a fancy one-step dealloying method. X-ray diffraction ( XRD) and scanning electron microscopy ( SEM) were used to examine the structure of the products. Electrochemical performance of as prepared CoO/NiO/CoNi was evaluated by galvanostatic cycling, the results show that the initial charge/discharge capacity is 417/617 mAh · g-1 at current density 200 mA·g-1 and the corresponding coulombic efficiency is about 67. 6;. A high capacity of 585 mAh·g-1 is obtained with the high capacity retention up to 500 cycles in the range 0. 01-3. 0 V, which indicates that the as prepared CoO/NiO/CoNi endowing good cycling performance.
    Preparation and Visible-light Photocatalytic Properties of One Dimensional Fe2 O3/α-MoO3 Heterostructures
    ZHEN Yan-zhong;WANG Jie;WANG Dan-jun;FU Feng;LI Jing;XUE Gang-lin
    2017, 46(1):  55-62. 
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    One Dimension ( 1D ) heterostructure photocatalyst Fe2 O3/α-MoO3 was fabricated by depositional method, which its composition, morphology and photo-adsorption properties of were characterized by XRD、SEM-EDS、STEM、XPS、UV-Vis-DRS, as so as, the performance of photocatalytic degradation RhB was also explored. The test results show that the Fe2 O3 modification not only broaden the absorption spectrum of α-MoO3 nanobelt to the visible light region, but also increase the photocatalytic activity. The optimum photocatalytic activity of MoO3 at Fe2 O3 weight content of 1; could reach 99;after visible light irradiation 40 minutes, which is almost 3. 8 and 26 times as high as that of the pure MoO3 nanobelts and Fe2 O3 .
    Effect of Complex Carbon Source on Synthesis and Chromaticity of C@ZrSiO4 Pigment
    ZHANG Xiao-jun;PAN Ting;JIANG Wei-hui;CHEN Ting;LIU Jian-min;XU Yan-qiao
    2017, 46(1):  63-68. 
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    C@ ZrSiO4 black encapsulation pigment was prepared by a nonhydrolytic sol-gel ( NHSG ) method, using the composite of rice husk and phenolic resin ( PF ) as carbon source, zirconium tetrachloride ( ZrCl4 ) and tetraethoxysilane ( TEOS ) as raw materials, lithium fluoride ( LiF ) as mineralizer, respectively. The phase composition and the morphology of the pigment were studied by means of X-ray diffraction patterns ( XRD) and transmission electron microscope ( TEM) , respectively, and the chromatic value of the pigment was investigated by CIE-L?a?b?color system. The experiment results indicate that the phenolic resin can be used as carbon resource and the dispersant for rice husk. The chromatic value of the pigment from carbon composite is lower than that of the single carbon resource, i. e. rice husk and PF. When the addition amount of PF is 15wt; and the compound colorants amount is 2. 50wt;, the C@ ZrSiO4 black pigment exhibited excellent chromatic performance after calcining under nitrogen atmosphere at 1000 ℃ for 1 h, as L?=39. 02, a?=1. 14, b?=2. 68.
    Synthesis and Spectroscopic Study of NaMn3 F10∶Yb/(Er,Tm,Ho) Nanoparticles
    YE Shuai;LIANG Hong-da;WANG Guang-sheng;SONG Jun;QU Jun-le
    2017, 46(1):  69-73. 
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    Due to low toxicity, high stability and high photoluminescence, lanthanide doped upconversion nanoparticles has a promising appliment in bioimaging and boilable. Here, monodispersed and uniform NaMn3 F10∶Yb/( Er,Tm,Ho) nanoparticles were synthesized by common thermal decomposited method. The sizes of all synthesized nanoparticles were lower than 10 nm. It was found that the NaMn3 F10∶Yb/Er NaMn3 F10∶Yb/Tm radiated single 660 nm and 800 nm under the excitation of 980 nm continue wave laser, respectively. It mainly attribute to the act of the 4 T1 level of Mn2+ ions, which could act as the intermediate energy and facilitate the non-radiative energy transfer from the 2 H11/2 and 4 S3/2 levels to the 2 F9/2 level of Er3+ ions so that the intensity of 2 F9/2 level ( red emission) were enhanced and the intensity of 2 H11/2 and 4 S3/2 levels ( green emission) were suppressed. Finally, it was found by incorporating the Mn2+ ions into NaYF4 nanoparticles that the emission color and red/green ratio were enhanced gradually as imcreasing the Mn2+ concentration. The nanoparticles with pure red emission were obtained when the Mn2+ ions comcentration was up to 58;.
    Preperation and Electrical Properties of MnO2/Graphene as Cathode for Thermal Battery
    YANG Xiao-wei;YANG Zhao-tang;LAN Wei;YANG Kun-kun;YANG Shao-hua
    2017, 46(1):  74-78. 
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    MnO2/graphene composites were synthesized by hydrothermal method. The surface morphology of the material was analyzed by scanning electron microscope ( SEM ) . The crystal phase structure and composition of the materials were characterized by X-ray diffraction ( XRD ) and X-ray photoelectron spectroscopy ( XPS ) . The electrical properties of LiSi/LiCl-KCl/ ( MnO2/G ) cell were tested by the method of constant current discharge. The test results show that adding of GO into the reaction system made the material is composed of nano-ball type and a large number of irregular nanorods structure woven together, and the α-MnO2 nanoclusters structure attach to graphene nanosheets. The disorder wide diffraction peaks of product during 2θ of 22°-27° is graphene. After oxidation of Mn element, the ion state of the Mn element is changed into Mn4+. The LiSi/LiCl-KCl/ ( MnO2/G) cell has two discharge platforms for 2. 58 V and 1. 96 V, respectively, when discharge voltage cut-off to 1. 0 V, the corresponding discharge specific capacity reach 1150. 2 mAh/g.
    Fabrication and Coloration Mechanism of CoAl2 O4 Ceramic Pigment by Co-precipitation Method
    SONG Yuan;ZHENG Yuan-lin;TANG Yu-fei;JIAO Yang-feng
    2017, 46(1):  79-84. 
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    Cobalt aluminate ( CoAl2 O4 ) ceramic pigment powders were fabricated by co-precipitation method. Compositions, morphologies and valence state of CoAl2 O4 ceramic pigment powders were characterized by XRD, SEM and XPS. Effects of Co/Al ratio, pH value and calcination temperature on color properties of the samples were also investigated. Finally, coloration mechanism of the pigment was discussed. The results show that the resulting samples are of the typical spinel structure. The blue CoAl2 O4 ceramic pigment with high chroma was obtained when the Co/Al ratio is 0. 7∶2, pH value is 11 and calcination temperature is 1200 ℃. And, the color change of CoAl2 O4 ceramic pigments is mainly related with the valence of Co elements in the products. CoAl2 O4 ceramic pigments contain Co3 O4 ( Co4+) when the Co content or pH of the precursor solution is high, then crystal lattice distortion could be occured when Co3 O4 entered into the CoAl2 O4 to form a solid solution, resulting in a green ceramic pigment.
    Exploration of WS2-SiO2 Saturable Absorbers Prepared by the Sol-gel Method
    LIN Tao;SUN Hang;LI Jing-jing;ZHANG Tian-jie;GUO En-min;SUN Rui-juan;WANG Xi;LI Lu;WANG Yong-gang;DUAN Yu-peng
    2017, 46(1):  85-93. 
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    Two-dimensional WS2 emerges as a competitive saturable absorber material because of its unique light absorber characteristics. As sol-gel method has the advantages of convenient operation, simple equipment, low cost and so on, so it will be cost-effective fabricating WS2-SiO2 films on the quartz substrate by sol-gel method to produce saturable absorbers. The optimum parameter combination forming the SiO2 film were determined by changing the ratio of raw materials, heat treatment conditions, coating speed and other experimental parameters in the experimental process. Then, WS2 solution was add in the process to prepare WS2-SiO2 saturable absorber based on the successful fabrication of the SiO2 film. After tested by the confocal microscopy, TEM, Raman and XRD methods, the WS2-SiO2 thin film saturable absorbers were found to have smoothing morphology, and WS2 particles in films were found in several layers dimension and polycrystalline structure with obvious crystal face preferred orientation of ( 002 )、(004)、(101)、(103)、(006)、(105).
    Preparation of Graphene Nanodisk Array by Reactive Ion Etching
    LI Hao;FU Zhi-bing;WANG Hong-bin;YI Yong;HUANG Wei;ZHANG Ji-cheng
    2017, 46(1):  94-97. 
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    High quality single layer graphene is formed on copper foil with ethnol as carbon source by CVD method then transferred on SiO2/Si substrate. Then the graphene surface is covered with a layer of sibgle layer PS microsphere array by self-assembly method. And it is etched by oxygen plasma, with the etching time increasing, PS microsphere will be gradually etched, and graphene will also be etched in the process. Regular graphene nanodisk arrays will be formed on SiO2/Si substrate after the the removal of impurities of PS microsphere. Field emission scanning electron microscopy ( SEM) , Raman spectroscopy are used to characterization test the graphene nanodisks and its forming process. And it has important reference meaning for preparation of high quality graphene nanoribbons, nanodot, nanodisk.
    Effect of Additive on Electrodeposition of Gold in DMH System
    YANG Xiao-wei;AN Mao-zhong
    2017, 46(1):  98-104. 
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    Effect of additives composed of C4 H6 O2、C7 H4 NNaO3 S and C12 H25 SO4 Na on electrodeposition and electrocrystallization behavior of gold from a cyanide-free bath with DMH as complexing agent were investigated. The results of cathodic polarization curves show that the optimized deposition potential range is -0. 60~ -1. 2 V, and additive concentration had tiny effect on cathodic polarization potential. Cyclic voltammetry curves indicate that the adsorption behaviors of additives on reaction surface can affect nucleation growth potential, and had inhibitive effects on the process of cathode deposition. Electrochemical impedance spectroscopy results indicate that after addition of additives to the bath, charge transfer process is more difficult. The results of SEM show that the grains is smaller and exhibited better flattening capability than the grains obtained in basic bath. The XRD results indicate that the gold electrodeposits plated in the baths both has a preferential orientation along Au ( 111 ) and Au ( 220 ) direction.
    Self-assembly of Polystyrene Microspheres at Air-water Interface of Emulsion Using Ethanol and Water as Mixed Dispersed Medium:the Rapid Fabrication of Monolayer Colloidal Crystals
    XU Ya-wei;YI Gui-yun;WANG Xiao-dong;ZHOU Li-xing;WEI Ying;CAO Jian-liang;SUN Guang;CHEN Ze-hua;MENG Hari-bala
    2017, 46(1):  105-111. 
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    A method for the preparation of polystyrene ( PS ) monolayer colloidal crystal ( MCC ) was presented in this paper. The sub-micrometer PS colloidal microspheres were self-assembled into MCC at the air-water interface of the emulsion using ethanol and water with certain mass ratio ( K, Mass ratio of ethanol and water) as mixed dispersed medium under definite temperature. The results indicate that the PS colloidal microspheres protrude easily from the water surface as a result of water convection. The strong attractive capillary force generated from the meniscus between two PS colloidal microspheres at the air-water interface causes the PS colloidal particles to assemble into the ordered regions ( nucleation ) . These ordered regions grow due to the convective transport of the particles to the ordered regions ( aggregation ) , and the MCC was obtained successfully. The attractive capillary force was changed correspondingly while the wettability between the dispersion medium and the PS colloidal microspheres at the air-water interface was adjusted by the K, therefore the K is a key factor in the formation of the MCC. The layer number of the colloidal crystal were influenced by the mass percentage concentration of the PS microspheres, however the MCC can't be obtained by reducing the concentration merely under the K<15∶1. The ordered arrangement and the number of defects of the MCC were related with temperature.
    Preparation of Gd3 (In,Al) 5 O12∶Ce Garnet Powder by Co-precipitation Method
    CAI Shuai;LV Bin;WU Guan-jie;WANG Zhen-hai;CHEN Hong-bing
    2017, 46(1):  112-116. 
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    The solution containing Cd3+ In3+, Al3+ and Ce3+ was acquired by dissolving the reagents of Gd2O3、In2O3、NH4Al(SO4)2·12H2O and Ce2(CO3)3 in diluted nitric acid. The precursor of sulfate carbonate basic hydrate was synthesised by means of co-precipitation method. GIAG∶Ce garnet powder with cubic crystallic system was prepared by sintering the precursor at the temperature above 950℃. The characteristic functional group and thermal chemical behavior of the precursor was investigated by infrared spectrum and differential thermal analysis. The phase transformation of the precursor samples subjected with the sintering treatment under the different temperatures was analysised by X-ray powder diffraction. The SEM images and grain size distribution of GIAG∶Ce powder was characterized by surface electron microscope and grain size analysis. The Fluorescence spectra of GIAG∶ Ce powder exhibites two luminescence peaks at the wavelength of 365 nm and 450 nm, which proved that Ce3+ ions has been doped into the crystalline lattice of garnet powder.
    Effect of Sm Doping on Structure and Visible Light Photocatalytic Properties of Nano-TiO2
    PENG Fu-chang;CUI Yan;GAO Hong-lin;LIU Qing-ju
    2017, 46(1):  117-123. 
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    The pure and Sm-doped TiO2 nanopowders were prepared by sol-gel method. The samples were characterized by XRD, XPS, FT-IR, UV-Vis, PL and Nano-sizer nano particle size analyzer, etc. The effects of Sm-doping on structure and visible photocatalytic properties of TiO2 photocatalyst was evaluated by photocatalytic degradation of methylene blue ( MB ) under the irradiation of fluorescent lamp. The results show that samarium appeared two kinds of Sm3+ and Sm2+ valence state on the surface of TiO2 . Samarium doping can restrain the phase transfer from anatase to rutile, prevent the grain growth, and increase the surface hydroxyl content. Appropriate doping amount of Sm can broaden TiO2 's, spectrum absorption region to visible light and effectively inhibit the recombination of photoelectron-hole pairs. Meanwhile, the photocatalytic activity of the 1. 0wt;Sm-doped TiO2 samples calcined at 500 ℃ is the better under the irradiation of fluorescent light, it is 97; within 6 h and significantly higher than 56; of P25 produced by Degussa under the same experimental conditions.
    Improvement of Efficiency of Infrafed Detector by Surface Plasmon
    LIU Chun-mei;WU Yuan-qing;ZHANG Jin-jing;ZHANG Yu-feng;LU Xiao-dong;ZHOU Tao
    2017, 46(1):  124-128. 
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    Surface grating was used, as the common method, to improve the performance of the uncooled infrared sensor, which has the problem of high reflectivity. To improve the absorption efficiency of the uncooled infrared sensor, its structure of inner surface-plasmon-resonance is proposed in this paper. By COMSOL, the variation of the infrared absorption efficient with the structure parameters is simulated and analyzed. Absorption efficient of 99. 9; within a specified spectral band and 37. 4; averaged within the whole wavelength range is reached by parameter optimization.
    Relationship of Etching Morphology and Crystal Symmetry of Hydrothermal BSO Crystals
    GUAN Chen-xue;CAO Yan-chao;HE Xiao-ling;ZHOU Hai-tao;ZHANG Chang-long
    2017, 46(1):  129-133. 
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    The etching morphology of two different crystalline habits of hydrothermal BSO crystals was studied. The characteristics of the etching morphology of {100}、{110}、{211}、{111}faces were shown. The three-dimensional model of etching morphology of BSO crystal was established. Though the different simple forms have different shapes of etching pits, it reflects the symmetry of BSO crystal. The etching difficult degree for different faces is related to the crystal structure.
    Preparation and Oil Absorption Properties of MoS2-modified PU Sponge
    CHANG Meng-jie;LIU Jun
    2017, 46(1):  134-138. 
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    MoS2 nanosheets were prepared from MoS2 powders through ultrasonic liquid exfoliation method. Hydrophobic polyurethane ( PU ) sponges for oil absorption were fabricated by subsequent modification with MoS2 nanosheets and polydimethylsiloxane ( PDMS ) . The contact angle and oil absorbent properties of the obtained sponges were measured. The results indicate that PU-MoS2 sponge shows good hydrophobicity and oil absorption capacity. PU-MoS2 sponge has absorbent capacities of 12-86 times of their own weight for different organic solvent. The PU-MoS2 sponge obtained by coating with smaller size MoS2 nanosheets has relatively higher absorption capacity. Moreover, the absorption capacity of the PU-MoS2 sponge did not deteriorate after it was reused for 20 times, so the PU-MoS2 sponge has excellent recyclability for future application.
    Solvothermal Preparation and Thermal Stability of Calcium Titanium Oxides with Porous Nanostructure
    DONG Wei-xia;BAO Qi-fu;GU Xing-yong;LI Zhou;CHEN Xin
    2017, 46(1):  139-142. 
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    Calcium titanium oxides porous nanostructure was prepared by using titanate butyl and anhydrous calcium chloride. The effects of solvothermal temperature on the properties of calcium titanium oxides porous nanostructure powders were studied. After calcium titanium oxides powder with porous nanostructure were pressed, firing temperature on the thermal stability of porous nanostructure were studied. The samples crystal phase, microstructure and thermal analysis were characterized by X-ray diffraction ( XRD) , scanning electron microscopy ( SEM) , transmission electron microscopy ( TEM) and differential thermal-thermogravimetric analyzer ( TG-DTA) . The porous properties were characterized by water absorption rate and apparent porosity. Experimental results show that when hydrothermal temperature is 180 ℃, the sample presents a porous structure. When the firing temperature is 600-1100℃, the sample after pressed present porosity with the apparent of 44 . 28;.
    Synthesis and Characterization of Yttrium Modifiedγ-alumina by Combustion Method
    YANG Xue-jiao;ZHANG Jin;CUI Xue-jiao;LI Dong-xia;JIA Han-yue;CHU Gang
    2017, 46(1):  143-147. 
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    Aluminum nitrate nonahydrate was used as oxidant, the combustion agent glycine was used as reducing agent, yttria nitrate was added as modifiers, the modified nanometer γ-alumina powder was prepared by combustion synthesis. The effects of the process parameters, such as modifier dosage, calcination temperature, calcination time on the final samples were studied. The results show that the optimal process conditions of preparing γ-alumina modified by yttrium with glycine was used as combustion agent, the mole ratio of yttria nitrate, aluminum nitrate nonahydrate is 0. 07∶ 1, the calcinations temperature is 950 ℃, the calcinations time is 4 h. Through X ray diffraction analysis ( XRD ) , Fourier Transform Infrared Spectrometer ( FTIR Spectrometer ) , scanning electron microscopy ( SEM) and specific surface area analysis of the samples, the samples surface area is larger, with weak acid, as a catalyst carrier can improve the precious metal dispersion and catalyst on the surface of the ability of resistance to carbon deposition.
    Influence of Annealing Process on Irradiation Effect of Silicon Controlled Rectifier
    CHEN Zu-liang;LI Zhao-long;WANG Hua-ming;YUE Wei;ZHANG Yue-hong;XIE Yu-ying
    2017, 46(1):  148-152. 
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    The annealing process of silicon controlled rectifier ( SCR) after irradiation were studied. SCR wafer was irradiated by 1. 4 MeV electronic beam with fixed fluence rates. Then the triggering current and minority carrier lifetime of SCR were measured. The experimental results show that the value of minority carrier lifetime is decrease and the value of triggering current is increase after irradiation. After annealing at 350℃, the triggering current of SCR was recovered to the level before irradiation. The minority carrier lifetime was recovered, but the value was far lower than that before irradiation. In irradiation fluence range of the experiment, the k was constant. After annealing process, the k coefficient was related to irradiation fluence. Under low irradiation fluence, the k coefficient was small. Storage at room temperature brought large influence on the irradiation effect of SCR. Long time storage had favorable influence on the annealing effect at 300 ℃, and unfavorable influence on the annealing effect at 200 ℃.
    Effect of Annealing Temperature on the Hydrophilicity of TiO2 Nanotube Arrays
    HU Wen-yue;ZHAO Xi-jin;GAO Jia-qi;SHEN Qian-qian;XUE Jin-bo;JIA Hu-sheng
    2017, 46(1):  153-157. 
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    TiO2 nanotube arrays were synthesized in the ethylene glycol electrolyte contains 0. 25wt;NH4 F and 2 mL H2 O by electrochemical anodization. The formed TiO2 nanotube arrays annealed at different temperatures were compared in terms of their morphologies, structures, element composition and hydrophilicity. The results show that the morphologies of the TiO2 nanotube arrays keep the same when the annealing temperature below 600 ℃, but some TiO2 nanotubes collapsed when the annealing temperature reached 600 ℃. Aa the annealing temperature increasing, the structure of TiO2 changes from amorphous to crystal, the contact angle and hydrophilicity become better. On the other hand, F element also has a clear effect on hydrophilicity of TiO2 nanotube arrays. Less F element content results in better hydrophilicity of TiO2 nanotube arrays.
    Influence of Methane Flow Rate on the Structure and Tribological Properties of Fullerene-like Hydrogenated Carbon Thin Films
    WU Kun-yao;ZONG Yan-xu;GONG Zhen-bin;YANG Chang-qing;Li Zhao;LU Yuan-yuan;MENG Zhi-xin
    2017, 46(1):  158-162. 
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    Fullerene like hydrogenated carbon ( FL-C∶ H ) thin films were deposited on the surface of monocrystalline silicon substrate by plasma enhanced chemical vapor deposition using methane as the precursors. The structure and morphology of the thin films were characterized by high resolution transmission electron microscopy and Raman spectroscopy. The machanical and tribological properties were investigated by nano-indentation and friction and wear testing machine in the case of different methane flow rate. The experimental results show that the thin films can be described as fullerene-like nanostructures. It is also found that increasing CH4 flow rate causes the decrease of fullerene-like nanostructures, elastic modulus and hardness. But the friction coefficient is not sensitive to the change of methane flow rate.
    Study on the Absorption Efficiency of PTB7∶PC70 BM Organic Solar Cells Enhanced by Metallic Gratings with Different Shapes
    ZHANG Ye;CHEN Ming;REN Jing-kun;SUN Qin-jun
    2017, 46(1):  163-167. 
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    The surface plasmon resonance was excited by metallic grating introduced into the organic solar cells, which made absorption increasing. The absorption of PTB7∶ PC70BM organic solar cells were improved by different optimized metallic grating. In this paper,enhancement absorption rate on condition metallic grating with different shape were studied by finite element method, such as square grating, circular grating, eliptic grating, was placed at the bottom of the active layer. The result reveal that the square grating can make the total active layer absorption increased to 52. 9; from 29;,compared with the planar device. The enhancement absorption is most obvious. Next to the square grating, the eliptic grating improve to 49;. Circular grating has little effect on the absorption of the active layer, increased to 45;.
    Structure and Photoluminescence Properties of a Eu(III) Complex with Two Ligands of Mixed Pyridinecarboxylic Acid
    WANG Hong-sheng;LI Gong-chun;ZHANG Wan-qiang;CHEN Xin-hua
    2017, 46(1):  168-173. 
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    A 3D europium coordination polymer {[Eu2(2,4,6-Hptc)( 3,5-pdc)2(H2O)8]·6H2O}n(1) (2, 4, 6-H3 ptc = 2, 4, 6-pyridinetricarboxylic acid;3, 5-H2 pdc = 3, 5-pyridinedicarboxylic acid ) was synthesized by hydrothermal method using europium perchlorate reacting with 3,5-pyridinedicarboxylic acid and 2,4,6-pyridinetricarboxylic acid. X-ray diffraction analysis of single crystal shows that the complex is crystallized in monoclinic system, C2/c space group. The cell parameters are as follows a=2. 0106(11) nm,b=1. 1048(6) nm,c=1. 7591(10) nm,β = 112. 117(8) °,α = γ = 90°. Eu3+ ions in the complex is coordinated with nine oxygen atoms. Five O atmos are from the carboxylate of lignds and the other four O atoms are from coordination water molecules. They are formed a distorted tricapped trigonal prism. The two carboxylates of each 3,5-pdc anion coordinates with Eu3+ by chelating way and a 1D chain structure is formed. 2,4,6-Hptc anions coordinate with Eu3+ by the 2-and 4-carboxylates. The 4-carboxylate does not coordinate. The 1D chain structres formed with 3,5-pdc anions and Eu3+ are further connected by 2,4,6-Hptc anions and 1D ladder shaped structure are constructed. The complex exhibits intense characteristic luminescence of Eu3+ with excitation of UV-rays.
    Discussion on Diamond Color Grading System
    CHENG You-fa;LIU Hai-bin;FAN Chun-li;ZHANG Cong-sen;WANG Yue;JIA Qiong
    2017, 46(1):  174-177. 
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    In accordance with the requirements of the national standard, a better instrument and method for diamond color grading has been developed, and the effect is very small by the detection of environmental conditions, personnel and sample size. This method is used to test the different standard stones, and the results show that the color uniformity is not ideal. So the conception of diamond quantization color gradation system is put forward, which makes the diamond grading quantitative. so that the diamond grading is really unified to a standard. The idea can unify the global diamond grading standards, make the diamond grading technology more scientific, fair and reasonable.
    Effect of MnO Addtion on 40(50Cu-Ni)-(NiFe2 O4-10NiO) Cermet Inert Anodes
    YANG Wen-jie;HE Liu-qing;LI Jing;ZHENG Xin;ZHOU Ke-chao
    2017, 46(1):  178-182. 
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    The modification experiments focuses on the 40(50Cu-Ni)-(NiFe2O4-10NiO) with MnO in powder metallurgy, The density and corrosion of electricity were studied by different amount of sample, results show that Mn2+ replace part of the matrix Ni2+ during sintering, lattice distortion occurs, increasing the sintering activity. The sample is 18. 5; shrinkage rate when the addition amount of 3wt;, density up to 97. 7;. The impurity content is lower after 24 h electrolysis,the content of Cu, Ni, Mn in aluminum liquid is 0. 069wt;,0. 121wt;,0. 115wt;,0. 028wt;,respectively.
    Review of 3 D Printing Technology of Ceramic
    YANG Meng-meng;LUO Xu-dong;XIE Zhi-peng
    2017, 46(1):  183-186. 
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    The preparation method, development status and application filed of ceramic 3D printing were introduction, and latest progress of ceramic suspension of oxide ( Al2 O3 , ZrO2 ) and non-oxide ( Si3 N4 , SiC) of direct 3D printing and stereolithography were reviewed. The effect of shaping method on the property of ceramic was demonstrated, and the development of 3D printing was prospected.
    Effect of Yb2 O3 Content on the Phase Composition, Microstructure and Mechanical Properties of Yttria Stabilized Zirconia Toughened Alumina Ceramics
    WU Hai-dong;LIU Wei;WU Zi-wei;WU Shang-hua
    2017, 46(1):  187-191. 
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    Effects of Yb2 O3 content on the phase composition, microstructural and mechanical properties of yttria stabilized zirconia toughened alumina were investigated. The density, mechanical properties, microstructure and physical composition were analyzed by Archimedes, three point bending, scanning electron microscope, and X-ray diffraction. The results show that the maximum value of fracture toughness, bending strength and hardness of ZTA was 7. 42 MPa·m1/2、623. 10 MPa and 1919. 60 HV without any addition of Yb2 O3 respectively. However, with Yb2 O3 addition, the phase and the mechanical properties of ZTA were changed. The pahse of zirconia from tetragonal to cubic and a new phase Yb3 Al5 O12 appeared. Finally, the mechanical properties of ZTA were reduced, especially, the fracture toughness reduced by 30. 7; compared to without additives.