Table of Content

15 June 2017, Volume 46 Issue 6

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Preparation and Thermoelectric Transport Properties of Sr3YCo4-xMgxO10.5+δ(0≤x≤0.04) Polycrystalline

TAN Wen-peng;YU Lan;PAN Peng;SONG Shi-jin;LIU Dan-dan

2017, 46(6):  957-961. 

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Sr3YCo4-xMgxO10.5+δ(0≤x≤0.04) polycrystalline samples were prepared by solid state reaction method.The Mg doping effects on the crystal structure, electrical transport property and thermopower were studied.The results of crystal structure indicate that Sr3YCo4-xMgxO10.5+δ is tetragonal structure.Due to Mg2+(0.066 nm) partly substitude Co3+/4+(0.053 nm/0.061 nm), and the Mg doping enlarge the lattice parameters.The Seebeck coefficient measurement at 340~830 K shows that the thermopower decreases with increasing temperature, and Mg doping does not much affect the thermopower and carrier concentration.The resistivity measurement at 100~300 K shows that the resistivity decreases with increasing temperature and resistivity decreases with increasing Mg content.Scanning electron microscope results show that the number of pores decreases and grains connect closely.Combining the results of scanning electron microscope and thermopower indicate that the main effects of Mg doping impact on the electrical transport property are weaken the scattering of pores and grain boundaries, and improve the carrier mobility.The effects of carrier concentration is secondary.

Effect of Ba on Structures of Cs1-xBaxAlSi2O6 Geopolymer and the Pollucite Ceramics

LI Jun;HOU Li;LU Zhong-yuan;DUAN Jian-xia

2017, 46(6):  962-969. 

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Geopolymer with chemical composition of about Cs1-xBaxAlSi2O6·nH2O was prepared by using metakaolin and CsOH·H2O partly replaced by BaCl2.And the Cs1-xBaxAlSi2O6 ceramics with pollucite structure were obtained through geopolymer precursors sintered at different temperatures.The crystal structures and morphologys of geopolymer and the pollucite were observed by X-ray diffraction (XRD) and scanning electron microscope (SEM).Results show that the addition of Ba has greatly influence on structures of Cs1-xBaxAlSi2O6·nH2O geopolymer and the pollucite.The CsCl and pollucite crystals would be formed in Cs1-xBaxAlSi2O6·nH2O geopolymers with increasing of Ba content.And the main crystal structures of Cs1-xBaxAlSi2O6 ceramics through geopolymer at different temperatures were pollucites.Part of Ba could enter into the lattice of pollucite and occupy the sites of Cs.But the content of Ba entered into the lattice of pollucite would be limited by the total amount of added Ba in Cs1-xBaxAlSi2O6 and the sinter temperature.

Preparation and Characterization of Yttrium Doping Modified LaMgB5O10 Powder by Combustion Method

LI Dong-xia;YANG Xue-jiao;JIA Han-yue;ZHANG Jin;CHU Gang

2017, 46(6):  970-974. 

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Yttrium doping modified LaMgB5O10 powder was synthetised with lanthanum nitrate hydrate (La(NO3)3·nH2O), yttrium oxide (Y2O3) as oxidant and magnesium nitrate hexahydrate (Mg(NO3)2·6H2O) as reductant by combustion method.The effects of Y doping amount, calcination temperatures and time on the synthesis of Y modified LaMgB5O10 were studied.The products were analyzed by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), photoluminescence spectroscopy (PL) and ultraviolet-visible diffuse reflectance spectroscopy (UV-Vis DRS).The results show that Y modified LaMgB5O10 has the best effect when the doping amount of Y is 5;, the calcination temperature is 900 ℃ and the calcination time is 5 h.Y modified LaMgB5O10 appear strong ultraviolet absorption peak at 212-317 nm and strong emission peaks at 280-355 nm and 368-435 nm.

Effect of TMIn Flow on Epitaxial Film of GaN-Based Blue Light Emitting Diodes

LI Tian-bao;ZHAO Guang-zhou;SHANG Lin;DONG Hai-liang;JIA Wei;YU Chun-yan

2017, 46(6):  975-979. 

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InGaN/GaN MQWs were grown on sapphire(Al2O3) substrates by Metal-Organic Chemical Vapor Deposition(MOCVD).The influence of TMIn flow on the alloy content, crystal quality and optical properties of InGaN/GaN MQWs were investigated by adjusting the TMIn flow in epitaxial growth process.Structural and optical properties of MQWs were characterized by high-resolution X-ray diffraction (HRXRD), atomic force microscopy (AFM) and photoluminescence (PL).HRXRD shows that with the increase of TMIn flow, the angle between the "0" peak and the GaN peak deviates from each other, and more In is incorporated into the film.HRXRD and AFM shows that with the increasing of TMIn flow, the density of dislocation and V-pits increases, and the crystal quality severely deteriorate.It is also found that the weaker PL intensity and larger FWHM value are presented with increasing TMIn fiow, which could be attributed to the deterioration of the crystal quality confirmed by HRXRD and AFM results.Thus, the structual and optical properties of InGaN/GaN MQWs are strongly affected by the TMIn flow.

Study on the Ceramic Fiber/mullite Whisker In-situ Reinforced Cordierite-mullite Lightweight Thermal Insulation Materials

QIN Meng-li;WANG Xi-tang;WANG Zhou-fu;MA yan;LIU hao

2017, 46(6):  980-986. 

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Cordierite-mullite lightweight thermal insulation materials were prepared by the starch consolidation molding process, using kyanite, clay, magnesium oxide as raw materials, starch as pore forming agent and curing agent, and addition of the suitable amount of ceramic fibers and AlF3.Cordierite-mullite lightweight thermal insulation materials have ceramic fiber/mullite whisker interlocking structure and mullite whiskers in situ formatted on the surface of ceramic fibers.The effects of introducing aluminum silicate fiber under the action of AlF3 on microstructure, mechanical properties at room temperature and thermal conductivity of the synthesized cordierite-mullite lightweight thermal insulation materials were investigated.The results show that: under the action of AlF3 mullite whisker in the vertical growth of the surface of the aluminum silicon fiber, part interspersed with well-developed cordierite grains;cordierite-mullite lightweight thermal insulation materials with fiber/mullite whisker interlocking structure had good mechanical properties and the minimum thermal conductivity.

Influence of Microwave Hydrothermal Synthesis Conditions on Crystal Properties of HZSM-5 from Direct Synthesis

YANG Wei-jia;YANG Kai-xu;ZHAO Ying;XU Zheng;CAO Jian-xin;LIU Fei

2017, 46(6):  987-995. 

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Nano HZSM-5 crystal was synthesized directly by microwave-assisted hydrothermal route.The obtained products were characterized by XRD, FT-IR, SEM, BET and NH3-TPD techniques, and the effect of various crystallization temperatures and time on the crystal properties of HZSM-5 were investigated.The results indicate that crystallization temperature and time has significant impact on the micromorphology, crystal size and dispersibility of the synthesized products.HZSM-5 crystals with regular morphology are hard to form at lower crystallization temperature or shorter crystallization time.As crystallization temperature increases, the synthetic sample gradually changes into spherical grains, the grain size increases and the degree of dispersion improved.When the crystallization temperature increases to 180 ℃, the grain size became larger and the specific surface area decreases slightly.With the extension of the crystallization time, the micropores, mesopores, specific surface area and pore volume of the samples increases.When the crystallization time was further prolonged, the possible shrinkage of the micropores in the crystal and the growth of the grains made the pore volume and specific surface area of the sample decrease.The HZSM-5 molecular sieve crystals with spherical crystal size about 60 nm and excellent dispersibility was synthesized at 160 ℃ for 1.5 h by microwave hydrothermal route, and the obtained HZSM-5 possessed distinct physicochemical properties including high specific surface area of 398.45 m2·g-1, pore volume of 0.63 cm3·g-1, average pore diameter of 6.27 nm and the weak acidity on the surface of crystal.

Preparation of Zn(O,S) Thin Films with Magnetron Sputtering Method and Application in CIGS Solar Cell

FAN Yu;LI Xiao-dong;LIN Shu-ping;ZHANG Yi;LIU Fang-fang;ZHOU Zhi-qiang;SUN Yun;LIU Wei

2017, 46(6):  996-1001. 

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Different Zn(O,S) thin films were prepared with various magnetron sputtering (MS) power and applied to the CIGS heterojunction solar cell, the Zn(O,S) thin films were investigated by XRD, XRF, profilometer, ultraviolet-visible-near infrared spectrophotometer, moreover, the analysis of MS-Zn(O,S)/CIGS heterojunction devices were completed by scanning electron microscope and wxAMPS simulation software.The results show that, the sulfur content within Zn(O,S) thin film and the optical band gap decreases significantly with lower sputtering power (<80 W).Meanwhile, α-ZnS generated in the amorphous or nano-crystalline Zn(O,S) thin film.With a higher sputtering power (>100 W), the sulfur content and optical band gap will increase and then become stable, moreover, α-ZnS can be removed within significant increased crystallization of Zn(O,S) thin film.According to the simulated results, the degradation of MS-Zn(O,S)/CIGS devices prepared under lower sputtering power (<80 W) are due to high offset between buffer layer and absorber layer which can lead to high recombination in SCR, while the degradation of the devices prepared under higher sputtering power (>100 W) are due to the high acceptor-like defect density at the interface of MS-Zn(O,S)/CIGS heterojunction which is induced by plasma bombing with higher sputtering power.

Study on the Crystalline Properties of the Pb(Zr0.52Ti0.48)O3 Thin Films with Different Thickness by Sputtering

ZHU Yan-xu;WANG Yue-hua;SONG Hui-hui;ZOU De-shu;LI Lai-long;SHI Dong

2017, 46(6):  1002-1008. 

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The influence of the thickness of Pb(Zr0.52Ti0.48)O3(PZT52/48) thin film on the crystallization and surface morphology during annealing crystallization was studied.First, the PZT molecular model was simulated by using the Materials Studio software, and the characteristic peak of PZT was obtained by X-ray diffraction;In the experiment, different temperatures and time annealing of PZT (52/48) thin films with different thickness were carried out by using annealing furnace;Then, crystalline phase of each sample was analyzed by XRD;The surface morphology of some samples was observed by FIB.The experimental results show that the impact of the thickness of the thin films and the annealing conditions on the crystalline state is consistent;For the thin films with certain thickness, the proper annealing conditions (650 ℃) can make it form a single PZT(52/48) phase;Secondary annealing has a certain effect on the crystallization of thick films, but the internal stress increases with the increase of the thickness of the sputtered film, the surface of the more thinck films that formed PZT (52/48) phase after the annealing show the more obvious cracks.

Synthesis and Photoluminescence Properties of Red-emitting Phosphor SrSnO3∶Eu3+

HAO Chen-hui;CUI Cai-e;HUANG Ping;WANG Lei;SHI Qiu-feng

2017, 46(6):  1009-1014. 

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A red-emitting phosphor SrSnO3∶Eu3+ was synthesized through the high temperature solid-state method in this article.The phosphors were characterized by X-ray powder diffraction.The characteristic photoluminescence properties were studied in detail by photoluminescence excitation, emission spectra and decay time.The red-emitting phosphor SrSnO3∶Eu3+ was proved to be a pure phase, and with good luminescent properties and thermal stability.Under excitation at 396 nm, sharp red light can be observed due to the 5D0→7F2 transition of the 0.05Eu3+ at 614 nm, the color coordinates(0.608, 0.386).The activation energy for thermal quenching was calculated that the value of ΔE was about 0.138 eV obtained from the fitting results.Above all, SrSnO3∶Eu3+ can be a potential red emitting phosphor for NUV/blue pumped white LEDs.

Sintering and Microwave Dielectric Properties of LiFeTiO4 Ceramics with Spinel Crystal Structure

GUO Teng;GUO Yu;DING Zhi-jie;HUI Zhen-zhen;YE Xiang-ju;CHEN Jun-hua;GU Yan

2017, 46(6):  1015-1020. 

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The synthesis characteristics of LiFeTiO4 ceramics were systematically investigated on the basis of solid-state reaction method, and crystal structures, microstructure and microwave dielectric properties were investigated for dense ceramics.It was found that single phase of LiFeTiO4 with spinel crystal structures can be obtained after the application of suitable sintering conditions, and the sintering temperature and holding time have obvious effects on the phase compositions.Critical values of sintering temperature and holding time were confirmed, for preparation of LiFeTiO4 ceramics with single phase, furthermore, ceramic materials with good dielectric properties can be obtained only when the sintering temperature and holding time had been well controlled.As the optimal sintering condition was 1090 ℃/2 h, the LiFeTiO4 ceramics have good microwave dielectric properties as ε=16.54, Q×f=15490 GHz (8.334 GHz), τf =-60.33×10-6/ ℃.

Influence of Hydrothermal Conditions on PZT Ceramic Powder Synthesized by Sol-Hydrothermal Method

HU Yan-hua;SONG Yan;LI-Lu;DING Bo-ming;YANG Yong-bing;JI Yao-wu

2017, 46(6):  1021-1025. 

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PbZr1-xTixO3 anti-ferroelectric ceramic powder with perovskite structure were synthesized by sol-hydrothermal method, and the influence of hydrothermal reaction temperatures and reaction times on crystallization, crystalline, microstructure were discussed.Experimental results illustrate that with the increasing of hydrothermal temperature T1 or the prolonging of hydrothermal reaction time τ1, the products of sol hydrothermal reaction is gradually change from amorphous to crystalline.When T1 is 180 ℃ and τ1 is 18 h, PZT ceramic powder with cubic morphology and perovskite structure are prepared.XRD diffraction peak of the PZT ceramic powder is enhance and the peak position is unchange when T1 is prolonge or τ1 is prolong.However, the particle size of PZT powder increase obviously when T1 increase and slightly increase by prolonging τ1.Therefore, the optimum hydrothermal conditions for the synthesis of PZT antiferroelectric ceramic powders by sol hydrothermal method in this experimental are ascertained as follows: the hydrothermal reaction temperature is 180 ℃ and the reaction time is 18 h.

Preparation and Thermal Shock Resistance of High-temperature Resistant Zirconia-corundum-mullite Composite Ceramics

XU Xiao-hong;CHEN Lin-lin;WU Jian-feng;TIAN Jiang-zhou;MI Kai-feng;ZHOU Shi-xiang

2017, 46(6):  1026-1033. 

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The high-temperature resistant zirconia-corundum-mullite composite ceramics were prepared from coal series kaolin, α-Al2O3 and partially stabilized zirconia (PSZ, 3;molY2O3).The phase composition and microstructure were determined by the XRD and SEM.The physical properties, pyroplastic deformation and thermal shock resistance were studied as the function of zirconia content (5wt;, 10wt;, 15wt;, 20wt;, 25wt; and 30wt;).The results reveal that the Y2O3, which introduced by PSZ, played as the role of sintering aids at high temperature and lowered the sintering temperature.The bending strength improve significantly as the increase of PSZ content and the bending strength of samples are 147.4 MPa, 161.3 MPa, 205.9 MPa, 234.4 MPa, 294.0 MPa and 385.0 MPa, respectively.The pyroplastic deformation and thermal shock test experiments show that the optimum addition of zirconia is 10wt;, and the pyroplastic deformation and thermal shock resistance would decrease while the content of zirconia increase further.SEM analysis show that with the increasing of zirconia content much denser samples could be obtained and the toughening effects are more obvious.XRD analysis shows that the composite ceramics have good high temperature resistance, for the phase composition of the samples before and after thermal shock is almost the same, namely corundum, mullite, m-ZrO2 and t-ZrO2.

Influence of Different Surfactants on the Activation Energy of Crystal Growth for La2Ce2O7 Nanocrystalline

WANG Chun-jie;JIE Ji-tao;LI Xue;WANG Yue

2017, 46(6):  1034-1037. 

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La2Ce2O7 nanocrystallines were prepared by hydrothermal method with La2O3 and Ce(NO3)3·6H2O as precursors, SDBS and CTAB as surfactants.The physicochemical performance of the products were investigated by XRD, Raman, SEM and TEM.The influence of different surfactants on the activation energy of crystal growth was also discussed.Qualitative analyses indicate that the sample with CTAB as surfactant shows cubic fluorite structure, the specific surface area and the average crystallite size are 187.53 m2 g-1 and 11.4 nm, respectively.In addition, the activation energy of crystal growth of CTAB (16.33±0.02 kJ·mol-1) is higher than that of SDBS (13.47±0.03 kJ·mol-1).

Properties of High Strength Silicon Carbide Foamed Ceramics by Phosphate Low-temperature Sintering

SUN Wen-fei;LIU Wei;LI Yang

2017, 46(6):  1038-1042. 

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High strength silicon carbide foam ceramics were fabricated at 950 ℃ by polymer sponge replicas method with aluminum dihydrogen phosphate as blinder.The effect of SiC contents and aluminum dihydrogen phosphate on microstructure and properties of the silicon carbide foam ceramics were investigated.The results show that the SiC particles were bonded by A-Al(PO3)3.The open cell porosity structure of silicon carbide foam ceramics was well-formed, the open porosity was from 75; to 91;.As the aluminum dihydrogen phosphate content increases, the linear shrinkage, volume density and flexural strength gradually increases, while the open porosity decreases.As the solid content increase, the linear shrinkage and open porosity declines, while the volume density and flexural strength gradually climbes.In particular, the flexural strength of silicon carbide foam ceramics is (2.22±0.26) MPa when the aluminum dihydrogen phosphate and SiC contents were 40; and 60;, respectively.

Effect of Hydrothermal Temperature on the Morphology and Ultraviolet Photocatalytic Activity of CaTi2O4(OH)2 Powders

HU Qi-guo;DONG Wei-xia;GU Xing-yong;LUO Ting;QIU Bo-xin

2017, 46(6):  1043-1047. 

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CaTi2O4(OH)2 powders with different ultraviolet photocatalytic properties were prepared by hydrothermal method using n-butyl titanate and anhydrous calcium chloride as raw materials.The phase structure, micro-morphologies, optical absorption properties and band gap width of as-prepared powders were characterized by X-Ray Diffraction(XRD), Field Emission Scanning Electron Microscope(FESEM) and UV-Vis absorption spectra(UV-Vis).The influence of different hydrothermal temperature on the phase structure, microstructure, crystal growth characteristics and ultraviolet photocatalytic properties of CaTi2O4(OH)2 were investigated.The results show that the pure CaTi2O4(OH)2 phase can be obtained at 160-200 ℃ for 36 h.The morphology of the powder from the sheet and pellet stack to develop into a complete sheet morphology process with the hydrothermal reaction temperature improved, and when the hydrothermal reaction temperature at 200 ℃, it can be found the film accumulation.The powder has the highest crystallinity when the temperature is 180 ℃, and the photocatalytic efficiency of rhodamine B is the best under UV-visible light for 5 h.

Design of Light-Trapping Structure for a-Si Thin Film Solar Cell with Optical Microcavity

SONG Yang;LU Xiao-dong;WANG Xin-xin;ZHAO Yang;WANG Ze-lai

2017, 46(6):  1048-1053. 

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Based on the Finite-Difference Frequency-Domain(FDFD) method and the range of effective absorption wavelength, the thickness of buffer layer and the size of optical microcavity clear aperture of optical microcavity light-trapping structure in a-Si solar cell that the thickness of active layer is 300 nm are optimized by using light field distribution, light throughput and active layer absorption spectra, and the photocurrent density spectrum, the total current density and the output parameter are analyzed.The results show that the active layer has a maximum absorption efficiency when the thickness of the buffer layer is 2.6 μm and the clear aperture diameter Φ=D×0.8/8;The short-circuit current of the optimized cell is 25.9225 mA/cm2, which is better than that obtained by other light-trapping structures.

Effect of Diamond Wiresaw Excited by Transverse Ultrasonic Vibration on Cutting Speed and Cutting Mechanism during Cutting Single Crystal SiC

LI Peng-yang;ZHAO Zhi-yuan;LI Lun;LI Shu-juan

2017, 46(6):  1054-1063. 

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Owing to the extremely high hardness and brittleness, the hard and brittle crystalline materials, such as SiC, Ge and Si, are very difficult to improve cutting efficiency and obtain better surface quality in conventional wiresaw cutting process.The transverse ultrasonic vibration was applied to the diamond wiresaw cutting single crystal SiC in this research.Based on analysing the characteristics of ultrasonic vibration cutting process, the necessary conditions for flexible vibrating wiresaw cutting SiC workpiece was studied and obtained.Furthermore, dynamic cutting process model for flexible diamond wiresaw excited by transverse ultrasonic cutting SiC workpiece was established, the influence of transverse vibrating wiresaw on intermittently cutting arc length and cutting speed was researched, and the mathematical expressions of increment of cutting speed in transverse vibrating wiresaw cutting process was derived.Based on the model of indentation cracking, the effect of conventional wiresaw cutting and ultrasonic vibrating wiresaw cutting on cutting speed, cutting force and surface roughness was analyzed.Comparative experiment of cutting SiC crystals by ultrasonic vibration wiresaw and by conventional wiresaw was conducted.The experimental result indicates that the surface roughness of wafers cut by transverse ultrasonic vibrating wiresaw is improved obviously, and the cutting speed in vibrating wiresaw cutting increases 45; than that in conventional wiresaw cutting, the cutting force reduces 28;-53; under the same machining conditions.Experimental result is more consistency with it in theoretical analysis.

Mechanism Study on Size Effects of Cluster Implantation on Silicon

WEI Ye;ZHOU Bing;SANG Sheng-bo;DENG Xiao;CHAI Jing;CHEN Ze-hua;ZHANG Wen-dong

2017, 46(6):  1064-1071. 

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Si cluster implantation was investigated using molecular dynamics (MD) simulation.Cluster ions'' motion was systematically investigated and compared, specifically its whole trajectory is tracked: scattering, irradiation and penetration.Subsequent long-time scale evolution of morphology on substrate surface was also monitored with visualized method.The established model straightforwardly reveals a range of novel features in low incident energy range.During the implantation, the cluster is composing variable numbers of atoms.The effect of size variations on the implantation process was examined to investigate the regime of motion of cluster.Simulation results indicate that the presented approach could be used to quantitatively predict the implanted cluster ions'' distribution.Our work could serve as references on generating surface feature of substrate materials or designing pattern in atomic scale and provide theoretical guidelines for controllable surface modification technique.

Study on Opto-Electrical Properties of Cu Thin Films Deposited by Magnetron Sputtering

FAN Zhi-qin;HE Yuan-yuan;LI Rui

2017, 46(6):  1072-1077. 

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Cu Thin films were prepared by magnetron sputtering on K9 optical glass substrate based on orthogonal test, and the effects of sputtering time, substrate temperature, and argon flow rate on the optical properties and electrical properties of copper films were studied.The research show that the transmission spectrum of Cu thin films has obvious absorption peak at 362 nm, but the absorption is weak in visible light, indicating that the Cu thin film is transparent to visible light.The transmittance decreases as the film thickness increases.The resistivity decreases with the increase of the film thickness, and the resistivity value changes rapidly when the thickness of Cu thin film is less than 1100 nm.When the thickness of Cu thin film is more than 1100 nm, the resistivity changes slowly to the fixed value.When the sputtering time is 25 min, the substrate temperature is 300 ℃ and the argon flow rate is 6.9 sccm, the obtained sample has not absorption peak in the ultraviolet-visible region and has good conductivity.

Influence of Different Morphologies on the Performance of CeO2 Humidity Sensor

WANG Chun-jie;LI Xue;WANG Yue

2017, 46(6):  1078-1082. 

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CeO2 nanocrystalline with different morphologies (nanobelts and nanoparticles) were synthesized via hydrothermal and sol-gel methods with Ce(NO3)3·6H2O as precursor.The phase structures and morphologies of products were investigated by XRD, SEM and TEM.The performance of humidity sensors fabricated by both samples were evaluated in detail.Qualitative analyses indicate that the morphologies of products has a significant effect on the properties of sensor.The sensor fabricated by nanobelts shows higher sensitivity, fast response (7 s) and rapid recovery (7 s) charateristics(15;-95;RH), and the maximum humidity hysteresis is 4; in the test humidity range compared with nanoparticles sample.The excellent performance of nanobelts sample can be attributed to the large specific surface area.

Influence of Temperature and Humidity on Electrical Resistivity of 96-Al2O3 Ceramics

LIU Jian;CHENG Li-xia;WU Hai-dong;TAN Yi-cheng;XIANG Qi-jun;WU Shang-hua

2017, 46(6):  1083-1087. 

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Al2O3 ceramics were pressureless sintered at 1500 ℃, 1550 ℃ and 1600 ℃ with 0.25wt; CaO, 1wt; MgO and 2.75wt; SiO2 as additives.The DC electrical resistivity of Al2O3 ceramics were investigated in the range of 150-400 ℃ and the relative humidity range of 40;-100; respectively.The phase composition and microstructure of Al2O3 samples were characterized by XRD and SEM.The results show that the temperature increases from 150 ℃ to 400 ℃, the DC resistivity of the samples decreases by about 2 to 2.5 orders of magnitude.The relative humidity increases from 40; to 100;, the DC resistivity of the samples decrease by about 3 to 4 orders of magnitude.At the same testing condition, the higher DC resistivity of Al2O3 samples sintered at 1500 ℃ is caused by the microstructure with smaller grain and higher porosity.

Influence of Calcined Magnesite with Suspension State and Accumulation State on Properties of Product

PENG Qiang;GUO Yu-xiang;QU Dian-li;SONG Yang;YAO Zhuo

2017, 46(6):  1088-1091. 

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Miniature analog suspended state calcination device and muffle furnace were utilized to prepare light calcined magnesia through the rapid calcination experiments of magnesite.The decomposition rate, XRD, SEM and activity of the calcined products in the suspended state and the accumulated state were analyzed, respectively, and the effects of two different calcination methods on the characteristics of light calcined magnesia were discussed.The results indicate that the decomposition rate reaches up to 98; after 1 min calcination in suspension state, which is much higher than that in accumulation calcination.In addition, the as produced light calcinedmagnesia shows the characteristics of small grain size, low crystallinity, large specific surface area, and high activity.Suspended calcination significantly enhances the heat transfer process, speeds up the reaction rate, which makes a significant contribution to increase the production efficiency, and improve the performance and stable quality of products.Suspended calcination can be applied to large-scale production of high activity light calcined magnesia.

Preparation of Manganese Dioxides by Redox Reactions as Electrode Materials for Supercapacitors

REN Qiang;KANG Li-tao;XIE Ling-li;SHI Ming-jie

2017, 46(6):  1092-1098. 

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Mesoporous manganese dioxides were prepared by a facile redox reaction using potassium permanganate (KMnO4) and polyvinyl pyrrolidone (PVP) as raw material.It is found that phases and microstructures of products are remarkably influenced by the concentration of KMnO4.As the concentration of KMnO4 increases from 0.1 mol·L-1 to 0.3 mol·L-1, the product transforms from crystalline Mn3O4 with a low surface area of 13.6 m2·g-1 to amorphous MnO2 with a relatively high surface area of 60 m2·g-1.Electrochemical tests suggest that the optimal amorphous MnO2 possesses a high specific capacitance of 442 F·g-1 at a current density of 1 A·g-1 in 2 mol·L-1 aqueous KOH electrolyte, along with 72.6;of the initial specific capacitance maintains after 1100 cycles at a current density of 5 A·g-1.

Synthesis and Characterization of EMT Molecular Sieves in the Presence of Trioxymethylene

ZHOU Jing;QIU Jun;LI Xin

2017, 46(6):  1099-1105. 

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EMT molecular sieves were synthesized by suspension aggregation aging method at room temperature using trioxymethylene as the organic additive, sodium silicate as the silicon source, and sodium aluminate as the aluminum source.The influence of gel composition, crystallization temperatures and crystallization time on the synthesis of EMT molecular sieves were investigated.The synthesized EMT molecular sieve was characterized by XRD, FT-IR, SEM, BET and ICP.The favorable synthetic conditions for the EMT zeolites are nNa2O∶nAl2O3∶nSiO2∶nH2O∶nTOX=18.5∶1∶5∶240∶0.5, crystallization temperature for 30 ℃, crystallization time for 72 h.EMT molecular sieves were synthesized under above condition, XRD characteristic diffraction peaks are stronger, consisted with typical characteristics of diffraction peaks of the EMT molecular sieve, andtherelative crystallinity is 80.1;, Si/Al is 2.01, BET specific surface area is 80.57 m2/g, pore volume and pore diameter are 0.03 cm3/g and 2.07 nm, respectively.SEM images show the spherical crystal particles grow together, with uniform size and compact arrangement.

Carbazole-Based Hole Transporting Material and Application in Perovskite Solar Cells

LI Hui;LI Zhan-feng;HAO Yu-ying;CHEN Zhi-liang;ZHANG Qi;ZHENG Xiao-lu

2017, 46(6):  1106-1111. 

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A novel carbazole-based molecule Cz-3Th was synthesized and successfully applied as hole-transporting material (HTM) of CH3NH3PbI3-based perovskite solar cells.The investigated hole-transporting material was synthesized in two steps from commercially available and relatively inexpensive starting reagents.The Cz-3Th was exploited in lead halide planar perovskite solar cells using low-temperature solution-processed SnO2 as the electron transporting layers, delivering a power conversion efficiency(PCE) of 2.68; with an open-circuit voltage(Voc) of 0.75 V under 100 mW/cm2 AM 1.5 G solar illumination.These promising results highlight the potential application of the Cz-3Th in the cost-effective and environment-friendly perovskite solar cells.

Preparation and Photocatalytic of CeO2/TiO2 Heterostructure Nanoflower

QIN Lei;XU Hai-feng

2017, 46(6):  1112-1116. 

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Due to the remarkable optoelectronic, photocatalytic properties and promising practical application in photodegrading environmental pollutions, heterostructure semiconductor nanomaterials have attracted wide attention.CeO2/TiO2 heterostructure nanoflower composites were prepared by hydrothermal method.Structure and morphology of the heterostructure semiconductor nanomaterials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscope (TEM), and ultraviolet-visible spectrum (UV-vis).It was found that the CeO2/TiO2 heterostructure nanoflower nanocomposites show excellent catalytic activity.There are about 98; degradation of methyl orange is degraded within 60 min.The enhanced photocatalytic activity may come from the special heterostructure.

Research in Preparation and Application of Graphene and Its Nanocomposites

LIN Sen;SUN Shi-yong;SHEN Ke-xuan

2017, 46(6):  1117-1121. 

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As a burgeoning two-dimensional carbon nano material, graphene has perfect crystal structure and many excellent physical and chemical properties.Graphene has broad application prospects due to its unique electrical, thermal, optical and mechanical properties, such as electronic devices, thermal materials, gas sensors, photosensitive components, environmental science and other fields.The development of graphene materials has become a hot research topic currently due to its potential value of practical applications.Graphene was introduced the source, structure, classifications and basic properties, then summarize the preparation methods and characteristics of graphene and its derivatives, and then introduce the latest research progress in electronics, materials, energy storage, environment and other fields of the nanocomposites of graphene and its derivatives.Lastly, the development prospect of graphene and its nanocomposites is prospected.

Oxidation Etching of Graphene Domains Prepared by Chemical Vapor Deposition

WANG Bin;LI Cheng-cheng;MENG Ting-ting;WANG Gui-qiang

2017, 46(6):  1122-1125. 

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Hexagonal graphene domains were synthesized on polished Cu substrate by chemical vapor deposition(CVD), and were etched with oxygen.After etching, reticular and short-line trenches were observed on the graphene domains as the result of etching on the wrinkles, and the density of trenches has great difference.The morphology and density of wrinkles were closely associated with the Cu crystal orientation indicated by the electron back-scattered diffraction.A different Cu crystal orientation led to variations in the morphology and density of wrinkles.The etching temperature has greater influence on the oxygen etching of graphene, and the etching rate increased obviously when the etching temperature exceed 250 ℃.The simple oxygen etching technology might be a convenient way to detect the distribution and morphology of wrinkles.

Synthesis and OLEDs Properties of High-efficient Deep-blue Materials Based on Fluorinated Bianthracene Derivatives

LYU Xiang;LI Zhan-feng;REN Jing-kun;HAO Yu-ying

2017, 46(6):  1126-1131. 

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A series of novel fluorinated bianthracene derivatives (BAnFs) were designed and synthesized with the aim of developing new multifunctional blue materials in organic electroluminescent (EL) devices.The photophysical properties, energy levels and thermal stability of these BAnFs were tuned by different substitution pattens of electron-withdrawing groups.On the one hand, the OLEDs using the host 4,4''-bis(N-carbazolyl)biphenyl (CBP) doped with the fluorophores BAnFs exhibited Commission Internationale de l''Eclairage (CIE) color coordinates in the range of (0.15, 0.08).In particular, the maximum current density and external quantum efficiency (EQE) of the BAn-(3,5)-CF3-doped device were 3.05 cd/A and 5.02;, respectively.On the other hand, BAnFs worked as the excellent fluorescent hosts for N,N-diphenylamino phenyl vinyl biphenyl (DPAVBi) dopant to obtain high-performance OLEDs with excellent EQE of 3.56;-5.43;.Thus, fluorinated bianthracene derivatives (BAnFs) will play an essential role in improving external quantum efficiency/color purity compromise for future multifunctional blue fluorophores.

Study on Mixed Crystal Properties of Potassium Ammonium Nitrate

LI Jian-yang;YUAN Jun-sheng

2017, 46(6):  1132-1137. 

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The single crystals of Kx(NH4)1-xNO3(0

Effect of 3D Cold Cathode Structure on Field Emission

HUO Hai-bo;YANG Wei-fei;MA Hua-li;DING Pei;ZENG Fan-guang

2017, 46(6):  1138-1142. 

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Cylinder and cuboid were fixed in circular copper by conductive silver glue to form 3D type cold cathode, surface electric field distribution of cylinder and cuboid was analyzed by finite element analysis software ANSYS.The cylinder diameter is 12.7 mm, the cuboid cathode surface is square and length is 12.7 mm.Two kinds of cathode have the same height.The carbon nanotube film (CNTs) were synthesized on the surface of cylinder and cuboid by chemical vapor deposition (CVD) and iron phthalocyanine (FePc) as catalyst.The morphology of carbon nanotubes were characterized by field emission scanning electron microscopy (FESEM).By using the diode structure and ITO conductive glass coated with phosphorpowder as anode, the field emission characteristics of two 3D type cold cathodes were measured in a vacuum chamber when the vacuum degree was 2×10-4 Pa.The results show that the field emission performance of the cuboid cathode is better than the cylinder cathode with the increase of the maximum ratio of the two cathode electric field intensity.

Synthesis of Ultrafine Magnesium Ammonium Phosphate Particles by Inverse Microemulsion Method

ZHANG Yong-xiang;LU Shan-xing;ZHANG Zhe-yi;WANG Jia;LIAO Jian-guo

2017, 46(6):  1143-1147. 

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Magnesium ammonium phosphate (MAP) was prepared by inverse microemulsion method and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared spectroscopy (FT-IR) and thermal analysis (TG-DSC).The results show that MAP prepared by inversed microemulsion method is narrower and smaller in size.MAPs with different crystal forms were obtained by different methods.Cetyl trimethyl ammonium bromide as a surfactant to prepare a magnesium ammonium phosphate has the smallest particle size distribution.Sodium dodecyl benzenesulfonate as a surfactant to prepare a magnesium ammonium phosphate has the smallest particle size and the best thermal stability.

Application of TiO2 Nanocrystalline Vesicle Microemulsion in the Polyurethane Coating System

ZHAO Xin;SUI Zhi-hui;ZHANG Jing-bin;SONG Xu-mei;SONG Wei-ming

2017, 46(6):  1148-1153. 

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Microemulsion of TiO2 nanocrystalline in vesicle was prepared using butyl titanate as raw materials.TiO2 nanocrystalline was gotted in vesicles micro-reactor formed by self-assembled of hexadecyl trimethyl ammonium bromide and sodium dodecyl benzene sulfonic acid.UPC/TVM composite leather finishing agent was gotted mixing TiO2 nanocrystalline vesicle microemulsion(TVM) and aqueous polyurethane (UPC).The dispersion, film forming and coating properties of finishing agent was studied when TiO2 vacuoles microemulsion with different ratio of polyurethane using TEM, melvin methods of grain size analysis and ultraviolet diffuse.The results show that the TiO2 vesicle microemulsion with polyurethane and hot wax slurry form uniform microemulsion with the particle size of about 80 nm.The tensile strength, elongation at break, water-absorbing quality, antibacterial ability and ultraviolet resistant of UPC/TVM3 membrane with TiO2 vesicle microemulsion were significantly increased comparing with UPC membrane.The applied experimental results of UPC/TVM composite leather finishing agent show that the water resistance of the coating and folding performance had been improved significantly.

Research Progress of TaC Coating on Carbon Materials

SHEN Xiao-song;WANG Song;LI Wei;JIANG Jin-ming

2017, 46(6):  1154-1159. 

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Oxidation of carbon materials limit their applications as structural materials in aerospace fields.TaC coating can improve the anti-ablation and against oxidation at high-temperature effectively.The new advancement of oxidation resistant TaC coatings, including single-phase, multi-layer composite coatings, gradient and the second phase toughening coatings were reviewed, the oxidation mechanism of TaC coatings in high-temperature(>2000 ℃) were also introduced.In addition, the main research direction of depend on the problem in present research were also proposed.

Research on Micro Fluidic Chips Used for Bioluminescence Detection

LIU Chun-mei;WANG Yang;WU Yuan-qing;ZHANG Jin-jing;YAO Su-ying;LU Xiao-dong;ZHOU Tao

2017, 46(6):  1160-1165. 

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The manufacture process of SU-8 photo resist mold for micro fluidic chips was described, and microfluidic chip which can realize single passing of micro balloons was successfully made.Processes including former bake, bake, lithography, imaging and other process have great impacts on SU-8 mold.A mold making process for reference was proposed, and anti-adhesive layer process was also discussed.Finally, through these studies on process, a mold was produced and used in fluid successfully, and micro balloon of 12 μm has finish its job of single pass and been detected.

Study on Ferroelectric Control of Magnetization Based Two-dimensional Ferroelectric Poly(Vinylidene Fluoride)

WANG Rui-qi

2017, 46(6):  1166-1169. 

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Using first-principles calculations with dispersion-corrected DFT-D2 method, magnetic moments and magnetic anisotropy energy flexibly by the ferroelectric polarization of PVDF were manipulated.In particular, by charge injection method, the spin-dependent screening of the ferroelectric polarization is proved to be responsible for this manipulation rather than the chemical bondings.The study is beneficial to electric-field controlled magnetic data storage.

Synthesis, Crystal Structure and Thermal Property of a 2D Coordination Polymer [Mn2(bppc)4(H2O)]n·2nH2O

SONG Juan;GE Hong-guang

2017, 46(6):  1170-1174. 

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A manganese coordination polymer [Mn2(bppc)4(H2O)]n·2nH2O was hydrothermally synthesized by Hbppc with MnCl2 .The coordination polymer was structurally characterized by single crystal X-ray diffraction,elemental analyses,IR and TGA.X-ray diffraction analysis of single crystal shows that the coordination polymer is crystallized in Monoclinic system with P2(1)/c space group.The cell parameters are as follows a=10.3918(9) nm, b=24.519(2) nm, c=7.0140(6) nm, β=105.0890(10)°, γ=90°.Each (bppc)-anion coordinates to one MnII atoms are bridged by the nitrogen atoms and carboxylate oxygen atoms of (bppc)-ligands to form a one line-like dimensional chain, and the carboxylate oxygen atoms of (bppc)-ligands further extended the 1D chain into 2D layer structure.Additionally, TGA results indicate it possess great thermal stability.

Research Progress on Synthesis of Monolayer Group-VIB Transition Metal Dichalcogenides by Chemical Vapor Deposition

ZHU Zu-song;ZHU De-quan;QIU Jun;YI Ming-fang;ZHANG Jie;WEN Jun

2017, 46(6):  1175-1183. 

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Since 2004, graphene have been under extensive investigation due to its excellent optical and electrical properties.But its applications were limited greatly because of the characteristics of the zero band gap.Monolayer VIB transition metal sulfide (TMDs) is a class of ideal two-dimensional direct band gap semiconductor,which has crystal structure analogues of graphene and controllable band structure.TMDs not only can be used to explore some other fundamental and advanced physical issues such as valley polarization, but also can be widely used in nanodevices, optoelectronics and photocatalysis.In recent years, chemical vapor deposition (CVD) technology is a more effective method to grow TMDs compared to traditional chemical synthesis or physical exfoliation.CVD can be used to synthesize a large area of continuous, uniform thickness and high crystal quality monolayer TMDs.Therefore, this review focuses on the recent progress of monolayer TMDs CVD growth technology.The influence of process parameters,such as the reaction temperature, the composition of carrier gas, the variable substrate and the precursor-substrate distance,to the growth and properties of monolayer TMDs were discussed also.Finally, it also prospects some available ways for realizing the control of the monolayer TMDs size, the coverage and thickness uniformity by using CVD technology.

Stress Distribution of Carbon Nanotubes Reinforced Magnesium Matrix Composites Containing Crack Defects under Tensile Loading

JIANG Yan;WANG Tian-shuang;WANG Jiao;SHEN Jie;LIU Gui-li

2017, 46(6):  1184-1190. 

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With the advent of the era of nanoelectronics,the unique electrical,optical and mechanical properties of carbon nanotubes as one-dimensional nanomaterials have attracted considerable interest and sparked discussion of their potential use in applications.Because of its good mechanical properties, carbon nanotubes can be used as the reinforcing materials with superior propertiesIn recent years,magnesium matrix composite of new high-strength lightweight composite materials developed rapidly.It has a high electrical and thermal conductivity, high specific strength and specific modulus, excellent damping properties, mechanical properties, high hardness and good wear resistance.In this paper, using the theory of continuum mechanics and ANSYS to solve carbon nanotubes reinforced magnesium matrix composite materials mechanics performance calculation.By using the finite element software ANSYS to contain crack defects of composite model, aims to study crack defects under the action of tensile load effect on the stress distribution of composite materials.The model without defects, magnesium matrix(vertical, transverse and circumferential defects) was selected respectively.Found in composite materials under tensile load, the vertical defects model is the most easy to fracture, and magnesium matrix contains circumferential defects is the most difficult to destroy.The model without defects is the most difficult to yield, while the magnesium matrix contains transverse defects is the easiest to yield, and the maximum yield stress appears at the junction of composite materials

Study on the Origin of Diamond Cutting Method

FAN Chun-li;CHENG You-fa;LIU Ji-yi;WANG Yue;ZHU Hong-wei;MA Xiao

2017, 46(6):  1191-1196. 

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First, a set of imitation diamond samples were processed, through the inspection to traceable to the national metrological verification department benchmark test, the test results verify the reliability of the results with the ratio of instrument, to achieve the purpose of indirect traceability.The uncertainty of the test results was calculated in detail.Experimental results show that the method is simple and feasible, and the cost is low.To form a method for diamond cutting traceability, and established the standard guide traceability work.The diamond cut grading standards to the national unified real.