Preparation of BN/SiO_2 ceramics by PIP method

1　INTRODUCTIONThe PIP method is a novel route to preparingceramic matrix composites ( CMC )[1]. Its basicprinciple is that the organic precursor is firstly syn thesized and then decomposed into inorganic ce ramics. The method to prepare ceramics from theorganic silicon compound precursor is widely used,because it possesses the following advantages ascompared with the conventional powder metallurgyroute: a lower heat treatment temperature, a ef fective control i…     

SiO2p／Ni和SiCp／Ni复合材料抗氧化性能研究

采用粉末冶金方法制备了SiO2p／Ni和SiCp／Ni复合材料，研究了两种复合材料在恒温氧化和循环氧化条件下的抗氧化性能。结果表明：两种复合材料比基体Ni有更好的抗氧化性能；复合材料SiO2p／Ni的抗氧化性能优于SiCp／Ni复合材料；复合材料的循环氧化速率高于恒温氧化速率。     

Molten Salt Synthesis of Ba（ Mgl／3Nb2／3 ）O3 Powder

The single-phrase Ba(Mgl/3Nb2/3)O3(BMN) powder was saccessfully prepared by the KCImolten salt synthesis(MSS) method. The temperature for single-phase BMN powders by MSS was about 400℃ lower than that by the solid-phase method. The average particle size (APS) was about 0.91,u.m at 900℃ and increased with increasing synhesis temperature. Based on the APS, the activation energy for particle growth in theMSS, whose value was 64. 1kJmol^-1.was attained. The sinterability of the powder prepared by MSS method wasbetter than that pretared by solid-phase method.     

纳米纤维素增强CMC/SiO2复合膜的性能研究

近年来膜技术不断在各个领域渗透,并且应用越来越广,成分单一的膜已经不能满足各领域的需求,尤其在航空航天、军事和国防等特殊领域,对所应用的膜的性能标准更高,通过将两种以上成分复合,使膜功能互补和优化,制备出性能优异的复合膜是当今时代发展的必然趋势。本工作研究将羧甲基纤维素（CMC）与SiO2纳米颗粒和纳米纤维素(CNF)混合,制备出具有较好的耐热性和机械强度的纳米复合薄膜。该复合膜可以在物质分离、生物传感器等方面被深入研究并加以应用。     

离子交换型Cu／SiO2催化剂的制备和表征

用离子交换法制备了Ｃｕ／ＳｉＯ２催化剂，并在催化活性与稳定性方面与浸渍型的Ｃｕ／ＳｉＯ２催化剂进行了对比，采用差热分析（ＤＴＡ）、Ｘ射线衍射（ＸＲＤ）、比表面测定等方法对催化剂进行了表征     

Structure and mechanical properties of ZrO2-mullite nano-ceramics in SiO2-Al2O3-ZrO2 system

ZrO2-mullite nano-ceramics were fabricated by in-situ controlled crystallizing from SiO2-Al2O3-ZrO2 amorphous bulk. The thermal transformation sequences of the SiO2-Al2O3-ZrO2 amorphous bulk were investigated by X-ray diffraction, infrared spectrum, scanning electron microscope and differential scanning calorimetric. And the mechanical properties of the nano-ceramics were studied. The results show that the bulks are still in amorphous state at 900 ℃ and the t-ZrO2 forms at about 950 ℃ with a faint spinel-like phase which changes into mullite on further heating. ZrO2 and mullite become major phases at 1 100 ℃ and an amount of m-ZrO2 occur at the same time. The sample heated at 950 ℃ for 2 h and then at 1 100 ℃ for 1 h shows very dense and homogenous microstructure with ball-like grains in size of 20-50 nm. With the increase of crystallization temperature up to 1 350 ℃, the grains grow quickly and some grow into lath-shaped grains with major diameter of 5 μm. After two-step treatment the highest micro-hardness, flexural strength and fracture toughness of the samples are 13.72 GPa, 520 MPa and 5.13 MPa·m1/2, respectively.     

高速气流冲击法制备BN包覆TiB2复合粉末

采用高速气流冲击式粉体表面改性装置Hybridization制备了BN包覆TiB2复合粉末，对包覆工艺参数进行了分析并得出了较适宜的包覆奈件。用JSM-5610LV型扫描电子显微镜和H-600STEM／EDS型透射电子显微镜对包覆体的显微结构进行研究。结果表明，包覆时间、转速、TiB2与BN的粒径比、原料预处理等均对包覆效果有显著影响；经球形化处理的TiB2粉末与BN预混合后再进行包覆处理，可以得到表面光滑、包覆致密、球形化效果显著的复合粉末。     

Fabrication and Microstructure of BN Matrix Composites with Electrical COnductivity

BN ceramic is advanced engineering ceramics with excellent thermal shock resistance,good workability and excellent dielectricity.TiB2 ceramic has excellent electric conductivity,high melting points,and corrosion resistance to molten metal.Therefore,the composite consisting of BN and TiB2 ceramics is expected to have a combination of above-mentionaed properties,thereby can be used as self-heating crucible.In this puper,hot pressing technology was used to fabricate the high performance BN-TiB2 composite materials,microstructure and electric conducting mechanism were studied,and the relationship between the microstructure and physical property was discussed.the results show that the microstructure of composites has a great influence on the physical property of composites.The BN-TiB2 composites with excellent mechanical strength and stable resistivity can be obtained by optimizing the processing parameter and controlling the microstructure of composites.     

Structure and internal stress of Au films deposited on SiO2／Si（100） andmica by dc sputtering

Au films with a thickness of about 300 nm were deposited on SiO2/Si(100) and mica substrates by dc sputtering. X-ray diffraction spectroscopy and field emission scanning electron microscopy were used to analyze the structure and internal stress of the Au films. The films grown on SiO2/Si(100) show a preferential orientation of [111] in the growth direction. However the films grown on mica have mixture crystalline orientations of [111], [200], [220] and [311] in the growth direction and the orientations of [200] and [311] are slightly more than those of [111] and [220]. An internal stress in the films grown on SiO2/Si(100) is tensile. For Au films grown on mica the internal stresses in the [111]-and [311]-orientation grains are compressive while those in the [200]- and [220]-orientation grains are tensile. Au films grown SiOJSi(100) have some very large grains with a size of about 400 nm and have a wider grain size distribution compared with those grown on mica.     

水热法制备SrBi2Ta2O9陶瓷及其介电性能研究

采用水热法合成SrBi2Ta2O9(SBT)纳米粉体,成型后采用常规烧结法制备SBT陶瓷.利用XRD和SEM研究陶瓷的物相和微观形貌;利用介电温谱研究陶瓷的介电性能.结果表明:采用水热法能够制备出颗粒细小均匀、结构致密且物相纯净的SBT陶瓷;其居里温度为375℃,对应的介电常数为114.54.     

Simulated Sunlight Irradiation Based Photocatalytic Degradation of Acrylonitrile by Sn-F Co-doped TiO2/SiO2 Nano Powder Catalyst

模拟阳光照射下Sn-F共掺杂TiO2/SiO2纳米粉体催化剂对丙烯腈的光催化降解

李翰良¹,苗诗雨²,邱露¹,Bandna Bharti¹,欧阳峰¹

（1．哈尔滨工业大学（深圳） 土木与环境工程学院, 深圳 518055;

2． 大连理工大学（盘锦） 生命科学与医学学院,辽宁 盘锦 124000）

创新点说明：

光催化降解污染物是一种绿色环保技术,其中F-TiO2/SiO2是本课题组研究比较成熟的技术,现通过进一步Sn-F共掺杂方式使得催化剂活性进一步提升,对光的吸收能力更强。

研究目的：

本研究致力于解决丙烯腈生产废水的光催化降解问题,由于丙烯腈存在碳氮三键,很难被生物降解,且丙烯腈生物毒性很强,常规方法很难达到彻底降解的目的。故本研究通过光催化技术产生强氧化能力的空穴将其氧化。

研究方法：

通过Sn-F共掺杂方式改性F-TiO2/SiO2催化剂,研究不同煅烧温度对其表面特性的影响,并进行XRD,SEM,EDS,XPS,BET,UV-Vis,PL等表征手段研究。

研究结果：

实验结果表明：通过Sn-F共掺杂,提升了光的吸收能力,增大了催化剂的比表面积,不同温度下煅烧均为锐钛矿相,且催化剂的分散性良好,电子-空穴对的分离得到改善,降解丙烯腈的能力比未掺杂前有很大的提高。

结论：

采用溶胶-凝胶法制备了Sn-F-TiO2/SiO2催化剂。在模拟光照条件下降解丙烯腈,评价其光催化活性。系统研究了Sn-F-TiO2/SiO2催化剂对丙烯腈降解的催化活性。Sn-F-TiO2 /SiO2催化剂对丙烯腈的降解率为67.7%。表征结果表明,Sn-F-TiO2/SiO2催化剂晶体尺寸小,颗粒表面小,颗粒疏松,有利于催化剂粉末在反应体系中均匀分散。PL也略有减弱,这意味着光生电子和空穴的复合受到抑制。吸收边发生红移,提高了光的利用率,并提高了光催化活性。XPS结果表明,催化剂晶格中成功掺杂了锡。在反应体系中加入牺牲剂表明,空穴是光催化活性中最重要的活性组分。

关键词：光催化,丙烯腈降解,Sn掺杂,F-TiO2/SiO2

     

Ca2+对SiO2-BSA混合体系膜污染行为的影响

为研究Ca²⁺对SiO₂-BSA混合污染物膜污染行为的影响,针对SiO₂与牛血清蛋白(BSA)共存体系,在不同Ca²⁺浓度下,使用原子力显微镜测定各污染物与聚偏氟乙烯(PVDF)超滤膜及各污染物之间的作用力,结合膜污染实验,探讨Ca²⁺对SiO₂-BSA混合污染物膜污染行为的影响.结果表明:随着Ca²⁺浓度的增大,SiO₂-BSA引起的膜污染逐渐减小,主要是因为Ca²⁺改变了SiO₂-BSA混合体系中各污染物与膜及污染物之间的相互作用力.针对污染物与膜之间的相互作用力,Ca²⁺的加入触发了PVDF膜与BSA及SiO₂之间的水合排斥力,从而削弱BSA在膜表面的吸附累计速率,有效减缓了运行初期的膜污染速率;针对污染物之间的作用力,Ca²⁺浓度的增加使得SiO₂-SiO₂及SiO₂-BSA之间作用力增大,从而导致污染物团聚形成大尺寸聚集体,在膜面形成松散多孔的污染层,进而伴随着膜污染速率以及污染幅度的减小.     

TiO2/ML-Ti3C2复合纳米材料的制备及其光催化性能

通过水热技术在二维(2D)多层材料Ti_3C_2 (multi-layer Ti_3C_2, ML-Ti_3C_2)的表面及层间原位晶化和生长锐钛矿相TiO_2纳米球,制备出TiO_2/ML-Ti_3C_2复合纳米材料。采用XRD、SEM、氮吸附等表征技术对TiO_2/ML-Ti_3C_2纳米复合材料进行分析表征,并以亚甲基蓝(MB)为模拟污染物,对纯TiO_2和TiO_2/ML-Ti_3C_2复合纳米材料的光催化性能进行了评价。实验结果表明,两种材料的耦合抑制了Ti O_2中光生电子-空穴对的湮灭,延长了复合光催化剂中载流子寿命,拓宽了复合材料的光谱响应范围。在紫外光照射下,以TiO_2/ML-Ti_3C_2复合纳米材料为光催化剂,200 mg/L的MB溶液在20 min内几乎完全脱色,降解率为98.98%。TiO_2/ML-Ti_3C_2纳米复合材料的光催化性能优于纯TiO_2和Ti_3C_2, Ti_3C_2优异的电子传输能力和超强的吸附性能优化了TiO_2的光催化性能。本研究为使用光催化技术处理废水提供了一种新的思路,具有一定的实际应用前景。     

Synthesis of γ-Al2O3 nanoparticles by chemical precipitation method

Highly pure active γ-Al₂O₃ nanoparticles were synthesized from aluminum nitrate and ammonium carbonate with a little surfactant by chemical precipitation method. The factors affecting the synthesis process were studied. The properties of γ-Al₂O₃ nanoparticles were characterized by DTA, XRD, BET, TEM, laser granularity analysis and impurity content analysis. The results show that the amorphous precursor Al(OH)₃ sols are produced by using 0.1 mol/L Al(NO₃)₃ · 9H₂O and 0.16 mol/L (NH₄)₂CO₃ · H₂O reaction solutions, according to the volume ratio 1.33, adding 0.024% (volume fraction) surfactant PEG600, and reacting at 40 °C, 1 000 r/min stirring rate for 15 min. Then, after stabilizing for 24 h, the precursors were extracted and filtrated by vacuum, washed thoroughly with deionized water and dehydrated ethanol, dried in vacuum at 80°C for 8 h, final calcined at 800 °C for 1 h in the air, and high purity active γ-Al₂O₃ nanoparticles can be prepared with cubic in crystal system, O _H ⁷ -FD3M in space group, about 9 nm in crystal grain size, about 20 nm in particle size and uniform size distribution, 131. 35 m²/g in BET specific surface area, 7 – 11 nm in pore diameter, and not lower than 99.93% in purity. Foundation item: Project(03JJY3015) supported by the Natural Science Foundation of Hunan Province     

Preparation of LiFePO4 for lithium ion battery using Fe2P2O7 as precursor

In order to obtain a new precursor for LiFePO4, Fe2P2O7 with high purity was prepared through solid phase reaction at 650 ℃ using starting materials of FeC2O4 and NH4H2PO4 in an argon atmosphere. Using the as-prepared Fe2P2O7, Li2CO3 and glucose as raw materials, pure LiFePO4 and LiFePO4/C composite materials were respectively synthesized by solid state reaction at 700 ℃ in an argon atmosphere. X-ray diffractometry and scanning electron microscopy（SEM） were employed to characterize the as-prepared Fe2P2O7, LiFePO4 and LiFePO4/C. The as-prepared Fe2P2O7 crystallizes in the Cl space group and belongs to β-Fe2P2O7 for crystal phase. The particle size distribution of Fe2P2O7 observed by SEM is 0.4-3.0 μm. During the Li^＋ ion chemical intercalation, radical P2O7^4- is disrupted into two PO4^3- ions in the presence of O^2-, thus providing a feasible technique to dispose this poor dissolvable pyrophosphate. LiFePO4/C composite exhibits initial charge and discharge capacities of 154 and 132 mA·h/g, respectively.     

Modification of LiCo1/3Ni1/3Mn1/3O2 cathode material by CeO2-coating

LiCo_1/3Ni_1/3Mn_1/3O₂ was coated by a layer of 1.0 wt% CeO₂ via sol-gel method. The bared and coated LiMn_1/3Co_1/3Ni_1/3O₂ was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), cyclic voltammogram (CV) and galvanotactic charge-discharge test. The results show that the coating layer has no effect on the crystal structure, only coating on the surface; the 1.0 wt% CeO₂-coated LiCo_1/3Ni_1/3Mn_1/3O₂ exhibits better discharge capacity and cycling performance than the bared LiCo_1/3Ni_1/3Mn_1/3O₂. The discharge capacity of 1.0 wt% CeO₂-coated cathode is 182.5 mAh·g⁻¹ at a current density of 20 mA·g⁻¹, in contrast to 165.8 mAh·g⁻¹of the bared sample. The discharge capacity retention of 1.0 wt% CeO₂-coated sample after 12 cycles reaches 93.2%, in comparison with 86.6% of the bared sample. CV results show that the CeO₂ coating could suppress phase transitions and prevent the surface of cathode material from direct contact with the electrolyte, thus enhance the electrochemical performance of the coated material.     

Characteristics of LiCoO2, LiMn2O4 and LiNi0.45Co0.1Mn0.45O2 as cathodes of lithium ion batteries

LiNi_0.45Co_0.10Mn_0.45O₂ was synthesized from Li₂CO₃ and a triple oxide of nickel, cobalt and manganese at 950 °C in air. The structures and characteristics of LiNi_0.45Co_0.10Mn_0.45O₂, LiCoO₂ and LiMn₂O₄ were investigated by XRD, SEM and electrochemical measurements. The results show that LiNi_0.45Co_0.10Mn_0.45O₂ has a layered structure with hexagonal lattice. The commercial LiCoO₂ has sphere-like appearance and smooth surfaces, while the LiMn₂O₄ and LiNi_0.45Co_0.10Mn_0.45O₂ consist of cornered and uneven particles. LiNi_0.45Co_0.10Mn_0.45O₂ has a large discharge capacity of 140.9 mA · h/g in practical lithium ion battery, which is 33.4% and 2.8% above that of LiMn₂O₄ and LiCoO₂, respectively. LiCoO₂ and LiMn₂O₄ have higher discharge voltage and better rate-capability than LiNi_0.45Co_0.10Mn_0.45O₂. All the three cathodes have excellent cycling performance with capacity retention of above 89.3% at the 250th cycle. Batteries with LiMn₂O₄ or LiNi_0.45Co_0.10Mn_0.45O₂ cathodes show better safety performance under abusive conditions than those with LiCoO₂ cathodes. Foundation item: Project(50302016) supported by the National Natural Science Foundation of China; Project(2005037698) supported by the Postdoctoral Science Foundation of China     

采用微生物覆铜板浸出液中铁离子制备 Fe2O3/石墨烯纳米复合材料的研究

针对微生物法覆铜板浸出液中的金属铁离子进行资源化处理,提高覆铜板浸出液的附加值。以水热法处理得到的铁离子溶液为原料,制备八面体和球形的Fe_2O_3/石墨烯复合材料,并将其作为锂离子电池负极材料,组装成扣式电池。结果显示:八面体形貌的Fe_2O_3/石墨烯复合材料的比容量高于球形的,其在100 mA/g电流下循环,首次放电和充电比容量分别高达1 343和970 mAh/g,在47次循环后,其放电及充电比容量分别为769和740 mAh/g。