氮化硼合成的工艺及性能研究

本论文采用硼酸和三聚氰胺按照一定的配比合成氮化硼的前驱体高聚物,氮化硼前驱体高聚物溶于甲酸溶液。将氮化硼前驱体高聚物在23 kV,正负极距离为15 cm条件下纺出细度均匀的纤维。对合成的前驱体高聚物放在马弗炉中按照10℃/min的升温速度升至800℃,保温一定时间得到氮化后的产物,氮化后产物成白色,硬度较大。利用扫描电镜、傅里叶红外光谱仪和TG-DSC热重分析仪对氮化后产物的性能特征进行了测试。     

类石墨氮化碳及其MCA杂化物的合成与阻燃

采用三聚氰胺作为原料,通过梯度加热制备了类石墨氮化碳(g-C3N4),再以三聚氰胺、氰尿酸和自制g-C3N4合成了三聚氰胺氰尿酸杂化物(CNMCA)。采用FTIR、XRP和TDA对g-C3N4和CNMCA的结构与热性能进行了表征。将CNMCA应用在聚酰胺6中制备了阻燃复合材料,同时,采用垂直燃烧和极限氧指数法分析了阻燃效果。结果表明,g-C3N4具有较高的热稳定性,其热失重5%(T-5%)的温度高达544.9℃。另外,g-C3N4的杂化不同程度地提高了MCA的热稳定性。当杂化比例为30%时,CNMCA的T-5%由345.5℃提升到352.3℃,在600℃下的残余质量由0.43%显著提升到23.45%。CNMCA的阻燃性能比MCA更佳,当添加到10%CNMCA30时,试样燃烧时的熔滴已无法使脱脂棉被引燃,因此,阻燃等级从UL94 V-2提升到UL94 V-0级,极限氧指数也从27.8%提升至31.3%。     

Influence of Hydrogenation on Morphology,Chemical Structure and Photocatalytic Efficiency of Graphitic Carbon Nitride

In this contribution, the effect of hydrogenation conditions atmosphere (temperature and time) on physicochemical properties and photocatalytic efficiency of graphitic carbon nitride (g-C₃N₄, gCN) was studied in great details. The changes in the morphology, chemical structure, optical and electrochemical properties were carefully investigated. Interestingly, the as-modified samples exhibited boosted photocatalytic degradation of Rhodamine B (RhB) with the assistance of visible light irradiation. Among modified gCN, the sample annealed at 500 °C for 4 h (500-4) in H₂ atmosphere exhibited the highest photocatalytic activity—1.76 times higher compared to pristine gCN. Additionally, this sample presented high stability and durability after four cycles. It was noticed that treating gCN with hydrogen at elevated temperatures caused the creation of nitrogen vacancies on gCN surfaces acting as highly active sites enhancing the specific surface area and improving the mobility of photogenerated charge carriers leading to accelerating the photocatalytic activity. Therefore, it is believed that detailed optimization of thermal treatment in a hydrogen atmosphere is a facile approach to boost the photoactivity of gCN.     

镁碱沸石结晶度及晶体形貌的影响因素

以硅溶胶为硅源,偏铝酸钠为铝源,乙二胺为模板剂制备镁碱沸石.考察了晶化温度、晶化时间、碱度、陈化时间和晶种加入量对镁碱沸石结晶度和晶体形貌的影响.用X射线衍射仪(XRD)、扫描电子显微镜(SEM)等对所合成的样品进行了表征.结果表明:在碱度为0.12~0.15、晶化温度为160 ℃、晶化时间为60 h的条件下能够合成出晶化良好的样品;随着晶化温度的升高样品结晶度先升高后降低,其晶体尺寸逐渐增加;随着晶化时间的延长样品的结晶度和晶体尺寸先增加后趋于稳定;适当温度的陈化可以减小晶体尺寸,而添加晶种则可以显著改变晶体的形貌和尺寸.     

混合碱液法生长氧化锌晶体的晶形、表面形貌及光致发光性质(英文)

以氢氧化钠和氢氧化锂作为助熔剂,采用常压混合碱液法成功生长了各种形貌的ZnO晶体。以Bravais-Friedel-Donnay-Harker法则为指导,获得了ZnO晶体的几种理论结构晶形;在考虑晶体内部结构和生长实验中外部生长条件下,得到了晶体的实验晶形。采用光学显微镜、扫描电子显微镜和原子力显微镜对六方片状晶体的表面形貌进行了研究。结果表明:晶体的理论结构晶形和实验晶形吻合良好;晶体具有二维螺旋生长的机制。此外,晶体在325 nm光激发的室温光致发光光谱显示,在380 nm处存在1个强的紫外发射峰和位于652 nm处的弱且窄的红光发射峰,说明生长的六方片状ZnO晶体结晶质量优良。     

Nanocrystalline Aluminum Nitride: II, Sintering and Properties

Nanocrystalline aluminum nitride powders obtained from gas condensation and in situ nitridation in a forced-flow reactor have been sintered successfully without pressure or additives. The resulting densified pellets showed good thermal conductivity and low oxygen content. A comparison of the improvement in densification with micrometer-size and nanocrystalline yttria additives was undertaken and it was found that the nanocrystalline yttria decreased the sintering temperature significantly. Besides spherical nanoparticles, needle-shaped nanocrystalline aluminum nitride particles that resulted in highly textured compacts when hot pressed could also be produced.     

Hot Isostatic Pressing of Silicon Nitride with Boron Nitride, Boron Carbide, and Carbon Additions

Si₃ N₄ test bars containing additions of BN, B₄C, and C, were hot isostatically pressed in Ta cladding at 1900° and 2050°C to 98.9% to 99.5% theoretical density. Room-temperature strength data on specimens containing 2 wt% BN and 0.5 wt% C were comparable to data obtained for Si₃ N₄ sintered with Y₂O₃, Y₂O₃ and Al₂O₃, or ZrO₂. The 1370°C strengths were less than those obtained for additions of Y₂O₃ or ZrO₂ but greater than those obtained from a combination of Y₂O₃ and Al₂O₃. Scanning electron microscope fractography indicated that, as with other types of Si₃N₄, roomtemperature strength was controlled by processing flaws. The decrease in strength at 1370°C was typical of Si₃N₄ having an amorphous grainboundary phase. The primary advantage of non-oxide additions appears to be in facilitating specimen removal from the Ta cladding.     

Composition and Microstructure of Chemically Vapor-Deposited Boron Nitride, Aluminum Nitride, and Boron Nitride + Aluminum Nitride Composites

The composition and microstructure of dispersed-phase ceramic composites containing BN and AIN as well as BN and AIN single-phase ceramics prepared by chemical vapor deposition have been characterized using X-ray diffraction, scanning electron microscopy, electron microprobe, and transmission electron microscopy techniques. Under certain processing conditions, the codeposited coating microstructure consists of small single-crystal AIN fibers (whiskers) surrounded by a turbostratic BN matrix. Other processing conditions resulted in single-phase films of AIN with a fibrous structure. The compositions of the codeposits range from 2 to 50 mol% BN, 50 to 80 mol% AIN with 7% to 25% oxygen impurity as determined by electron microprobe analysis.     

Synthesis, Properties, and Oxidation of Alumina-Titanium Nitride Composites

Al₂O₃-TiN composites varying from 60 to 66.6 mol% TiN were prepared by an in situ reaction between TiO₂ and AlN. N₂ or O₂ evolution takes place, depending on the composition selected. A pseudobrookite (PB) phase appears in the reaction product, the amount decreasing as the TiO₂:AlN ratio becomes poor in AlN. The in situ reaction product can be pressureless sintered to 94% to 97% theoretical density at 1600°C in N₂. The four-point flexural strength varies from 280 to 430 MPa at room temperature. The fracture toughness is 3 to 4.7 MPa.m^1/2. Oxidation of a 94% dense TiN-Al₂O₃ composite in the temperature range 710° to 1050°C was also studied. A layer of TiO₂ (rutile) protects the composite at 710°C from further oxidation with a weight gain of 0.08 mg/cm² in 90 min. In the temperature range 820° to 1050°C, the initial oxidation kinetics are parabolic, with an activation energy of 216.5 kJ/mol. Linear oxidation kinetics with an activation energy of 113.7 kJ/mol pertain at longer times.     

Study on Tribological Properties of Carbon/Aramid Fabric Coatings Modified by Boron Nitride of Single Layer

Carbon/aramid fabric composite coatings modified with boron nitride of single layer were fabricated through a dip-coating method. The composite coatings were cured with successive heating processes in an oven. The friction and wear properties of those as-prepared coatings were studied on a block-on-ring tester. The obtained results showed that the wear life of the coatings increased obviously after inclusion of boron nitride of single layer; however, the values of friction coefficients of the coatings almost remained constant. The optimal loadings of boron nitride of single layer in our experiments was 5 wt.%, and the wear life of the modified coating increased by ca. 360% compared with that of pristine fabric composite coating. The worn morphology of the sliding surface for both pristine fabric coating and the composite coatings filled with boron nitride of single layer was discussed, and the wear mechanisms were illuminated.     

NMMO工艺纤维素膜结晶度与强度性能初探

以纤维素为原料,N-甲基吗啉-N-氧化物(NMMO)为溶剂,采用相转化法制备非对称纤维素膜。利用X-射线衍射仪对NMMO工艺纤维素膜的结晶状况进行检测,并利用拉力机检测出薄膜的拉伸强度。结果表明:随着铸膜液中纤维素含量的增加,薄膜结晶度与拉伸强度均提高;随着溶解纤维素的温度提高,薄膜结晶度与拉伸强度降低;随着刮膜剪切力增大,薄膜结晶度和拉伸强度提高;并且薄膜结晶度的增加有利于薄膜拉伸强度的提高。     

氮化硼/碳纤维复合织物的性能研究

将氮化硼粉末负载于碳纤维织物上,用扫描电镜和紫外分光光度计观察和测试了氮化硼/碳纤维复合织物的表面形貌和紫外漫反射性能。结果显示:有大量氮化硼负载于碳纤维织物上;在250～600 nm波长范围,氮化硼/碳纤维复合织物的紫外漫反射性能比纯碳纤维织物的更好。用网络分析仪测试了氮化硼/碳纤维复合织物的电磁屏蔽性能,发现负载了氮化硼的碳纤维织物的电磁屏蔽性能略弱于纯碳纤维织物。     

Fabrication of Low-Shrinkage, Porous Silicon Nitride Ceramics by Addition of a Small Amount of Carbon

Successful net-shape sintering offers a significant advantage for producing large or complicated products. Porous Si₃N₄ ceramics with very low shrinkage were developed, in the present investigation, by the addition of a small amount of carbon. Carbon powders (1–5 vol%) of two types, with different mean particle sizes (13 nm and 5 μm), were added to α-Si₃N₄−5 wt% Y₂O₃ powders. SiC nanoparticles formed through reaction of the added carbon with SiO₂ on the Si₃N₄ surface or with the Si₃N₄ particles themselves. Such reaction-formed SiC nanoparticles apparently had an effective reinforcing effect, as in nanocomposites. Sintered Si₃N₄ porous ceramics with a high porosity of 50%–60%, a very small linear shrinkage of ∼2%–3%, and a strength of ∼100 MPa were obtained.     

氮化硅陶瓷在现代制造业中的应用

本文论述了氮化硅结构陶瓷材料的性能,着重介绍了此种材料在国内外制造业中的应用现状,也讨论了氮化硅陶瓷的缺陷及研究方向。     

PTFE改性树脂立方氮化硼磨具性能的研究

为了解决钛合金磨削高温和模具黏附问题,提高其切削加工性能,通过在树脂立方氮化硼(CBN)磨具中加入不同含量的聚四氟乙烯(PTFE)作为固体润滑剂,并对其进行力学性能测试,研究PTFE添加量对树脂CBN磨具磨削性能的影响。结果表明:PTFE润滑作用明显;当PTFE添加量为6 g时,树脂CBN磨具的摩擦力和摩擦系数显著降低,磨具磨削性能显著改善。     

高结晶性带状氧化锰的制备及其电容性质

以KMnO4和乙醇经氧化还原反应所得γ-MnOOH为前驱物,在10 mol/L KOH溶液中于140℃水热条件下反应72 h,制得了比表面积为53 m2/g的带状Birnessite型层状氧化锰.应用XRD、SEM和氮气吸脱附等技术对制备产物进行了结构和形貌表征.同时,在1.0 mol/L Na2SO4水溶液中研究了带状氧化锰的电容性质.结果显示,当扫描速度为5 mV/s时,其比电容为180F/g.循环测试2000圈后,比电容保持率为72％.     

氟化钡晶体点阳极电注入着色光谱特性

利用自行研制的电注入实验装置,在不同温度和电压条件下,对氟化钡(BaF2)晶体进行点阳极电注入着色。测定了点阳极电注入着色时的电流随时间的变化关系;测量和分析了着色BaF2晶体室温下的吸收光谱。结果表明:着色BaF2晶体中产生大量F色心。按照传统电注入机理,晶体经点阳极电注入不可能产生F色心。借助电流–时间曲线对经点阳极电注入BaF2晶体中F色心的形成机理进行了分析,即V色心首先在阳极附近被产生,F色心是由V色心吸收光子转化而来。     

Synthesis of Pure Hydroxyapatite and the Effect of Synthesis Conditions on its Yield,Crystallinity, Morphology and Mean Particle Size

Abstract

Hydroxyapatite (HAP) is a calcium phosphate compound with the chemical formula Ca₅(PO₄)₃OH. This compound is especially significant in biomedical applications since it resembles the mineral constituents of the hard tissue in the human body. Its biocompatibility, castability, and sinterability make it a very attractive material for simulating bones and therefore for implantations. The objective of this study was to produce HAP with a high purity and to determine quantitatively the exact percentage of HAP in the synthesized powder. Hydrothermal methods have been used to produce HAP. In the present work, Hydroxyapatite powder was produced using the chemical precipitation method in a batch and semi‐batch modes of operation. The effect of temperature, pH, and reactant addition rates on the mean particle size was studied. Results showed a maximum in the mean particle size at pH 9, while a minimum was observed at around 45°C. As the reactant addition rate increased the mean particle size increased as well. The purity of the obtained powder was characterized using both quantitative and qualitative techniques. The quantitative results were performed using the powerful Rietveld refinement method. The quantitative results were obtained for three samples. Results showed that pure HAP was produced at a temperature of 85°C, pH 9 and reactant addition rate of 1.3 mL/min.     

TPI结晶性对DCP硫化TPI胶料性能的影响

研究了反式-1,4-聚异戊二烯（TPI）结晶性对不同用量过氧化二异丙苯（DCP）硫化的TPI性能的影响。结果表明,拉伸前后TPI试样的XRD曲线上结晶峰有明显不同。TPI预拉伸冷冻试样的拉伸性能与冷冻前后原始试样的差异明显。随着DCP用量的增加,500mm/min和50mm/min拉伸速率下测得的拉伸强度之间的差异变得越来越小;同一压缩率时,试样的压缩强度不断降低。在tanδ-温度曲线上,随着交联密度的提高,TPI低温损耗峰的tanδ值不断增大,而其高温损耗峰的tanδ值呈下降趋势。     

氮化硅陶瓷的无压烧结工艺优化及性能研究

以α-Si3 N4为原料,Y2 O3和MgO为复合烧结助剂,通过无压烧结制备出氮化硅陶瓷。为了优化实验配方和工艺参数,采用正交实验研究了成型压力、保压时间、保温时间、烧结温度、烧结助剂含量以及配比对氮化硅陶瓷气孔率和抗弯强度的影响规律。结果表明,影响氮化硅陶瓷气孔率的主要因素是烧结助剂含量和配比,而影响其抗弯强度的主要因素是烧结助剂配比和烧结温度。经分析得出,最佳工艺参数为成型压力16 MPa,保压时间120 s,保温时间2 h,烧结温度1750℃,烧结助剂含量12wt％,烧结助剂配比1∶1;经最佳工艺烧结后的氮化硅陶瓷,相对密度为94．53％,气孔率为1．09％,抗弯强度为410．73 MPa。