碳纤维表面 h-BN 耐高温涂层的制备及表征

目的在碳纤维表面制备六方氮化硼涂层,以提高纤维的抗氧化、耐高温性能,拓宽其在高温领域的应用。方法以硼酸、尿素、氨气和氮气作为原始材料,先通过浸渍法在碳纤维表面涂覆硼酸和尿素的混合溶液,然后将其放置在氨气和氮气氛围中进行高温热解。采用电子显微镜分析涂层的形貌,观察涂层与碳纤维的结合是否良好;采用傅里叶红外光谱、X射线电子能谱及X射线衍射等测试技术对涂层的成分和结构进行表征。结果碳纤维表面的涂层连续,形貌良好。红外光谱中,在1399,799 cm-1处存在B—N键和B—N—B键的特征峰。X射线衍射图谱中,在43.64°和53.93°存在六方氮化硼(001)晶面和(004)晶面的特征峰。X射线电子能谱分析表明,涂层中存在O,B,C和N四种元素,且B与N的原子比接近1∶1。结论实验中成功制备了h-BN涂层碳纤维,且涂层和碳纤维结合较好。涂层中的h-BN结晶度良好,纯度较高,但少量氧化物的存在会对h-BN涂层碳纤维耐高温性的提升有所影响,如何进一步提高h-BN涂层的纯度有待研究。     

六方氮化硼在防腐涂料中的应用研究进展

六方氮化硼(h-BN)具有优异的热稳定性、阻隔性、耐高温性等性能,日益受到各国研究人员的广泛关注.将h-BN引入到当前防腐涂料体系中,有助于提升防腐涂料的性能,因此成为当前防腐涂料领域的研究热点之一.首先介绍了h-BN及其纳米片(BNNSs)的物化性质.接着对BNNSs的"自上而下"和"自下而上"制备方式进行了介绍,并对其优缺点进行了分析比较,重点结合当前使用较为广泛的超声辅助液相剥离技术,对其研究进展进行了概述,并介绍了近年来涌现的BNNSs制备新策略.h-BN应用于防腐涂料中,其"分散性"和"相容性"是当前首要解决的问题,功能化修饰可以有效地改善BNNSs在涂料体系中的"分散性"和涂膜的"相容性",因此对BNNSs的"共价功能化"和"非共价功能化"修饰方法进行了分析、对比和总结,并介绍了等离子气体处理制备功能化BNNSs的新技术.结合目前在防腐涂料领域中应用较为广泛的环氧涂料、聚氨酯涂料、丙烯酸涂料,对h-BN在防腐涂料中的应用进展进行了介绍,并结合相关研究进展对其增强涂层防腐的机理进行了说明.最后,基于当前h-BN在防腐涂料领域中的应用现状,对其今后研究的侧重点提出相关建议.     

高结晶度六方氮化硼的制备及表征

以硼酸和三聚氰胺为原料,在新型高温感应电炉中加热1 800 ℃进行热处理,制备六方氮化硼粉体样品,并通过扫描电镜、X射线衍射仪等设备,以及激光粒度分析、化学分析等手段对所制样品进行表征。结果表明:在设定的工艺条件下制备出结晶度高、纯度高、晶粒大的六方氮化硼。      

微波水热法合成花状纳米ZnO及其光催化活性(英文)

使用氯化锌和精氨酸作为反应物,通过简单的微波水热技术制备花状纳米氧化锌。利用X射线衍射(XRD)和扫描电镜(SEM)对所合成的纳米氧化锌进行晶体结构和形貌的表征。通过拉曼光谱和光致发光(PL)光谱对纳米氧化锌的光学性能进行研究,证实了合成物为高结晶度的纳米氧化锌。在紫外光辐射下,合成的ZnO光催化降解亚甲基蓝(MB)有较好的效果,紫外光催化2h后亚甲基蓝的降解率达到95.60%。ZnO光催化降解亚甲基蓝可以描叙为一级动力学反应,降解速率常数在1.0675～1.6275h-1的范围中,这与所合成的ZnO形貌有关。     

少层石墨烯的微波辐照法快速制备及表征(英文)

以可膨胀石墨为原料制备少层石墨烯,通过初次微波辐照3 min、混酸(浓硫酸与浓硝酸的体积比为1:1)浸泡处理24 h及二次微波辐照剥离3 min的工艺流程,得到了少层石墨烯。用扫描电镜(SEM)、X射线衍射(XRD)、拉曼光谱(Raman)、原子力显微镜(AFM)、X射线光电子能谱(XPS)、红外光谱(FTIR)和燃烧法元素分析对实验产物进行表征。结果表明:经过初次微波辐照处理,伴随闪光及爆裂声,可膨胀石墨层片结构被剥离,迅速形成疏松、多孔的蠕虫形貌。通过混酸浸泡、二次微波辐照和超声分散等后续处理,可快速制得厚度约为4.7 nm的约十几层的石墨烯,且石墨烯未被严重氧化,纯度高,结晶度高。     

Fe_3O_4/壳聚糖/纳米石墨微片纳米复合材料的制备和表征

采用原位水热法制得Fe_3O_4/壳聚糖/纳米石墨微片纳米复合材料。研究实验过程中水热反应时间对复合材料制备的影响。通过X射线衍射仪(XRD)、场发射扫描电子显微镜(SEM)、傅里叶变换红外光谱仪(FTIR)及热失重分析仪(TGA)等测试手段对制得的复合材料样品进行了表征。XRD结果表明,实现了Fe_3O_4/壳聚糖/纳米石墨微片纳米复合材料的制备。水热反应时间对复合材料的形貌产生明显影响,水热反应时间有利于促进壳聚糖炭化,四氧化三铁均匀分布在纳米石墨微片片层上。采用FTIR和TG对壳聚糖的炭化程度进行表征,表现为热失重由36%降低到32%。     

不同h-BN含量Ni-P-WS2-BN化学镀层的组织结构及磨损性能

目的 通过化学镀共沉积技术在Ni-P-WS2镀层中引入六方氮化硼(h-BN)纳米粉末,以进一步提升其硬度和耐磨性,改善其摩擦学性能。方法 将六方氮化硼(h-BN)纳米粉末与二硫化钨(WS2)纳米粉末共沉积制备Ni-P-WS2-BN复合镀层,并对其进行400 ℃×1 h的惰性气氛热处理。采用扫描电镜、X射线衍射仪、摩擦磨损试验机等对镀层的化学成分、组织结构及摩擦学性能进行表征,考察h-BN用量及热处理对复合镀层的影响。结果 随着镀液中h-BN用量的增加,镀层中h-BN含量持续上升,镀层的表面粗糙程度先升高、后降低,胞块结构有致密化倾向,硬度由321HV0.1上升至522HV0.1,磨损率从1.82×10^–13 m³/(N.m)降至0.95×10^–13 m³/(N.m),平均摩擦因数介于1.61~2.00,且呈先降后升的趋势(h-BN用量为3.0 g/L时达到最小值)。经热处理后,镀层硬度可达457~822HV0.1,磨损率从1.24×10^–13 m³/(N.m)降至0.31×10^–13 m³/(N.m),平均摩擦因数降至0.93~1.29。复合镀层的磨损以磨粒磨损机制为主。结论 h-BN粉末的共沉积和400 ℃退火处理可显著提高复合镀层的硬度和耐磨性,大幅度降低摩擦因数和磨损率,改善复合镀层的综合性能。     

六方、立方氮化硼的制备和热传导性质研究进展

随着微电子技术的不断进步,电子芯片集成化电路越来越密集。性能提高的同时,其内部热流密度不断攀升,对电子器件的散热能力提出了更高的要求。低热耗散材料严重制约了电子设备的性能和功效,有效的热传递和热管理已成为下一代微处理器、集成电路、发光二极管等设备稳定工作的重要保障,因此亟需具有更高热导率的半导体材料以提高电子器件的使用寿命。近年来,六方氮化硼(h-BN)和立方氮化硼(c-BN)引起了人们极大的研究兴趣,h-BN具有与石墨类似的层状晶体结构,常被称为“白石墨”,散热、绝缘性能良好;而c-BN为闪锌矿结构,具有类似于金刚石的晶体结构,热导率仅次于金刚石,是第三代半导体中禁带宽度最大的材料。研究表明,2种晶体均具有良好的导热性能,可成为新一代电子芯片散热材料,是当前热管理领域的研究热点。本文对h-BN薄膜和c-BN单晶制备方法的研究进展进行了综述,介绍了h-BN和c-BN热传导性质的研究成果,并对h-BN和c-BN面临的挑战和未来的发展方向进行了展望。     

微波水热法制备分等级空心球状CdS纳米结构(英文)

以氯化镉和硫代硫酸钠为原料,以乙二胺四乙酸(EDTA)为模板剂,采用微波水热(M-H)法成功制备了空心球状 CdS 纳米结构。采用 X 射线衍射仪(XRD)、场发射扫描电子显微镜(FE-SEM)、能量弥散X射线谱(EDS)和高分辨透射电子显微镜(HRTEM)对所制备的CdS 纳米结构进行表征。采用紫外-可见吸收光谱研究所制备的分等级空心球状 CdS 纳米结构的光学性能。结果表明:得到的CdS是具有纤锌矿结构的直径为 400～600nm的分等级空心球状纳米结构,这种结构由30nm左右的纳米颗粒自组装构成。EDTA和微波辐射在分等级空心球状 CdS纳米结构的形成过程中起了重要作用,讨论了这种作用并提出可能的生长机理。所制备的分等级空心球状CdS纳米结构具有较好的蓝光发射性能。     

石英纤维表面氮化硼涂层的制备及表征

以硼酸和尿素为原料，分别采用埋入法、一步法、两步法在石英纤维表面制备了氮化硼涂层。利用XRD，FTIR测试技术分析了涂层的物相和结构，结合DTA曲线分析了涂层产物的热稳定性，观察了涂覆BN涂层后的显微组织，对反应原理进行了初步探讨。结果表明：3种方法都能够在石英纤维表面形成良好的BN涂层，其中两步法是最好的涂层方法，涂层均匀平整，涂层产物为单一的h-BN，纯度很高，在1000℃以内具有良好的热稳定性。合成氮化硼的反应比较复杂，反应过程主要受尿素的化学性质控制。     

BN与LPSO相混杂增强的镁基复合材料制备及性能

研究了六方氮化硼(h-BN)颗粒增强镁基复合材料的制备工艺及其性能。通过化学镀法在h-BN颗粒表面包覆一层纯镍,镀镍处理能显著改善h-BN与镁合金熔体的润湿性,改善其与基体的界面结合。通过向基体合金中加入Y元素,利用镀镍层熔入熔体中的Ni获得了由Mg-Ni-Y组成的LPSO结构(长周期堆垛有序结构),制得了h-BN+LPSO混杂增强的镁基复合材料。超声处理后,hBN增强相体积分数为3%的镁基复合材料热导率为99.92W/(m·K),室温(RT)至100℃的平均热膨胀系数为18.36×10^-6K^-1,抗拉强度为171MPa,伸长率为3.9%,获得了兼具较高力学性能和优异热物性能的镁合金材料。     

Synthesis of cubic boron nitride thin films by low-energy ion beam assisted deposition by applying substrate bias

Cubic boron nitride (c-BN) films are synthesized with low-energy ions of 100eV from a gridless ion gun by applying negative substrate bias. Boron is evaporated by an electron beam at rates of 0.8 to 2.3Å/sec onto silicon substrate. Substrate temperature and bias are varied from 400 to 800°C and from 0 to -700V, respectively. Due to the low-operating pressure of the ion beam assisted deposition (IBAD) process, applying substrate bias efficiently accelerates ions enough for synthesis of the c-BN phase. With increasing substrate bias, the major phase changes in the sequence of hexagonal boron nitride (h-BN) to c-BN to h-BN. The reappearance of the hexagonal phase at high bias voltage is thought to be due to the stress annealing effect. Intermediate temperatures have produced higher c-BN contents. Far-off stoichiometric film (N/B≈0.72) consists of h-BN phase even under the c-BN parameter but a little off stoichiometry has led to higher c-BN contents. The maximum contents of c-BN phase is about 70%. DC type bias and oxygen/hydrogen incorporation into the films are presumed to limit the content. The IBAD process with proper substrate bias is promising for large areas of and high rate growth of the c-BN phase.     

Synthesis and characterization of Ni–P coated hexagonal boron nitride by electroless nickel deposition

Electroless plating has been receiving a steady progress over the last decade on the modification of the surface properties of ceramic materials in order to produce composite coatings with unique characteristics for critical tribological systems. In this work, an electroless nickel deposition process was used to deposit nickel-phosphorous (Ni–P) coating on hexagonal boron nitride (h-BN) particles via hypophosphitereduced acid bath solution. The substrate particles were initially subjected to series of pre-treatment operation in order to ensure that the particles are cleaned and catalytically active prior to electroless plating. The characterization of the as-received and Ni-coated powder was studied through scanning electron microscopy (SEM), energy dispersive X-ray (EDX) spectroscopy and field emission scanning electron microscopy (FESEM). The result reveals that the pretreatment of h-BN powder provides substrate particle surfaces with coarse and roughened structures which are normally considered suitable for Ni–P deposition. Moreover, the result of the EDX analysis confirms the existence of nucleating agents and Ni–P coating on the surface of the treated h-BN powder. The cross-sectional microstructure of the coated powder shows that the h-BN particles were embedded in a continuous matrix layer of Ni–P deposit. The EDX mapping profiles further indicate that the deposited Ni–P alloy mass was uniformly distributed on the surface of the Ni–P codeposited h-BN particles (Ni–P–h-BN). The successful development of Ni coated h-BN powder will raise the potential of h-BN as a high-performance coating material.     

多种硼源的复合添加对含硼金刚石单晶的影响

本文使用碳化硼、六方氮化硼和硼砂三种硼源材料复合添加的铁基触媒在高温高压下合成含硼金刚石,通过对金刚石结构与性能的表征,探讨多种硼源复合添加对含硼金刚石的影响。实验发现,采用多种硼源复合添加的铁基触媒合成金刚石可以有效地稳定金刚石的硼源供给,提高金刚石的含硼量。随着硼含量的增加,金刚石的结晶习性逐渐以（111）晶面为主,主要的机械性能和热稳定性得到了明显的提高。实验结果充分说明,多种硼源复合添加更有利于提高含硼金刚石的品级。     

The microstructural characteristics and mechanical properties of Ni-Al/h-BN coatings deposited using plasma spraying

Hexagonal boron nitride (h-BN) material was added to a nickel aluminum alloy (Ni-Al), which was deposited as plasma spray coatings, and the resultant enhanced tribological properties of these coatings were investigated. The microstructures of the coatings were analyzed using a scanning electron microscope (SEM) to monitor the morphologies of both the powders and the coatings. After wear testing, the surface morphologies of the scratched coatings were analyzed using an SEM to monitor the fracture mode of the coatings. The results of this study indicate that the addition of h-BN material to Ni-Al results in coatings with enhanced tribological properties.     

Wetting Behavior and Reactivity of Molten Silicon with h-BN Substrate at Ultrahigh Temperatures up to 1750 °C

For a successful implementation of newly proposed silicon-based latent heat thermal energy storage systems, proper ceramic materials that could withstand a contact heating with molten silicon at temperatures much higher than its melting point need to be developed. In this regard, a non-wetting behavior and low reactivity are the main criteria determining the applicability of ceramic as a potential crucible material for long-term ultrahigh temperature contact with molten silicon. In this work, the wetting of hexagonal boron nitride (h-BN) by molten silicon was examined for the first time at temperatures up to 1750 °C. For this purpose, the sessile drop technique combined with contact heating procedure under static argon was used. The reactivity in Si/h-BN system under proposed conditions was evaluated by SEM/EDS examinations of the solidified couple. It was demonstrated that increase in temperature improves wetting, and consequently, non-wetting-to-wetting transition takes place at around 1650 °C. The contact angle of 90° ± 5° is maintained at temperatures up to 1750 °C. The results of structural characterization supported by a thermodynamic modeling indicate that the wetting behavior of the Si/h-BN couple during heating to and cooling from ultrahigh temperature of 1750 °C is mainly controlled by the substrate dissolution/reprecipitation mechanism.     

硼膜多步骤注N的镀层结构研究

用离子束溅射硼靶，在W6o5Cr4V2钢上宙积一层硼膜，再用反冲注入法注氮以形成氮化硼（BN），注入时采用逐次递减能量（即50kV,30keV,10keV0的多步骤注入。用XPS分析膜的成分深度分布及元素的化学价态；用傅立叶红外（FTIR）反射谱分析膜的结构，结果表明：膜基界面产生混合，与用单一能量注入相比，多步骤注入时，膜层的N／B分布比较均匀；硼在膜中以BN形式存在，膜深度较大处为a-BN或h-BN，并且随着深度的降低，膜有向c-BN转化的趋势。     

钛合金表面激光熔覆 h-BN 固体润滑涂层

目的优化钛合金激光熔覆固体润滑涂层的熔覆工艺参数,提高钛合金表面耐磨性能。方法采用Nd∶YAG激光器,分别在高功率和低功率条件下,在TC4钛合金表面制备h-BN固体自润滑涂层。观察分析熔覆陶瓷层的宏观形貌、物相组成、显微组织和硬度,采用摩擦磨损试验仪对熔覆层的摩擦学性能进行研究。结果低激光功率下,熔覆材料上浮流失严重,熔覆层的相成分主要是Ti N,Ti B,Ti B2等硬质相,硬度较高,存在裂纹。高激光功率下,基材的熔化稀释较好地抑制了润滑相h-BN的上浮,减少了溅射损失,发生了包晶反应,生成了单质金属Ti,熔覆层硬度低,但摩擦磨损试验表明,涂层中润滑相h-BN含量的增加使得形成了更好的润滑膜,降低了摩擦系数。结论在输出电流400 A,脉宽5 ms,频率12Hz,扫描速度120 mm/min,搭接率50%~60%的条件下进行激光熔覆,所得熔覆层的表面状态平整,耐摩擦性能最好。