Effect of nitriding atmosphere on the morphology of AlN nanofibers from solution blow spinning

High purity AlN fiber is a promising thermal conductive material. In this work, AlN fibers were prepared using solution blow spinning followed by nitridation under N₂ or NH₃ atmosphere. Soluble polymer, such as polyaluminoxane, and allyl-functional novolac resin were adopted as raw materials to form homogeneous distribution of Al₂O₃ and C nanoparticles within the fibers, which could inhibit the growth of alumina crystal and promote their nitridation process. The effect of nitriding atmosphere on the fiber morphology was investigated. XRD results showed that complete nitridation was achieved at 1300 °C in the NH₃ or at 1500 °C in the N₂ atmosphere. Hollowed fiber structure was observed when fiber was nitrided in N₂ at high temperature, which was caused by gaseous Al gas diffusion, and this phenomenon was eliminated in NH₃ atmosphere. The nitridation mechanisms in different atmosphere were analyzed in detail. It was demonstrated that the nitridation of Al₂O₃ fibers in the NH₃ atmosphere offered the favored AlN morphology and chemical quality. Flexible AlN fiber with O content of 0.7 wt% was achieved after nitriding in NH₃ at 1400 °C. The high quality AlN can be used in thermal conductive composite materials.     

Low-temperature hot-press sintering of AlN ceramics with MgO–CaO–Al2O3–SiO2 glass additives for ceramic heater applications

Aluminum nitride (AlN) is used a ceramic heater material for the semiconductor industry. Because extremely high temperatures are required to achieve dense AlN components, sintering aids such as Y₂O₃ are typically added to reduce the sintering temperature and time. To further reduce the sintering temperature, in this study, a low-melting-temperature glass (MgO–CaO–Al₂O₃–SiO₂; MCAS) was used as a sintering additive for AlN. With MCAS addition, fully dense AlN was obtained by hot-press sintering at 1500 °C for 3 h at 30 MPa. The mechanical properties, thermal conductivity, and volume resistance of the sintered AlN–MCAS sample were evaluated and compared with those of a reference sample (AlN prepared with 5 wt% Y2O3 sintering aid sintered at 1750 °C for 8 h at 10 MPa). The thermal conductivity of AlN prepared with 0.5 wt% MCAS was 91.2 W/m?K, which was 84.8 W/m?K lower than that of the reference sample at 25 °C; however, the difference in thermal conductivity between the samples was only 14.2 W/m?K at the ceramic-heater operating temperature of 500 °C. The flexural strength of AlN–MCAS was 550 MPa, which was higher than that of the reference sample (425 MPa); this was attributed to the smaller grain size achieved by low-temperature sintering. The volume resistance of AlN–MCAS was lower than that of the reference sample in the range of 200–400 °C. However, the resistivity of the proposed AlN–MCAS sample was higher than that of the reference sample (500 °C) owing to grain-boundary scattering of phonons. In summary, the proposed sintering strategy produces AlN materials for heater applications with low production cost, while achieving the properties required by the semiconductor industry.     

Reactive wetting behavior and mechanism of AlN ceramic by CuNi-Xwt%Ti active filler metal

In order to propel the application of the developed CuNi-Xwt%Ti active filler metal in AlN brazing and get the universal reactive wetting mechanism between liquid metal and solid ceramic, the reactive wetting behavior and mechanism of AlN ceramic by CuNi-Xwt%Ti active filler metal were investigated. The results indicate that, with the increasing Ti content, surface tension for liquid CuNi-Xwt%Ti filler metal increases at low-temperature interval, but very similar at high-temperature interval, which influence the wetting behavior on AlN ceramic obviously. CuNi/AlN is the typical non-reactive wetting system, the wetting process including rapid wetting stage and stable stage. The wettability is depended on surface tension of the liquid CuNi filler metal completely. However, the wetting process of CuNi-8wt.%Ti/AlN and CuNi-16 wt%Ti/AlN reactive wetting system is composed by three stages, which are rapid wetting stage decided by surface tension, slow wetting stage caused by interfacial reaction and stable stage. For CuNi-8wt.%Ti/AlN and CuNi-16 wt%Ti/AlN reactive wetting system, although the surface tension of liquid filler metal is the only factor to influence the instant wetting angle θ₀ at rapid wetting stage, the reduced free energy caused by interfacial reaction at slow wetting stage plays the decisive role in influencing the final wettability.     

AlN对铁基合金等离子喷焊层组织和摩擦磨损性能的影响

目的 加入AlN提高铁基合金的摩擦磨损性能。方法 采用PTA-400E3-HB等离子喷焊设备在Q235钢表面制备添加AlN的铁基合金喷焊层。通过光学显微镜、扫描电镜（SEM）和X射线衍射仪（XRD）研究喷焊层的组织和相结构。利用显微硬度计、摩擦磨损试验机和台阶仪对喷焊层的硬度和摩擦磨损性能进行测试。结果 添加AlN的喷焊层主要物相为α-Fe、γ-Fe和(Fe,Cr)7C3。未添加AlN的喷焊层由等轴晶组成，添加AlN的喷焊层呈现柱状树枝晶，且随AlN量增加，树枝晶组织愈加粗大。添加1%AlN喷焊层的平均显微硬度最高，为(890.1±46.8)HV0.3，比铁基喷焊层的显微硬度高131.6HV0.3；当AlN含量增加，未转变奥氏体量增加，导致喷焊层的硬度降低。加入AlN的喷焊层的摩擦系数均降低，摩擦系数稳定在0.40~0.57之间。当AlN添加量为3%时，喷焊层的磨损形貌最光滑，磨损率为1.15×10-14 m3/(N?m)。添加AlN后，喷焊层的磨损机理从之前的粘着磨损变为磨粒磨损。结论 添加AlN能提高铁基喷焊层的摩擦磨损性能。     

以物理气相传输法自支撑生长氮化铝单晶的表征

本文提出了以物理气相传输法自支撑生长氮化铝单晶的新方法，此方法可以在氮化铝烧结体表面一次性获得大量生长的氮化铝单晶。本研究中，在2373–2523 K的温度条件下经过100 h生长的氮化铝单晶，其最大尺寸为7 × 8 × 12 mm3，典型直径为5–7 mm。这些原生晶体的表面形貌及结晶质量分别通过扫描电子显微镜、拉曼光谱和高分辨X射线衍射进行表征分析。其中，拉曼光谱E2峰位的半高全宽为5.7 cm-1，高分辨X射线衍射得到的对称摇摆曲线的半高全宽为93.6角秒。经过选择性化学腐蚀后的晶体，其表面的平均腐蚀坑密度为7.5 × 104 cm-2。逸出气体分析和辉光放电质谱分析结果表明，碳和氧为晶体内部的主要杂质元素，含量分别为28 ppmw和120 ppmw。此方法为高质量氮化铝单晶的获取提供了一个新的途径，这些单晶可以被切成晶片作为后续氮化铝同质外延生长的优良籽晶。使用这些小的籽晶，我们首次成功制备出了直径高达60 mm的氮化铝单晶体/晶圆，并具有良好的深紫外光透过性。     

导热PE-LD复合材料的制备与性能研究

采用低密度聚乙烯(PE-LD)为基体材料,石墨、Al N为导热填充材料,通过双辊混炼、模压制备了导热复合材料,并对该复合材料的导热性能、力学性能、热行为进行了分析。结果表明,随着石墨或Al N含量的增加,PE-LD/石墨复合材料和PE-LD/Al N复合材料的热导率逐渐增大;PE-LD/石墨复合材料的热导率高于PE-LD/Al N复合材料的热导率。当石墨与Al N的总质量分数为50%、石墨与Al N的质量比为4∶1时,PE-LD/石墨/Al N复合材料的拉伸强度、弯曲强度均达到最大值,分别为12.8,17.15 MPa;此时PE-LD/石墨/Al N复合材料的热导率达到最大值,为0.618 W/(m·K),略低于添加质量分数50%的石墨时的PE-LD/石墨复合材料的热导率[0.634 W/(m·K)];当石墨与Al N质量比为1∶4时,PE-LD/石墨/Al N复合材料的热导率为0.488 W/(m·K),高于只添加质量分数50%Al N的PE-LD/Al N复合材料的热导率[0.410 W/(m·K)]。当石墨和Al N总质量分数为50%时,随着Al N含量的增加,PE-LD的结晶度增大。     

工艺参数对氮化铝陶瓷表面激光金属化层电阻的影响

目的 提高氮化铝陶瓷表面激光金属化层的导电性能。方法 采用正交试验设计方案,使用30 W纳秒光纤激光打标机制备了氮化铝陶瓷表面激光金属化试样,测量了金属层的电阻。通过极差分析和方差分析方法分析了激光工艺参数及其交互作用对氮化铝陶瓷表面激光金属化层电阻值的影响规律。结果 在本研究激光工艺参数及其取值范围内,激光功率对氮化铝表面激光金属化层电阻的影响最为显著,增大激光功率有利于降低氮化铝表面激光金属化层的电阻值。采用优化工艺参数(激光功率30 W、频率30 kHz、扫描速度100mm/s)单次激光扫描制备激光金属化层的电阻为2.25?/mm。随着重复扫描次数的增加,功率不同的激光表面金属层的电阻值向相反方向转变：小功率激光表面金属层电阻值随扫描次数增加而迅速减小,大功率激光表面金属层电阻值随扫描次数增加而增大。经10次重复扫描后,激光功率3 W(相应的激光能量密度约为15.3 J/cm²)激光金属化层的电阻值低于功率分别为30 W和18.75 W激光金属化层的电阻值。结论 采用30 W激光单次扫描,或者采用3 W激光多次扫描,有利于提高氮化铝表面激光金属化层的导电性。     

镁铝钆合金在空气中的氧化与燃烧

研究了在镁铝质量比为20:80的镁铝合金中加入稀土金属钆后,合金在空气中的氧化与燃烧特性。借助TG-DSC,SEM,XRD,EDS以及高速摄像仪等仪器对Mg-Al-Gd合金的氧化、燃烧过程及产物进行分析。结果表明:相对于不含钆的Mg-Al合金,Mg-Al-Gd合金在空气中的点火温度较低,约为487.6℃。在TG-DSC实验中,镁铝钆合金的氧化分为2个阶段,第1个阶段为镁的氧化反应,第2个阶段为氧化镁、铝以及氧气的反应,反应生成MgAl_2O_4。当Mg-Al-Gd合金在空气中燃烧时,合金粒子表面会形成一层薄的致密的氧化层,氧化层限制了合金粒子固相或液相的氧化,促进其气相燃烧,同时也导致燃烧出现喷射现象。燃烧没有生成MgAl_2O_4,而是形成了一种新的产物AlN。     

流延成型用AlN无苯浆料的制备及其性能研究

氮化铝(AlN)陶瓷具有优良的热、电、力、光学性能,具有广阔的应用前景,已经引起了国内外研究者的广泛关注。以无水乙醇和异丙醇为混合溶剂,研究了分散剂添加量、Y值(表示粘结剂和增塑剂质量之比)、固含量及溶剂种类对AlN浆料性能的影响。在不添加二甲苯的前提下,当分散剂添加量为1.0%(质量分数)、Y值为0.75时,制备了固含量为39.5%(体积分数)的低黏度AlN浆料,并利用流延成型制备了AlN生坯,在氮气气氛中1 825℃,保温4 h烧结后得到相对密度为99.8%、热导率为178 W·m–1·K–1的AlN陶瓷。