Fabrication and characterization of aluminum nitride thick film coated on aluminum substrate for heat dissipation

For effective heat dissipation in high-power LED applications, aluminum nitride (AlN) thick films as thermally conductive dielectric layers were developed, which were deposited on an Al substrate by aerosol deposition (AD). The aerosol-deposited AlN thick films on Al substrates have advantages over conventional polymer-based dielectric substrates or ceramic substrate mounted heatsink systems including an epoxy adhesive, such as excellent heat dissipation capacity and low thermal resistance. AD is an effective method to fabricate high-quality AlN thick film without the Al₂O₃ phase because the film is formed at room temperature. Highly dense and well-adhered, pure AlN thick films with thicknesses up to 30 µm were deposited on an Al substrate. AlN-Al₂O₃ and AlN-polyvinylidene fluoride (PVDF) composite films were also deposited on an Al substrate in order to investigate the effect of Al₂O₃ and polymer on the microstructure and thermal properties. Among the films, pure AlN thick film exhibited the highest dielectric strength, the highest thermal conductivity, and the lowest thermal resistance. Therefore, it can be expected that the aerosol-deposited AlN thick film on Al substrate could be used as a powerful heatsink.     

On the Use of Silver Plated Nano Aluminum Nitride and Silver Plated Chopped Carbon Fiber to Prepare Electrically Conductive Adhesives with High Thermal Conductivity

To satisfy the high electrical and thermal conductivity required for the development of microelectronic products, silver plated aluminum nitride (Ag/AlN) and silver plated chopped carbon fiber (Ag/CF) were added into an acrylate resin to prepare electrically conductive adhesives (ECAs) with high thermal conductivity. The Ag/AlN was prepared by subjecting AlN to an electroless silver plating using a Pb-free activation method. The Ag/AlN has good electrical and thermal conductivity compared to the AlN without treatment. When the weight fraction of Ag/AlN is 45 ωt%, the electrical conductivity of ECAs based on acrylate resin filled with Ag/AlN is 1.5 S/cm, and the thermal conductivity reaches 2.1 W/(m · K). With the addition of 3 ωt% Ag/CF as supplement filler, the electrical conductivity has a sharp increase to 17.8 S/cm because of the formation of conductive networks in the ECAs. However, the shear strength has an apparent loss, falling from 4.2 to 1.1 MPa.     

AIN陶瓷烧结技术研究进展

氮化铝（AIN）因其具有高热导率，作为基片材料在电子元器件中得到日益重视。本文主要论述了氮化铝陶瓷制备过程中各种烧结参数，包括烧结助剂、烧结气氛、保温时间、常压烧结、热压烧结、微波烧结和等离子烧结等对氮化铝陶瓷性能的影响。并指出可通过合适的AIN粉体制备技术，结合快速烧结方法可得到具有晶粒细小、结构均匀、高致密度和高导热率的AIN陶瓷。     

Mechanical performances of AlN/Al metallized ceramic substrates fabricated by transient liquid phase bonding and pre-oxidation treatment

For the miniaturization of high-power electronic components, AlN/Al is a promising metallized ceramic substrate due to its superior mechanical and thermal performances. Numerous bonding processes have been proposed for fabricating the metallized ceramic substrate. Unfortunately, the influences of various bonding techniques on the mechanical performance of AlN/Al metallized ceramic substrate remain undetermined to date. The objective of this study was thus to investigate the effects of the transient liquid phase (TLP) technique and pre-oxidation treatment on the bonding, microstructure, and mechanical strength of the AlN/Al metallized ceramic substrate.The results indicated that the three-layered AlN/Al/AlN specimen could be effectively bonded by the TLP process and pre-oxidation treatment. However, the bending strengths of the specimens fabricated by the two techniques were obviously divergent. The bending strength of raw AlN substrate was 333 MPa. In contrast, the bending strengths of the three-layered specimens with AlN substrates pre-oxidized at 1050 °C, 1150 °C, and 1250 °C were 292 MPa, 250 MPa, and 224 MPa, respectively. Raising the pre-oxidation temperature of the AlN substrate from 1050 °C to 1250 °C obviously increased the thickness of the Al₂O₃ layer and deteriorated the bending strength, for the fracture propagated along the Al₂O₃ layer and the Al₂O₃/AlN interface. For the TLP bonding, the Cu film deposited on the AlN substrate contributed to the generation of Al–Cu transient liquid and to bonding. The bending strength of the three-layered specimens fabricated by TLP at 650 °C was 417 MPa, which was 25% and 43% better than those of the raw AlN substrate and the three-layered specimens prepared by the pre-oxidation treatment, respectively.     

Densification and properties of AlN ceramic bonded carbon

To obtain light and tough materials with high thermal conductivity, AlN ceramic bonded carbon (AlN/CBC) composites were fabricated at temperatures from 1600 to 1900 °C in a short period of 5 min by the spark plasma sintering technique. All AlN/CBCs (20 vol% AlN) have unique microstructures containing carbon particles of 15 μm in average size and continuous AlN boundary layers of 0.5-3 μm in thickness. With an increase in sintering temperature, AlN grains grow and anchor into carbon particles, resulting in the formation of a tight bonding layer. The AlN/CBC sintered at 1900 °C exhibited a light weight (2.34 g/cm³), high bending strength (100 MPa), and high thermal conductivity (170 W/mK).     

Improvement in fracture strength in electrically conductive AlN ceramics with high thermal conductivity

It is possible to impart electrical conductivity to insulating aluminum nitride (AlN) ceramics by precipitating a yttrium oxycarbide grain boundary phase with electrical conductivity. However, previously, sintering at high temperature was required to increase the electrical conductivity through the transformation of the grain boundary phase from yttrium aluminum oxide (Al₂Y₄O₉) to rare-earth oxycarbide. As a result, the increase in electrical conductivity was accompanied with a considerable decrease in the fracture strength due to grain growth of AlN. In this study, sintering temperature and additive compositions were investigated to maintain the high strength of electrically conductive AlN without losing the high thermal conductivity.     

Extracting the Optical Parameters of the Fabricated (Al/Bare Borosilicate Crown Glass,BK-7/Ag) Multiple Layers

Significant effort has been devoted in this work to convert bare glass substrate with high transmittance, into reflective layers to know its suitability for modern applications. The glass substrate has been carefully chosen for its durability, high permeability, and ability to withstand any external stresses as a result of the accumulation of layers that reduce its permeability to convert it with the thin films coated on it into reflective materials. In parallel, the thin layer to be coated on the substrate is selected from films that can withstand external influences and their great optical properties, not to mention that they are cheap and can produce highly reflective surfaces. The optical measurements (transmittance and reflectance spectra) have been performed in the UV, Vis and NIR regions of the spectrum, that is, in the range between 300 and 1200 nm. Such measurements have been made for the bare glass substrate, the glass substrate with the Al (top side), and the glass substrate with Ag on it (bottom side), and then the optical measurements have been made for the three layers. The corresponding optical parameters of each layer have been calculated and ultimately a reflective layer with high electrical conductivity and excellent optical properties has been obtained that can be adapted for different application purposes.

     

AlN基板材料研究进展

氮化铝(AlN)以其优异的高热导率、低介电常数、与Si相匹配的热膨胀系数及其它优良的物理化学性能受到了国内外学术界和生产厂家的广泛关注，被誉为新一代高密度封装的理想基板材料。详细综述了AlN基板在导热机理、基片制备、金属化和烧结工艺方面的研究进展，展望了AlN基板的发展趋势和前景。     

High infrared emissivity of SiC-AlN ceramics at room temperature

SiC-AlN ceramics were fabricated by pressureless sintering with B₄C-C as sintering additives. The effects of AlN contents on infrared emissivity, thermal conductivity and electrical properties of SiC ceramics were investigated. The improvement of total emissivity is slight before 3 wt%AlN, but impressive after 3 wt%AlN. The significant increase of the emissivity for AlN content higher than 3 wt% could be explained via DFT calculation, that the impurity energy level formed by N atom doping into 4H-SiC and the lattice distortion are mainly responsible for it. Besides, the highest total emissivity is 0.775 when the content of AlN is 5 wt%. Additionally, more AlN solid solution results in a decrease in thermal conductivity and an enhancement in electrical resistivity. There is always a compromise among the three properties of SiC-AlN ceramics.     

Method for fabricating microwave absorption ceramics with high thermal conductivity

In this work, a high-performance microwave absorption ceramic together with high thermal conductivity was proposed through the introduction of phenolic resin as the carbon source into AlN ceramic substrate. The phenolic resin was initially mixed with AlN powder and sintering additives in ethanol to form homogeneous slurries, followed by drying, pyrolysis, dry pressing and pressureless sintering to develop nano carbon in situ in AlN substrate. The well controlled microstructure with homogeneous distribution of nano sized carbon lead to the high thermal conductivity and excellent microwave absorption properties. by adjusting the phenolic resin content, the ceramic showed a minimal reflection coefficient of about ?30 dB with an effective bandwidth of about 2 GHz together with a high thermal conductivity of about 135.1 W/m K.     

Improved thermal conductivity of ceramic-epoxy composites by constructing vertically aligned nanoflower-like AlN network

Ceramic-polymer composites with good thermal conductivity, low dielectric constant and low dielectric loss have significant applicability in microelectronics and wireless communication systems. However, traditional thermal conductivity ceramic-polymer composites – realized simply through the random dispersion of spherical or near-spherical ceramic powder fillers – cannot have both high thermal conductivity and good electrical insulation, which greatly hinders their practical application. In this study, we first used metallic Al powder corroded by ultrasonic cavitation as the aluminium source, and then prepared spherical aluminium nitride (AlN) powders with many nano petals grown on the surface using the melamine-assisted nitriding method; subsequently, the ice-template method was utilized to construct a three-dimensional (3D) AlN framework with vertical columnar holes, and finally, nanoflower-like AlN-epoxy (EP) composites were prepared by vacuum infiltration. The unique nano petal structures on the surface of AlN powder and the welding between AlN nano-petals during vacuum sintering increased the contact area between nanoflower-like AlN powders and lowered their contact thermal resistance. Moreover, the construction of vertical AlN channels was conducive to the formtion of thermally conductive pathways in AlN-epoxy composites. As a result, we obtained ceramic-polymer composites with improved thermal conductivity, among which the composites with 20 vol% nanoflower-like AlN powder had the highest thermal conductivity – 2.26 W/m·K – compared to a pure matrix, which is equivalent to an enhancement of 830%.     

High-strength Ti2AlN ceramics prepared by pulse electric current sintering based on powders synthesized by molten salt method

Ti₂AlN powders were synthesized through molten salt method and re-calcination process using TiH₂, Al and TiN powders as raw materials at 1100 ℃. The composition of final composite was directly influenced by the initial Al and TiH₂ content in the starting mixture. The purity of the synthesized Ti₂AlN powder could reach 97.1 wt% when the Al molar ratio was 1.05. Then high strength Ti₂AlN ceramics were successfully prepared in different modes, including two forms of pulse electric current sintering (PECS/SPS) and hot-pressing sintering (HP). A record-high flexural strength of 719 MPa was obtained for the PECS/SPS with an electrical insulating die (PECS/SPS II) sintered sample, based on the synthesized powder in which the initial molar ratio of Al was 1.1. The sintering behaviors in various modes were analyzed, confirming the shrinkage of particles starting at lower temperature in PECS/SPS II. The density, microstructure, Vickers hardness and elastic modulus of sintered ceramics were also investigated. Therefore, the present work provided the new methods about powder preparation and ceramic sintering of Ti₂AlN, making it possible to be used as high strength structural ceramics.     

Effect of hot-pressing sintering on thermal and electrical properties of AlN ceramics with impedance spectroscopy and dielectric relaxations analysis

The effects of hot-pressing sintering on the phase composition, microstructure, thermal and electrical properties of AlN ceramics with CeO₂–CeF₃ additives were studied. During hot-pressing sintering, high pressure reduced the grain boundary phase CeAlO₃ and decreased the concentration of oxygen in AlN ceramics. The hot-pressing sintered AlN samples had a much higher thermal conductivity of 191.9 W/m·K than pressureless sintered ones because of the great reduction of grain boundary phases and oxygen impurities in AlN ceramic. As the carbon content in hot-pressing sintered sample was very high, carbon contamination led to the decrease in electrical resistivity and changes in polarization mechanisms for AlN ceramics. The relaxation peak in the dielectric temperature spectrum with an activation energy of 0.64 eV for hot-pressing sintered samples was caused by electrons from free carbon at low temperature. Overall, hot-pressing sintering can effectively increase the thermal conductivity and change the electrical properties of AlN ceramics.     

不同烧结气氛下制备的AlN陶瓷结构和电性能的差异

以AlN粉末为原料、Y2O3粉末为烧结助剂,分别在氮气气氛下和真空气氛下,采用放电等离子烧结方法在1700℃、25MPa条件下保温10min制备AIN陶瓷。X-射线衍射、扫描电镜和X-射线光电子能谱分析表明：不同烧结气氛下制备的AlN陶瓷的结构和体积电阻率各有不同。真空气氛AlN陶瓷与氮气气氛AlN陶瓷相比较,除舍有主晶相AlN和第二相Y3Al5O12外,还含有微量Al2Y相。正是由于微量Al2Y相的存在,使得真空气氛下得到的AlN陶瓷比氮气气氛下得到的A1N陶瓷的体积电阻率低约2个数量级。     

Controlled synthesis of ultra-long AlN nanowires in different densities and in situ investigation of the physical properties of an individual AlN nanowire

The controlled synthesis of different growth densities of ultra-long AlN nanowires has been successfully realized by nitridation of Al powders for the first time. These AlN nanowires have an average diameter of about 100 nm and their mean length is over 50 μm. All the synthesized ultra-long nanowires are pure single crystalline h-AlN structures with a growth orientation of [0001]. We preferred the self-catalyzing vapor-liquid-solid (VLS) mechanism to illustrate their growth process. Although the sample with the middle growth density (3.2×10(7) per cm2) of AlN nanowire performs the best field emission (FE) properties, the emission uniformity is not good enough for field emission display applications, which may be attributed to their low intrinsic conductivity. Moreover, the electrical transport and FE properties of an individual ultra-long AlN nanowire are further investigated in situ to find the decisive factor responsible for their FE behaviors. An individual AlN nanowire is observed to have a mean 1 nA field of 440 V μm(-1) and 1 μA field of 480 V μm(-1) as well as an average electrical conductivity of about 2.7×10(-4)Ω(-1) cm(-1), which is lower than that of some cathode materials with excellent FE properties. Therefore we come to the conclusion that the electrical conductivity of the AlN nanowire must be improved to a higher level by some effective ways in order to realize their practical FE device applications.     

Thin Ag films adhesive onto flexible substrates with excellent properties for multi-application

Here, thin Ag films with excellent properties were successfully prepared on flexible substrates through surface grafting and assembling followed by simple spray-assisted deposition process. The constructed molecule brushes provide the interfacial adhesion for Ag layers onto polymer substrates. The mechanical and electrical properties of the conductive Ag coated PET could be tuned by changing the spraying passes. As the electromagnetic interference shielding material, the composite PET possesses a highest shielding efficiency of 45 dB. In addition, the Ag coated PET with the thickness of 0.1 mm would maintain the 72% electrical conductivity even been folded even at a minimum diameter of 0.2 mm. It was demonstrated that uniform and fine cracks would generate when the Ag coated PET was stretching, but Ag films still retain continuous networks to maintain the high electronic conductivity even stretching to 100%. Simple finite element modeling results prove that the stress by stretching would concentrate in corner of the crack and the deformation is mainly at stress side. The Ag layers were also produced on TPU substrates to detect the stretching, showing its potential applications for strain sensors and health monitoring systems.     

Electrically conductive ceramic composites prepared with printer toner as the conductive phase

Conductive ceramic composite was prepared by sintering the mixture of clay and printer toner at 1050°C and in the N₂ atmosphere. The microstructure and mineral phases of the ceramic composite were characterised by SEM, EDX, TG and XRD, and its electrical conductivity and mechanical properties were also investigated. The results show that, in the sintering process, a series of physical and chemical reactions take place, and mineral phases with excellent electrical conductivity, such as metal iron, carbon and Fe–Al solid solution material, are formed. The electrical conductivity mechanism can be explained by the percolation theory. The threshold value for electrical conductive percolation is between 3.5 and 7.0?wt-%. At the content of printer toner 10?wt-%, the volume electrical resistance of the ceramic composite is as low as 8.5?Ω?cm, and the composite exhibits excellent flexural strength higher than 14?MPa.     

Effects of doping Al-metal powder on thermal,mechanical and dielectric properties of AlN ceramics

In this work, the influence of Al-metal powder addition upon that thermal, mechanical and dielectric properties of aluminium nitride (AlN) ceramic was studied. The findings show that adding Al-metal powder improves not only the mechanical and thermal properties of the AlN ceramic but also has no negative impact on its dielectric properties. Based on Y₂O₃ as sintering aid, the AlN ceramic with 1.0 wt% Al doping were 14.35% higher thermal conductivity, 11.73% higher flexural strength and 59.50% higher fracture toughness than those doped without Al, respectively. This study showed that the addition of Al-metal powder may favor the purifying of the AlN lattice and the formation of homogenous and isolated second phase, which would increase the AlN–AlN interfaces and improve the thermal conductivity. Furthermore, the grain boundaries of AlN ceramics might be strengthened by the isolated second phases due to the thermal mismatch between the second phases and AlN grains, thus strengthening and toughening the AlN ceramic doped with Al. However, the large additive amount of Al powder (>1.0 wt%) was not help the isolation and homogenization of the second phase, giving a deterioration in an AlN ceramic's mechanical and thermal properties. These results suggest that the introduction of an appropriate dose of aluminium metal powder is a simple method that can be used to improve the AlN ceramic's mechanical and thermal properties simultaneously.     

Heat-conducting LSN:Ce-in-glass film on AlN substrate for high-brightness laser-driven white lighting

Laser diodes (LDs) combined with color converters have been considered as new-generation high-brightness white light source. Whereas, the luminescence of phosphor materials is easily influenced by accumulated heat originating from laser-driven conversion. In order to alleviate the thermal effect under focused laser of high-power, we proposed a high-luminescence laser-driven color converter of heat-conducting La₃Si₆N₁₁:Ce³⁺ (LSN:Ce) phosphor-in-glass (PiG). The LSN:Ce nitride phosphor exhibits excellent opto-thermal property. The LSN:Ce-PiG-AlN converter was fabricated by sintering the LSN:Ce-PiG layer (～50 μm) upon a AlN ceramic substrate. Due to excellent luminescence of LSN:Ce and high thermal conductivity of AlN, the LSN:Ce-PiG-AlN converter achieves a luminous flux (LF) of 376.1 lm, a luminous efficiency (LE) of 158 lm/W, and a correlated color temperature (CCT) of 4462 K under 2.39 W laser excitation. In addition, the temperature of PiG film surface still stays low level (<150 °C) when driven by 4.82 W laser irradiation. The proposed LSN:Ce-PiG-AlN converter is a high-performance and promising phosphor converter for high-luminescence white laser lighting.     

电子基板用玻璃/陶瓷复合材料的低温共烧与性能

玻璃/陶瓷低温共烧复合材料具有高导热性、快速电子信号传输性能、热膨胀系数与硅匹配、力学性能良好等优点,被广泛应用作电子基板材料。本文简要阐述了玻璃/陶瓷复合材料的烧结机理和影响因素,综述了主要的制备方法,指出了烧结过程中可能存在的关键问题,并讨论了玻璃/陶瓷复合材料的性能调控方法。最后,展望了玻璃/陶瓷复合材料在电子信息领域的发展方向和应用前景。