前驱体制备与氮化还原法合成AIN粉的物相分析

采用溶胶凝胶工艺制备了铝源和碳源的均匀混合物,分析了铝源与碳源的比例对合成氮化铝物相的影响规律,研究表明,在一定的碳铝比范围内生成很纯的氮化铝粉体,比值较小时含有较多的氧化铝相,较大时含有的碳很难排除完全,并且也容易发生氮化铝粉体的氧化,使纯度降低.对铝源与碳源的混合物通过高温氮化还原煅烧处理,分析了煅烧温度与合成物相的关系,随着温度的提高,形成的氮化铝峰明显增强,直至合成纯的氮化铝相.并与氧化铝通过氮化还原法制备氮化铝粉体的煅烧温度进行了比较,明显降低了合成纯氮化铝粉体的煅烧温度.     

溶胶-凝胶法制备氮化铝粉体

先利用溶胶-凝胶法制备氮化铝前驱体,然后采用碳热还原法煅烧得到氮化铝粉体,制备的氮化铝粉体纯度较高,单晶细小,小于1μm。     

sol-gel法制备六方相ZnTiO3粉体的研究

首次采用溶胶-凝胶工艺得到了纯六方相ZnTiO3粉体。以Zn(NO3)2·6H2O和Ti(OC4H9)4为原料,通过溶胶-凝胶法制备了纯六方相ZnTiO3粉体。采用DSC-TG,XRD,FT-IR和Raman等现代测试分析手段,对凝胶粉体的热分解和相转变过程进行了研究。实验结果表明,800℃煅烧处理凝胶粉末可获得纯六方钛铁矿相ZnTiO3粉体;但是,这种六方相ZnTiO3的高温稳定性较差,当煅烧温度超过900℃时,六方相ZnTiO3分解为立方结构Zn2TiO4和金红石TiO2。     

熔盐法制备ZnTiO3粉体的研究

以分析纯ZnO和TiO2为原料,NaCl-KCl为熔盐,采用熔盐法合成了纯相ZnTiO3粉体.研究了煅烧温度,保温时间以及盐与原料的质量比等因素对所制粉体的微观结构的影响.结果表明:当盐与原料质量比为1∶1,800℃煅烧1 h后所得粉体显微形貌较好,晶粒生长充分,呈片状,无明显团聚,尺寸分布均匀.     

前驱体溶液pH值对柠檬酸盐法合成Na_(0.5)Bi_(0.5)TiO_3微粉的影响

采用柠檬酸盐法合成了钙钛矿相的Na0.5Bi0.5TiO3粉体,利用TG-DTA、XRD、SEM及激光粒度仪对Na0.5Bi0.5TiO3粉体进行了分析表征,讨论了前驱体溶液pH值对合成粉体的影响。结果表明,当前驱体溶液pH=8.5,柠檬酸与金属离子摩尔比r(C/Mn+)=1.25,水浴温度为80℃,煅烧温度为600℃时,所制备出的Na0.5Bi0.5TiO3晶体呈球形,其颗粒细小,粒径为100~200 nm。相同条件下,当pH=2.5时产物主要是富含Na、Ti、O的棒状物质。pH=6.5时所得粉体主要是Na0.5Bi0.5TiO3相,粉体颗粒呈球状,粒径为500~600 nm,其中存在少量的块状颗粒,粒径分布不均匀。pH=10.5时产物中含有较多Bi3Ti4O12杂相,粒径较大。     

氮化铝-铝复合封装基板的制备

采用磁控溅射法在阳极氧化预处理过的铝板上沉积氮化铝薄膜,制备氮化铝-铝复合基板。制备的氮化铝为非晶态,抗电强度超过700 V/μm,阳极氧化铝抗电强度达75 V/μm。当阳极氧化铝膜厚约10μm、氮化铝膜约1μm时,制备的复合封装基板击穿电压超过1350 V,绝缘电阻率1.7×106 MΩ·cm,氮化铝与铝板的结合强度超过8 MPa;阳极氧化铝膜作为缓冲层有效缓解了氮化铝与铝热膨胀系数失配的问题,在260℃热冲击下,铝板未发生形变,氮化铝膜未破裂,电学性能无明显变化。氮化铝与阳极氧化膜的可见光高透性保持了镜面抛光金属铝的高反射率,当该复合基板应用于LED芯片COB封装时,有助于提高封装光效。     

Co-Ni-Fe-Cr系红外辐射材料自蔓延燃烧合成与应用

采用溶液自蔓延燃烧合成法及煅烧法制备了Co-Ni-Fe-Cr系红外辐射粉体材料,对前驱体和煅烧样品的晶体结构、微观形貌和红外发射率进行了表征分析。结果表明,自蔓延燃烧得到的燃烧产物呈无定形态,显微结构为多孔薄片状。燃烧产物经800～1 000℃煅烧处理后转变为尖晶石相,随煅烧温度升高晶粒长大并趋近尖晶石相八面体形貌。1 000℃煅烧得到的粉体团聚较少且粒径分布均匀(平均粒径为0.6μm)。获得的Co_0.5Ni_0.5(Fe_0.375Cr_0.625)₂O₄粉体全波段法向红外发射率为0.92,添加质量分数20%的Ca-Mg-Zr-Al-Si玻璃粉配制成丝网印刷浆料,经施釉、干燥和800℃釉烧在氧化铝黑瓷基板表面形成致密釉层,釉层红外发射率达到0.87,材料可用于氧化铝陶瓷基红外加热器的研制。     

BiFeO_3粉体的固相合成及其微观结构研究

采用固相反应法制备了BiFeO3陶瓷粉体,研究了BiFeO3粉体在不同煅烧条件下的相结构与微观形貌的演变。结果表明,过低的煅烧温度和过短的煅烧时间得到的产物以杂相Bi25FeO40为主,提高煅烧温度和延长煅烧时间使杂相逐渐减少,有效地促进BiFeO3相的合成,但过高的煅烧温度和过长的煅烧时间则生成大量杂相Bi2Fe4O9并出现颗粒异常团聚及长大现象,800℃、1h为最佳的煅烧条件。另外,利用稀硝酸可有效清除产物中的杂相,获得较均匀、纯净的BiFeO3粉体,有利于进一步研究和应用。     

静态煅烧法除SiC微粉中碳杂质的工艺研究

由于SiC在电子半导体方面有较大应用,纯度要求就成为主要限制,尤其是碳杂质的影响。本实验对SiC微粉首先经过不同温度的煅烧测定烧失率确定最佳煅烧温度,然后在最佳煅烧温度下通过不同保温时间测定烧失率确定最佳保温时间,对粉体进行DTA-TG测定分析样品质量变化与温度的关系,最后对实验前后的样品进行XRD物相分析,最终得到除碳最佳煅烧温度900℃,最佳保温时间3h。     

氮化铝粉末的制备研究

本文详细综述了国内外氮化铝粉末制备的主要方法；直接氮化法、碳热氮还原法及化学气相淀积法。通过比较不同制备方法得到高频等离子体化学气相淀积是制备氮化铝超细粒子的优良方法。     

Al(H_2PO_4)_3和H_3PO_4改性AlN粉末的研究

采用机械球磨法,以Al(H2PO4)3和H3PO4为改性剂,制备了具有较高抗水解能力的AlN粉末,研究了改性AlN粉末在水基球磨过程中的稳定性。通过XRD,FT-IR,SEM,TG-DSC和氮含量测定对改性前后AlN粉末进行了表征。改性AlN粉末在60℃水中浸泡24h后,其w(N)为32.97%,且其XRD谱中未发现Al(OH)3相,其抗水解能力得到显著提高。改性AlN粉末在水中高速球磨16h后,其w(N)约为32%,AlN悬浮液的pH值约为6,说明改性AlN粉末在水中球磨过程中具有较好的稳定性。     

NH4Cl对机械活化Al粉燃烧合成AlN的控制

添加NH4Cl到经由高能球磨制得的机械活化铝粉中后,铝粉在空气中于室温下即可发生自燃反应.本研究通过含有不同量NH4Cl的机械活化铝粉的自燃制得了Al2O3-AlN疏松粉末,并研究了NH4CL添加量对燃烧产物成分和结构的控制.结果表明:NH4Cl不仅控制了产物的形貌,而且改变了铝粉的氮化初理.在NH4Cl添加量为3%～...     

单晶生长用AlN粉料的烧结提纯工艺实验研究

使用自主研发的钨系统中频感应加热炉对AlN粉料进行了烧结提纯处理实验,并用XRD、SEM、IGA和GDMS等表征方法分析了烧结后的样品.实验发现,高温(2 250℃)长时间(50 h)烧结提纯工艺效果显著,但AlN粉料损耗高达47.37％;而低温(小于2 000℃)分段式短时间(每段10h)烧结提纯工艺粉料损耗低于2％,但是提纯效果一般.通过对实验结果的综合分析,提出了一种AlN粉料烧结提纯的改进工艺,最终得到了氧含量仅238 ppm、碳含量135 ppm的高质量AlN单晶生长原料,并且显著增加了原料的利用率.     

Ammonothermal synthesis of aluminum nitride crystals on group III-nitride templates

Polycrystalline aluminum nitride (AlN) crystals were synthesized using the ammonothermal technique at temperatures between 525°C and 550°C. The growth of AlN was conducted in alkaline conditions with potassium azide (KN₃) as the mineralizer. The growth mechanism was found to be reversegradient soluble, necessitating the placement of the GaN and AlN seeds at a higher temperature than the aluminum metal source. Growth on the GaN seeds varied from 100 to 1500 μm in thickness at a gestation period of 21 days. Additionally, scanning electron micrographs revealed varying microstructure ranging from pointed hexagonal rods, which are approximately 5 μm wide and 20 μm long, to highly densified and contiguous films. Formation of hexagonal AlN was verified using x-ray powder diffraction measurements. Oxygen was detected at 3.7 at.% by inert gas fusion analysis on AlN nucleated on the walls of the autoclave and a qualitative indication of unintentionally incorporated impurities in the AlN grown on the GaN seeds was obtained using energy-dispersive x-ray analysis. Photoluminescence spectroscopy conducted at 20 K revealed a deep-level emission at 3.755 eV due to unintentionally incorporated impurities.     

不锈钢表面溅射氮化铝陶瓷膜工艺参数的研究

工业生产中需要测量机械零件的润滑油膜厚度,利用超声波检测可实现无损检测的目的。利用氮化铝(AlN)陶瓷膜制成的压电换能器对超声波发射和接收。利用射频磁控溅射技术,在不锈钢表面沉积AlN薄膜。利用X线衍射仪(XRD)和原子力显微镜(AFM)等设备对AlN薄膜结构表征,并对结果进行了讨论。     

Preparation of Oriented Aluminum Nitride Thin Films on Polyimide Films and Piezoelectric Response with High Thermal Stability and Flexibility

c‐Axis oriented aluminum nitride (AlN) thin films are successfully prepared on amorphous polyimide films by radiofrequency magnetron reactive sputtering at room temperature. Structural analysis shows that the AlN films have a wurtzite structure and consist of c‐axis oriented columnar grains about 100 nm wide. The full width at half maximum of the X‐ray diffraction rocking curves and piezoelectric coefficient d₃₃ of the AlN films are 8.3° and 0.56 pC N^–1, respectively. The AlN films exhibit a piezoelectric response over a wide temperature range, from –196 to 300 °C, and can measure pressure within a wide range, from pulse waves of hundreds of pascals to 40 MPa. Moreover, the sensitivity of the AlN films increases with the number of times it was folded, suggesting that we can control the sensitivity of the AlN films by changing the geometric form. These results were achieved by a combination of preparing the oriented AlN thin films on polyimide films, and sandwiching the AlN and polymer films between top and bottom electrodes, such as Pt/AlN/polyimide/Pt. They are thin (less than 10 μm), self powered, adaptable to complex contours, and available in a variety of configurations. Although AlN is a piezoelectric ceramic, the AlN films are flexible and excellent in mechanical shock resistance.     

Effect of the Sapphire-Nitridation Level and Nucleation-Layer Enrichment with Aluminum on the Structural Properties of AlN Layers

The effect of atomic aluminum deposited onto sapphire substrates with different nitridation levels on the quality of AlN layers grown by ammonia molecular-beam epitaxy is investigated. The nitridation of sapphire with the formation of ~1 monolayer of AlN is shown to ensure the growth of layers with a smoother surface and better crystal quality than in the case of the formation of a nitrided AlN layer with a thickness of ~2 monolayers. It is demonstrated that the change in the duration of exposure of nitrided substrates to the atomic aluminum flux does not significantly affect the parameters of subsequent AlN layers.     

An integratable dual metal gate CMOS process using an ultrathin aluminum nitride buffer layer

We propose and demonstrate a novel approach for dual metal gate CMOS process integration through the use of a very thin aluminum nitride (AlN/sub x/) buffer layer between metal and gate oxide. This buffer layer prevents the gate oxide from being exposed to a metal etching process which potentially causes oxide thinning and damage. Subsequent annealing consumes the very thin AlN/sub x/ layer and converts it into a new metal alloy film by reacting with gate metals, resulting in no increase in EOT due to this buffer layer. The work function of the original gate metal is also modified as a result of its reaction with AlN/sub x/, making this approach extremely attractive for engineering the work function for dual metal gate CMOS applications.     

几种高强铝合金的激光填粉焊接

采用2500W Nd:YAG激光加工系统,利用填充粉末激光焊接技术进行了几种高强铝合金的焊接;送粉头采取的是一种新型同轴三层结构形式。结果表明,采用He:Ar=4:1左右的混合气作为焊接时的保护气比单纯使用He气和Ar气保护效果好,而试板背面保护气采用He气或Ar气均可。高速摄像显示,采用填充粉末的激光焊接过程比没有填充粉末的稳定,熔池金属表面的波动性小;在优选的焊接工艺规范下,含有AlSi12合金粉末的焊缝没有发现热裂纹。焊接接头的拉伸强度实验显示,采用填充粉末、激光焊接优化工艺参数获得的2219、2024、LF3、6061等铝合金试件断裂都发生在母材一侧;即使焊接性差的7075铝合金,其焊缝正反表面平滑连续、成型良好,无明显外观缺陷。焊缝强度较未填粉时有大幅度提高,达到了母材的78%。     

X-Ray Photoelectron Spectroscopy Characterization of Aluminum Nitride Surface Oxides: Thermal and Hydrothermal Evolution

Oxidized surfaces of aluminum nitride (AlN) epilayers grown on sapphire substrates and of AlN bulk crystals grown by physical vapor transport were studied by x-ray photoelectron spectroscopy (XPS). Analysis of the oxygen core level spectra showed approximately equal contributions from oxygen in two bonding states, which were identified by the binding energies and relative separation of the fitted peaks as OH⁻ and O²⁻. The oxide on air-exposed AlN surfaces was identified as aluminum oxide hydroxide. Systematic annealing experiments were conducted in vacuum to study the thermal evolution of hydroxide layers, and a dehydration mechanism resulting in the formation of Al₂O₃ at high temperature was identified.