脉冲激光沉积制备TiN/AlN多层薄膜的研究

采用脉冲激光沉积(PLA)法,在单晶Si试样表面沉积制备了一系列TiN/AlN硬质多层膜,并采用基于免疫算法的免疫径向基函数(IRBF)神经网络对AlN厚度建立预测模型,设计出具有可控调制周期和调制比的TiN/AlN多层膜。X射线衍射(XRD)结果表明,小调制层周期下,过高或过低的工艺条件下薄膜通常为非晶态,适当的工艺条件下TiN、AlN形成具有强烈织构的超晶格柱状晶多层膜;与此相应,纳米多层膜产生了硬度和弹性模量异常增高;随着调制比增加,使纳米多层膜形成非晶AlN层和纳米晶TiN层的多层结构,多层膜的硬度和弹性模量逐渐下降。XPS结果表明,薄膜界面由Ti+4、Ti+3离子组成,N的负二价、三价亚谱结构预示着非当量TiN、AlN的形成。AFM研究显示,薄膜的调制周期均在10~200 nm范围内,且薄膜表面较均匀;当多层薄膜调制周期在50 nm以下时,薄膜的纳米硬度值明显高于TiN和AlN的混合硬度值,达30 Gpa。     

脉冲偏压对TiAlN/TiN多层膜生长及熔滴的影响

针对直流脉冲负偏压对PVD涂层形成过程和熔滴造成很大影响的问题,通过施加脉冲偏压有利于实现低温沉积.研究发现,沉积速率随直流脉冲负偏压峰值的提高先升高后降低,在-300V偏压时沉积速率最大;熔滴密度和直径随脉冲负偏压峰值的提高递减;随偏压升高,加大了元素溅射产额的差异,使涂层中铝元素和钛元素的含量发生变化.     

脉冲激光沉积AlN薄膜的工艺优化与机械性能

采用脉冲激光沉积(PLD)方法在单晶Si衬底上制备AlN薄膜.利用扫描电子显微镜(SEM)、X射线衍射仪(XRD)对薄膜的形貌和微观结构进行了分析;采用显微硬度仪、球-盘式磨损试验机和涂层自动划痕仪测试了薄膜的机械性能.通过正交实验,分析了工艺参数与AlN薄膜硬度之间的关系,得出沉积气压是对薄膜硬度影响大的因素,并研究了沉积气压对AlN薄膜表面形貌、微观结构、沉积速率、硬度、结合力和摩擦性能的影响.实验结果表明:所制备的薄膜均为非晶结构,随着沉积气压的上升,薄膜沉积速率降低,薄膜表面粗糙度降低,摩擦系数变小,当气压由0.1Pa增加到1Pa时,薄膜的硬度和耐磨性提高,但是随着气压进一步增大,其硬度和耐磨性下降.     

CrAlN/TiAlN 纳米多层膜的微结构及其性能研究

采用磁控反应溅射法制备了不同调制周期的CrAlN/TiAlN纳米多层膜,并通过X射线衍射仪 、显微硬度计、扫描电镜分析了调制周期对多层膜的微结构、力学性能和高温抗氧化性能的影响。结果表明：CrAlN/TiAlN纳米多层膜共格外延生长,呈现CrAlN（或TiAlN）面心立方结构,且呈（111）择优取向;CrAlN/TiAlN纳米多层膜在某些调制周期出现硬度异常升高的超硬度效应;CrAlN/TiAlN纳米多层膜比CrAlN, TiAlN单层膜具有更好的高温稳定性,高温时仍具有较高的硬度。     

铜合金表面Ti/TiN多层膜的制备、结构及其性能

为了研究多层膜的腐蚀性能,促进多层膜在生产中的应用,采用电弧离子镀技术,通过调整环境N₂和Ar气的时间比例在铜衬底上成功制备了不同调制周期的Ti/TiN多层膜.利用x 射线衍射谱和交流阻抗谱研究了该多层膜的结构和腐蚀性能.表面形貌显示,沉积的Ti/TiN多层膜具有明显的周期性,环境中N2和Ar气的时间比例决定了多层膜的调制周期,N₂气时间越长,多层膜中TiN相层越厚.腐蚀性能测定表明,多层膜的调制周期影响其耐蚀性,当调制周期为550nm时,沉积膜的耐腐蚀性最好.     

AIB用于改进PLD沉积在机械瓣膜上的类金刚石膜的质量

用脉冲激光沉积(PLD)法在热解C制作的人工心脏机械瓣膜上沉积类金刚石(DLC)薄膜,并用3KeV的氩离子轰击(AIB)DLC薄膜。采用拉曼(Raman)光谱和X射线光电子能谱(XPS)分别对AIB前后的DLC薄膜进行检测分析,用光学显微镜观察AIB前后的DLC薄膜表面。实验结果表明:AIB不影响薄膜的黏附性。但是可以在一定程度上导致薄膜微观结构的变化和sp3/sp2比值的提高,可以在薄膜中掺杂微量的Ar元素,可以有效消除薄膜表面吸附的O,但对薄膜中C-O、C=O和COOH的影响较小。因此,离子轰击法可以作为一种改进类金刚石薄膜质量的方法。     

活塞环表面Cr/CrN纳米多层膜的微观结构

为改善发动机活塞环的摩擦学性能,提高其使用寿命,采用多弧离子镀技术在活塞环表面制备了Cr/CrN纳米多层膜.采用x 射线衍射（XRD）、透射电子显微镜（TEM）、俄歇能谱仪（AES）、纳米硬度仪和CETR摩擦磨损试验机,系统分析了不同调制周期Cr/CrN纳米多层膜的微观结构、成分分布、纳米硬度和抗滑动磨损性能.结果表明：Cr/CrN多层膜由CrN、Cr2N和Cr相组成,在CrN（200）方向上出现择优取向.随调制周期的减小,多层膜的硬度和残余应力增大,当调制周期为80nm时,多层膜的硬度值最高达到21.5GPa;当调制周期为120nm时,H³/E²值达到最高,此时划痕临界载荷值最高.根据摩擦磨损试验结果可知,与电镀Cr和CrN涂层相比,Cr/CrN多层膜具有相对较好的抗滑动磨损性能,其磨损机制主要以磨粒磨损为主,有可能替代原活塞环Cr电镀层.     

CrAIN／TiAIN纳米多层膜的微结构及其性能研究

采用磁控反应溅射法制备了不同调制周期的CrAIN／TiAIN纳米多层膜,并通过x射线衍射仪、显微硬度计、扫描电镜分析了调制周期对多层膜的微结构、力学性能和高温抗氧化性能的影响。结果表明：CrAIN／TiAIN纳米多层膜共格外延生长,呈现CrAIN（或TiAIN）面心立方结构,且呈（111）择优取向;CrAIN／TiAIN纳米多层膜在某些调制周期出现硬度异常升高的超硬度效应;CrAIN／TiAIN纳米多层膜比CrAIN,TiAIN单层膜具有更好的高温稳定性,高温时仍具有较高的硬度。     

多层喷射沉积过共晶Al—Si—Cu—Mg合金的微观组织及力学性能

多层喷射沉积技术具有冷速快、工艺简单、氧化程度低、制备的材料组织细小且分布均匀等特点。而使高硅铝合金充分发挥实用价值的关键蚴化初晶硅。作者用多层喷射沉积技术制备了过共晶Ａｌ－Ｓｉ－Ｃｕ－Ｍｇ合金,并与传统的铸态冶金制备的相同化学成分的合金进行了比较。对合金的沉积坯、热挤压处理后的微观组织进行了观察与分析。结果表明,多层喷射沉积合金的初晶硅大小只有２５μｍ左右。并对合金的拉伸性能、扫描断口进行了测试     

磁控溅射AI／Pb纳米多层膜调制结构研究

用磁控交替沉积制备Al／Pb纳米多层膜,运用XPS,AFM,TEM考察表面状况及膜结构．结果表明,实验条件下,当Al层厚60nm时,Pb子层标定厚度从20nm增至30nm,可形成较完整埋层调制结构．随Pb层厚度增加,连续性变好、表面糙度降低,Al层对Pb层表面糙度克服能力提高,改善层状结构完整性．多层膜中Al,Pb子层均存在（111）择优取向特征,由fcc结构的表面自由能最小化引起．     

脉冲激光沉积CN_x薄膜的微观组织结构表征

利用脉冲激光烧蚀CNx靶,在室温至450℃基片温度时沉积CNx薄膜.利用扫描电镜(SEM)、X射线衍射(XRD)、X射线光电子谱(XPS)和拉曼光谱(Raman)等对CNx薄膜的表面形貌、化学成分、结晶性以及价键状态进行了分析.结果表明:所得CNx薄膜呈非晶状态,表面形貌与沉积温度密切相关,基片温度高于150℃时薄膜表面较为光滑.随着基片温度的增加,薄膜中C—N键的面积分数从31.2%逐渐减少至14.1%,N—sp3C和N—sp2C键的面积分数随之减少,300℃时最利于形成sp3键.Raman光谱中比值ID/IG总体呈上升趋势,G峰的位置向高波数(高频)方向移动且半高宽(FWHM)下降,薄膜由CNx薄膜的无序结构逐渐向高有序化程度类石墨结构转变,石墨化程度增加.     

Investigations of ZnO thin films deposited by a reactive pulsed laser ablation

Highly transparent ZnO thin films were deposited at different substrate temperatures by pulsed laser deposition in an oxygen atmosphere. The thin films were characterized by various techniques including X-ray diffraction, scanning electron microscopy, optical absorption, and photoluminescence. We demonstrated that oriented wurtzite ZnO thin films could be deposited at room temperature using a high purity zinc target. Variable temperature photoluminescence revealed new characteristics in the band edge emission. The underlying mechanism for the observed phenomena was also discussed.     

电弧离子镀TiN/TiAlN复合涂层摩擦磨损性能研究

利用阴极电弧离子镀技术,在硬质合金基体上制得5层和20层TiN/TiAlN复合涂层.研究表明,这两种涂层均为典型的B1-NaCl面心立方结构,且均呈(200)择优取向.两种涂层表面光滑平整,粗糙度分别为0.32和0.11,硬度为1 470HV和2 000HV .20层复合涂层的摩擦系数和比磨损率低于5层,表明增加复合层数有利于提高涂层的耐磨损性能,涂层的磨损机理为磨粒磨损.     

Property improvement of multilayer TiN/Ti films with C+ implantation

Using the MEVVA ion source, carbon ions have been implanted in TiN coatings deposited by multiarc ion plating. The Vickers microhardness of the C⁺-implanted TiN films increased with the increase in the ion flux and dose. X-ray diffraction (XRD) analysis showed that the TiC phases had been formed in the films. In addition, the films had the preferred growth orientations of TiN and TiC, both of which were (111) orientation after annealing at 500°C for 30 min. Auger electron spectra analysis indicated that C⁺-implanted profile was in typical Gaussian-like distribution in single films. The distribution with multipeaks of C atoms was obtained in multi-layer TiN/Ti. The possibility of the multilayer films (Ti(C,N)/TiN/Ti(C,N)/TiN and Ti(C,N)/TiC/Ti(C,N)/TiC) forming using the C-implanted TiN/Ti films is presented for the first time. Project supported by the National Natural Science Foundation of China and the “863” Hi-Tech Program of China.     

Property improvement of multilayer TiN/Ti films with C~+ implantation

Using the MEVVA ion source, carbon ions have been implanted in TiN coatings deposited by multi-arc ion plating The Vickers microhardness of the C+ -implanted TiN films increased with the increase in the ion flux and dose. X-ray diffraction (XRD) analysis showed that the TiC phases had been formed in the films. In addition, the films had the preferred growth orientations of TiN and TiC, both of which were (111) orientation after annealing at 500℃ for 30 min. Auger electron spectra analysis indicated that C+ -implanted profile was in typical Gaussian-like distribution in single films. The distribution with multipeaks of C atoms was obtained in multi-layer TiN/Ti. The possibility of the multilayer films (Ti (C, N)/TiN/Ti(C, N)/TiN and Ti(C, N)/TiC/Ti(C, N)/TiC) forming using the C-implanted TiN/Ti films is presented for the first time.     

Preparation and Properties of IrO2 Thin Films Grown by Pulsed Laser Deposition Technique

Highly conductive IrO2 thin films were prepared on Si （100） substrates by means of pulsed laser deposition technique from an iridium metal target in an oxygen ambient atmosphere. Emphasis was put on the effect of oxygen pressure and substrate temperature on the structure, morphology and resistivity of IrO2 films. It was found that the above properties were strongly dependent on the oxygen pressure and substrate temperature. At 20 Pa oxygen ambient pressure, pure polycrystalline IrO2 thin films were obtained at substrate temperature in the 300-500℃ range with the preferential growth orientation of IrO2 films changed with the substrate temperature. IrO2 films exhibited a uniform and densely packed granular morphology with an average feature size increasing with the substrate temperature. The room-temperature resistivity variations of IrO2 films correlated well with the corresponding film morphology changes. IrO2 films with the minimum resistivity of （42 ±6）μΩ·cm was obtained at 500℃.     

块体Ti_2AlN/TiN复合材料的制备

在合成Ti2Al N配比的基础上原位引入15%体积含量的Ti N,在原位热压(HP)和放电等离子(SPS)两种烧结工艺条件下合成了块体Ti2Al N/Ti N复合材料。通过X射线衍射(XRD)分析烧结产物的相组成,用扫描电镜(SEM)和电子探针(EPMA)结合能谱仪(EDS)研究材料的显微结构特征。原位热压工艺合成Ti2Al N/Ti N复合材料的最佳温度为1 300℃,烧结试样的密度为4.30 g/cm3,达到理论密度的96.2%;放电等离子烧结工艺合成Ti2Al N/Ti N复合材料的最佳温度为1 200℃,烧结试样的密度为4.23 g/cm3,达到理论密度的94.7%。Ti2Al N和Ti N相均有团聚现象,Ti2Al N为片状形貌,晶粒发育完善,具有明显的层状结构特征;Ti N为尺寸1～2μm的四方小颗粒。     

激光能量对掺铒纳米Si晶薄膜形貌的影响

采用XeCl脉冲准分子激光器,保持激光脉冲比为1:2,分时烧蚀Er靶和高阻抗单晶Si靶。改变激光能量,在真空中沉积了掺Er非晶Si薄膜。在氮气保护下,分别在950℃,1010℃和1100℃温度下进行30min热退火处理,得到掺Er纳米晶Si薄膜。扫描电子显微镜的结果表明,高的退火温度或高的激光能量均会导致迷津结构的形成。