偏压对反应磁控溅射TiN薄膜结构以及性能的影响

本文采用直流反应磁控溅射技术,以Ar和N2为反应前驱气体制备了TiN功能装饰薄膜.重点研究了衬底负偏压对沉积TiN薄膜的色泽、性能及微结构的影响.采用台阶轮廓仪、X射线衍射仪、EDS能谱仪、纳米压痕仪等分析了薄膜的粗糙度、晶相、组分、纳米硬度以及弹性模量.结果表明,采用适宜的衬底负偏压调控轰击离子能量,能够有效阻止薄膜结构中空位以及缺陷的产生,从而有效避免薄膜表面的紫黑色氧化钛的生成,有利于表面光滑的金黄色TiN薄膜制备,同时使薄膜具备更优异的力学性能.实验结果还表明基体偏压可显著影响TiN薄膜的择优生长取向:随偏压增加,薄膜由(111)晶相择优生长转变为(200)晶相的择优生长,(200)晶相的薄膜比(111)晶相薄膜具有更佳的力学性能.     

偏压方式对金刚石薄膜生长的影响研究

采用脉冲偏压和直流偏压辅助热丝化学气相沉积装置在硅片表面制备了金刚石薄膜,对比研究了两种方式施加的偏压大小对薄膜表面形貌以及质量的影响.利用扫描电子显微镜和拉曼光谱分别表征了薄膜的形貌和质量,采用等离子体光谱诊断分析了薄膜生长过程的气相化学反应.结果表明:两种偏压方式下偏压的大小对薄膜的形貌及品质均有较大影响.相比直流...     

直流热阴极PCVD法掺氮纳米金刚石薄膜形貌及结构的影响

采用直流热阴极等离子体化学气相沉积(PCVD)技术,通过在CH4/H2的混合反应气源中通入不同流量的N2,合成了掺氮纳米金刚石薄膜。结果表明随着氮气流量的增加,金刚石薄膜表面形貌发生明显变化:晶粒细化,晶界和缺陷有所增多,膜层由尺寸较大微晶颗粒转向纳米级菜花状结构,并且薄膜表面粗糙度相应变小。同时薄膜中非金刚石组份相对逐渐增多。氮气的引入可以促进金刚石二次形核,抑制金刚石大颗粒生长,对薄膜的生长取向、形貌及结构都产生一定影响。     

基底负偏压对直流磁控溅射CrN薄膜择优取向及表面形貌的影响

直流磁控溅射法制备不同基底负偏压下的CrN薄膜,采用XRD分析薄膜相结构,EDS分析薄膜表面成分,SEM观察薄膜表面形貌,并对偏压作用机制进行了探讨。结果表明,当Ar流量6ml/min、N2流量30ml/min时,在基底负偏压增大过程中,CrN薄膜始终由CrN相组成,但薄膜生长发生了(111)(-50V)向(200)(-125V)再向无明显择优生长(-225V)的转变。低偏压时,CrN薄膜[111]向[200]取向转变主要是轰击表面氮离子浓度增加导致;高偏压时,薄膜中Ar浓度大幅增长,高能离子长时间轰击破坏晶粒取向性,使薄膜呈无择优取向。同时,负偏压增加使薄膜表面形貌从具有棱角的不规则形状逐渐变为粒状结构,且晶粒逐渐细小。     

基底温度复合控制对化学气相沉积纳米金刚石薄膜的影响

采用自主研制的具有基底温度开-闭环复合自动控制系统的直流弧光放电PCVD设备,当开环流量不同时,在硬质合金基体表面分别进行了纳米金刚石薄膜制备研究。并采用SEM、XRD、激光Raman光谱仪对所制备薄膜的形貌、物相和品质进行了分析。研究结果表明,当开环流量从10→5→15→20mL/min变化时,所制备纳米金刚石薄膜的表面粗糙度及石墨成分会随之增加,金刚石晶粒转变为以(110)面生长为主,且尺寸增大;并加剧了硬质合金基体中Co相粘结剂向基体表面的扩散。温控中基底温度的波动(稳定性)是影响纳米金刚石薄膜生长性能的主要原因。     

原子氢在纳米金刚石薄膜生长中的作用

探索了原子氢在各类制备条件下对纳米金刚石薄膜生长所起的作用,指出贫氢环境并不是纳米金刚石薄膜制备的必备条件,原子氢与Ar在贫氢环境和富氢环境中的作用机理不尽相同.通过施加衬底偏压能促进氢离子的产生,氢离子刻蚀sp²碳的能力比刻蚀sp³碳能力强很多,同时能产生表面缺陷,因而富原子氢环境更有利于纳米金刚石薄膜成核与生长.     

直流负偏压对类金刚石薄膜结构和性能的影响

利用直流-射频-等离子体增强化学气相沉积技术在单晶硅表面制备了类金刚石薄膜，采用原子力显微镜、Raman光谱、X射线光电子能谱、红外光谱、表面轮廓仪和纳米压痕仪考察了直流负偏压对类金刚石薄膜表面形貌、微观结构、沉积速率和硬度等性能的影响。结果表明：无直流负偏压条件下，薄膜呈现有机类聚合结构，具有较低的SP3含量和硬度；叠加上直流负偏压后，薄膜具有典型的类金刚石结构特征，SP3含量和硬度得到了显著的提高；但随着直流负偏压的升高，薄膜的沉积速率和H含量逐渐降低，而SP3含量和硬度在直流负偏压为200V时出现最大值，此后逐渐降低。     

直流脉冲磁控溅射铜膜的结构与性能研究

采用直流脉冲磁控溅射法制备铜膜,利用X射线衍射法分析薄膜相结构,通过扫描电镜观察薄膜形貌,基于纳米压痕载荷-位移曲线计算薄膜的硬度、弹性模量和接触刚度,同时采用显微硬度法测量薄膜硬度,系统研究了溅射功率和偏压对铜膜结构和力学性能的影响。结果表明,通过纳米压痕载荷-位移曲线计算薄膜力学性能是可靠的。随着溅射功率的增大,铜膜生长取向几乎无变化,均呈无择优生长状态,弹性模量、接触刚度基本不变,硬度略有减小;偏压增大会使铜膜呈现明显的(111)取向生长,接触刚度、弹性模量和硬度呈下降趋势。     

沉积参数对化学气相沉积纳米金刚石薄膜的影响

用强电流直流伸展电弧化学气相沉积金刚石薄膜装置,在CH4-Ar和CH4-H2-Ar气氛中沉积了纳米金刚石薄膜,研究了沉积气氛中H2加入量和沉积压力对金刚石薄膜显微组织和生长机制的影响.沉积气氛中H2含量对金刚石薄膜的表面形貌、晶粒尺寸和生长速度有显著影响,随着H2含量增加,金刚石晶粒尺寸增大,薄膜生长速度提高.在1%CH4-Ar气氛中沉积的纳米金刚石薄膜,晶粒尺寸细小,薄膜表面形貌光滑平整.在1%CH4-少量H2-Ar气氛中沉积的金刚石薄膜,晶粒尺寸小于100nm,薄膜表面形貌较平整.随着沉积压力提高,金刚石薄膜的生长速度增大.用激光Ram an对金刚石薄膜进行了表征.     

探索人工干预诱导二次形核技术制备纳米金刚石膜

围绕纳米金刚石膜生长的二次形核理论,利用直流热阴极PCVD技术,在微晶金刚石膜连续生长模式常用的一些生长条件下,通过改变工作气压,改变生长温度,同时采取人工干预间歇生长模式进行金刚石膜生长实验,探索纳米级金刚石膜制备的新途径.实验表明:在金刚石膜生成的过程中,降低工作气压或生长温度,可使等离子体激励能量减弱,导致二次形核基团比例增加,成为人工干预二次形核的内在诱因;通过调节激励电压,使等离子体能量状况改变,有利于二次形核行为的引导,成为人工干预二次形核的外在诱因,在此内外因素共同作用下,可以实现二次形核现象的有效诱导,制备出纳米金刚石膜.人工干预诱导二次形核技术制备纳米金刚石膜的实现,使纳米金刚石膜制作方法得到了扩展,也拓宽了直流热阴极PCVD技术的应用范围.     

On the dependence on bias voltage of the structural evolution of magnetron- sputtered nanocrystalline Cu films during thermal annealing

The nanostructural evolution during heat treatments of DC magnetron-sputtered Cu films deposited at different substrate bias voltages was experimentally studied. A growth chamber equipped with two magnetrons and Kapton windows for in-situ X-ray diffraction was mounted on a six-circle goniometer at a synchrotron beam line. Using Bragg-Brentano X-ray diffraction, the grain size, the texture, and the lattice constant were monitored during thermal annealing. Increasing the substrate bias voltage, the grain growth rate lowered, and the change in texture with time became smaller due to a decrease in the defect concentration. Furthermore, the grain size in the as-deposited films decreased with increasing bias voltage. The activation energy for grain growth was, within experimental errors, the same in all the films.     

The effects of pulse frequency and substrate bias to the mechanical properties of CrN coatings deposited by pulsed DC magnetron sputtering

The chromium nitride coatings have been prepared by the bipolar symmetric pulsed DC magnetron reactive sputtering process at 2 kHz and 20 kHz pulse frequencies, respectively. Different substrate bias was applied with a pulsed DC bias unit with 50 kHz pulse frequency. Oscilloscope traces of the I–V waveforms indicate high power and high current density outputs during the symmetric bipolar pulsed mode. It is concluded that the (200) orientation of CrN films is observed. The grain size decreases with increasing pulse frequency and substrate bias. The substrate bias has a strong influence on the mechanical properties of CrN films. The scratch tests of the CrN coatings show that almost only tiny chipping failure is occurred. Sufficient adhesion strength quality of the coating is also observed. The substrate bias for the deposition of CrN films with sufficient hardness and adhesion properties combination is − 290 V at 20 kHz and − 408 V at 2 kHz pulse frequency, respectively.     

Deposition,structure and hardness of Ti–Cu–N hard films prepared by pulse biased arc ion plating

In this work, Ti–Cu–N hard nanocomposite films were deposited on 304 stainless steel (SS) substrate by using pulse biased arc ion plating system with Ti–Cu alloy target. The effects of negative substrate pulse bias voltages on chemical composition, structure, morphology and mechanical properties were investigated. The composition and structure of these films was found to be dependent on the pulse bias, whereas the pulse biases put little influence on hardness of these films. The XPS spectra of Cu 2p showed that obtained peak values correspond to pure metallic Cu. Cu content in Ti–Cu–N nanocomposite films changed with pulse bias voltage. In addition, X-ray diffraction analysis showed that a pronounced TiN (111) texture is observed under low pulse bias voltage while it changed to TiN (220) orientation under high pulse bias voltage. Surface roughness of the Ti–Cu–N nanocomposite films achieved to the minimum value of 0.11 μm with the negative pulse bias voltage of −600 V. The average grain size of TiN was less than 17 nm. The mechanical properties of Ti–Cu–N hard films investigated by nanoindentation revealed that the hardness was about 22–24 GPa and the hardness enhancement was not obtained.     

Deposition,structure and hardness of Ti–Cu–N hard films prepared by pulse biased arc ion plating

In this work, Ti–Cu–N hard nanocomposite films were deposited on 304 stainless steel (SS) substrate by using pulse biased arc ion plating system with Ti–Cu alloy target. The effects of negative substrate pulse bias voltages on chemical composition, structure, morphology and mechanical properties were investigated. The composition and structure of these films was found to be dependent on the pulse bias, whereas the pulse biases put little influence on hardness of these films. The XPS spectra of Cu 2p showed that obtained peak values correspond to pure metallic Cu. Cu content in Ti–Cu–N nanocomposite films changed with pulse bias voltage. In addition, X-ray diffraction analysis showed that a pronounced TiN (111) texture is observed under low pulse bias voltage while it changed to TiN (220) orientation under high pulse bias voltage. Surface roughness of the Ti–Cu–N nanocomposite films achieved to the minimum value of 0.11 μm with the negative pulse bias voltage of ?600 V. The average grain size of TiN was less than 17 nm. The mechanical properties of Ti–Cu–N hard films investigated by nanoindentation revealed that the hardness was about 22–24 GPa and the hardness enhancement was not obtained.     

偏压对直流磁控溅射Fe-N薄膜结构及性能的影响

为了揭示偏压对溅射态Fe-N薄膜磁学行为的影响规律及机理,采用直流磁控溅射工艺在不同偏压下制备了Fe-N薄膜.利用掠入射X射线衍射、小角X射线散射技术和振动样品磁强计研究了薄膜的相结构、厚度、表面粗糙度以及磁性能.结果表明,增加偏压有利于薄膜中非晶的形成,且随着偏压的增大,薄膜的厚度增加,表面粗糙度降低.Fe-N薄膜的磁性能表明,随着偏压的增加,薄膜的饱和磁化强度和矫顽力均有不同程度的减小.偏压的增加导致Fe-N薄膜由晶态向非晶态转变,从而引起磁性能的改变.     

CVD金刚石薄膜热,导率的研究

研究了直流等离子体喷射沉积金刚石膜的晶粒尺寸、晶粒取向、膜厚、杂质和缺陷对金刚石膜的热导率的影响。结果表明，随着晶粒尺寸的增大，金刚石膜的热导率先慢后快逐渐增大；随着膜的增厚，热导率先大幅度提高，达到一定值后，变化率变小；晶粒（111）取向对金刚石膜的热导率最有利，其次是（110）；非金刚石碳相和缺陷都降低膜的热导率，但晶间空隙对热导率的影响比非金刚石碳相大。     

金刚石膜内晶粒尺寸和取向对其热导率的影响

研究了金刚石膜内晶粒尺寸和取向程度对金刚石膜热导率的影响。通过对衬底表面进行不同研磨时间的处理和适当的工艺条件，采用灯丝热解化学气相沉积（ＨＦＣＶＤ）的方法在单晶硅衬底上形成了具有不同晶粒尺寸和不同程度（１００）晶面取向的金刚石膜，并研究了其热导率。结果表明，由大晶粒和较高程度（１００）晶面取向的晶粒构成的金刚石膜具有热导率特性。     

大面积高质量金刚石自支撑膜热导率的影响因素研究

通过Raman、XRD、SEM分析方法分别对大面积高质量金刚石自支撑膜的质量、晶体结构、晶粒尺寸进行研究,分析它们对金刚石自支撑膜热导率的影响.研究结果表明,金刚石自支撑膜的质量对热导率的影响较大,质量越好,热导率越接近于天然金刚石的热导率;并且金刚石自支撑膜中晶体[220]取向度越高,热导率越高.形核面晶粒尺寸越大,晶粒间的晶界就减少,有利于提高金刚石自支撑膜的热导率.     

正偏压对纳米金刚石薄膜结构和电阻率的影响

采用电子辅助热丝化学气相沉积工艺, 在1kPa反应气压和施加不同的偏流条件下, 沉积了纳米金刚石薄膜. 用X射线衍射, 场发射扫描电镜和半导体特性表征系统对该薄膜进行了表征和分析. 结果表明, 施加偏流可以使薄膜晶粒呈现明显的(110)晶面择优取向, 表面形貌发生较大变化. 当偏流为8A时, 薄膜晶粒达到最小值, 约为20nm, 薄膜表面也最光滑. 本文讨论了在低气压和电子轰击条件下(110)晶面择优取向的形成机制及其对薄膜显微形貌和电阻率的影响关系.