同质缓冲层厚度对磁控溅射法制备玻璃基AZO薄膜的结构与光电性能影响

室温下在玻璃基片上用射频磁控溅射法制备了不同厚度的ZnOAl(AZO)缓冲层,并在该同质缓冲层上溅射生长了AZO薄膜.用XRD测试了薄膜结构,用四探针法测量了薄膜方块电阻,用紫外-可见光谱仪测试了薄膜透过率,用双光束红外分光光度计测试了薄膜在中红外范围内的红外反射率.并比较并分析了引入同质缓冲层前后薄膜结构与性能的变化.结果表明,与没有缓冲层的样品相比较,适当厚度的同质缓冲层能降低AZO薄膜中的残余应力,使薄膜晶粒尺寸变大,降低AZO薄膜的方块电阻,使薄膜的紫外截止边发生蓝移,增加薄膜的红外反射率,并不明显影响薄膜的可见光透过率.     

掺钨氧化钒薄膜的制备及研究

采用复合靶磁控溅射法在SiO2玻璃、普通玻璃和Si(100)上沉积氧化钒薄膜,然后对其进行真空退火.分别利用X射线衍射、原子力显微镜、紫外可见光分光光度计和红外光谱仪分析样品的物相、表面形貌和光透过率.结果表明:500 ℃下退火1 h,SiO2玻璃衬底上沉积40 min的薄膜主要物相为VO2和V2O5,退火时间延长到2 h,薄膜主要物相为VO2,薄膜晶粒尺寸均匀,晶粒大小约为100 nm;Si (100)上沉积40 min的薄膜在500 ℃下退火2 h后,物相为低于+4价的钒氧化物;掺钨后薄膜可见光和红外光的透过率都有提高.     

ZL109铝合金表面多弧离子镀TiN薄膜的制备及性能

利用正交设计试验探讨了基体温度、偏压、溅射时间、沉积时间对ZL109表面沉积TiN涂层时,对薄膜显微硬度和膜/基结合力的影响.结果表明,在ZL109表面多弧离子镀制备TiN薄膜的最佳工艺为:基体温度260 ℃、偏压200 V、沉积时间30 min、溅射时间8 min、Ti靶电流80 A、炉内总压1 Pa(Ar和N_2流量比为1∶2).在此工艺下制备的TiN薄膜显微硬度达到1500 HV0.05,膜/基结合力达到36 N,膜厚约2～3 μm.     

磁控溅射温度与时间对ZrN薄膜附着力的影响

采用非平衡磁控溅射技术在1Cr18Ni9Ti不锈钢上制备了ZrN薄膜。用SEM、EDS观察并分析了薄膜的表面形貌和成分,用光电轮廓仪测量了膜层厚度。并采用划格法测试不同溅射时间和温度制备的薄膜附着力大小。分析不同溅射时间和温度对薄膜附着力的影响规律。结果表明,通过调节磁控溅射时间和温度可以得到具有一定厚度,成分稳定,结构致密的ZrN薄膜,且溅射时间在1～20 min范围内时间越长薄膜附着力越大,溅射时间超过20 min,附着力趋于稳定;溅射温度在30～90℃范围内温度越高薄膜附着力越大,超过90℃溅射温度继续升高附着力减小。     

高熵合金AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7扩散阻挡层的制备与性能研究

目的 验证15 nm厚度AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7的势垒层热稳定性和扩散阻挡性能。方法 采用直流磁控溅射技术在n型Si(111)基片上真空溅射沉积15 nm的AlCrTaTiZrRu(3 nm)/(AlCrTaTiZrRu)N0.7 (12 nm)双层阻挡层,随后在双层AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7薄膜的顶部沉积50 nm厚的Cu膜,最终制得Cu/AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7/Si复合薄膜试样。将样品在真空退火炉中分别进行600~900 ℃高温退火30 min,以模拟最恶劣的应用环境。用场发射扫描电镜(FE-SEM)、X射线衍射仪(XRD)、能谱分析仪(EDS)、四探针电阻测试仪(FPP)以及原子力显微镜(AFM)对试样的表面形貌、物相组成、化学成分、方块电阻和粗糙度进行表征分析。结果 沉积态AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7薄膜呈现非晶结构,与Cu膜和Si衬底的结合良好。在800 ℃退火后,Cu/AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7/Si薄膜系统结构完整,膜层结构界面之间未出现分层现象,表面Cu颗粒团聚现象加剧,Si衬底和Cu膜表面未发现Cu-Si化合物生成,薄膜方阻保持在较低的0.070 ?/sq;900 ℃退火后,薄膜系统未出现层间分离和空洞现象,Cu膜表面形成孤立的大颗粒Cu-Si化合物,薄膜电阻率大幅上升。结论AlCrTaTiZrRu/(AlCrTaTiZrRu)N0.7双层结构在800 ℃退火后仍能有效抑制Cu与Si相互扩散,其非晶结构增强了Cu/HEA/HEAN0.7/Si体系的热稳定性和扩散阻挡性。     

Nd-Fe-B薄膜的磁控溅射法制备与组织结构

对直流磁控溅射法制备Nd-Fe-B薄膜工艺进行了研究.在不同的溅射功率、溅射气压、溅射时间等条件下制备薄膜,并对薄膜进行了AFM、XRD分析.结果表明,Nd-Fe-B薄膜的沉积速率、表面形貌及相结构与溅射功率、溅射气压、溅射时间密切相关.薄膜的沉积速率随磁控溅射功率的增加而增加,薄膜表面晶粒尺寸和表面粗糙度随溅射功率增加而增大.沉积速率随溅射气压的升高先增大后减小.低功率溅射时,薄膜中出现α-Fe、Nd2Fe14B相相对较少,随溅射功率增加,α-Fe相消失,Nd2Fe14B相增多.综合考虑各种因素,最佳溅射功率为100～130 W.     

溅射气压对磁控溅射TiN薄膜光学性能的影响

采用直流反应磁控溅射方法在Si(111)基底上沉积了氮化钛薄膜。研究了在溅射沉积过程中,改变腔体气压对所制备的薄膜结构及性能的影响。研究发现:在保持其它工艺参数不变的条件下,沉积的TiN薄膜在不同溅射气压下生成的物相不同,薄膜的主要成分是立方相TiN,薄膜的结晶均显示出明显的TiN(200)择优取向。在腔体气压为0.5 Pa时出现的TiN(200)衍射峰最强、择优取向最明显。随着腔体气压的增加,薄膜厚度变小,而衍射峰则呈减弱的趋势,TiN薄膜的生长可能无择优取向。当腔体气压为0.35 Pa时,膜层致密均匀,没有大尺寸缺陷且粗糙度好,薄膜的结晶度最好,表面也最光滑,在测试波长范围内对光的平均反射率最大,可满足光学薄膜质量方面的要求。     

溅射沉积Cu-Mo薄膜的结构和性能

用磁控溅射法制备含钼2.19%～35.15%(摩尔分数)的Cu-Mo合金薄膜,运用能谱仪(EDX)、X射线衍射仪(XRD)、透射电镜(TEM)、扫描电镜(SEM)、显微硬度仪和电阻计对薄膜成分、结构和性能进行研究.结果表明Mo添加使Cu-Mo薄膜晶粒显著细化,Cu-Mo膜呈纳米晶结构,存在Mo在Cu中的FCCCu(Mo)非平衡亚稳过饱和固溶体;随Mo含量的增加,Mo固溶度逐渐增加,而薄膜微晶体尺寸则逐渐减小,Mo的最大固溶度为30.6%.与纯Cu膜对比表明,Cu-Mo膜的显微硬度和电阻率随Mo含量的上升而持续增加.经200、400和650℃热处理1h后,Cu-Mo膜的显微硬度和电阻率均降低,降幅与热处理温度呈正相关;经650℃退火后,Cu-Mo膜基体相晶粒长大,并出现亚微米-微米级富Cu第二相.在Cu-Mo膜的XRD谱中观察到Mo(110)特征峰,Cu-Mo薄膜结构和性能形成及演变的主要原因是添加Mo引起的晶粒细化效应以及热处理中基体相晶粒的生长.     

磁控溅射氧化钒薄膜的相组成及性能

采用反应磁控溅射法在玻璃基底上沉积氧化钒薄膜,分别利用X射线衍射(XRD)、原子力显微镜(AFM)和红外光谱仪分析样品的物相、表面形貌和红外光透过率。结果表明:氧气体积分数低于15%时,薄膜为低价钒氧化物,高于20%时薄膜为V2O5;氧气体积分数等于15%时,溅射功率由150W增加到200W,薄膜中钒的价态变低;当溅射功率为250W时,薄膜物相变成VO2。随着沉积时间从30min增加到60min,原子力显微分析显示VO2颗粒尺寸从约200nm增加到400nm;红外光透过率范围从55%～65%减小到45%～55%。     

沉积温度对Ge2Sb2Te5溅射薄膜结构、电/光性质的影响

在衬底加热条件下利用磁控溅射法制备Ge2Sb2Te5薄膜,利用X射线衍射仪表征各种沉积温度下薄膜的结构,差示扫描量热法(DSC)确定的薄膜晶化温度为168℃(加热升温速率为5℃/min)。用四探针法测试薄膜的方块电阻,分光光度计测试薄膜的反射率谱,并根据反射率数据讨论在波长为405和650nm时薄膜的反射率对比度同沉积温度关系。结果表明:室温沉积的薄膜为非晶态;在衬底温度为140℃条件下薄膜已完全转变为晶态Ge2Sb2Te5,在300℃时出现少量的六方相;低于140℃时易形成非Ge2Sb2Te5组分的其它晶相,它们对薄膜的电/光性质有很大的影响,可能是导致此类相变光存储薄膜使用过程中反射率对比度下降的原因。     

新型等离子体磁控溅射技术

介绍了等离子体磁控溅射原理和矩形磁控靶,探讨了几种新型等离子体非平衡磁控溅射技术,其中包括脉冲磁控溅射和离子辅助溅射,重点分析了工艺要点,并就存在的问题提出了解决思路.     

CORRELATION BETWEEN CONSTITUENT AND SPUTTERING RATE OF BINARY ALLOYS IN GLOW DISCHARGE LAMP

Investigation was made of the sputtering rate in glow discharge lamp with relaion toconstituent of 25 different specimens of 6 binary systems.namely,Cr-Fe,Bi-Sb,Cu-Zn,Ag-Cu,Al-Zn and Cd-Sn.by measuring mass loss sfter each sputtering under constantAr pressure and voltage applicd.The correlation.in general,between sputtering rate andconcentration of constituent of these non-intermetallic binary alloys obeys the hyperboliclaw under steady state,that may be approximately regarded as linear correlation only oncertain special condition if the two components of the alloys with similar sputte ringrates.     

Comparative study of high-power pulsed sputtering (HPPS) glow plasma techniques using Penning discharge and hollow-cathode discharge

Plasma-ion processing enhances the functionality of films used in various industrial and life-science fields, where high-efficiency metal-plasma sources are indispensable for facilitating this process. In this paper, a new sputtering plasma source is proposed. The plasma source is called high-power pulsed sputtering (HPPS) plasma; more than 10 kW of electric power is easily consumed in the plasma despite its compact size. The characteristics are compared with those of a hollow-cathode discharge (HCD) in the same source configuration. In the case of HPPS plasma generated in a magnetic field, the plasma is confined in the magnetic field and as much as 8 kW of power is consumed. When a set of permanent magnets are removed, the plasma changes from a confined state to an expanded state. Thus, a hollow-cathode discharge plasma is generated. As a result, efficient sputtering of the target material ceases; the consumed power decreases to approximately 20% of that of HPPS plasma, which causes the power density to decrease to 5%. The metallic components observed in the optical emission spectrum are significantly less common in the HCD plasma. In the HPPS plasma, the contributions to the optical emission spectrum from titanium- and argon-related species are significant, while no specified emissions are detected in the HCD plasma. Based on the optical emission spectrum intensity, the activated titanium species are not uniformly distributed at the gap. Some parts of the species are commonly on the outer edge of the target, while the argon species are relatively uniformly distributed in the plasma region.     

磁控溅射中溅射电流对Ti薄膜膜基结合性能的影响

研究在磁控溅射工艺中工作压强和溅射时间恒定的情况下,溅射电流的变化对钛膜与基底Gd结合能力的影响.通过拉伸法测量薄膜与基体间的附着强度,利用扫描电镜观察Ti膜表面形貌.结果表明:溅射电流达到3 A时,Ti膜表面平整,与基体的结合力最强.由此说明,溅射电流的变化对钛膜与基底Gd结合能力的影响较大.     

功率对磁控溅射TbDyFe薄膜磁致伸缩性能的影响

采用直流磁控溅射工艺制备TbDyFe磁致伸缩薄膜，通过考察薄膜成分及其微结构，分析研究了溅射功率对薄膜磁致伸缩性能的影响。结果表明，同一薄膜内部成分相当均一，但不同溅射功率条件下的薄膜成分相异。溅射功率较低，薄膜内部微柱状体结构导致了磁各向异性的产生，磁致伸缩性能下降；溅射功率提高到120W，微柱状体结构消失，薄膜内部趋于均一连续，磁致伸缩性能较好。     

An XPS and ellipsometry study of Cr-O-Al mixed oxides grown by reactive magnetron sputtering

Cr-O-Al thin film mixed oxides grown on Si (100) substrates by reactive magnetron sputtering using different target compositions from 90% Cr (10% Al) to 10% Cr (90% Al) and oxygen fluxes in the range from 0 to 15 sccm have been investigated using ex situ XPS, XPS depth profiles and ARXPS. The chemical information obtained with XPS as well as the observed chemical shift of the Cr 2p, Al 2s and O 1s bands points to the formation of mixed substitutional Me₂O₃ oxides (Me = Al + Cr) instead of the formation of single oxide phases. Compositions and stoichiometries obtained from concentration depth profile measurements (CDP) simultaneously using XPS and Ar⁺ bombardment confirm the formation of such a type of substitutional mixed oxides. ARXPS allows ruling out oxygen preferential sputtering during Ar⁺ bombardment. Finally, it is shown that the optical properties of the films like their refractive index can be controlled through their chemical composition.     

辉光放电灯中二元合金溅射率与化学组成的关系

在恒定气压和电压条件下,用测量溅射减量的方法,系统研究了Cr—Fe,Bi-Sb,Cu—Zn,Ag—Cu,Al-Zn和Cd—Sn六个系统的25个试样在辉光放电灯中溅射率与组分的关系结果表明;阴极溅射在稳态时,二元合金(不形成金属间化合物)的溅射率与组元浓度的普遍关系是双曲线,只有在某些特殊情况下,两组元的溅射率相差不大时,可以近似看成线性关系。     

Modelling of sputtering yield amplification effect in reactive deposition of oxides

Many reactive sputter deposition applications require high deposition rates. The primary limiting parameters in magnetron sputtering are the target power dissipation and sputtering yields of the target elements. In reactive deposition of oxides, the deposition rate is of particular interest due to the low sputtering yield of most commonly used oxides. Traditional high rate techniques rely on a feedback control of the oxygen partial pressure to prevent formation of oxide on the target and hence enable operation in the transition area. An alternative approach, based on target doping, is presented in this paper.By doping the sputtering target with heavy elements, it is possible to substantially enhance the sputtering yield and hence the deposition rate. Simulations of the partial sputtering yield values for aluminium from doped targets sputtered in reactive atmosphere have been carried out. The Monte Carlo based TRIDYN computer code has been used for simulations. The program has been used to find out optimum alloying conditions to obtain maximum partial sputtering yield for deposition of Al₂O₃. Our simulations indicate that the sputtering yield amplification in reactive sputtering may lead to much higher relative deposition rate increase than in a nonreactive case. The highest relative increase may be achieved in the transition region but substantial increase is predicted also in the oxide mode.     

Microstructure control of CrNx films during high power impulse magnetron sputtering

The microstructure and composition of CrN_x (0 ≤ x≤ 1) films grown by reactive high power pulsed magnetron sputtering (HIPIMS or HPPMS) have been studied as a function of the process parameters: N₂-to-Ar discharge gas ratio, (f_N2/Ar), negative substrate bias (V_s), pulsing frequency, and energy per pulse. The film stoichiometry is found to be determined by the composition of the material flux incident upon the substrate during the active phase of the discharge with no nitrogen uptake between the high power pulses. Scanning electron microscopy investigations reveal that for 0 < f_N2/Ar < 0.15 and 150 V bias, a columnar film growth is suppressed in favor of nano-sized grain structure. The phenomenon is ascribed to the high flux of doubly charged Cr ions and appears to be a unique feature of HIPIMS. The microstructure of column-less films for 100 V ≤ V_s ≤ 150 V is dominated by the CrN and hexagonal β-Cr₂N phases and shows a high sensitivity to V_s. As the amplitude of V_s decreases to 40 V and self-biased condition, the film morphology evolves to a dense columnar structure. This is accompanied by an increase in the average surface roughness from 0.25 nm to 2.4 nm. CrN_x samples grown at f_N2/Ar ≥ 0.3 are columnar and show high compressive stress levels ranging from −7.1 GPa at f_N2/Ar = 0.3 to −9.6 GPa at f_N2/Ar = 1. The power-normalized deposition rate decreases with increasing pulse energy, independent of f_N2/Ar. This effect is found to be closely related to the increased ion content in the plasma as determined by optical emission spectroscopy. The HIPIMS deposition rate normalized to DC rate decreases linearly with increasing relative ion content in the plasma, independent of f_N2/Ar and pulsing frequency, in agreement with the so-called target-pathways model. Increasing frequency leads to a finer grain structure and a partial suppression of the columnar growth, which is attributed to the corresponding increase of the time-averaged mean energy of film-forming ions arriving at the substrate.