氮气流量对磁控溅射制备类金刚石薄膜性能的影响

采用磁控溅射法以石墨为靶材在玻璃衬底上沉积了类金刚石(DLC)薄膜,用原子力显微镜表征了不同氮气流量条件下生长薄膜的形貌,用拉曼光谱仪、X射线光电子能谱仪和分光光度计分析了样品的微结构、元素的价态和透光性能.结果表明:沉积的薄膜均为非晶结构.通入2sccm氮气时,薄膜的光学透过率大大提高,此时DLC薄膜内的氮元素含量为5.88%,sp3键百分比为64.65%,ID/IG值为1.81;掺氮DLC薄膜在可见光范围内光学透过率达到95.69%.随着氮气流量增加,DLC薄膜光学透过率呈现出下降的趋势.退火2h后不掺氮DLC薄膜光学透过率呈小幅度下降,而掺氮DLC薄膜的光学透过率几乎没有变化.     

热退火对等离子体增强化学气相沉积SiCOH薄膜结构与性能的影响

热退火是多孔低介电常数薄膜制备过程中的重要一环, 对薄膜结构及性能具有重要影响. 本文以四乙氧基硅烷和双戊烯为前驱体, 采用等离子体增强化学气相沉积方法制备了SiCOH薄膜, 对其进行了氮气氛围下的热退火处理, 分析了热退火对薄膜结构与性能的影响, 探究了退火过程中薄膜结构变化的可能的反应机理. 傅里叶变换红外光谱和固体核磁共振谱结果表明, 沉积薄膜是一种有机无机杂化薄膜. 退火过程中, 薄膜中的-CH₂, -CH₃等有机组分被分解除去, 形成了以稳定的Si-O-Si等无机组分为骨架的多孔结构, 并通过氮气吸附/脱附等温线测试得到了验证. 在此期间, 薄膜骨架微结构亦发生一系列调整, C=C, Si-C含量增加, Si、O、C等元素间发生进一步键合. C=C 含量的提高, 使得薄膜的消光系数和漏电流密度增大. 实验证明, 退火后薄膜具有低折射率、低介电常数特性, 是一类具有优异的介电性能和力学性能的材料, 作为芯片后端互连层间介质具有极大的应用潜力.     

镶嵌有纳米硅的氮化硅薄膜键合特性分析

采用螺旋波等离子体化学气相沉积(HWPCVD)技术制备了非化学计量比的氢化氮化硅薄膜,对所沉积样品及氮气环境中920 ℃退火样品的微观结构及键合特性进行了分析。Raman散射结果表明,薄膜中过量硅以非晶纳米粒子形式存在,退火样品呈现纳米晶硅和氮化硅的镶嵌结构。红外吸收和可见光吸收特性比较结果显示,薄膜样品的微观结构依赖于化学计量比以及退火过程,硅含量较低样品因高的键合氢含量而表现出低的纳米硅表面缺陷态密度;退火过程将引起Si—H和N—H键合密度的减少,因晶态纳米颗粒的形成,退火样品表现出更高的结构无序度。     

对基于磁控溅射方法沉积的HfO_2薄膜的紫外光学特性及薄膜结构的研究（英文）

本文基于磁控溅射方法,功率从160 W增加到240 W,在石英衬底上沉积氧化铪薄膜(HfO_2),并对沉积后的薄膜进行退火处理.利用X射线衍射谱、X射线光电子能谱、紫外-可见-近红外透射谱和椭圆偏振仪对Hf02薄膜进行研究,对比了退火前后Hf02薄膜的光学特性及薄膜结构的变化.实验结果显示,HfO_2薄膜对波长大于200 nm的入射光具有很低的吸收系数.优化退火温度和时间,可以将沉积后的Hf02薄膜从非晶态转化成多晶态.退火有助于结晶生成和内应力的增加,同时退火可以优化薄膜的化学计量比,提升薄膜的光学密度及折射率.对功率在220 W左右沉积的薄膜进行退火,获得的Hf02薄膜具有较高并且稳定的光学折射率(2)和紫外光透射率,可在紫外波段减反膜系统中得到应用.     

钙钛矿薄膜的微结构和光电特性优化

分别以纯二甲基甲酰胺、纯二甲基亚砜以及二者不同比例的混合物作为前驱体溶剂,制备钙钛矿薄膜样品.将薄膜样品分为两组,分别将其置于氮气氛围中进行热退火和二甲基亚砜蒸汽氛围中进行溶剂退火,并对薄膜样品的微观结构和光电特性进行系统研究分析.结果表明,与热退火相比,经溶剂退火后样品的平均晶粒尺寸和均匀性显著提升,从而减小了薄膜中晶粒边界或界面的体积分数.采用混合前驱体溶剂和后续溶剂退火增加了薄膜的厚度和可见光的利用率,有效改善了薄膜形貌,优化了结晶质量.同时薄膜光致发光强度的增加,表明薄膜缺陷态密度降低.采用优化后的钙钛矿薄膜作为吸收层制备太阳电池,其光电转换效率达到15.7%.     

O2流量对磁控溅射N掺杂TiO2薄膜成分及晶体结构的影响

利用直流脉冲磁控溅射方法在室温下通过改变O₂流量制备具有不同晶体结构的N掺杂TiO₂薄膜,利用台阶仪、X射线光电子能谱仪、X射线衍射仪、紫外-可见分光光度计等设备对薄膜沉积速率、化学成分、晶体结构、禁带宽度等进行分析.结果表明:所制备的薄膜元素配比约为TiO_1.68±0.06N_0.11±0.01,N为替位掺杂,所有样品退火前后均未形成Ti—N相结构,N掺杂TiO₂薄膜的沉积速率、晶体结构等主要依赖于O₂流量.在O₂流量为2 sccm时,N掺杂TiO₂薄膜沉积速率相对较高,薄膜为非晶态结构,但薄膜内含有锐钛矿(anatase)和金红石(rutile)相晶核,退火后薄膜呈anatase和rutile相混合结构,禁带宽度仅为2.86 eV.随着O₂流量的增加,薄膜沉积速率单调下降,退火后样品禁带宽度逐渐增加.当O₂流量为12 sccm时,薄膜为anatase相择优生长,退火后呈anatase相结构,禁带宽度为3.2 eV.综合本实验的分析结果,要在室温条件下制备晶态N掺杂TiO₂薄膜,需在高O₂流量(＞10 sccn)条件下制备. 关键词： 2薄膜')" href="#">N掺杂TiO₂薄膜 磁控溅射 化学配比 晶体结构     

NiFe2O4外延薄膜的制备及后退火效应研究

本文利用脉冲激光沉积方法制备了NiFe2O4磁性绝缘薄膜.X-射线衍射线性扫描测量表明,在MgO(110)单晶衬底上可以生长出高质量的NiFe2O4外延薄膜,原子力显微镜显示其具有平整的表面形貌.我们还研究了后退火处理对样品结构、表面形貌和磁性的影响.结果表明,后退火后薄膜的结构和表面形貌都发生了明显的改变,样品的磁性得到增强.这些效应可归结为在氧气氛下退火处理导致的氧含量的变化以及退火过程中阳离子分布和价态发生改变.     

热致晶化高反射率SbOx薄膜的结构分析和光学性质

利用直流磁控反应溅射法制备了SbOx薄膜,利用X射线衍射分析仪和光谱仪分别研究了这种薄膜热致晶化的微观结构和光学性质的变化,并通过非晶态薄膜粉末的示差扫描量热实验测出不同加热速度条件下结晶峰温度,研究了这种薄膜的结晶动力学。发现沉积态SbOx薄膜为非晶态,非晶态SbOx薄膜在热致晶化过程中发生了两种变化,分别对应为较低温度下Sb晶体和较高温度下立方Sb2O3相的生成。退火后晶态薄膜中出现了单质Sb和Sb2O3,300℃退火后Sb2O3相含量最大。晶态薄膜的反射率均高于沉积态,在晶态薄膜中200℃退火的薄膜反射率最大。     

Ag/Fe/Ag 纳米颗粒膜磁特性和微结构

"利用对靶磁控溅射法制备了一系列Ag/Fe/Ag纳米薄膜,沉积态样品Fe层厚度固定为35 nm,Ag层厚度为1、2、3、4、5 nm．随后对沉积态样品进行了退火处理,退火温度分别为200、300、400、500、600 ℃ , 退火30 min． 利用VSM测量了样品的磁特性, 利用SPM观察样品表面形貌和磁畴结构,并且利用XRD分析了样品的晶体结构．研究结果表明,沉积态样品随Ag层厚度的变化,垂直和平行膜面矫顽力均先增加后减小．当Ag层厚度为3 nm时,垂直膜面矫顽力最大约为260 Oe,样品颗粒分布均     

Ti-B-C-N纳米复合薄膜结构及力学性能研究

利用反应磁控溅射方法在单晶硅和高速钢(W18Cr4V)基片上制备出不同C含量Ti-B-C-N纳米复合薄膜. 使用X射线衍射和高分辨透射电子显微镜研究了Ti-B-C-N纳米复合薄膜的组织和微观结构,用纳米压痕仪测试了它们的硬度和弹性模量. 结果表明,利用往真空室通入C₂H₂气体的方法制备得到的Ti-B-C-N纳米复合薄膜中,在所研究成分范围内只发现TiN基的纳米晶. 当C₂H₂流量较小时,C元素的加入可以促进Ti-B-C 关键词： Ti-B-C-N薄膜 磁控溅射 微观结构 力学性能     

Microstructure and Mechanical Properties of Multilayer α-AlN/α-BCN Coating as Functions of the Current Density during Sputtering of a B<Subscript>4</Subscript>C Target

Multilayer AlN/BCN coating of nanometer scale have been prepared by magnetron sputtering of Al and B₄C targets in an argon–nitrogen atmosphere during deposition on a Si substrate. These coating have an X-ray amorphous structure and the maximum Knoop hardness of 27 GPa (at the current density 100 mA). The first-principle molecular dynamics calculations show that the B4–BN layer is dynamically unstable; thus, it will not be epitaxial and will be amorphous or have a structure different from the B4–BN structure. The thermal vacuum annealing from 600 to 800°C of samples with multilayer nanosized coating leads to the decrease in the Knoop hardness to 18 GPa; however, the coating structure is retained X-ray amorphous.     

The effects of Si3N4 interlayer on the thermal stability and hardness of Ti/TiNx (x = 0.5-1) nanolayered coatings

The polycrystalline Ti/TiN_x multilayer films were deposited by magnetron sputtering, and the as-deposited multilayer coatings were annealed at 500-800 °C for 2-4 h in vacuum. We investigated the effects of annealing temperature and annealing time on the microstructural, interfacial, and mechanical properties of the polycrystalline Ti/TiN_x multilayer films. It was found that the hardness increased with annealing temperature. This hardness enhancement was probably caused by the preferred crystalline orientation TiN(1 1 1). The X-ray reflectivity measurements showed that the layer structure of the coatings could be maintained after annealing at 500 °C and the addition of the Si₃N₄ interlayer to Ti/TiN_x multilayer could improve the thermal stability to 800 °C.     

Influence of high temperature annealing on the structure, hardness and tribological properties of diamond-like carbon and TiAlSiCN nanocomposite coatings

Diamond-like carbon (DLC) and TiAlSiCN nanocomposite coatings were synthesized and annealed at different temperatures in a vacuum environment. The microstructure, hardness and tribological properties of as-deposited and annealed DLC-TiAlSiCN nanocomposite coatings were characterized by X-ray diffraction, X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), Raman spectroscopy, nano-indentation and friction tests. The TEM results reveal that the as-deposited DLC-TiAlSiCN coating has a unique nanocomposite structure consisting of TiCN nanocrystals embedded in an amorphous matrix consisting of a-Si₃N₄, a-SiC, a-CN and DLC, and the structure changed little after annealing at 800 °C. However, XPS and Raman results show that an obvious graphitization of the DLC phase occurred during the annealing process and it worsened with annealing temperature. Because of the graphitization, the hardness of the DLC-TiAlSiCN coating after annealing at 800 °C decreased from 45 to 36 GPa. In addition, the DLC-TiAlSiCN coating after annealing at 800 °C has a similar friction coefficient to the as-deposited coating.     

溅射压强对TiN/SiNx纳米多层膜微观结构及力学性能的影响

利用磁控溅射方法在不同溅射压强条件下制备了TiN/SiN_x纳米多层膜.多层膜的微观结构及力学性能分别用X射线衍射仪、原子力显微镜及纳米压痕仪来表征.结果表明随着溅射压强的增大,多层膜的界面变模糊,TiN层的择优取向由(200)晶面过渡到(111)晶面.与此同时,多层膜的表面粗糙度增大,硬度和弹性模量随溅射压强的增大而减小.多层膜力学性能的差异主要是由于薄膜的周期性结构及致密度存在差异所致. 关键词： x多层膜')" href="#">TiN/SiN_x多层膜 界面宽度 表面形貌     

Tribological characterization of chromium nitride coating deposited by filtered cathodic vacuum arc

CrN coatings were prepared by filtered cathodic vacuum arc (FCVA) technique. The influence of the deposition parameters (nitrogen partial pressure PN₂, substrate bias voltage V_s and preheating of the substrate) on the structural, mechanical and tribological properties of the FCVA CrN coatings was investigated. Further, the FCVA CrN coating was compared in dry reciprocating sliding with commercial multi-arc ion plating (MAIP) CrN coating as to friction and wear properties. Profilometer, scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDX) were used to evaluate the wear scars and the wear mechanisms were discussed. The results showed that the structural, mechanical and tribological properties of the FCVA CrN coatings were significantly dependent on the deposition parameters. The FCVA CrN coating deposited with PN₂ of 0.1 Pa, V_s of −100 V and without preheating exhibited the optimal mechanical and tribological properties. The FCVA CrN coating exhibited much better anti-abrasive and anti-spalling properties than the MAIP CrN coating, which was resulted from significant reduction of macroparticles and pitting defects by the FCVA technique. The MAIP CrN coating suffered severe concentrated wear by a combination wear mechanisms of delamination, abrasive and oxidative wear when high normal load was applied, while for the FCVA CrN coating the wear mechanisms were ultra-mild abrasive and oxidative wear.     

退火对Ge诱导晶化多晶Si薄膜结晶特性的影响

本文采用磁控溅射法, 衬底温度500 ℃下在硅衬底上分别制备具有Ge填埋层的a-Si/Ge 薄膜和a-Si薄膜, 并进行后续退火, 采用Raman光谱、X射线衍射、原子力显微镜及场发射扫描电镜等对所制薄膜样品进行结构表征. 结果表明, Ge有诱导非晶硅晶化的作用, 并得出以下重要结论: 衬底温度为500 ℃时生长的a-Si/Ge薄膜, 经600 ℃退火5 h Ge诱导非晶硅薄膜的晶化率为44%, 在相同的退火时间下退火温度提高到700 ℃, 晶化率达54%. 相同条件下, 无Ge填埋层的a-Si薄膜经800 ℃退火5 h薄膜实现晶化, 晶化率为46%. 通过Ge填埋层诱导晶化可使在相同的条件下生长的非晶硅晶薄膜的晶化温度降低约200 ℃. Ge诱导晶化多晶Si薄膜在Si(200)方向具有高度择优取向, 且在此方向对应的晶粒尺寸约为76 nm. 通过Ge诱导晶化制备多晶Si薄膜有望成为制备高质量多晶Si薄膜的一条有效途径.     

Microstructure, microhardness and dry friction behavior of cold-sprayed tin bronze coatings

In this paper, two types of tin bronze coatings (Cu-6 wt.% Sn and Cu-8 wt.% Sn) were prepared by cold spray process. The as-sprayed coatings were subjected to a vacuum heat treatment at 600 °C for 3 h. The coating microstructure, microhardness and tribological performance were characterized. The effects of the tin content and the vacuum heat treatment on the microstructure, microhardness and tribological behavior of the coatings were investigated. It is found that the as-sprayed CuSn6 (As6) and CuSn8 (As8) coatings exhibit practically an identical porosity. Meanwhile, As8 presents a higher microhardness than As6. In addition, the increase of the tin content in the powder feedstock leads to a lower wear rate. After a heat treatment, coating porosities are significantly reduced. However, the coating hardness is significantly decreased and the coating presents a much decreased wear resistance. For the as-sprayed coatings, such factors as ploughing and particle delamination could determine the sliding process. The heat treatment results in a distinct modification of the tribological behavior. For the annealed coatings, the adhesion, between the coating and the counterpart, could play a dominant role in the sliding process.     

Nanolayered multilayer coatings of CrN/CrAlN prepared by reactive DC magnetron sputtering

Single-phase CrN and CrAlN coatings were deposited on silicon and mild steel substrates using a reactive DC magnetron sputtering system. The structural characterization of the coatings was done using X-ray diffraction (XRD). The XRD data showed that both the CrN and CrAlN coatings exhibited B1 NaCl structure with a prominent reflection along (2 0 0) plane. The bonding structure of the coatings was characterized by X-ray photoelectron spectroscopy and the surface morphology of the coatings was studied using atomic force microscopy. Subsequently, nanolayered CrN/CrAlN multilayer coatings with a total thickness of approximately 1 μm were deposited on silicon substrates at different modulation wavelengths (Λ). The XRD data showed that all the multilayer coatings were textured along {2 0 0}. The CrN/CrAlN multilayer coatings exhibited a maximum nanoindentation hardness of 3125 kg/mm² at a modulation wavelength of 72 Å, whereas single layer CrN and CrAlN deposited under similar conditions exhibited hardness values of 2375 and 2800 kg/mm², respectively. Structural changes as a result of heating of the multilayer coatings in air (400-800 °C) were characterized using XRD and micro-Raman spectroscopy. The XRD data showed that the multilayer coatings were stable up to a temperature of 650 °C and peaks pertaining to Cr₂O₃ started appearing at 700 °C. These results were confirmed by micro-Raman spectroscopy. Nanoindentation measurements performed on the heat-treated coatings revealed that the multilayer coatings retained hardness as high as 2250 kg/mm² after annealing up to a temperature of 600 °C.     

Fabrication of coaxial nanowire heterostructures: SiO x nanowires with conformal TiO2 coatings

Silica nanowires, grown via the active oxidation of a silicon substrate, have been coated with TiO₂ using two coating methods: solution-based deposition of Ti-alkoxides and atomic layer deposition. Analysis of as-deposited and annealed films shows that it is possible to produce stable conformal coatings of either the anatase or rutile phases of TiO₂ on nanowires with diameters greater than 100 nm when annealed between 500–600°C and 800–900°C, respectively, with annealing at higher temperatures (1050°C) producing coatings with a highly facetted rutile morphology. The efficacy of the process is shown to depend on nanowire diameter, with nanowires having diameters less than about 100 nm fusing together during solution-based coating and decomposing during TiO₂ atomic layer deposition. The use of a suitable buffer layer is shown to be an effective means of minimizing nanowire decomposition. Finally, annealing coated nanowires under active oxidation conditions (1100°C) is shown to be an effective technique for depositing additional conformal SiO _x coatings, thereby providing a means of fabricating multi-layered coaxial nanostructures.