磁场非平衡度对CrN_x镀层性能的影响

使用具有不同非平衡度的磁控管直流磁控溅射技术沉积CrN_x镀层,并用Langmuir探针诊断、高斯仪测量、Ansys软件模拟等手段进行表征,研究了磁场非平衡度对溅射等离子体的空间分布状态以及CrN_x镀层的微观结构、硬度及摩擦性能的影响。结果表明:低非平衡度磁控管（K为2.78）将多数离子束缚在靶材表面大约6 cm范围内,而对于高非平衡度磁控管（K为6.41）则在此区域没有类似的高密度等离子体存在。随着磁场非平衡度的增大,CrN_x镀层的厚度递增,物相结构也从Cr+Cr₂N依次向Cr+Cr₂N+CrN和Cr₂N+CrN转化,且镀层的平整度和致密性随之明显改善。同时,CrN_x镀层的硬度随着非平衡度的增大而提高,摩擦系数则随之减小。     

多弧离子镀CrN薄膜的耐腐蚀性能

单相CrN薄膜较难制取,国外已形成商用,而国内相关研究尚处于起步阶段。采用多弧离子镀技术在45钢表面沉积CrN薄膜,通过扫描电镜观察了CrN薄膜的表面形貌,采用X射线衍射仪对其相结构进行了分析,分别讨论了CrN薄膜在3.5%NaCl溶液、1 mol/L NaOH溶液和1 mol/L H2SO4溶液中的电化学腐蚀性能,在其他制备参数不变的条件下,考察了氩氮流量比对薄膜组织结构以及性能的影响。结果表明:随着氩氮流量比的减小,CrN薄膜表面的液滴尺寸和数目逐渐减小;薄膜主要以CrN相为主,随着氩氮流量比的增大,CrN(110)的峰值逐渐减弱,CrN(200)的峰值逐渐增强;随着氩氮流量比的减小,CrN薄膜在3.5%NaCl溶液、1 mol/L NaOH溶液和1mol/L H2SO4溶液中的耐蚀性均得到提高,在氩氮流量比1∶3时,薄膜的耐腐蚀性最佳。     

电弧离子镀Cr/CrN多层膜的耐腐蚀性研究

采用电弧离子镀技术制备了Cr/CrN多层膜,通过控制每个Cr层和CrN层的沉积时间获得不同调制比,从微观组织和腐蚀行为两方面研究了调制比对Cr/CrN多层膜的影响。结果表明,引入Cr层对CrN薄膜沉积过程中生长的柱状结构有抑制作用,孔隙率更低,结构更加致密。动电位极化曲线和电化学阻抗谱表明,与纯CrN薄膜相比,Cr/CrN多层膜的腐蚀电位增加了约100 mV,腐蚀电流密度降低一个数量级以上,多层膜的耐腐蚀性能得到明显提升。     

Cr/CrN多层膜的结构及腐蚀性能研究

利用电弧离子镀设备,在45#钢基体上制备了两种调制比的Cr/CrN多层膜.采用X射线衍射技术(XRD)、扫描电子显微镜(SEM)、电子探针(EPMA)、M273A电化学系统等技术分析了薄膜的相结构、表面形貌、横截面元素分布、模拟海水中的抗腐蚀性能.结果表明:膜层主要由CrN、Cr2N和Cr组成,以Cr2N(111)为择优取向;膜层为Cr层-过渡层-CrN层的"三明治"调制结构;Cr/CrN多层膜结构与中间Cr层的存在可以显著提高基体和单层CrN抗腐蚀性能,45#钢+Cr/CrN(5/10)的防护体系抗腐蚀性能最佳.     

氮分压对电弧离子镀CrNx薄膜结构与性能的影响

采用电弧离子镀技术,在不同n2分压下沉积Cr/CrNx薄膜.X射线衍射技术、努氏硬度计和UMT型球-盘摩擦试验机、M342-2型腐蚀测量系统分别测试了薄膜相结构、显微硬度、摩擦磨损和抗腐蚀性能.研究了N2分压对薄膜相组成、硬度、摩擦磨损和抗腐蚀性能的影响.结果表明随着N2分压的升高,薄膜由Cr2N(211)相过渡到CrN(220)相;薄膜硬度出现两个极值,对应于单相Cr2N和CrN;与钢基体相比,N2分压为0.35 Pa时制备的CrNx薄膜具有良好的耐磨性能和抗腐蚀性能.     

304不锈钢表面Cr/a-C:H薄膜的制备及其抗腐蚀性能

采用直流反应磁控溅射技术在304不锈钢表面制备Cr/a-C:H薄膜进行表面改性,有望提高其在NaCl溶液中的耐蚀性能。采用Raman光谱仪、X射线衍射仪(XRD)、场发射扫描电子显微镜(SEM)和原子力显微镜(AFM)研究了Cr/a-C:H薄膜的微观结构和表面形貌;利用接触角测量仪和动电位极化曲线研究了304不锈钢表面沉积Cr/a-C:H薄膜前后的润湿性和抗腐蚀性能。结果表明:所制备薄膜为Cr_3C_2纳米晶镶嵌非晶碳的典型纳米晶/非晶复合薄膜;薄膜表面光滑、结构均匀致密;沉积Cr/a-C:H薄膜后304不锈钢表面由亲水性转为疏水性,水接触角达到95°;在3.5%NaCl溶液中304不锈钢表面沉积Cr/a-C:H薄膜体系的自腐蚀电位约为-0.06 V,腐蚀电流密度为2.95×10~(-8)A/cm~2,极化电阻为14.07×10~5Ω·cm~2,相比于表面无薄膜防护的304不锈钢,该体系的抗腐蚀性能得到明显提升。     

金属过渡层类型对非晶碳膜结构性能的影响

采用直流磁控溅射技术制备不同金属过渡层(Cr, Ti, W)的类石墨非晶碳膜(GLC), 研究过渡层类型对非晶碳膜微结构的影响, 并考察其在人工海水中摩擦性能的变化。研究结果表明: Cr/GLC薄膜sp²杂化键含量最高, 沿GLC表面到铬碳界面方向, sp²杂化键含量逐渐增大, Ti过渡层和W过渡层的sp²杂化键含量变化不明显。Cr/GLC薄膜较高的sp²杂化键含量有助于其在摩擦过程中产生可以充当润滑相的石墨化转化摩擦转移膜。在三种涂层中, Cr/GLC薄膜表现出最高的腐蚀电位-0.16 V和最低的腐蚀电流密度4.42×10^-9 A/cm²。因此相较于Ti, W作过渡层的GLC薄膜, Cr/GLC薄膜在海水环境下表现出优异的摩擦学特性。     

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。     

生物可降解Fe-O薄膜的制备及性能表征

纯铁由于其可降解性和无毒性,在血管支架材料领域具有潜在的应用前景.本文采用等离子体浸没离子注入与沉积(PⅢ&D)方法,在纯铁表面沉积一层Fe-O薄膜以改善纯铁表面的抗腐蚀性,用X射线光电子能谱和X射线衍射研究了薄膜表面成分和物相结构,用极化腐蚀试验研究了薄膜在模拟体液中的腐蚀行为,采用划痕试验法评价了薄膜与基体的结合力.结果表明:采用PⅢ&D法制备Fe-O薄膜,不同氧流量下沉积的薄膜具有不同的物相结构,当氧流量较小时,在纯铁表面形成一层FeO薄膜,随着氧流量的增加,FeO相逐渐转变为Fe3O4相.通过划痕试验和腐蚀试验发现,氧流量为3.4sccm时,形成的FeO薄膜与基体具有较好的结合力,并可对基体产生较好的保护作用,从而大大提高了纯铁表面在模拟体液中的抗腐蚀性能.     

微波-ECR等离子体辅助沉积Zr-N薄膜结构和性能研究

在不同氮流量下,利用微波-ECR等离子体溅射沉积技术在45#钢基体上制备了ZrN薄膜.XRD、TEM分析结果表明:随着充入N2流量的改变,薄膜结构由单一的ZrN结构向ZrN和ZrNx复合结构转变,然后出现非晶态结构.当N2流量在(2～8) sccm之间,薄膜为ZrN结构;在(10～12) sccm时,为ZrN和正交的ZrNx(a=0.3585 nm,b=0.4443 nm,c=0.5798 nm)混合型结构;14 sccm时出现非晶化趋势.俄歇电子谱仪(AES)和探针分析表明:薄膜中氮含量为7.73%～66.96%.同时对薄膜的硬度进行了测试,薄膜硬度在19.82 GPa～26.32 GPa之间,随氮值的变化,先增加后降低.对硬度最高的4#样品进行了摩擦性能测试,磨损率约4.5×10-8 mg/min.薄膜这些性能的变化是由于不同氮流量下薄膜结构发生变化造成的.     

CrN和CrNiN涂层在模拟质子交换膜燃料电池环境中的电化学性能及疏水性能EI北大核心CSCD

用闭合场非平衡磁控溅射离子镀在304不锈钢表面沉积CrN和CrNiN涂层。采用X射线衍射和场发射扫描电镜表征涂层的结构和形貌。采用电化学测试、界面接触电阻测试以及疏水性测试等方法,研究两种不同涂层在模拟质子交换膜燃料电池(Proton Exchange Membrane Fuel Cell,PEMFC)环境下的电化学腐蚀性能、界面接触电阻以及疏水性能。结果表明:CrN涂层主要包含CrN和Cr2N相,CrNiN涂层中CrN和Cr2N相较少,Ni在CrNiN涂层中以单质形式存在;动态极化测试表明涂层的耐蚀性能较好,其中CrNiN涂层的耐蚀性能较CrN涂层差,恒电位极化测试表明CrN和CrNiN涂层的电流密度相当;CrN和CrNiN涂层都显著降低了304不锈钢的界面接触电阻,其中CrN涂层的接触电阻最小;CrNiN涂层疏水性能优于CrN涂层,更有利于质子交换膜燃料电池中的水管理。     

Influence of nitrogen flow rates on materials properties of CrN x films grown by reactive magnetron sputtering

Chromium nitride (CrN) hard thin films were deposited on different substrates by reactive direct current (d.c.) magnetron sputtering with different nitrogen flow rates. The X-ray diffraction patterns showed mixed Cr₂N and CrN phases. The variations in structural parameters are discussed. The grain size increased with increasing nitrogen flow rates. Scanning electron microscopy image showed columnar and dense microstructure with varying nitrogen flow rates. An elemental analysis of the samples was realized by means of energy dispersive spectroscopy. The electrical studies indicated the semiconducting behaviour of the films at the nitrogen flow rate of 15?sccm.     

氮化银铬和氮化钨铬纳米薄膜在微型钻头上的应用

为了了解氮化银铬和氮化钨铬纳米复合薄膜涂层应用于微型钻头加工的潜能,采多靶材非平衡磁控溅射方式制备薄膜,分别将钨(W)和银(Ag)掺杂于氮化铬(CrN)中,形成氮化钨铬(Cr-W-N)和氮化银铬(Cr-Ag-N)纳米复合薄膜,研究其基本特性及涂层于微型钻头表面加工电路板性能.结果表明,虽掺杂Ag导致硬度降低,仍可改善微型钻头加工性能;掺杂W形成W2N化合物混杂于CrN中,因而整体涂层硬度增加,同时大幅提升微型钻头加工性能.经由本研究,确认氮化银铬和氮化钨铬纳米复合薄膜具备改善微型钻头加工电路板的能力.     

Preparation of CrN thick films by high-rate middle-frequency unbalanced magnetron sputtering

A middle-frequency (MF) unbalanced magnetron sputtering system equipped with an electron source was designed and used for deposition of CrN thick films under various MF power (1.4–14 kW) at fixed temperature, pressure, and gas flow rate. The deposition rate was increased with increasing MF power and the structure and N/Cr ratio of the deposited CrN films exhibited a complicated behavior, where the CrN films were a polycrystalline structure and the films deposited under optimized conditions exhibited a dense columnar structure and a micro-hardness of 16 GPa. The dependence of the structure and micro-hardness on MF power was interpreted by the power deposition efficiency.     

Preparation of CrN thick films by high-rate middle-frequency unbalanced magnetron sputtering

A middle-frequency (MF) unbalanced magnetron sputtering system equipped with an electron source was designed and used for deposition of CrN thick films under various MF power (1.4–14 kW) at fixed temperature, pressure, and gas flow rate. The deposition rate was increased with increasing MF power and the structure and N/Cr ratio of the deposited CrN films exhibited a complicated behavior, where the CrN films were a polycrystalline structure and the films deposited under optimized conditions exhibited a dense columnar structure and a micro-hardness of 16 GPa. The dependence of the structure and micro-hardness on MF power was interpreted by the power deposition efficiency.     

Structural,Wettability and Optical Investigation of Titanium Oxynitride Coatings:Effect of Various Sputtering Parameters

The objective of the present work is to investigate the effect of various sputtering parameters such as nitrogen flow rate,deposition time and sputtering pressure on structural,wettability and optical properties of titanium oxynitride films deposited on glass substrate by reactive magnetron sputtering.The X-ray diffraction graphs of titanium oxynitride films show evolution of various textures of TiO_xN_y and TiN phases with increasing nitrogen flow rate and deposition time,but an increase in sputtering pressure from 4.0 to 8.0 Pa results in decline of various textures observed for TiO_xN_y and TiN phases.The stress and strain calculated by sin~2Ψ method are compressive,which decrease with increasing nitrogen flow rate from 55 to 100 sccm(standard cubic centimeter per minute) and increase with increasing deposition time from 80 to 140 min due to atomic penning effect and increasing thickness of the deposited films.The titanium oxynitride films have contact angle values above 90 deg.,indicating that films are hydrophobic.The maximum contact angle of 109.1 deg.is observed at deposition time of 140 min.This water repellent property can add value to potential protective,wear and corrosion resistant application of titanium oxynitride films.The band gap decreases from 1.98 to 1.83 eV as nitrogen flow rate is increased from 55 to 100 sccm;it decreases from 1.93 to 1.79 eV as deposition time is increased from 80 to 140 min as more nitrogen incorporation results in higher negative potential of valence band N2p orbital.But it increases from 2.26 to 2.34 eV for titanium oxynitride films as sputtering pressure increases from 4.0 to 8.0 Pa.     

工艺参数对磁控溅射ZrN膜耐腐蚀性能的影响

为寻求真空磁控溅射ZrN膜耐蚀性与其溅射工艺间的规律,在1Cr18Ni9Ti不锈钢表面以不同的工艺参数真空磁控溅射了系列ZrN膜。通过中性盐雾试验确定了不同工艺参数所得ZrN膜的耐蚀性等级。结果表明:ZrN膜耐蚀性随N2流量的增加先增加,但超过15 mL/min后,膜的耐蚀性反而下降;ZrN膜耐蚀性随反应温度升高而增强;ZrN膜的耐蚀性随反应时间的增加越来越好,但超过15 min后,膜的耐蚀性不再增强;以ZrN膜的耐蚀性为依据,最佳溅射工艺参数为N2流量15 mL/min,反应时间15 min,反应温度200℃。     

The influence of Cr-based coating on the adhesion force between epoxy molding compounds and IC encapsulation mold

The surface properties of IC encapsulation molds such as anti-sticking, wear and corrosion resistances can be improved by hard surface coating. The unbalanced magnetron sputtering method is used to deposit Cr, Cr₂N, and CrN phase individual. Of the three coatings, the Cr₂N coating has the lowest surface energy and the highest contact angle of water, which reaches as high as 120°. High water-repellency of Cr₂N coating is due to the CH groups on the film surface, and the N-H or O-H bonds are found to be the effective adsorption sites for carbon substances. The experimental results also show the correlation of coating's surface energy and its adhesion force with EMC. Performance evaluation showed that the Cr₂N coating could increase the number of molding injections in the IC package production lines by 50%.     

Influence of the N2 partial pressure on the characteristics of CrZrN coatings synthesized Using a segment CrZr target

In this study, CrZrN films were synthesized by unbalanced magnetron sputtering (UBM) under various N2 partial pressures and their characteristics such as crystalline structure, surface morphology, microstructure and mechanical properties as a function of the N2 partial pressures were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), nanoindentation, wear tests, and corrosion tests. Results revealed that, with increasing the N2 partial pressure from 0.05 to 0.21 Pa, the nitrogen content of the films increased from approximately 40.9 to 53.7 at%, the deposition rate decreased from approximately 100 to 59 nm/min and the surface roughness (Rms value) was increased from approximately 0.57 to 1.79 nm. The Cr37.3-Zr9.0-N53.7 film has the highest hardness, elastic modulus, and plastic deformation resistance of 36 GPa, 380 GPa, and 0.41, respectively. The Cr37.3-Zr9.0-N53.7 film also has the lowest friction coefficient and wear rate of 0.19 and 3.01 (10(-6)m3/Nm) at room temperature. In addition, the potentiodynamic test results showed the corrosion resistance of the CrZrN films became increased significantly and their corrosion current density (i(corr)), corrosion potentials (Ecorr) and corrosion rate decreased with increasing N2 partial pressure.     

铀表面非平衡磁控溅射离子镀Ti基薄膜的组织结构与腐蚀性能

金属铀的化学性质十分活泼,极易发生氧化腐蚀。本文采用磁过滤多弧离子镀在金属铀表面制备Ti过渡层,然后采用非平衡磁控溅射离子镀技术制备了Ti、TiN单层膜及Ti/TiN多层薄膜,以期改善基体的抗腐蚀性能。采用X射线衍射、极化曲线、盐雾腐蚀试验对镀层的结构、表面形貌、抗腐蚀性能进行了分析。结果表明,采用磁控溅射在金属铀表面制备一层Ti/TiN多层膜后,多层膜界面较清晰,大量的界面可终止柱状晶的生长,细化晶粒,提高镀层的致密性,有效地改善了基体的抗腐蚀性能。