基于X射线反射研究溅射工艺对CrAlN/TiAlN周期膜界面结构的影响

为研究X射线反射技术在纳米多层膜界面微结构表征中的应用,采用反应磁控溅射技术在单晶硅基片上制备CrAlN/TiAlN纳米周期膜,利用X射线反射技术系统研究溅射工艺参数对CrAlN/TiAlN纳米周期膜界面微结构的影响规律。结果表明:增加铝靶功率可提高膜层的溅射速率和降低膜层的界面粗糙度,然而较高的铝靶功率会使膜层界面出现严重的弥散;较大和较小的负偏压都不利于形成完整的周期膜调制结构和光滑的界面;提高Ti/Cr靶电流可有效改善周期膜的调制界面结构,但太大的靶电流会导致膜层间扩散加重,形成弥散界面。N2流量与Ar流量对膜层界面粗糙度具有相反的影响作用。试验得到的优化工艺参数为:铝靶功率80W,溅射负偏压-200 V,Ti/Cr靶电流0.2A,N2流量30cm~3/min,Ar流量10cm~3/min。     

Estimation of Transformation Temperatures in Ti–Ni–Pd Shape Memory Alloys

The present study focused on estimating the complex nonlinear relationship between the composition and phase transformation temperatures of Ti–Ni–Pd shape memory alloys by artificial neural networks (ANN). The ANN models were developed by using the experimental data of Ti–Ni–Pd alloys. It was found that the predictions are in good agreement with the trained and unseen test data of existing alloys. The developed model was able to simulate new virtual alloys to quantitatively estimate the effect of Ti, Ni, and Pd on transformation temperatures. The transformation temperature behavior of these virtual alloys is validated by conducting new experiments on the Ti–rich thin film that was deposited using multi target sputtering equipment. The transformation behavior of the film was measured by varying the composition with the help of aging treatment. The predicted trend of transformational temperatures was explained with the help of experimental results.     

反应磁控溅射制备的Cr-N薄膜的成相行为

采用反应磁控溅射在不锈钢衬底上制备Cr-N薄膜，并研究了基片温度、氮气分压和溅射功率变化对薄膜相组成的影响。结果表明，基片温度升高使薄膜由单一的CrN相变成CrN和Cr2N两相共存，同时使有效的沉积速率下降；在基片温度为373K、溅射功率约45W时，氮气和氩气流量比在1：4到3：2的范围内变化时，薄膜的相组成几乎没有明显的变化；过高的溅射功率使薄膜以非晶态的形式存在。热处理后的Cr-N薄膜通常有CrN和Cr2N两相共存。     

MICROSTRUCTURE AND COMPRESSIVE PROPERTIES OFTi_(50)Al_(48)Mn_2 AND Ti_(50)Al_(48)Cr_2

The microstructure and compressive properties of Ti_(500Al_(48)Mn_2and Ti_(50)Al_(48)Cr_2 alloys are studied in this paper Existence of αx y transforntation in TiAl alloys is confirnted by metallographic examincttion,the transformation temperatuses of Ti_(50)Al_(48)Mn_2 and Ti_(500Al_(48)Cr_2,are 1375and 1373C respeclively,After treating withic x y phase field,themicrostructure of alloys consists of lamellar zones(L)and bulk y_p.,The vohme ratio of L/y_p inctrases with increasing solution treatnient temperature.The third alloying ele-ments of Mn and Cr distribute perfentially over αphase at solution treatment tempera-tures and result in that α_2 and γ lamellae become thicker.The yield strength of Ti_(50)Al_(48)Mn_2 and Ti_(500Al_(48)Cr_2 alloys decreases and the compressibllity increases with in-creasing γ_p volume fraction.     

On the Ti2Ni precipitates and Guinier–Preston zones in Ti-rich Ti–Ni thin films

After heat treatment, there may exist different types of precipitates in Ti-rich thin films, i.e. spherical Ti₂Ni precipitates and plate-like Guinier–Preston (GP) zones. While the Ti₂Ni precipitates impede the shear deformation of martensitic transformation, the GP zones do not stop both the shear deformation of martensitic transformation and the twinning shear of (001) deformation twin in the martensite phase. An elastic deformation model of the GP zone during martensitic transformation and subsequent deformation in the martensite was built up. The model can explain the GP zones-related shape memory properties self-consistently. These results supply microstructural explanation for the previous results that Ti-rich Ti–Ni thin films with GP zones show a large transformation strain despite the presence of the GP zones, while thin films with Ti₂Ni precipitates show a relatively small transformation strain.     

Microstructural characterizations of magnetron sputtered Ti films on glass substrate

Magnetron sputtered Ti thin films deposited on glass substrates under varying deposition parameters were characterized by X-Ray Diffraction, Scanning Electron Microscopy and Atomic Force Microscopy. The textures of the Ti films characterized by X-ray diffraction revealed the initial (1 0 0) preferred orientation but it transformed in to (0 0 2) and (1 0 1) orientation with increase in sputtering power and substrate temperature, respectively. The preferred orientations of (0 0 2) and (1 0 1) were observed for the films deposited with the sputtering pressure of 5 mTorr and 20 mTorr, respectively. The average surface roughness of the Ti films showed an increasing trend with power, pressure, and temperature from the Atomic Force Microscopy analysis. The dense film morphology was observed in the Scanning Electron Microcopy images of Ti thin films deposited with higher substrate temperature (500 °C). X-ray diffraction analysis revealed that the grain size of the Ti thin films exhibits an increasing trend with varying deposition parameters.     

Ti_(50+x)Pd_(30)Ni_(20-x)高温形状记忆合金的弹性行为

制备了三种 Ｔｉ５０＋ｘＰｄ３０Ｎｉ２０－ｘ高温形状记忆合金,使用热分析测试了合金的相变温度发现当 Ｔｉ的原子分数偏离５０％时,合金的相变温度随 Ｔｉ成分的升高而降低,并对这种合金的力学性能进行了测试．合金在奥氏体转变结束温度以上变形仍具有形状记忆效应,应力诱发的马氏体在应力去除后不能恢复到奥氏体研究了这种合金在不同的重复加载条件下的弹性行为,实验表明,弹性回线的形状特征与加载历程有关在奥氏体转变结束温度附近加载可以获得完全的线性伪弹性;而对于处于稳定单相的试样,在重复加载的条件下也可以获得弹性滞后回线     

磁控溅射中工作压强对钛膜沉积的影响

为了研究在磁控溅射工艺中溅射电流和溅射时间恒定的情况下,氩气工作压强的变化对钛膜在基底表面沉积的影响,通过用原子力显微镜分析钛膜的厚度和均方根粗糙度的方法来进行.结果表明:工作压强达到1.1Pa后, Ti膜的厚度及均方根粗糙度都随压强的增大而减小.由此说明,工作压强的变化对钛膜沉积有较大影响.     

Microstructure and properties of indium tin oxide thin films deposited by RF-magnetron sputtering

Tin-doped indium oxide （ITO） thin films were prepared using conventional radio frequency （RF） planar magnetron sputtering equipped with IR irradiation using a ceramic target of In2O3/SnO2 with a mass ratio of 1：1 at various IR irradiation temperatures T1 （from room temperature to 400℃）. The refractive index, deposited ratio, and resistivity are functions of the sputtering Ar gas pressure. The microstructure of ITO thin films is related to IR T1, the crystalline seeds appear at T1= 300℃, and the films are amorphous at the temperature ranging from 27℃ to 400℃. AFM investigation shows that the roughness value of peak-valley of ITO thin film （Rp-v） and the surface microstructure of rio thin films have a close relation with T1. The IR irradiation results in a widening value of band-gap energy due to Burstein-Moss effect and the maximum visible transmittance shifts toward a shorter wavelength along with a decrease in the film＇s refractive index. The plasma wavelength and the refractive index of ITO thin films are relative to the T1. XPS investigation shows that the photoelectrolytic properties can be deteriorated by the sub-oxides. The deterioration can be decreased by increasing the oxygen flow rote （fo2）, and the mole ratio of Sn/In in the samples reduces with an increase info2.     

反应溅射Ti(0，N)涂层的微结构与力学性能

采用反应磁控溅射方法在Ar、N2和O2混合气氛中制备了一系列Ti(O,N)涂层,并采用EDS、XRD、SEM、AFM和微力学探针研究了氧分压对涂层的化学成分、微结构和力学性能的影响.结果表明:随混合气氛中氧分压的提高,涂层中的氧含量逐步增加,氮含量相应减少,但涂层始终保持与TiN相同的NaCl结构.少量氧的加入,可以改善涂层的结晶状态,涂层的硬度也相应升高,明显高于未含氧的TiN涂层的硬度.氧含量为8.0%(原子数分数)时,涂层硬度达到最大值26.2 GPa.进一步增加氧含量,涂层的硬度基本保持不变.     

磁控溅射工艺参数对钛钨合金膜电阻温度特性的影响

采用直流磁控溅射方法在载玻片上制备钛钨合金热敏感薄膜,测试了所制备的钛钨合金热敏薄膜在不同温度下的方块电阻,并根据测试曲线计算薄膜的电阻温度系数(TCR)。研究了工作气压、氩气流量以及溅射电流对钛钨合金膜TCR的影响,获得了最佳沉积工艺参数,即:溅射电流0.32A,工作气压0.8Pa,氩气流量60cm3/min。在此参数下制备的钛钨合金膜TCR为0.2%/K。测试结果也表明钛钨合金膜的时间稳定性好。     

磁控溅射和退火制备ZnO/SiO2复合薄膜

采用射频磁控溅射和退火处理的方法在单晶硅衬底上制备了ZnO/SiO2复合薄膜,利用X射线衍射(XRD)、扫描电镜(SEM)、能谱分析(EDS)和接触角测量等测试手段研究溅射气压、溅射功率、氧氩比和退火温度等对复合薄膜成分组成、组织结构及润湿性能的影响。研究表明,复合薄膜中主要有ZnO、SiO2、Zn2SiO4 3种物相,且分别以六方纤锌矿结构、无定形态和硅锌矿型等形式存在。随着溅射和退火工艺的改变,复合薄膜的接触角在41°～146°间变化,组织形态由颗粒状向纳米竹叶状变化。溅射气压0.5 Pa,溅射功率120 W,氧氩比(O2∶Ar)为0∶30,退火温度为700℃的条件下获得具有六方纤锌矿结构的ZnO纳米组织,该组织呈现出竹叶状,在薄膜表面交错排列形成了无序多空隙的微观形貌,使复合薄膜具有超疏水性,接触角为146°。     

Cu content and annealing temperature dependence of martensitic transformation of Ti36Ni49−xHf15Cux melt spun ribbons

The martensitic transformation in Ti₃₆Ni_49−xHf₁₅Cu_x (x = 1, 3, 5, 8) ribbons has been investigated. Only B2 to B19′ transformation was detected in all the present ribbons. The martensitic transformation temperatures do not change obviously with increase in the Cu content except that they decrease when the Cu content is 3 at.%. The lattice parameters of B19′ martensite, a and c increase, b almost remains constant, while the monoclinic angle β decreases with increase in the Cu content. For the ribbons with Cu content of 1 and 3 at.%, the martensitic transformation temperatures change slightly when the annealing temperature increases. For the ribbons with Cu content of 5 and 8 at.%, with increase in the annealing temperature, the martensitic transformation temperatures almost do not change and then decrease rapidly when the annealing temperature is higher than 873 K. TEM observation shows that the microstructure of the ribbons with Cu content of 1 and 3 at.% contains the martensite matrix and the (Ti,Hf)₂Ni particles with the size of about 150 nm, which does not change obviously when the annealing temperature increases. This results in that the martensitic transformation temperatures are not sensitive to the annealing temperature in the ribbons with 1 and 3 at.% Cu content. However, nano-scale (Ti,Hf)₂Ni particles precipitate in the ribbons with Cu content of 5 and 8 at.% when the annealing temperature is 773 and 873 K, and then the (Ti,Hf)₂Ni particles grow and coarsen rapidly with further increase in the annealing temperature. The coarsening of the (Ti,Hf)₂Ni particles should be responsible for the dramatic decrease of the martensitic transformation when the annealing temperature is higher than 873 K. For all the present ribbons, the substructure of B19′ martensite is (001) compound twins, and the inter-variant relationship is mainly (011) type I twinning.     

Study on adhesion and electro-optical properties of ITO films on flexible PET substrate

High-quality ITO films on flexible PET substrate were prepared by RF magnetron sputtering at low deposition temperature with different Ar gas sputtering pressure.Adhesion and electro-optical properties of ITO films were investigated as a function of Ar partial pressure.The sputtering conditions provide very uniform ITO films with high transparency (＞85% in 400-760 nm spectra) and low electrical resistivity (1.408×10-3-1.956×10-3 Ω·cm).Scratch test experiments indicate that there is a good adhesion property between ITO films and PET substrate, the critical characteristic load increases from 16.5 to 23.2 N with increasing Ar sputtering pressure from 0.2 to 1.4 Pa.     

Ti49.4Ni50.6超弹性弹簧的相变和形变特性

用示差扫描量热仪、拉伸实验和应力-应变循环实验系统研究了退火温度、变形温度以及热循环和室温应力-应变循环对Ti49．4Ni50．6超弹性(SE)弹簧的相变和形变特性的影响。冷加工加中温退火态Ti49．4Ni50．6合金冷却→←加热时的相变类型为母相B2→←R相→←马氏体B19′。随退火温度升高，马氏体转变温度升高，R相转变温度降低。623-773K退火态Ti49．4Ni50．6弹簧室温下可获得SE特性，随变形温度升高，SE弹簧剐度增加；当退火温度超过823K后，SE持性变差。热循环时SE弹簧的切变量取值越小，其应变恢复率越高。预循环训练可增强SE的稳定性。     

氩离子溅射刻蚀对Ti-Si-C纳米复合薄膜XPS分析的影响

通过中频非平衡磁控溅射Ti80Si20复合靶在氩气和甲烷混合气氛中沉积Ti-Si-C复合薄膜。采用X射线衍射仪、Raman光谱和X射线光电子能谱分析薄膜微结构。结果显示:制备的薄膜为非晶碳(a-C:Si:H)包裹约10 nm TiC晶粒的复合结构,氩离子溅射刻蚀对XPS分析结果有显著影响。随氩离子刻蚀溅射刻蚀时间增加,薄膜表面C、O原子含量明显降低,而Ti、Si原子含量增加。氩离子溅射刻蚀导致薄膜非晶碳相发生石墨化转变,即sp3C-C(H)/sp2C-C比率减小,同时,C-Ti*/C-Ti和C-(Ti+Ti*)/C-C强度比明显增加。     

Structure of martensite in Ti-rich Ti–Ni–Cu thin films annealed at different temperatures

After annealing at different temperatures, there are different types of precipitates in Ti-rich Ti–Ni–Cu thin films: plate-like Guinier–Preston (GP) zones, Ti₂Cu precipitates and spherical Ti₂Ni precipitates. The (0 1 1) compound twins and (1 1 1) type I twins are dominant in Ti-rich Ti–Ni–Cu thin films annealed at different temperatures, which suggests that the precipitates do not change the twinning modes of the B19 martensite. However, the amount of the (0 1 1) compound twin increases with increasing annealing temperature due to its small twinning shear. In thin films with GP zones or Ti₂Ni precipitates, the amount of martensite with a single-pair morphology is less than that in thin films without precipitates. And in thin film with Ti₂Cu + Ti₂Ni precipitates, hardly any martensite with a single-pair morphology is observed. For the different types of precipitates at the different annealing temperatures, the obstacle of the precipitates to the growth of the B19 martensite plate also varies. The GP zones slightly hinder the growth in the width of martensite, resulting in wavy twin boundaries at the martensite variant tip. The Ti₂Cu precipitates can change both the width and the direction of the martensite plates. Ti₂Ni precipitates also significantly disturb or impede the growth of the martensite variants. These effects lead to a decrease in the maximum shape recoverable strain with increasing annealing temperature.     

Room temperature deposition of Al-doped ZnO thin films on glass by RF magnetron sputtering under different Ar gas pressure

Al-doped ZnO (AZO) thin films were deposited on glass substrates at room temperature by RF magnetron sputtering. The effects of Ar gas pressure on the structural, optical, and electrical properties were investigated. As the Ar gas pressure increased, the resistivities of the AZO thin films increased, the mobilities decreased, and the carrier concentrations were constant. X-ray photoelectron spectroscopy (XPS) showed that higher Ar gas pressures promoted O-Zn bond formation and reduced the number of oxygen vacancies. The reduction in mobility, which increased the resistivity, was attributed to increased lattice scattering by the oxygen atoms. In AZO thin films deposited at room temperature, the conduction characteristics are primarily influenced by the mobility.     

高温、短时Pd/Ti之间相互扩散行为的研究

为了研究高温下短时间Pd/Ti间的互扩散行为,在Ti表面利用磁控溅射技术沉积了Pd膜层,然后分别对Pd/Ti试样进行500℃/5 h,550℃/5 h,600℃/5 h和700℃/5 h高温处理,用XRD、SEM和EDS研究合金层的相组成、微观组织和元素分布。研究发现:当Pd/Ti试样经500℃/5 h处理后,Pd/Ti之间有极轻微的互扩散发生。当温度升高到550℃时,Pd/Ti间产生了连续的扩散层,随着温度升高,膜层之间的互扩散加剧。并且,当温度升高到700℃时,Pd/Ti之间形成了相图中除Ti3Pd5相和Ti3Pd相以外的其余各化合物相。还分析了Pd/Ti界面扩散反应动力学。结果表明,扩散层厚度的增加经历了一个由界面反应动力学控制到扩散控制的过渡。     

制备工艺对超磁致伸缩Fe-Ga合金薄膜表面形貌的影响

采用JZCK-600F型多功能镀膜设备制备了Fe-Ga合金薄膜,研究了溅射工艺对Fe-Ga合金薄膜沉积速率及表面形貌的影响。用SEM、EDS研究了Fe-Ga合金薄膜的表面形貌和薄膜成分。当其他工艺参数不变时,溅射时间、溅射功率是影响Fe-Ga合金薄膜的厚度和生长速率的主要因素。随溅射时间和功率的增加,薄膜厚度和沉积速率也随之增加,并且薄膜厚度与溅射时间和功率呈现出正比例关系;但是薄膜厚度过大,加大的内应力会使薄膜剥离。溅射功率过大时,内应力同样会使薄膜内部出现裂纹。所制备Fe-Ga合金薄膜的磁畴图像明暗对比明显。磁畴形状呈现不太规则的团圈状,类似珊瑚结构。薄膜的结晶化生长良好,薄膜形貌为较均匀致密的颗粒状结构。优化的薄膜溅射工艺参数为溅射功率80 W、溅射工作气压0.6 Pa、溅射时间60 min、Ar气工作流量25 mL/min。采用此优化工艺制备的Fe-Ga合金磁致伸缩薄膜悬臂梁偏移量为69.048 μm,可满足制备微器件所需性能。