N2分压对ZrN/WN纳米多层膜缺陷性质与力学性能的影响

利用射频磁控溅射系统在不同N2分压的条件下,制备了一系列ZrN/WN纳米多层膜.借助慢正电子湮没技术分析了样品的缺陷性质,采用纳米压痕仪研究了多层膜的力学性能.结果发现:N2分压为0.4 Pa的多层膜具有最小的空位型缺陷浓度,其中心层和膜基结合层的平均S参数分别为0.4402和0.4641,而较低或较高的N2分压都可能导致空位型缺陷浓度的增加.随着空位型缺陷浓度的减小,多层膜的硬度和临界载荷增大.对于空位型缺陷浓度最小的多层膜,其硬度和临界载荷达到最大值,分别为34.8 GPa和100 mN,说明较低的缺陷浓度有利于提高多层膜的力学件能.     

反应磁控溅射ZrN/AlON纳米多层膜的晶体生长和超硬效应

采用Zr靶和Al₂O₃靶通过在Ar，N₂混合气氛中进行反应磁控溅射的方法制备了不同AlON调制层厚和不同ZrN调制层厚的两个系列的ZrN/AlON纳米多层膜.利用X射线能量色散谱仪、X射线衍射仪、高分辨透射电子显微镜和微力学探针研究了多层膜的成分、微结构和力学性能.结果表明，在Ar，N₂混合气氛中对Al₂O₃进行溅射的过程中，N原子会部分取代Al₂O₃中的氧原子，形成AlON化合物.在ZrN/AlON纳米多层膜中，由于受到ZrN晶体调制层的模板作用，溅射条件下以非晶态存在的AlON层在其厚度小于0.9nm时被强制晶化并与ZrN层形成共格外延生长；相应地，多层膜的硬度明显提高，最高硬度达到33.0GPa.进一步增加多层膜中AlON调制层的厚度，AlON层形成非晶结构，破坏了多层膜的共格外延生长，导致其硬度逐步降低. 关键词： ZrN/AlON纳米多层膜 外延生长 非晶晶化 力学性能     

Hg1-xCdxTe晶体缺陷的正电子湮没寿命

利用正电子(e⁺)湮没寿命谱实验研究了Hg_1-xCd_xTe晶体样品的空位缺陷.碲溶剂法生长的样品，不论是n型导电还是p型导电都存在大量的Hg空位.经过合适的退火工艺，p型材料转为n型，同时对正电子的俘获效应减小，表现为正电子湮没平均寿命值减小14—17ps.若退火温度高于350℃，正电子湮没寿命值又增大，表明Hg空位浓度增加.得到HgCdTe中正电子的体寿命为τ_b=272ps.根据正电子湮没寿命和电参数的测量结果，得出 关键词：     

界面和择优取向对TiN/ZrN纳米多层膜硬度变化的影响

利用射频反应磁控溅射方法，制备了调制比约为4，调制周期不同的一系列TiN/ZrN纳米多层膜. 利用X射线衍射仪(XRD)、高分辨电子显微镜(HRTEM)和纳米压痕仪(Nanoindentation)对多层膜的调制结构、界面状态和力学性能进行了表征. 研究结果表明TiN/ZrN多层膜具有很好的调制结构，但是在TiN层和ZrN层之间存在一定厚度的界面混合层. 力学性能分析表明：当调制周期小于15 nm时，TiN/ZrN多层膜的硬度介于单一TiN和ZrN薄膜的硬度之间；当调制周期为15.24 nm时，硬度达到最大，但随着调制周期增加，多层膜的硬度基本上保持为常数. 分析了TiN/ZrN多层膜硬度变化的机制，认为界面厚度和择优取向是导致硬度变化的主要原因. 关键词： TiN/ZrN多层膜 界面宽度 择优取向 硬度变化     

掺镧PbWO4闪烁晶体的缺陷研究

利用正电子湮没寿命谱(PAT)和X射线电子能谱(XPS)研究了掺镧所引起的PbWO₄ 晶体缺陷的变化.结果表明：掺镧后,PbWO₄晶体中的正电子捕获中心铅空位(V< sub>Pb)浓度增加,并进一步诱导低价氧浓度的增加.讨论了掺La的作用机制,认为掺 La将抑制晶体中的氧空位,增加铅空位浓度. 关键词： 掺镧钨酸铅晶体 正电子湮没寿命谱 X射线电子能谱 缺陷     

反应溅射VN/SiO2纳米多层膜的微结构与力学性能

采用V和SiO₂靶通过反应溅射方法制备了一系列具有不同SiO₂和VN调制层厚的VN/SiO₂纳米多层膜. 利用X射线衍射、X射线能量色散谱、高分辨电子显微镜和微力学探针表征了多层膜的微结构和力学性能. 结果表明：在Ar，N₂混和气体中，射频反应溅射的SiO₂薄膜不会渗氮. 单层膜时以非晶态存在的SiO₂，当其厚度小于1nm时，在多层膜中因VN晶体层的模板效应被强制晶化，并与VN层形成共格外延生长. 相应地，多层膜的硬度得到明显提高，最高硬度达34GPa. 随SiO₂层厚度的进一步增加，SiO₂层逐渐转变为非晶态，破坏了与VN层的共格外延生长结构，多层膜硬度也随之降低. VN调制层的改变对多层膜的生长结构和力学性能也有影响，但并不明显. 关键词： 2纳米多层膜')" href="#">VN/SiO₂纳米多层膜 共格外延生长 非晶晶化 超硬效应     

Co掺杂纳米ZnO微结构的正电子湮没研究

利用正电子湮没技术研究了10 at.% Co掺杂的Co₃O₄/ZnO纳米复合物中退火对缺陷的影响. 利用X射线衍射(XRD)测量了Co₃O₄/ZnO纳米复合物的结构和晶粒尺寸. 随着退火温度升高,Co₃O₄相逐步消失,ZnO晶粒尺寸也有显著增加. 经过1000 ℃以上退火后,Co₃O₄相完全消失,并出现了CoO的岩盐结构. 正电子湮没寿命测量显示出Co₃O₄ /ZnO纳米复合物中存在大量的Zn空位和空位团. 这些空位缺陷可能存在于纳米复合物的界面区域. 当退火温度达到700 ℃后Zn空位开始恢复,空位团也开始收缩. 900 ℃以上退火后,所有空位缺陷基本消失,正电子寿命接近ZnO完整晶格中的体态寿命值. 符合多普勒展宽谱测量也显示Co₃O₄ /ZnO纳米复合物经过900 ℃以上退火后电子动量分布与单晶ZnO基本一致,表明界面缺陷经过退火后得到消除. 关键词： ZnO 界面缺陷 正电子湮没     

TiN/Al2O3纳米多层膜的共格外延生长及超硬效应

采用多靶磁控溅射法制备了一系列具有不同Al₂O₃调制层厚度的TiN/Al₂O₃纳米多层膜. 利用X射线能量色散谱、X射线衍射、扫描电子显微镜、高分辨透射电子显微镜和微力学探针表征了多层膜的成分、微结构和力学性能. 研究结果表明，在TiN/Al₂O₃纳米多层膜中，单层膜时以非晶态存在的Al₂O₃层在厚度小于1.5 nm时因TiN晶体层的模板效应而晶化，并与TiN层形成共格外延生长，相应地，多层膜产生硬度明显升高的超硬效应，最高硬度可达37.9 GPa. 进一步增加多层膜中Al₂O₃调制层的层厚度，Al₂O₃层逐渐形成非晶结构并破坏了多层膜的共格外延生长，使得多层膜的硬度逐步降低. 关键词： 2O₃纳米多层膜')" href="#">TiN/Al₂O₃纳米多层膜 外延生长 非晶晶化 超硬效应     

SiO2的赝晶化及AlN/SiO2纳米多层膜的超硬效应

采用反应磁控溅射法制备了一系列不同SiO₂层厚度的AlN/SiO₂纳米多层膜，利用X射线衍射仪、高分辨透射电子显微镜和微力学探针表征了多层膜的微结构和力学性能，研究了SiO₂层在多层膜中的晶化现象及其对多层膜生长方式及力学性能的影响. 结果表明，由于受AlN六方晶体结构的模板作用，溅射条件下以非晶态存在的SiO₂层在其厚度小于0.6 nm时被强制晶化为与AlN相同的六方结构赝晶体并与AlN形成共格外延生长. 由于不同模量的两调制层存在晶格错配度，多层膜中产生了拉、压交变的应力场，使得多层膜产生硬度升高的超硬效应. SiO₂随层厚的进一步增加又转变为以非晶态生长，多层膜的外延生长结构受到破坏，其硬度也随之降低. 关键词： 2纳米多层膜')" href="#">AlN/SiO₂纳米多层膜 赝晶化 应力场 超硬效应     

TiN/TiB2异结构纳米多层膜的共格生长与力学性能

采用多靶磁控溅射法制备了一系列具有不同TiB₂调制层厚度的TiN/TiB_{2纳米多层膜.利用x射线衍射仪、高分辨电子显微镜和微力学探针研究了TiB2层厚变化对多层膜生长结构和力学性能的影响.结果表明，在fcc-TiN层(111)生长面的模板 作用下，原为非晶态的TiB2层在厚度小于2.9nm时形成hcp晶体态，并与fcc-TiN 形成共格外延生长；其界面共格关系为{111}TiN//{0001}TiB2，〈110〉TiN//〈1120〉TiB2.由于共格界面存在晶格失配 度，多层膜中形成拉、压交变的应力场，导致多层膜产生硬度和弹性模量升高的超硬效应， 最高硬度和弹性模量分别达到46.9GPa和465GPa.继续增加TiB2层的厚度，TiB2形成非晶态并破坏了与TiN层的共格外延生长，多层膜形成非晶TiN层和非晶TiB< sub>2层交替的调制结构，其硬度和弹性模量相应降低. 关键词： 2}纳米多层膜')" href="#">TiN/TiB₂纳米多层膜 共格生长 晶体化 力学性能     

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     

Improvement of mechanical and tribological properties in steel surfaces by using titanium-aluminum/titanium-aluminum nitride multilayered system

Improvement of mechanical and tribological properties on AISI D3 steel surfaces coated with [Ti-Al/Ti-Al-N]_n multilayer systems deposited in various bilayer periods (Λ) via magnetron co-sputtering pulsed d.c. method, from a metallic binary target; has been studied in this work exhaustively. The multilayer coatings were characterized in terms of structural, chemical, morphological, mechanical and tribological properties by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), scanning electron microscopy, nanoindentation, pin-on-disc and scratch tests, respectively. The failure mode mechanisms were studied by optical microscopy. Results from X-ray diffraction analysis revealed that the crystal structure of TiAl/TiAlN multilayer coatings has a tetragonal and FCC NaCl-type lattice structures for Ti-Al and Ti-Al-N, respectively, i.e., it was found to be non-isostructural multilayers. An enhancement of both hardness and elastic modulus up to 29 GPa and 260 GPa, respectively, was observed as the bilayer periods (Λ) in the coatings were decreased. The sample with a bilayer period (Λ) of 25 nm and bilayer number n = 100 showed the lowest friction coefficient (∼0.28) and the highest critical load (45 N), corresponding to 2.7 and 1.5 times better than those values for the coating deposited with n = 1, respectively. These results indicate an enhancement of mechanical, tribological and adhesion properties, comparing to the [Ti-Al/Ti-Al-N]_n multilayer systems with 1 bilayer at 26%, 63% and 33%, respectively. This enhancement in hardness and toughness for multilayer coatings could be attributed to the different mechanisms for layer formation with nanometric thickness such as the novel Ti-Al/Ti-Al-N effect and the number of interfaces that act as obstacles for the crack deflection and dissipation of crack energy.     

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.     

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.     

Structural and mechanical properties of compositionally gradient CrNx coatings prepared by arc ion plating

Compositionally gradient CrN_x coatings were fabricated using arc ion plating by gradually increasing N₂ flow rate during the deposition process. The effect of substrate bias, ranging from 0 to −250 V, on film microstructure and mechanical properties were systematically investigated with XRD, SEM, HRTEM, nanoindentation, adhesion and wear tests. The results show that substrate bias has an important influence on film microstructure and mechanical properties of gradient CrN_x coatings. The coatings mainly crystallized in the mixture of hexagonal Cr₂N, bcc Cr and fcc rock-salt CrN phases. N₂ flow rate change during deposition results in phase changes in order of Cr, Cr + Cr₂N, Cr₂N, Cr₂N + CrN, and CrN, respectively, along thickness direction. Phase fraction and preferred orientation in CrN_x coatings vary with substrate bias, exerting an effective influence on film hardness. With the increasing of bias, film microstructure evolves from an apparent columnar structure to a highly dense one. The maximum hardness of 39.1 GPa was obtained for the coatings deposited at a bias of −50 V with a friction coefficient of 0.55. It was also found that adhesion property and wear resistance of gradient CrN_x coatings were better than that of homogeneous CrN coatings.     

Influence of bilayer periods on structural and mechanical properties of ZrC/ZrB2 superlattice coatings

ZrC/ZrB₂ multilayered coatings with bilayer periods ranging from 4.4 to 35.5 nm were synthesized by r.f. magnetron sputtering. X-ray diffraction, scanning electron microscopy and nanoindention were employed to investigate the microstructure and mechanical properties of the nanoscale multilayers. The results indicated that all coatings had the clear multilayered structure with mixed ZrB₂(0 0 1), ZrB₂(0 0 2) and ZrC(1 1 1) preferred orientations. The maximum hardness (41.7 GPa) was observed in the multilayer with 27.5-nm thick period, which is about 25% higher than the rule-of-mixture value of the monolithic ZrC and ZrB₂ coatings. It also exhibited the best adhesion. Its critical load was over 70 mN. While through insert ZrB₂ into ZrC layer periodically, higher residual stress built in ZrC layer can be released.     

Enhancement of surface mechanical properties by using TiN[BCN/BN]n/c-BN multilayer system

The aim of this work is to improve the mechanical properties of AISI 4140 steel substrates by using a TiN[BCN/BN]_n/c-BN multilayer system as a protective coating. TiN[BCN/BN]_n/c-BN multilayered coatings via reactive r.f. magnetron sputtering technique were grown, systematically varying the length period (Λ) and the number of bilayers (n) because one bilayer (n = 1) represents two different layers (t_BCN + t_BN), thus the total thickness of the coating and all other growth parameters were maintained constant. The coatings were characterized by Fourier transform infrared spectroscopy showing bands associated with h-BN bonds and c-BN stretching vibrations centered at 1400 cm⁻¹ and 1100 cm⁻¹, respectively. Coating composition and multilayer modulation were studied via secondary ion mass spectroscopy. Atomic force microscopy analysis revealed a reduction in grain size and roughness when the bilayer number (n) increased and the bilayer period decreased. Finally, enhancement of mechanical properties was determined via nanoindentation measurements. The best behavior was obtained when the bilayer period (Λ) was 80 nm (n = 25), yielding the relative highest hardness (∼30 GPa) and elastic modulus (230 GPa). The values for the hardness and elastic modulus are 1.5 and 1.7 times greater than the coating with n = 1, respectively. The enhancement effects in multilayered coatings could be attributed to different mechanisms for layer formation with nanometric thickness due to the Hall-Petch effect; because this effect, originally used to explain increased hardness with decreasing grain size in bulk polycrystalline metals, has also been used to explain hardness enhancements in multilayered coatings taking into account the thickness reduction at individual single layers that make up the multilayered system. The Hall-Petch model based on dislocation motion within layered and across layer interfaces has been successfully applied to multilayered coatings to explain this hardness enhancement.     

Microstructure and mechanical properties of alumina coatings prepared by double glow plasma technique

Low-temperature growth (600 °C) of α-Al₂O₃ coatings on the stainless steel substrate by double glow plasma technique was achieved. The compositions and microstructures of the coatings prepared at different oxygen flow rates were characterized, respectively, by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectrometry. A phenomenological mechanism for the formation of the Al₂O₃ ceramic coatings during the oxidation process was proposed on the basis of the experimental results. It was obvious that the oxygen flow rates had a great effect on the surface structure of the prepared Al₂O₃ coatings. The dense and smooth Al₂O₃ coatings were prepared at the oxygen flow rate of 15 sccm. In addition, the correlations between the mechanical properties of Al₂O₃ coating and oxygen flow rates were also discussed. The coating prepared at 15 sccm oxygen flow rate exhibited the best mechanical properties with a maximum hardness of 31 GPa and elastic modulus of 321 GPa. The corresponding critical load of scratch adherence for this sample was 47 N.     

Nano indentation measurements on nitrogen incorporated diamond-like carbon coatings

Nanoindentation testing was performed on nitrogen (N₂) incorporated diamond-like carbon (N-DLC) films and deposited using radio-frequency plasma-enhanced chemical vapor deposition technique, with varied percentage of nitrogen partial pressures of 0, 44.4, 66.6, and 76.1%. The values of nanohardness (H) and elastic modulus (E) of these films were obtained from 38 to 22 GPa and 462 to 330 GPa, respectively, as the partial pressure of N₂ increases from 0 to 76.1%. Further, these films were studied for % elastic recovery, ratio between residual displacement after load removal and displacement at maximum load (d _res/d _max), plastic deformation energy and plasticity index parameter (H/E). Both hardness per unit stress and plasticity index per unit stress were found to be maximum at N₂ partial pressure of 76.1%. X-ray photoelectron spectroscopy measurements confirmed the presence of N₂ in these films.     

Micro- and nanocomposite Ti-Al-N/Ni-Cr-B-Si-Fe-based protective coatings: Structure and properties

A new type of nanocomposite Ti-Al-N/Ni-Cr-B-Si-Fe-based coatings 70–90 μm thick produced by combined magnetron sputtering and a plasma detonation technology is created and studied. Phases Ti₃AlN + Ti₃Al₂N₂ and the phases caused by the interaction of plasma with a thick Al₃Ti + Ni₃Ti coating are detected in the coatings. The TiAlN phase has a grain size of 18–24 nm, and other phases has a grain size of 35–90 nm. The elastic modulus of the Ti-Al-N coating is E = 342 ± 1 GPa and its average hardness is H = 20.8 ± 1.8 GPa. The corrosion rate of this coating is very low, 4.8 μg/year, which is about three orders of magnitude lower than that of stainless steel (substrate). Wear tests performed according to the cylinder-surface scheme demonstrate high wear resistance and high adhesion between the thick and thin coatings.