BCN薄膜的结构及性能

采用直流磁控溅射法制备了B-C-N薄膜.通过改变基体偏压,研究其对薄膜的成分、结构和力学性能的影响.X射线光电子谱(XPS)和傅里叶变换红外光谱(FTIR)试验结果表明薄膜中存在着B-C,B-N,C-C和C-N键,说明薄膜中B,C,N 3种元素达到了原子级化合.随基体偏压增大,薄膜无序化程度增强.纳米硬度测试结果表明,随着基体偏压的增,纳米硬度和弹性模量不断增加.     

磁控溅射沉积参数对硼碳氮薄膜沉积速率的影响

利用直流磁控溅射技术制备了三元硼碳氮(B-C-N)薄膜,通过改变靶功率、基体偏压、沉积温度和励磁线圈电流,在相同沉积时间内得到不同厚度的薄膜.采用纳米压入仪分析了沉积参数改变对B-C-N薄膜沉积速率的影响规律.结果表明,在低靶功率和高励磁电流的条件下沉积的薄膜,随着靶功率和励磁电流的增加薄膜沉积速率呈线性增长;薄膜的沉积速率随基体偏压的增加呈抛物线状下降;薄膜的沉积速率受基体是否升温影响很大,而受基体所加温度大小影响较小.     

基体负偏压对四面体非晶碳膜结构和性能的影响

采用自主研制的45°单弯曲磁过滤阴极电弧沉积系统于Si基体表面制备了四面体非晶碳(ta-C)膜,研究了基体负偏压对薄膜沉积速率、成分、力学性能及摩擦学性能的影响规律。结果表明,随基体负偏压升高,ta-C膜sp3键含量呈先增后减的变化趋势,在-50V时达到最大值(约64%);其硬度和弹性模量呈相似的变化规律,在-50V偏压下获得最大值(48.22GPa和388.52GPa)。ta-C薄膜的摩擦学性能与其sp3碳杂化键的含量密切相关,在-50V偏压下制备的薄膜具有最小平均摩擦因数值(0.10)。可见,采用单弯曲磁过滤阴极弧电弧制备ta-C薄膜的力学和摩擦学特性主要受薄膜中sp3键含量的制约。     

不同氮含量BCN薄膜的微观结构与摩擦学行为

用电弧增强反应磁控溅射方法(AEMS)在高速钢(W18Cr4V)基体上制备出具有耐磨减摩性能的BCN薄膜。用X射线衍射仪(XRD)、高分辨透射电镜(HRTEM)和X射线光电子能谱(XPS)研究了氮含量对薄膜微观结构的影响;用显微硬度计和销盘式摩擦磨损仪研究了薄膜硬度和摩擦学行为。结果表明:用AEMS方法制备的BCN薄膜为非晶结构,薄膜中的B-N键的含量随氮含量增加而增加;薄膜中氮含量的增加使薄膜的硬度和摩擦系数升高,磨损率降低。     

基体负偏压对四面体非晶碳膜结构和性能的影响

采用自主研制的45°单弯曲磁过滤阴极电弧沉积系统于Si基体表面制备了四面体非晶碳(ta–C)膜,研究了基体负偏压对薄膜沉积速率、成分、力学性能及摩擦学性能的影响规律。结果表明,随基体负偏压升高,ta–C膜sp3键含量呈先增后减的变化趋势,在-50 V时达到最大值（约64%）;其硬度和弹性模量呈相似的变化规律,在-50 V偏压下获得最大值(48.22 GPa和388.52 GPa)。ta–C薄膜的摩擦学性能与其sp3碳杂化键的含量密切相关,在-50 V偏压下制备的薄膜具有最小平均摩擦系数值（0.10）。可见,采用单弯曲磁过滤阴极弧电弧制备ta–C薄膜的力学和摩擦学特性主要受薄膜中sp3键含量的制约。     

基体脉冲偏压对TiN/Cu纳米复合薄膜组织结构、力学及耐磨性能的影响

本文采用轴向磁场增强电弧离子镀在高速钢基体上沉积了TiN/Cu纳米复合薄膜,研究了基体脉冲偏压幅值对薄膜成分、结构、力学性能及耐磨性能的影响。结果表明,薄膜中铜含量随着脉冲偏压幅值的增加先增加而后降低,在一个较低的范围内(1.3-2.1at.%)。X射线衍射结果表明所有的薄膜均出现TiN相,并未观察到Cu相。薄膜的择优取向随着脉冲偏压幅值的增加而改变。薄膜的最高硬度为36GPa,是在脉冲偏压幅值为-200V时得到的,对应了1.6at.%的Cu含量。与纯的TiN薄膜相比,Cu的添加明显增强了薄膜的耐磨性能。     

静电纺丝制备连续SiC亚微米/纳米纤维

采用镶嵌靶反应磁控溅射技术,通过调节氮分压及基体偏压在M2高速钢基体表面制备了一系列耐热的(Ti,Al)N硬质薄膜,并用XRD,EDS及纳米压入法、划痕法等方法研究了(Ti,Al)N薄膜的成分、相结构与力学性能的关系。结果表明,氮分压和基体偏压对(Ti,Al)N薄膜取向及Ti、Al、N原子含量有明显影响,从而导致薄膜硬度及膜基结合性能发生变化。研究中,在氮分压为33.3×10-3Pa、基体偏压为-100V时制备的(Ti,Al)N薄膜力学性能最优,其纳米硬度为43.4GPa,达到40GPa超硬薄膜的要求。     

脉冲偏压对TiAlCN薄膜结构与力学性能的影响

利用多弧离子镀-磁控溅射复合技术通过改变脉冲偏压在Si片与SS304基体表面制备了TiAlCN薄膜,研究了不同脉冲偏压对薄膜结构和力学性能的影响。薄膜成分、表面形貌、相结构及力学性能分别利用能量弥散X射线谱(EDS)、扫描电镜(SEM)、X射线衍射(XRD)和纳米压痕仪等设备进行表征。结果表明,随着脉冲负偏压的增加,薄膜中Ti元素的含量先减小后增大,而Al元素有相反的变化趋势。适当增大脉冲偏压,薄膜表面颗粒、凹坑等缺陷得到明显改善。物相分析表明TiAlCN薄膜主要由(Ti,Al)(C,N)相,Ti4N3-x相和Ti3Al相组成。薄膜平均硬度与弹性模量随脉冲负偏压的增加先增大后减小,在负偏压-200 V时达到最大值分别为36.8 GPa和410 GPa。     

负偏压对电弧离子镀复合TiAlN 薄膜的影响

采用电弧离子镀技术,以W18Cr4V高速钢为基体,调整基体负偏压,制得多个复合TiAlN薄膜试样,研究了基体负偏压对薄膜微观组织形貌、物相组成、晶格位向、硬度、厚度和沉积速率的影响。结果表明,过高或过低的负偏压会使得膜层表面不平整,显微硬度下降。当负偏压为200 V时,膜层的沉积速率最大;负偏压为150 V时,有利于薄膜(111)晶面的择优取向生长,且TiAlN膜的硬度最高。     

偏压对DLC薄膜结构及摩擦学性能的影响

目的通过调节偏压,改善无氢DLC薄膜的微观结构,提高其力学性能和减摩抗磨性能。方法采用离子束辅助增强磁控溅射系统,沉积不同偏压工艺的DLC薄膜。采用原子力显微镜(AFM)观察薄膜表面形貌,采用拉曼光谱仪对薄膜的微观结构进行分析,采用纳米压痕仪测试薄膜硬度及弹性模量,采用表面轮廓仪测定薄膜沉积前/后基体曲率变化,并计算薄膜的残余应力,采用大载荷划痕仪分析薄膜与不锈钢基体的结合力,采用TRB球-盘摩擦磨损试验机评价薄膜的摩擦学性能,采用白光共聚焦显微镜测量薄膜磨痕轮廓,并计算薄膜的磨损率。结果偏压对DLC薄膜表面形貌、微观结构、力学性能、摩擦学性能都有不同程度的影响。偏压升高导致碳离子能量升高,表面粗糙度呈现先减小后增加的趋势,-400V的薄膜表面具有最小的表面粗糙度且C─C sp^3键含量最多,这也导致了此偏压下薄膜的硬度最大。薄膜的结合性能与碳离子能量大小呈正相关,-800 V时具有3.98 N的最优结合性能。不同偏压工艺制备的薄膜摩擦系数随湿度的增加,均呈现减小的趋势,偏压为-400V时,薄膜在不同湿度环境中均显示出最优的摩擦学性能。结论偏压为-400 V时,DLC薄膜综合性能最优,其表面粗糙度、硬度、结合力和摩擦系数分别为2.5 nm、17.1 GPa、2.81 N和0.11。     

沉积温度和退火处理对BCN薄膜结构的影响

采用脉冲激光沉积技术,在Si(100)基片上制备了BCN薄膜,研究了沉积温度和退火处理对BCN薄膜组分和结构的影响。利用傅里叶变换红外光谱(FTIR)和X射线光电子能谱(XPS)对制备的BCN薄膜进行了表征。结果表明:沉积温度升高时,BCN薄膜的组分无明显改变。所制备的BCN薄膜包含B—N,C—B和C—N化学键,是由杂化的B—C—N键构成的化合物。真空退火温度为700℃时,BCN薄膜结构稳定;大气退火温度达到600℃时,BCN薄膜表面发生氧化分解,同时有C≡N键形成,表明C≡N键具有较好的高温热稳定性。     

Effect of nitrogen pressure on structure and optical properties of pulsed laser deposited BCN thin films

Amorphous boron carbon nitride (BCN) thin films were deposited on Si (100) and quartz substrates by laser ablation of a boron carbide (B₄C) target in nitrogen atmosphere. The effects of the nitrogen pre ssure (p_N2) on the film deposition rate, composition, structure and optical properties were investigated. The film deposition rate was measured by a surface profiler, which increased from 3.4 to 6.25 nm/min at elevated p_N2. Structure and composition of the films were investigated by X-ray photoelectron spectroscopy (XPS) and Fourier-transform infrared (FTIR) spectroscopy. FTIR and XPS analyses indicated that the as-deposited BCN films contained B-C, N-C and B-N chemical bonds, implying the formation of ternary BCN compounds. The nitrogen content in the films increased gradually and then saturated up to ∼ 26 at.% at 10 Pa p_N2. The optical band gap (E_g) increased from 3.78 to 3.92 eV with increasing p_N2 from 2 to 15 Pa. The evolution of E_g is in accordance with the change of film compositions and bonding states.     

具有TiN过渡层的BCN薄膜制备与力学性能

用电弧增强磁控溅射(AEMS)装置在高速钢(W18Cr4V)和Si(100)基体上制备了具有TiN过渡层的BCN薄膜,用X射线衍射(XRD)仪和傅里叶红外光谱(FTIR)分析了薄膜的微观结构,用划痕仪测试了薄膜的结合力,用显微硬度计和销盘式摩擦磨损实验仪测试了薄膜的硬度和摩擦学性能。结果表明:本实验条件下制备的具有Ti N过渡层的BCN薄膜的硬度为23 GPa,薄膜与GCr15钢球对磨的摩擦系数为0.3,具有TiN过渡层的BCN薄膜的结合力和摩擦学性能较BCN单层薄膜有明显提高。     

PECVD OF HARD AND ELASTIC BCN COATINGS

Compounds of the B-C-N system are very promising to produce superhard coatings with good tribological, chemical and thermal properties. Consequently, BCN films were prepared by plasma enhanced chemical vapor deposition (PECVD). The films were deposited from gaseous mixtures of BCl3-C2H4-N2-H2-Ar in different unipolar and bipolar pulsed glow discharges at 550℃ and analyzed with respect to composition, electronic structure and mechanical properties. The micro structure and composition of the BCN films were determined by scanning electron microscopy (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and reflection electron energy loss spectroscopy (REELS). Mechanical properties were characterized using both the traditional Vickers method and nanoindentation. The films, that were deposited using a bipolar pulsed generator, were weak and had a sponge-like structure, whereas the films prepared using an unipolar generator were well adherent, had a hardness of more than 11GPa and very high e     

Tuning bond contents in B–C–N films via temperature and bias voltage within RF magnetron sputtering

Using radio frequency reactive magnetron sputtering technique with boron and graphite targets, amorphous B–C–N films were synthesized on the silicon (100) substrate applied with different temperatures and bias voltages. The structural and bonding characteristics of the synthesized films were characterized by Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS). The bond contents in the B–C–N films show remarkable dependence on the bias voltage applied to the substrate at 400 °C.     

Effect of radio-frequency electric power applied to a boron nitride unbalanced magnetron sputter target on the deposition of cubic boron nitride thin film

Cubic boron nitride (c-BN) films were deposited by an unbalanced magnetron sputtering method. A (100) Si wafer with a nanocrystalline diamond thin film as a surface coating layer or that without it was used as a substrate. The target power was varied from 100 to 400 W. A boron nitride target was used, which was connected to a radio frequency power supply. High frequency power connected to a substrate holder was used for self-biasing. The deposition pressure was 0.27 MPa with a flow of Ar (18 sccm) — N₂ (2 sccm) mixed gas. The existence of threshold bias voltages for c-BN formation and resputtering were observed irrespective of target power. The bias voltage window for c-BN formation broadened with increased target power. The deposition rate decreased with enhanced bias voltage and decreased target power. Residual stresses of the films did not vary noticeably with target power within the target power range of c-BN formation. A parameter space for c-BN formation according to the target power and the bias voltage, as two variables, was suggested.     

Composition and mechanical properties of AlC, AlN and AlCN thin films obtained by r.f. magnetron sputtering

Aluminum carbide (Al-C), aluminum nitride (Al-N), and aluminum carbonitride (Al-C-N) thin films were grown onto Si [100] substrates by r.f. reactive magnetron sputtering at 400 °C. The Al-N coatings were obtained by sputtering of Al (99.9%) target in Ar/N₂ atmosphere and the Al-C and Al-C-N by co-sputtering of a binary (50% Al, 50% C) target in argon and in Ar/N₂ mixture, respectively. The d.c. bias voltage was varied between 0 and − 150 V. The films were characterized by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), Fourier transformed infrared spectroscopy (FTIR) and the mechanical properties by nanoindentation. The structure of the films has been determined by XRD, which shows that amorphous films are formed in all cases. The variation of polarization bias voltage produced chemical differences in the films. As the bias voltage is increased, the Al content is reduced in all three materials. The nitrogen content also varied between 10 and 14 at.% for Al-N coatings, remaining practically constant (21 at.%) for the Al-C-N films. The Berkovich hardness results were 7.0, 17.2 and 9.2 GPa for Al-C, Al-N, and Al-C-N films, respectively.