残余氧对TiN+Si3N4纳米复合薄膜硬度的影响

用直流等离子体增强化学气相沉积设备在不锈钢表面沉积纳米晶TiN和纳米非晶Si3N4复相薄膜．主要研究了氧元素对薄膜硬度的影响．结果表明，薄膜中极其微量的氧含量就会使nc—TiN α-SiaN4薄膜的硬度大幅降低．薄膜中氧含量小于0.2％(原子分数)，薄膜硬度可以达到45～55GPa，而氧含量升至1％—1．5％后，薄膜硬度降至30GPa左右．其原因与晶界处形成SiOx相有关。     

Si3N4／铁基结合剂氮化金刚石薄膜涂层节块

本介绍Si3N4(代替部分金刚石浓度）配合铁基（以Fe代Co)结合剂氮化金刚石薄膜涂层节块,可大大降低成本,该节块性能良好,有较高使用效果及经济效益。     

β-Si3N4晶种的制备和自增韧Si3N4陶瓷

分别以Yb2O3和MgO为添加剂，通过对原始α-Si3N4粉热处理的方法，分别在1700℃和1650℃的温度下，制备出了具有柱状形貌的β-Si3N4晶体颗粒。并将这2种β-Si3N4晶粒在未经酸或碱处理的情况下，作为晶种添加到原始α-Si3N4粉中，采用热压烧结工艺，以Yb2O3作为烧结添加剂，在1800℃下制备了自增韧Si3N4陶瓷材料。研究结果表明，以Yb2O3和MgO为添加剂都可以在较低的温度下获得适合于作晶种的β-Si3N4晶体颗粒。2种晶种引入到Si3N4陶瓷中都可以有效地改善材料的断裂韧性，但晶种中的残留相对自增韧Si3N4陶瓷的高温强度产生了强烈的影响。XRD和TEM分析结果表明，含Mg相的存在是导致Si3N4陶瓷高温强度的剧烈降低和促进晶间相析晶的主要原因。     

TiAl与Si3N4f/Si3N4复合材料钎焊接头界面结构及性能研究

采用AgCuTi钎料实现了TiAl与Si3N4f/Si3N4复合材料的钎焊,确定了钎焊接头的典型界面组织结构为TiAl/AlCuTi/Ag(s,s)/TiN/Si3N4f/Si3N4。钎焊过程中,液相钎料在Si3N4f/Si3N4复合材料表面发生较好润湿,钎料中活性元素Ti与Si3N4基体及纤维发生反应形成连续的TiN化合物层。过高的钎焊温度或过长的保温时间导致钎缝中脆性的AlCuTi化合物增加,且由于接头应力的作用在钎缝中产生微裂纹甚至开裂,严重地降低了钎焊接头性能。当钎焊温度T=850℃,保温时间为10min时,接头抗剪强度达到最大,为9.4MPa,超过Si3N4f/Si3N4母材层间抗剪强度的60%。断口分析表明:压剪过程中,断裂发生在Si3N4f/Si3N4复合材料一侧。     

TiN/Si3N4纳米多层膜硬度对Si3N4层厚敏感性的研究

通过反应磁控溅射制备了一系列不同Si3N4层厚的TiN/Si3N4纳米多层膜,利用X射线衍射仪、高分辨透射电子显微镜、扫描电子显微镜和微力学探针表征了多层膜的微结构和硬度,研究了其硬度随Si3N4层厚微小改变而显著变化的原因.结果表明,在TiN调制层晶体结构的模板作用下,溅射态以非晶存在的Si3N4层在其厚度小于0.7 nm时被强制晶化为NaCl结构的赝晶体,多层膜形成共格外延生长的{111}择优取向超晶格柱状晶,并相应产生硬度显著升高的超硬效应,最高硬度达到38.5GPa.Si3N4随自身层厚进一步的微小增加便转变为非晶态,多层膜的共格生长结构因而受到破坏,其硬度也随之降低.     

无压浸渗制备Si3N4／Al复合材料的反应浸渗机理

采用“中断浸渗”方法获得保留了“浸渗前沿”的样品，应用扫描电子显微镜和X射线能谱分析了浸渗界面上的形貌和成分变化，深入讨论了浸渗界面推进过程中的物理、化学反应过程。采用扫描电镜等微观分析手段观察了复合材料显微形貌，探讨了界面反应机理。研究结果表明：浸渗界面推进过程中熔体中的Mg富集在浸渗前沿的预制体上，并与预制体发生反应；Al／Si3N4界面反应产物AlN相形成“楔形”向Si3N4单元心部推进，细观上呈现含毛细通道的胞状辐射形貌，大量毛细通道确保了Al和Si3N4之间的置换反应持续进行：Al与Si3N4的置换反应产物Si绝大部分溶解在铝镁合金熔体中。     

Si_3N_4/Ni和Si_3N_4/Ni_3Al的界面固相反应

使用扫描电子显微镜、电子能谱仪、X射线衍射等研究了在N2气氛中1150℃×10 h等温热处理的Si3N4/Ni,Si3N4/Ni3Al平面偶界面固相反应区的形貌、成分分布、显微结构及相组成。结果表明:Si3N4/Ni界面固相反应形成约20μm厚的反应区,反应区主要由Ni3Si构成,其中分布着大量细密的孔洞;而Si3N4/Ni3Al界面固相反应形成约2μm厚的反应区,反应区具有比Ni3Al高得多的Al含量,反应区由NiAl及Ni3Si构成。Si3N4/Ni3Al具有比Si3N4/Ni高得多的界面化学相容性。     

Si3N4／Cu68Ti20Ni12的界面结构及连接强度

采用Cu68Ti20Ni12钎料进行了Si3N4／Si3N4的活性钎焊连接。结果表明：钎焊温度和时间对连接强度有重要影响；在1373K，10min的连接条件下，Si3N4/Si3N4连接强度达到最大值289MPa。通过对Si3N4／Cu68Ti20Ni12界面区的微观分析：发现Ti，Ni明显向Si3N4方向富集，相对Ni而言，Ti的富集区更靠近Si3N4陶瓷，而Si则向钎料方向扩散，Cu在接头中心富集：界面区存在2层反应层，反应层Ⅰ为TiN层，而反应层Ⅱ则由TiN，Ti5Si4，Ti5Si3，Ni3Si及NiTi化合物组成。     

Csf／Si3N4复合材料的力学性能和微波介电性能研究

采用热压烧结的方法，以α-Si3N4粉和短切碳纤维为主要原料，以Y2O3和La2O3为烧结添加剂，制备Csf／Si3N4复合材料，研究了其力学性能和微波介电性能。结果表明，该Csf／SiaN。复合材料的抗弯强度随纤维含量的增加呈现下降的趋势，是由于碳纤维氧化所产生的缺陷所致；当纤维含量较低时，断裂韧性随纤维含量增大而增大，由于纤维氧化产生的缺陷阻止了裂纹进一步的扩展或使裂纹发生了偏转。当纤维含量超过1％（质量分数）后，随着纤维含量的增大，氮化硅显微结构发生变化，氮化硅陶瓷本身断裂韧性减小，使Csf／Si3N。复合材料断裂韧性逐步降低。当碳纤维含量在0～1％（质量分数）时，随着碳纤维含量的增加，介电常数ε’，ε＂和介电损耗tanδ均随着纤维含量的增加而增大，而且所制得的复合材料表现出较强的频散效应：当纤维含量继续增加时，在相同的频率下，介电常数下降，材料的频散效应逐渐消失。     

TiN/Si3N4纳米复相陶瓷电加工表面质量的正交试验研究

通过对TiN/Si3N4纳米复相陶瓷电火花线切割加工电参数的优化试验,找出了影响表面粗糙度值的主要因素和较优组合,为进一步开发TiN/Si3N4纳米复相陶瓷材料的应用提供了依据。     

低频机械谱术测量薄膜切变模量及微量油膜探测

描述了工作在共振和次共振模式下的低频机械波谱仪的基本原理．主要介绍了研究金属衬底上薄膜的物理性质的两种方法：第一种方法，用于测量沉积在钼丝上的TiN／Ti(C，N)多层膜的切变模量和内耗；第二种方法，用于探测钢片表面微量油膜的存在．尽管这两种技术有着各自不同的应用目的及对象，但它们均源自能够导致机械能损耗的表面效应。     

共析转变过程中内耗与复模量行为的对比

通过系统地改变振动频率和变温速率，用低频强迫振动模式，测量了Ｚｎ－２２％Ａｌ合金的动力力学性能，观测到析析转变时具有典型一级相变特征的内耗，峰；结合实验结果；从复模量的实部和虚部随振动频率和变温速率的变化关系出发，讨论了界面的稳定性和低频相变内耗的特征。     

CARBON NITRIDE FILMS PREPARED AT DIFFERENT N2／Ar RATIOS BY CLOSED FIELD UNBALANCED REACTIVE MAGNETRON SPUTTERING

Carbon nitride ( CNx thin films have been deposited onto Si(100) (for structural and mechanical analyses) and M42 high-speed-steel (for tribological measurements) substrates at room temperature by closed-field unbalanced magnetron sputtering. The mechanical and tribological properties of these films were highly dependent on the N/C concentration ratio that was adjusted by the F(N2)/F(Ar) flow-rate ratio at fixed substrate biasing of -60V during deposition. The films were characterized by employing scanning electron microscopy (SEM), atomic force microscopy (AFM), nano-indentation measurements, X-ray photoelectron spectroscopy (XPS), Raman scattering and Fourier transform infrared (FTIR) spectroscopy, pin-on-disc tribometer, scratch tester, and Rockwell-C tester. The results showed that the N content in the films increased with the N2 pressure. However, the maximum N/C ratio obtained was 0.25. The nanohardness was measured to be in the range of 11.7-20.8 GPa depending on the N/C ratios. The XPS N 1s spectra showed the existence of both N-C sp^2 and N-C sp^3 bonds in films. Raman and FTIR spectra exhibited that N-C bonds were fewer when compared to other N-C bonds. The friction coefficient of the film deposited onto steel substrate with N/C=0.26 was measured to be -0.08 and for film with N/C=0.22 a high critical load of 70N was obtained. The tribological data also showed that the wear rates of these films were in the range of -10^-16m^3/Nm, indicating excellent wear resistance for CNx films.     

PREPARATION AND SURFACE CHARACTERIZATION OF TiO_2 THIN FILMS ON GLASS BY MAGNETRON SPUTTERING METHOD

1. IntroductionTiOz thin films have excellent properties sucl1 as l1igh ref1actitre il1dex, outstal1diugoptical tra11sl11ittallce, high dielectric constant and physical chemical stabilityll'2]. Recently',the TiO2 thi1l films have drawn more attel1tions oll photocatalysis, optical coating, al1dsolar cell fab.ication[3'4l. In this work we deposited Ti thin film on glass substrate b}-nlagl1etroll sputterillg lllethod and allllealing Ti tl1in fi1l11 to fOrlll TiO2 tl1ill fi1m.2. ExperimelltalT…     

EFFECT OF AGING ON INTERNAL FRICTION,ELASTIC MODULUS AND MECHANICAL PROPERTIES OF TERNARY Mn-Cu-Al ALLOYS

Internal friction and elastic modulus of ternary Mn-Cu-Al alloys containing 56—60wt-% Mn,0-3.59 wt-% Al were measured with acoustic frequency,1 kHz,in the tempera-ture range of-150 to 150℃.It was found that when the specimen was aged in the temperaturerange under the spinodal curve within the miscibility gap(400—500℃),the internal fric-tion increases with an increase of the aging time and reaches a maximum value at a certain ag-ing time which is shorter with a higher aging temperature.Two internal friction peaks whichdid not appear before the aging were observed above room temperature after a definite agingtime.These are respectively the martensitic tranformation peak and the relaxation peak orig-inating from the stress-induced movement of the twin boundaries.The former peak shifts to-ward higher temperatures with an increase of the aging time,whereas the relaxation peak ap-pearing at 15℃,is independent of the aging time and temperature.The activation energy as-sociated with the relaxation peak was found to be 0.56 eV which is about the same as that ofthe relaxation peak in binary alloy containing 90 wt-% Mn.It was also found that thehardness,strength and the brittleness of the specimen increase when aged below the spinodalcurve within the miscibility gap.The addition or Al enhances the strength but reduces the in-ternal friction of the specimen.A choice of suitable aging time and temperature can give anoptimum compromise of high strength and high internal friction.Analysis of experimental re-sults suggests that spinodal decomposition leads to Mn-rich zones in the specimen and thuscauses the phase transformation and the change of mechanical properties of the specimen.     

CHARACTERISTICS OF INTERNAL FRICTION AND MODULUS ASSOCIATED WITH NON-EQUILIBRIUM DIFFUSION-TYPE PHASE TRANSFORMATION IN EUTECTOID Al-Zn ALLOY

The characteristics of the low frequency internal friction and the modulus effect associatedwith the non-equilibrium spinodal pretransformation and the following discontinuous trans-formation was investigated in an as-quenched eutectiod Al-Zn alloy.It was observed that theloss of the stability in the lattice,which corresponded to the large-amplitude long-wavelengthstatic concentration wave in the non-equilibrium spinodal pretransformation,did not induceany effect of localized soft modulus.Although there are two aging internal friction peaks inphase transformation which correspond to the appearance and disappearance of the coherencyin spinodal pretransformation and the maximum of the interface area in the discontinuoustransformation respectively,the effect of localized soft modulus did not take place yet.     

时效对Mn-Cu-Al三元合金的内耗、杨氏模量和力学性能的影响

测量了Mn-Cu-Al三元合金(含56-60wt-％Mn,0-3.59wt-％Al)在-150—150℃的声频内耗,发现当试样在调幅线的温度范围内进行时效时,内耗随着时效时间的增加而增加,并在特定的时间内达到极大值.时效温度越高,达到极大值的时间越短.在时效一定的时间后出现马氏体相变峰和孪晶界面弛豫峰.相变峰随着时效时间的增加而向高温移动;弛豫峰则出现在15℃左右(频率约1kHz),测得其激活能是0.56eV. 在调幅线内时效使合金的硬度、强度及脆性墙加,Al元素有增加合金的强度而降低其内耗的作用.实验结果表明,在450℃时效2—3h,可得到合金的内耗和强度的最佳综合指标. 根据内耗、模量、金相检验和X射线分析的结果,认为调幅分解后产生的富Mn区是合金发生相变和高内耗的来源,也是合金的强度增加和韧性降低的原因.     

磁电复合材料CuFe2O4/PbZr0.53Ti0.47O3的内耗与介电损耗

制备了组分为xCuFe2O4-(1-x)PbZr0.53Ti0.47O3(其中x=0．1，0．2，0．3，1．0)的磁电复合材料，XRD实验表明，样品中只存在着CuFe2O4和PbZr0.53Ti0.4703相．利用多功能摆测量了样品在低频下(0.1--6．4Hz)的内耗，同时利用HP4194A阻抗分析仪测量了样品低频(100Hz--1 MHz)的介电损耗，分析了复合物中CuFe2o4和PZT对内耗及介电损耗分别所作的贡献．     

复合体材料CuFe2O4-Pb(Mg1/3Nb2/3)O3的内耗和介电损耗

用传统的固相反应方法制备了CuFe2O4-Pb(Mg1／3Nb2／3)O3复合体材料陶瓷，用X射线衍射确定了复合体材料中各相的存在．用双端振动簧法研究了样品在-200—400℃的音频内耗谱，在37．6℃发现一个很大的内耗峰P1，并伴随着约9％的模量的软化，表明了相变的存在．在室温下，测量了介电常数ε′和介电损耗tanδ随频率变化的关系；同时，测量了复合体材料的介电常数和介电损耗随温度的变化关系，进一步验证P1峰由立方到四方的相变引起．最后给出样品的磁滞回线。     

TiCx/Ni3Al复合材料相界面显微结构及界面纳米硬度与弹性模量分布

采用SEM,EDS等对融渗工艺制备的C/Ti比x分别为0.6,0.7,0.8和0.9的四种不同TiCx/Ni3Al复合材料进行了研究，证实Ti元素向金属相存在较强的扩散，而Ni和Al元素几乎没有向陶瓷相中扩散，扩散的结果形成了两相界面之间直接的原子结合，增加了复合材料相界面结合的强度和韧性，利用纳米压痕技术研究了复合材料相界面附近的纳米硬度H和弹性模量E，二者在相界面附近均呈连续梯度分布特征，并且TiC0.7/Ni3Al复合材料在界面处具有较高的纳米硬度值。