用含添加剂硫的粉末触媒合成金刚石

本文分别用铁镍触媒、含添加剂硫的铁镍触媒在国产六面顶压机上合成了优质金刚石单晶，利用光学显微镜观察，发现所合成的金刚石多为六八面体，晶形完整；在大多数用含添加剂硫的铁镍触媒合成的金刚石的{100}面，有熔坑出现，而用铁镍触媒合成的金刚石没有这种现象；用电子显微镜对熔坑的形貌进行了细致的观察。另外，还发现用含添加剂硫的铁镍触媒合成的金刚石中的包裹体要明显少于用铁镍触媒合成的金刚石中的包裹体。     

金刚石表面电镀镍铁合金工艺研究

在金刚石表面镀一层均匀的镍铁合金镀层,以增强金刚石颗粒的物理化学性能.重点介绍了在金刚石颗粒上实现高质量镍铁合金镀层需要注意的一些问题.设计一种改进的滚镀装置,解决了传统金刚石电镀装置的弊病.在金刚石表面化学镀一层很薄的金属镍,然后利用滚镀装置并严格控制一定的工艺,在60～70目的金刚石颗粒表面获得了一层镀层均匀、厚度达10～200μm、含铁量在20%～25%的高硬度镍铁合金.试验的关键因素是要控制好温度、pH值、电流密度以及防止铁阳极污染镀液.     

感应加热金刚石/镍基复合涂层微观组织与性能

采用感应加热的方式,在65Mn钢基体表面制备了金刚石质量分数为10%的复合镍基涂层,利用SEM、EPMA、XRD对钎涂接头的微观组织和相组成进行了分析,研究了感应钎涂中金刚石/钎料界面的元素扩散机制和形成机制。并利用干砂橡胶轮磨损试验机测试了涂层的耐磨性能,分析了金刚石/镍基涂层的耐磨增强机制。结果表明,钎涂层中钎料合金物相主要为Ni₄B₃、(Ni,Fe)固溶体、Ni₃Si₂、CrB;金刚石与钎料合金发生了冶金反应,金刚石/钎料合金界面的C元素分布促使金刚石表面出现了双层碳化物结构,分别为金刚石侧的Cr₃C₂和在Cr₃C₂表面生长的Cr₇C₃。金刚石复合涂层的耐磨性能显著优于钢基体,涂层60min磨损失重仅0.25g,为钢对比试样磨损失重的1/12,金刚石在磨损过程中起到了阻挡犁沟扩展的作用,涂层的失效机制为镍基合金磨损和金刚石的脱落。     

Magnetic properties and structure of Ni80Fe20/Ni48Fe12Cr40 bilayer films deposited on SiO2/Si（100） by electron beam evaporation

Ni80Fe20/Ni48Fe12Cr40 bilayer films and Ni80Fe20 monolayer films were deposited at room temperature on SiO2/Si（100） substrates by electron beam evaporation. The influence of the thickness of the Ni48Fe12Cr40 underlayer on the structure, magnetization, and magnetoresistance of the Ni80Fe20/Ni48Fe12Cr40 bilayer film was investigated. The thickness of the Ni48Fe12Cr40 layer varied from about 1 nm to 18 nm while the Ni80Fe20 layer thickness was fixed at 45 nm. For the as-deposited bilayer films the introducing of the Ni48Fe12Cr40 underlayer promotes both the （111） texture and grain growth in the Ni80Fe20 layer. The Ni48Fe12Cr40 underlayer has no significant influence on the magnetic moment of the Ni80Fe20/Ni48Fe12Cr40 bilayer film. However, the coercivity of the bilayer film changes with the thickness of the Ni48Fe12Cr40 undedayer. The optimum thickness of the Ni48Fe12Cr40 underlayer for improving the anisotropic magnetoresistance effect of the Ni80Fe20/Ni48Fe12Cr40 bilayer film is about 5 nm. With a decrease in temperature from 300 K to 81 K, the anisotropic magnetoresistance ratio of the Ni80Fe20 （45 nm）/Ni48Fe12Cr40 （5 nm） bilayer film increases linearly from 2.1% to 4.8% compared with that of the Ni80Fe20 monolayer film from 1.7% to 4.0%.     

High temperature tribology of heavily boron doped diamond films against steel

Despite the fact that Fe, Co, and Ni catalyze the phase transition of diamond into graphite, the question of the applicability of diamond as a functional coating of a metal-cutting tool is still open. For this reason, our work contains investigation of wear and friction of heavily boron doped diamond films against steel at elevated temperature, as well as influence of boron concentration on diamond film oxidation resistance. The obtained data indicated that minimum CoF value is achieved in the temperature range within 570–670 °C and strongly depends on boron concentration in coating (CoF decreases with increasing of boron concentration). Wear rate has the same dependence as the CoF, whereas oxidation resistance decreases with increasing of boron concentration. Besides, the presented results are first obtained for boron doped diamond films synthesized under high B/C ratio conditions (of up to 333 ppb).     

Structure and characteristics of Si-coated diamond grits

IntroductionThe properties of diamond tools are determined bythe quality of diamond abrasive and the adhesion betweenthe diamond grits and the bond[1-3].However,duringsintering process,metal bond containing graphitizing ele-ments seriously erodes diamond grits,which reduces thestrength of the diamond grits.Furthermore,diamondstend to be oxidated when the temperature reaches as highas 700℃.Therefore,sintering process of diamond toolsleads the diamond grits to oxidization,significantly de-creas…     

CVD金刚石薄膜及膜-基界面形态

采用直流等离子体财流CVD法在硬质合金基体上沉积了多晶金刚石薄膜,借助XRD、Raman光谱、SEM和EPMA等对金刚石薄膜及膜-基界面的结构、形貌和成分进行了研究.结果表明,结晶度高的刻面型金刚石薄膜质量、纯度较好,膜-基界面处较致密,机械锚固作用明显,结合性能较好沉积前后基体表面形貌变化很大,存在数十微米厚的脱钴-等离子体刻蚀层,等离子体刻蚀导致脱钻表面更加凹凸不平,为金刚石形核提供了有利条件.     

CVD金属石薄膜及膜——基界面形态

采用直流等离子体射流ＣＶＤ法在硬质合金基体上沉积了多晶金刚石薄膜,借助ＸＲＤ,Ｒａｍａｎ,光谱、ＳＥＭ和ＥＰＭＡ等对金刚石薄膜及膜－基界面的结构、形貌和成分进行了研究,结果表明,结晶度高的刻面型金刚石薄膜质量、纯主较好,膜－基界面处较致密,机械锚固作用明显,结合性能较好,沉积前后基体表面形貌变化很大,存在数十数米厚的脱钴－等离子体刻蚀层,等离子体刻蚀导致脱钴表面更加凹凸不平,为金刚石形核提供了有利     

钎焊法制造单层金刚石取孔钻及其界面微观结构

使用钎焊法制造了单层金刚石取孔钻,并与电镀单层金刚石取孔钻的加工性能进行了比较.发现由于具有高的金刚石出刃和结合强度,钎焊取孔钻的锋利度和寿命都优于电镀取孔钻.通过光学显微镜、扫描电子显微镜(SEM)、能谱分析(EDX)和X射线衍射等对钢基体-钎料合金-金刚石的界面微观结构和成分进行了观察和分析,发现钎料合金中的Ni,Cr元素向钢基体中有一定的扩散;而在钎料合金和金刚石上分别存在反应层.钎料合金反应层主要是金刚石表面的C原子扩散进入液相后与Cr反应生成的Cr3C2和Cr7C3,而金刚石反应层是石墨化金刚石表面的位错通道与Cr反应形成Cr3C2并渗透到一定的深度形成的.     

镍改性层增强铜基底沉积金刚石膜的形核(英文)

在铜基底溅射约100nm厚的镍改性层,然后置入纳米金刚石悬浮液中超声震荡加载籽晶,随后在热丝化学气相沉积设备中制备出晶体颗粒接近热力学平衡形态的高质量金刚石膜,其中sp2碳相含量低于5.56%。分别采用激光拉曼光谱、扫描电镜与X射线衍射对金刚石膜的形核与生长进行研究。实验结果表明:在溅射有镍改性层的铜基底上,金刚石的形核密度比在无改性层的铜基底上的形核密度高10倍。镍改性层的增强机制主要来源于两个方面:镍改性层的纳米级粗糙表面增强金刚石籽晶颗粒的吸附;镍改性层的强催化效应加速铜基底上金刚石形核生长所需的石墨过渡层的形成,从而促进金刚石的快速形核。     

Investigations on kinetics of formation of fcc-free surface layers on cemented carbides with Fe-Ni-Co binders

The formation of surface layers free of face centered cubic (Ti,Ta,Nb,W)(C,N) carbonitrides and enriched in ductile binder phase (fcc-free surface layers) was investigated on cemented carbides containing Fe-Ni-Co binders. Cemented carbide alloys with varying Fe-Ni-Co binders were sintered in vacuum atmospheres at 1450 °C for 2, 3 and 5 h. Independent of the binder composition the growth of fcc-free surface layers obeys a parabolic law. For same sintering conditions, fcc-free layer growth kinetics is enhanced by the addition of Fe to Co and Ni binders. Thermodynamic calculations showed that adding Fe to Co and Ni binders increases the solubility of the element nitrogen in the liquid binder phase. The higher solubility of N in Fe-containing binder phases promotes the formation of larger fcc-free surface layers, so that the width of fcc-free surface layers can be modified by controlling the Fe content in the binder phase.     

The oxidation behaviour of 304 stainless steel in oxygenated high temperature water

Characteristics of the oxide films formed on 304 stainless steel immersed in 290 °C oxygenated water for different duration time were examined. The results show that the oxide film is mainly composed of outer irregularly shaped α-(Fe, Cr)₂O₃ and minor spinel in the inner layer. The morphology and chemical composition of the oxide film evolve with increasing immersion time. The surface layer is first enriched in Cr and then enriched in Fe. It is proposed that the oxide nucleated by solid-state reactions with the selective dissolution of Fe and Ni, and grew up through precipitation of extraneous metallic ions from solution.     

电火花沉积Ni/Ti(C,N)金属陶瓷复合涂层的组织及性能研究

目的提高H13模具钢的表面耐磨性,探索金属陶瓷涂层的应用。方法分别用Ti(C,N)基金属陶瓷棒和纯镍棒作为电极,氩气为保护气体,在H13钢表面电火花沉积制备Ni/Ti(C,N)金属陶瓷复合涂层。使用X射线衍射仪对涂层的相组成进行了分析,并用扫描电子显微镜及能谱仪观察涂层的微观结构和元素分布情况,采用显微硬度计和CSM球盘式摩擦计对涂层的显微硬度和不同载荷下的耐磨性进行测试。结果涂层表面为单脉冲沉积斑点堆积而成的溅射状形貌,Fe和Ti元素整体上呈现出分区富集的特征,强化层主要物相包括TiC(0.7)N(0.3)、Ni(17)W3、Ni-Cr-Co-Mo和Fe3Ni2。涂层截面组织均匀,缺陷较少,厚度约为31μm,Fe、Ti和Ni元素均在界面处发生扩散,形成了良好的冶金结合,过渡层与基体相互混合,呈现出机械式的咬合结构。涂层的显微硬度实测最高值达1420HV,约为基体的5.4倍。涂层具有比基体更低的摩擦系数,且30 min内的磨损质量损失仅为基体的1/2,涂层磨损机理主要为粘着磨损和轻微的磨粒磨损。结论在H13钢表面电火花沉积制备的Ni/Ti(C,N)金属陶瓷复合涂层可提高其表面的硬度、耐磨性,且具有一定减摩性,可以起到延长模具寿命的作用。     

Effects of Ti- and Zr-based interlayer coatings on hot-filament chemical vapor deposition of diamond on high-speed steel

The prospect of obtaining good adhesion of diamond films onto steel substrates is highly exciting because the achievement of this objective will open up numerous new applications in industry. However, a major problem with depositing diamond onto steel is high diffusion of carbon into steel at chemical vapor deposition (CVD) temperatures leading to a very low nucleation density and cementite (Fe₃C) formation. Therefore, the study of the nucleation and growth processes is timely and will yield data that can be utilized to get a better understanding of how adhesion can be improved. This work focuses on the adhesion of thin diamond films onto high speed steel previously coated with various interlayers such as ZrN, ZrC, TiC, and TiC/Ti(C,N)/TiN. The role of seeding on nucleation density and the effect of diamond film thickness on stress development and adhesion has been investigated using scanning electron microscopy (SEM), x-ray diffraction (XRD), and Raman spectroscopy (RS). The main emphasis in this study lies with TiC, which for the first time proved to be a suitable layer for diamond CVD on high-speed steel (HSS). In fact, different from other interlayer materials investigated, no delamination was observed after 3 h of CVD at 650 °C when TiC was used. Nevertheless, the increase of diamond film thickness on TiC-coated HSS substrates led to delamination of small areas. This occurrence suggests that there was a distribution of adhesive toughness values at the diamond/TiC interface with the stress development being dependent on film thickness. This paper was presented at the fourth International Surface Engineering Congress and Exposition held August 1–3, 2005 in St. Paul, MN.     

EFFECTS OF ACTIVE ELEMENTS Y AND Ce ON HIGH TEMPERATURE OXIDATION OF Fe-25Cr-40Ni ALLOY

The effects of small amount(≥0.05%)of active elements Y and Ce in Fe-25Cr-40Ni al-loy have been investigated on the kinetics of early stage of high temperature oxidationas well as composition and microsructure of oxide film by ion backscattering and slowpositron beam.The results show that Y and Ce can reduce evidently the high tem-perature oxidation rate of FeCrNi alloy at early stage and can effectively enhance theCr_2O_3 formation and retard the oxide formation of Fe and Ni in the surface layer thusthe microstructure of the oxide film is improved.Y and Ce enter the oxide film andconcentrate within several tens nanometres from surface of the outer layer.The mech-anism of oxidation resistance for Ce is different from Y.Ce can decrease the densityof vacancy defects in oxide layer,so the cations are restrained from diffusion outwardthrough vacancies.While Y can control the outward diffusion of cations through va-cancies at the early statge of oxidation(shorter than 12 min),aften that restrained thecations from diffusion outward along grain boundaries up to 60 min oxidation.     

压痕法研究镶嵌结构界面金刚石膜粘附性能

在铜基体上沉积Cu(Cr)-diamond复合过渡层,用热丝CVD法在复合过渡层上沉积出金刚石膜。用压痕法对沉积的金刚石膜/基结合性能进行了研究。结果表明,在Cu-diamond上沉积的金刚石膜,用147 N压痕时压痕边缘出现大面积崩落,并在基体表面留下被拔出的金刚石凹坑;在Cu-diamond中掺入微量Cr,压痕边缘只形成环形裂纹,增大压痕载荷至441 N,环形裂纹区域增大,并出现部分崩落,崩落区域有被切断的金刚石残留。在Cu-diamond复合层中掺入微量Cr能显著提高金刚石膜/基结合力。     

不锈钢／Al固液轧制复合板材界面的精细结构

应用场发射透射电子显微镜研究了不锈钢／Ａｌ固液轧制复合板材界面的精细结构。结果表明,在钢－Ａｌ之间存在主要由两种金属间化合物组成的界面反应层。靠近钢处由一层细小的（Ｆｅ,Ｃｒ,Ｎｉ）２Ａｌ５纳米晶组成,靠近Ａｌ处由纳米级的（Ｆｅ,Ｃｒ,Ｎｉ）４Ａｌ１３柱状晶组成。反应层附近的Ａｌ中有各种形态的（Ｆｅ,Ｃｒ,Ｎｉ）４Ａｌ１３相析出,并对界面结构的形成进行了初步的分析。     

一种钛基钎料钎焊TiAl/GH536的接头界面组织及性能

采用Ti-Zr-Fe-Cu-Ni-Co-Mo钎料实现了TiAl合金与GH536合金的有效钎焊连接. 运用SEM,EDS,XRD等手段对钎焊接头的界面组织进行了分析,并检测了钎焊接头的抗剪强度. 结果表明,钎焊接头的典型界面组织由TiAl合金一侧到GH536合金一侧包括Ⅰ层(Ti₃Al + TiAl)、Ⅱ层(Al₃NiTi₂)、Ⅲ层(以AlNi₂Ti为主,并含有富铬(Cr,Ni,Fe)_SS、富镍(Cr,Ni,Fe)_SS和(Ni)_SS + TiNi₃)和Ⅳ层(以富铬(Cr,Ni,Fe)_SS为主,并含有富镍(Cr,Ni,Fe)_SS,AlNi₂Ti和(Ni)_SS + TiNi₃). 当钎焊时间为10 min时,在1 110 ~ 1 170 ℃的钎焊温度范围内,随着钎焊温度的升高,钎焊接头的抗剪强度先升高后降低. 钎焊温度对原子扩散和金属间化合物的形成有较大的影响,较低或较高的温度都会导致接头强度偏低. 1 150 ℃钎焊10 min获得的接头抗剪强度最高,为183 MPa,接头主要断裂在Ⅱ层.     

微波功率对(100)晶面取向金刚石薄膜制备的影响

以H2和CH4的混合气体为气源,使用实验室自制10 kW新型装置,采用微波等离子体化学气相沉积法(MPCVD)在Si(100)基体上沉积金刚石薄膜,然后采用扫描电镜(SEM)、Raman光谱以及XRD光谱,以得到表面形貌、样品质量和晶面取向等信息,由此获得微波功率对金刚石薄膜取向的影响。结果表明,微波功率对金刚石膜的质量、表面形貌和晶面取向都有明显地影响,随着微波功率升高,金刚石薄膜的形貌变得规则,薄膜中Isp3/Isp2由1.52提高到6.58,其沉积晶面的I(100)/I(111)由0.38提高到3.93。当微波功率为4 900 W时,所得沉积样品晶面以(100)为主,形貌规则,纯度很高。     

高温钎焊过程中Ni-Cr合金对金刚石磨粒静压强度的影响

采用C类(Ni82Cr7Si4.5B3.1Fe3)和E类(BNi76Cr15P9)两种钎料对金刚石进行真空炉中钎焊。通过静压强度测试对各种状态下的金刚石钎焊性能进行评价,并借助SEM以及拉曼光谱仪对金刚石表面碳化物的形貌和金刚石的石墨化进行检测分析。结果表明:钎焊高温对金刚石强度的影响较合金钎料的化学侵蚀作用而言小很多;触媒元素Ni、Fe和强碳化物形成元素Cr等引起的化学侵蚀,是导致金刚石静压强度降低的两个主要原因;不同品质的金刚石经过高温钎焊后,静压强度值出现不同程度的降低。