表层钴含量对基体/涂层界面组织结构和刀具切削性能的影响

本文采用五种预处理工艺对硬质合金刀片表面进行了处理,制备了具有不同表面Co含量的刀片。在此基础上,研究了刀片表层Co含量对基体与涂层界面组织结构和切削性能的影响。采用扫描电镜(SEM)分析了表层钴含量及其微观形貌;借助压痕剥落试验来评价基体与涂层的结合情况;通过切削实验对比涂层刀片的耐磨性能和抗冲击性能。实验结果表明:不同预处理工艺处理的刀片表层钴含量在其基体标称钴含量±100%范围内变化。随着表层钴含量的提高,其显微形貌差异较大:在基体表层钴含量低于标称含量时,基体/涂层界面组织松散,基体与涂层的结合情况较差,随着钴含量提高,基体/涂层界面组织逐渐致密,界面结合力也提高,当钴含量高至其标称钴含量后,基体/涂层界面平整度又逐渐下降,界面结合力又下降。随着基体表层钴含量的提高,涂层刀片的耐磨性能降低,抗冲击性能提高。     

细晶粒硬质合金预处理工艺优化及金刚石涂层性能研究

为了进一步拓展金刚石涂层刀具的产业化应用,提升金刚石涂层刀具的结合力性能,本文开展了细晶粒钨钴类硬质合金的化学预处理研究,考察了三步法预处理工艺对不同晶粒度基体形貌和成分的影响,实现了金刚石涂层与基体的高结合强度。利用扫描电子显微镜和EDS能谱仪对预处理后基体的表面形貌和钴含量以及涂层形貌进行分析,采用拉曼光谱、X 射线衍射光谱对涂层物相结构进行分析表征,并利用固体颗粒冲刷评价金刚石涂层的抗冲刷性能。结果表明:酸处理对Co的去除起着重要作用,WC晶粒越小所需酸处理的时间越长,碱处理对WC的刻蚀能力表现出先增大后减小的趋势,在3min时达到最大Co暴露量。由此分别确定了WC-6%Co(0.2,0.4,1.0 μm)基体三步法最佳工艺,三步法预处理后的基体均获得均匀致密,晶粒取向为(111)面,抗冲刷性能优异,膜基结合性能好的金刚石涂层。     

利用中间阻碍层在硬质合金上沉积高粘结强度的金刚石 …

能完全阻止钴由基体渗入表面而且大可与ＷＣ－Ｃｏ硬质合金相比的阻碍底层在本研究中取得了进展，这些底层连续无缺陷，沉积时硬质合金基体没有损坏和脱碳现象，底层上沉积 钛基中间层。对以此方法涂覆后的硬质合金基体采用特殊的激光照射工艺进行纳米晶金刚石引晶处理和用等离子体ＣＶＤ法进行金刚石涂层。引晶过程采用超声波处理，可以将石墨碳从基体表面除去。用此方法获得的金刚石涂层与基体表面粘结牢固，这是在中间层，金刚石     

硬质合金表面化学脱钴对金刚石涂层的影响

以CH3COCH3和H2为反应气源,采用热丝CVD法在经过一步法和碱酸两步法预处理的YG6硬质合金(WC-6％Co)基体上沉积了金刚石涂层.采用扫描电镜、能谱仪、硬度计等对样品进行了分析检测,着重考察了一步法和两步法化学腐蚀脱钴预处理工艺对硬质合金基体表面形貌、钴含量以及其对所得金刚石涂层的形核密度、晶粒尺寸、膜基附着性能等的影响.实验结果表明:无论是一步法还是两步法脱钴预处理工艺,都能去除YG6硬质合金基体表面的钴元素,一步法最佳腐蚀时间为15 min,两步法最佳腐蚀时间为5min,两步法效果强于一步法.在经两步法5min酸蚀脱钴预处理的YG6基体上,获得了膜基粘着性能良好、结晶性能好的微米金刚石涂层.     

前处理工艺对NdFeB表面真空蒸镀Al薄膜结构及性能的影响

为了开发烧结钕铁硼磁体表面低损伤、环境友好型镀膜前处理工艺,在分别采用抛光、酸洗(50 s)、吹砂、吹砂+酸洗(5 s)4种不同工艺处理的烧结NdFeB磁体表面真空蒸镀Al薄膜。经不同工艺前处理的NdFeB基体和涂层的形貌采用扫描电子显微镜进行观察;采用拉伸试验对Al涂层和基体之间的结合力进行测试;NdFeB基体的自腐蚀行为采用电化学极化曲线进行表征。结果表明:吹砂前处理后NdFeB基体表面存在一层晶粒损伤层,导致镀Al薄膜试样镀层与基体之间的结合力(9.54 MPa)最差。而采用吹砂+酸洗(5 s)前处理后NdFeB表面镀Al试样镀层与基体之间结合力可达13.58 MPa。酸洗(50 s)及喷砂+酸洗(5 s)前处理后基体试样的自腐蚀电流密度基本相同(21μA·cm~(-2)),仅为抛光及喷砂前处理基体试样的20%。在4种工艺当中,吹砂+酸洗(5 s)前处理工艺获得最高的结合力和优异的耐腐蚀性能。     

酸浸+等离子体刻蚀YG6微米-纳米金刚石复合涂层工具研究

金刚石涂层工具一直是金刚石膜工具应用研究的主流.制约其产业化的主要因素是涂层的附着力低和微晶金刚石涂层工具的加工精度差.通过对衬底的有效预处理和CVD沉积过程控制的研究,开发在硬质合金基体上沉积高结合强度、低粗糙度的金刚石涂层新技术,对于实现CVD金刚石涂层刀具高效、高精度切削加工具有重要意义.对旨在提高金刚石涂层附着力的预处理技术,本文探索了将酸蚀脱钴+等离子体刻蚀处理衬底法.利用优化的沉积工艺,在酸浸+等离子刻蚀处理的YG6刀片上沉积的两层金刚石复合膜表面粗糙度为0.13μm,附着力压痕测试临界载荷大于1500N.金刚石涂层工具的切削加工性能明显高于无涂层硬质合金工具.在加工ZAlSi12合金时,单层和两层金刚石涂层车刀片的切削寿命分别是无涂层车刀片切削寿命的21倍和28倍.     

酸浸＋等离子体刻蚀YC6微米-纳米金刚石复合涂层工具研究

金刚石涂层工具一直是金刚石膜工具应用研究的主流。制约其产业化的主要因素是涂层的附着力低和微晶金刚石涂层工具的加工精度差。通过对衬底的有效预处理和CVD沉积过程控制的研究，开发在硬质合金基体上沉积高结合强度、低粗糙度的金刚石涂层新技术，对于实现CVD金刚石涂层刀具高效、高精度切削加工具有重要意义。对旨在提高金刚石涂层附着力的预处理技术，本文探索了将酸蚀脱钴＋等离子体刻蚀处理衬底法。利用优化的沉积工艺，在酸浸＋等离子刻蚀处理的YG6刀片上沉积的两层金刚石复合膜表面粗糙度为0．13μm，附着力压痕测试临界载荷大于1500N。金刚百涂层工具的切削加工性能明显高予无涂层硬质合金工具。在加工ZAlSi12合金时，单层和两层金刚石涂层车刀片的切削寿命分别是无涂层车刀片切削寿命的21倍和28倍。     

WC-(W,Ti)C-(Ta,Nb)C-Co涂层硬质合金的组织与性能

用控制烧结工艺制备了均质基体结构与梯度基体结构的WC-(W,Ti)C-(Ta,Nb)C-Co硬质合金,采用化学气相沉积工艺在合金表面涂上TiCN/Al203/TiN涂层,制备成相应的涂层硬质合金及刀片.运用金相观察、扫描电镜分析、三点抗弯强度测试及切削性能测试,研究了梯度基体结构对涂层WC-(W,Ti)C-(Ta,Nb)C-Co硬质合金的组织与力学性能影响.结果表明,采用梯度烧结工艺,可以在合金的表层形成梯度韧性区,该韧性区可以提高裂纹扩展阻力.所制备的梯度基体结构合金的抗弯强度明显超过均质基体结构合金,而相应涂层硬质合金刀片在保持耐磨性能的同时能显著提高抗冲击性能.     

YG6金刚石涂层刀片衬底真空渗硼预处理新技术研究

本文研究了真空渗硼预处理硬质合金基体的表面组织、形貌、粗糙度，并在处理过的YG6刀片基体上，用强电流直流伸展电弧等离子体CVD法沉积金刚石薄膜涂层。结果表明，真空渗硼预处理不仅可以有效的消除或控制钴在金刚石沉积时的不利影响，而且，还显著粗化硬质合金基体表面。因此，提高了金刚石薄膜的质量和涂层的附着力。     

脱β层厚度对CVD涂层硬质合金性能的影响

通过对WC-TiC-(Ta,Nb)C-Co硬质合金在1 300～1 380℃的渗氮气氛处理和随后的脱N烧结制得了不同脱β层厚度的合金基体,通过化学气相沉积(CVD)工艺制成从内到外依次为TiN/MT-TiCN/Al2O3/TiN的涂层硬质合金。采用光学显微镜、扫描电镜和能谱仪、抗弯(TRS)和切削试验对合金基体涂层前后的组织特征与性能进行了研究。结果表明,随着脱β层厚度的增加,试样涂层前后的抗弯强度均增加,在厚度达到20μm以上时,增加不明显。CVD涂层硬质合金可转位刀片的抗冲击性能也有相应的规律,而耐磨性则基本上保持一致。     

Complicated hollow turbine blades and surface grain refinement process

The control of grain size in superalloys is critical in the manufacture of gas turbine blades. The aim of the present research is to provide the technology for producing complicated hollow turbine blades with fine surface grains and better comprehensive mechanical properties. By melt superheating treatment and coating the internal surfaces of shell mould using a cobalt aluminate-bearing coating material, the influence of cobalt aluminate as inoculant on the surface grain sizes of turbine blade was studied with addition of cobalt aluminate: 0, 35%, 45% - 65% and 100% respectively. At the same time, the effects of cooling circumstances of the blades on surface grain sizes were also experimented under the same addition of cobalt aluminate. The results showed that the melt superheating treatment plays a significant role in the grain size and carbide morphology; and fine surface grains were obtained when the internal surfaces of shell mould were coated using cobalt aluminate coatings. When the addition of cobalt aluminate in coating is between 45% - 65%, and the melt is poured into preheated shell moulds with fine silica sand as backing sand, the blades satisfied the surface grain size requirement is over 90%. In addition, comparisons of the surface grain size and the mechanical properties were also conducted between home-made and foreign-made blades.     

INVESTIGATION OF SURFACE GRAIN REFINEMENT OF SUPERALLOY CASTINGS

本文对国内外关于高温合金铸件表面晶粒细化机理的几种观点作了验证;用X射线,显微镜和电子探针法对效果不同的型壳作了分析,发现铸件晶粒的细化与铝酸钴的分解以及合金中的活性元素有关;从浇铸后的型壳表面、铸件表面以及铝酸钴粉加不同活性元素的真空加热后的产物中均发现了Co(高温型)粒子。本文也做了铝酸钴加Al粉的真空差热分析并作了热力学计算,证明Co粒子的生成并不伴随着吸热,实际却是一个不大的放热效应。综合诸实验,作者认为铸件表面晶粒细化主要是由于Co粒子的核心作用;据此也探讨了合理的工艺,并巳用于工厂生产中,效果显著。     

Microstructure evolution of cobalt coating electroless plated on SiC whisker during electroless plating and heat treatment

SiC_w/Co nanocomposite particles were prepared by electroless plating cobalt on SiC whiskers and the microstructure evolution of the plated coating was investigated by SEM and XRD. SEM images show that growth occurs on the surface of the clusters at the initial stage; as they grow larger, the clusters converge to form a continuous coating, which is actually stacking of cobalt clusters. After heat treated at 500 °C in a hydrogen atmosphere, the cobalt coating transforms from an amorphous to a crystalline state. The thermal stability of SiC_w/Co composite is low because of the weak bonding between the substrate and the cobalt coating. The continuous coating aggregates to clusters through surface diffusion during heat treatment.     

The pre-oxidation process of electropolishing for the textured {113} <121> Ag substrate for Tl-1223 superconductor substrate

The surface roughness of a substrate is typically influenced by grain boundaries, grooves and voids. In an effort to improve the surface roughness, a textured {113} <121> Ag substrate was electropolished using a new method that causes the formation of an oxidation layer at the constant current density before electropolishing at a constant voltage of 1.75 V vs. SCE. The constant current density and potential were determined using the anodic polarization method. The pH effect for the optimized electropolishing condition was also investigated by adding phosphoric acid. The edges of the grain boundaries, grooves and voids became smoother when a constant current density was supplied with the pre-oxidation. A RMS (root mean square) value of 5.90-nm regarding the surface roughness of the Ag substrate was obtained without a final surface treatment before electropolishing, while a RMS surface roughness value of 34.12-nm was obtained for an Ag substrate that was given a final surface treatment for mechanical polishing.     

钴含量对电铸镍钴合金模芯微纳结构复制质量的影响

为探明电铸液中钴含量对仿荷叶表面镍钴合金模芯微纳结构复制质量的影响,采用阴极竖直旋转的微电铸技术,制备不同钴含量的仿荷叶表面镍钴合金模芯,采用扫描电子显微镜（SEM）、能谱仪（EDS）分析仿荷叶表面镍钴合金模芯表面的复制质量及成分。结果表明：由于铸层表面内应力的影响,在常规镍电铸中添加钴以后,仿荷叶镍钴合金模芯表面出现了波纹型的褶皱;观测模芯微观形貌发现其表面微米级的孔洞沿特定方向出现不同程度的拉伸,随着电铸液中钴含量（体积分数）的增加,拉伸程度先增加后降低（拉伸程度：钴含量0 g/L<钴含量40 g/L<钴含量10~30 g/L）;铸层中添加元素钴有利于晶粒细化,随电铸液中钴含量的增加,模芯表面微纳结构越细小,复制质量越高。     

电积钴板微观组织结构及力学性能对比

研究了3种电积钴板的微观组织结构和力学性能之间的差异，采用X射线衍射仪和扫描电子显微镜分析了3种电积钴板的择优取向、晶体结构和微观组织形貌；并分析了3种电积钴板的强度、硬度和韧性。结果表明：3种电积钴板均是密排六方结构（hcp）的纯钴相，晶粒取向随机。A-Co板沉积层均匀致密、孔洞较少，而B-Co板和C-Co板的沉积层较为分散且存在大量的孔洞。同时A-Co板表面的平均晶粒尺寸最小，沉积层晶粒大小分布均匀，B-Co板表面的平均晶粒尺寸最大，沉积层晶粒大小分布不均匀。3种电积钴板截面的始极片都是柱状晶结构，且始极片两侧的生长方式不同。由力学性能分析发现A-Co板的抗拉强度和硬度均高于其它2种钴板，但是韧性较差。综上所述，A-Co板的品质要明显优于B-Co板和C-Co板的品质。     

Real-time SEM/FIB studies of whisker growth and surface modification

We report on real-time measurements that enable us to watch the morphology of whiskers and hillocks forming in real-time and provide insight into the mechanisms controlling their growth and initiation. These measurements show that whiskers appear to grow out of a single grain on the surface with little lateral growth. To understand why whiskers initiate at specific sites, we modified the surface using the focused ion beam to remove the oxide in selected areas. Whiskers did not grow out of these uncovered areas, indicating that the underlying grain structure is important to whisker growth and it is not sufficient to just remove the oxide barrier. In comparison with whiskers, we found that hillock formation is accompanied by a large amount of grain growth and often by grain rotation at the surface.     

不同烧结温度下超细合金烧结体的密度、钴磁和晶粒度

本文研究了钴质量分数为10.5%的超细硬质合金在不同的烧结温度下的致密度、钴磁、晶粒长大等方面的变化趋势。研究结果表明:含量为10.5%的超细硬质合金,当烧结温度达到1 350℃时合金已基本致密化;在经典的WC-Co伪二元状态图表明的固相烧结阶段,随着温度升高,钴磁降低,晶粒长大以并合方式为主,可能存在少许的溶解-析出现象;在液相烧结阶段,钴磁达到稳定值后基本不变,晶粒长大以溶解-析出为主。     

复杂空心涡轮工作叶片表面细晶工艺研究

针对由K465合金制造的复杂、空心涡轮工作叶片表面细晶的不同要求,研究了制备叶片陶瓷型壳时,采用在精铸型壳内表面均匀涂挂一层350号铝酸钴作为表面细晶孕育剂,其加入量分别为0、35%、45%～65%及100%时对叶片表面低倍晶粒度的影响;同时研究了细晶孕育剂加入量一定时,浇注叶片时冷却环境对叶片表面低倍晶粒度的影响.研究结果表明,未经孕育处理的试片表面晶粒粗大,而经铝酸钴细晶孕育剂处理后试片表面晶粒细小.当铝酸钴加入量为45%～65%时,叶片采用热型浇注,型壳细砂做填砂,能够使复杂、空心涡轮工作叶片表面低倍晶粒度的合格率达到90%以上.另外,工艺可行性验证结果也表明,中、外叶片显微组织、力学性能相当.     

The Application of Surface Response Methodology to the Pretreatment of WC Substrates Prior to Diamond Coating

High cobalt (Co) content greater than 10% in tungsten carbide is desirable because Co improves the toughness of the cutting tool. However, the additional Co poses a huge challenge in surface preparation given that the Co content must be reduced to less than 1% on the substrate surface prior to applying a diamond coating. The excessive presence of Co on the substrate surface during coating suppresses diamond nucleation and causes the deterioration of diamond film adhesion. Many attempts have been made to overcome this issue, including the use of chemical etching, mechanical blasting, and heat treatment, but the successful pretreatment of WC-12%Co is still very limited. In this paper, a single-step chemical pretreatment using a mixture of sulfuric acid and hydrogen peroxide solutions was carried out on WC-12%Co. Two independent variables, i.e., etching time and acid temperature, were varied in the experiments to reduce Co contents as well as to roughen the substrate surface. The experimental plan was based on a central composite design. Variance analysis was employed to verify the precision of the mathematical models and their relative parameters. The predicted models generated by the response surface methodology (RSM) were compared with the experimental results, and close agreement was observed. The models demonstrated the significance of both factors, namely, acid temperature and etching time, in reducing Co contents to less than 1% as well as a roughening of the substrate surface within the desirable range.