金刚石薄膜涂层钻头加工高硬度钢的实验研究

为提高金刚石薄膜涂层的韧性，避免金刚石薄膜涂层脆性断裂，以自贡硬质合金厂生产ZK-10型号硬质合金钻头为基体，采用厚度大约为3μmTiC作为过渡层，在表面涂覆4μm～5μm厚度的金刚石薄膜制成金刚石薄膜涂层钻头。用于加工硬度为HRC61的经热处理的GCrl5钢板，分别与未涂层硬质合金钻头、TiC-TiN涂层钻头对比，结果表明，金刚石薄膜涂层钻头由于加工速率高，摩擦发热量少，有效地避免了铁元素在高温下将金刚石转化石墨的作用，结果使用寿命比未涂层硬质合金钻头提高10倍以上，同TiC-TiN涂层钻头相比，初期加工性能明显优越，加工速率成倍数提高．但使用过程中，性能衰减更快，导致总体使用寿命同TiC-TiN涂层钻头相差不大。在表面喷砂处理中，金刚石薄膜涂层大部分易于脱落，剩余部分呈岛状分布，说明金刚石薄膜与基体的结合力分布很不均匀，这可能与金刚石薄膜的形核过程密切相关。     

脱钴预处理对金刚石/硬质合金附着性能的影响

采用不同的两步处理方式浸蚀YG3和YG6低钴硬质合金基体表面，随后在热丝化学气相沉积装置上沉积了金刚石薄膜，分别用扫描电子显微镜、能谱仪以及洛氏硬度计对样品进行了分析检测。结果表明先采用Murakami剂30min腐蚀碳化钨相，再用3H2SO4 7H2O230s混合酸去除钴相，样品金刚石薄膜形核密度高，结晶质量较好，金刚石涂层与硬质合金基体结合良好。同一处理工艺，YG6系列样品处理效果更好。基体钴含量的降低对改善硬质合金与金刚石涂层间的附着性能有利。     

金刚石涂层用低钴硬质合金基体表面二步浸蚀法的研究

研究了先用Murakami剂浸蚀WC相，再用（H2O2＋H2SO4）酸混合液除去o相的2步法浸蚀YG6硬质合金基体表面预处理的过程，并在浸蚀过的硬质合金基体上，用热丝法沉积了金刚石薄膜，结果表明：2步浸蚀法可在基体表面深度为6μm-12μm的范围内，使Co含量从6％降低到0．54％－3．22％，并使硬质合金基体的表面粗糙度增加到Ra=1.0μm，但会导致硬质合金基体表面的硬度从89．9HRA降低至88．1HRA，在该硬质合金基体沉积金刚石薄膜之后，发现金刚石薄膜试样的组织结构具有明显的｛111｝面取向，金刚石涂层与硬质合金基体具有较高的粘结强度。     

渗硼+两步处理硬质合金微米-纳米金刚石复合涂层工具研究

研究了固体粉末渗硼＋碱酸两步预处理硬质合金基体的表面组织、形貌、粗糙度。实施优化的微米．纳米为0．1402μm金刚石复合涂层沉积工艺，得到表面平整、光滑、平均粗糙度的优质金刚石复合涂层。该涂层与基体附着力高，压痕测试其临界载荷大于1500N，金刚石复合涂层刀具加工ZAlSi12合金试验表明其切削寿命是无涂层刀具的41倍。     

等离子体技术在提高硬质合金工具上金刚石薄膜附着力方面的应用

金刚石薄膜具有优异的性能，作为切削工具表面的保护性涂层，可以大幅度提高工具的使用寿命以及加工精度。硬质合金是一种广泛使用的工具材料，在其表面沉积高附着力的金刚石薄膜时存在着困难。等离子体中离子、原子或分子具有高的反应活性，等离子体技术在金刚石薄膜的制备中有着广泛应用。利用等离子体技术可以极大的消除因金刚石薄膜与硬质合金基体之间存在热应力以及由硬质合金中的钴粘结剂在化学气相沉积金刚石薄膜过程中的促石墨化作用而产生的不利影响，提高金刚石薄膜与硬质合金基底之间附着力。本文综述了等离子体技术在提高硬质合金工具表面金刚石薄膜附着力方面的研究进展。     

热丝CVD金刚石薄膜涂层工具的制备技术及应用研究

本文通过电子增强热丝CVD方法在硬质合金基体上沉积金刚石薄膜 ,对硬质合金基体进行酸洗、表面研磨处理后用气相沉积方法沉积约 1μm厚的金属W膜层 ,在形核初期采用逐渐升高的偏流以去除表面形成的非晶C膜 ,并增加金刚石的形核密度和增强W的扩散作用 ,形成多种W -C化合物以增强金刚石薄膜与硬质合金基体的结合力 ,通过这种工艺制备了与基体结合力良好的金刚石薄膜。采用两种途径制备金刚石薄膜涂层工具 ,其一为在YG6硬质合金圆片上沉积约 80 μm的金刚石薄膜 ,经激光切割成 6mm× 6mm的合金片 ,用砂轮抛光 ,焊接在钢制刀柄上 ,经刃磨后制作成木工工具刀头 ;另一是直接在YG6硬质合金钻头这种复杂形状工具上沉积约 10 μm厚的金刚石薄膜制成金刚石工具。对两种工具分别进行使用性能测试 ,木工工具用于加工Al2 O3 复合木地板 ,测试结果表明金刚石薄膜涂层木工工具与硬质合金工具相比 ,使用性能有明显提高 ,寿命提高一倍以上 ,但由于刀刃后角处无金刚石层保护 ,使用中出现明显的后角磨损 ,未能达到理想效果 ;金刚石涂层钻头用于加工硬质合金时在使用初期有明显效果 ,但由于磨损很快 ,使用寿命低 ,经观察分析 ,主要是由于金刚石膜晶粒粗大造成表面光洁度不高 ,使用中刀刃处的金刚石薄膜涂层易于出现应力集中     

等离子体溅射对微型钻头表面ta-C涂层结合特性及摩擦性能的影响

无氢类金刚石涂层（ta-C）常用于提高刀具表面润滑性，提升极细微型钻头的排屑性能，降低断刀率。但ta-C涂层内应力大，与硬质合金钻头间的结合力较差，等离子溅射是提升涂层与基体之间结合力的有效方法。本文利用离子源产生的氩离子对硬质合金微型钻头和样块表面进行等离子体溅射，研究基体电流密度对基体表面形貌的影响；再利用阴极弧技术在等离子体溅射后的硬质合金表面制备ta-C涂层，研究不同溅射基体电流密度对ta-C涂层结合特性的影响。利用球盘式摩擦磨损试验机对溅射后的硬质合金表面以及ta-C涂层摩擦系数进行测试。通过钻孔测试，研究钻孔过程中基体电流密度对涂层与基体结合特性以及涂层微型钻头断刀率的影响。结果表明，随着溅射基体电流密度的增加，基体表面钴含量逐渐减少。压痕测试结果显示，合理的溅射基体电流密度（19.1 mA/cm2）下，可得到高结合力等级（HF1）。高结合力等级的ta-C涂层，摩擦系数最低为0.096。涂层钻头加工通信印制电路板1000孔后，高结合力ta-C涂层钻头的槽内涂层无异常脱落，测试1000支后无断刀。     

硬质合金微型钻头金刚石涂层预处理工艺对其断裂强度的影响

系统研究了直径为0.5mm的细晶粒微型钻头金刚石涂层前预处理工艺对其断裂强度的影响,并尝试使用线形同轴耦合式微波等离子体CVD方法对预处理后的微型钻头进行了金刚石涂层.其中,预处理采用Murakami溶液(10gKOH 10gK3[Fe(CN)6] 100gH2O)对微型钻头进行表面侵蚀,使其表面适当粗化;其后采用硫酸-双氧水溶液(10mL 98wt% H2SO4 100mL 38%m/v H2O2)对微型钻头表面进行侵蚀,以去除其表面的Co.实验表明,被广泛采用的上述两步法表面预处理技术对尺寸较小的硬质合金微型钻头的断裂强度会造成显著的影响.即使是很短时间的预处理,也会对硬质合金表面造成显著的损伤,引起微型钻头断裂强度的大幅度下降.其中,酸处理过程由于会引起表层组织疏松,其造成的断裂强度的下降更为严重.这表明,两步法预处理方法并不适用于尺寸较小的硬质合金工具.针对小截面硬质合金工具金刚石涂层的需求,需要发展更为适用的表面预处理方法.     

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。     

微型硬质合金钻头上金刚石涂层研究

WC-Co硬质合金钻头经过短时间酸腐蚀和微波等离子体硼氮化处理后,利用热丝CVD方法生长金刚石薄膜,并在电路板和玻璃板上进行了附着力测试.研究表明:钻头垂直于热丝放置,钻头端部为最高硬度的(111)面,有利于改善钻头切削加工性能;短时间酸腐蚀只去掉了钻头表面的钴,不降低表面硬度.同时酸腐蚀手段提高了表面粗糙度,避免了在随后的硼氮化处理时在WC表层形成低附着力的硼化物层,提高了金刚石薄膜附着力.在电路板及玻璃板上钻孔的测试结果表明,金刚石薄膜涂层钻头具有更高的寿命.     

CVD金刚石薄膜涂层整体式刀具的制备与应用

化学气相沉积(chemical vapor deposition,CVD)金刚石薄膜具有硬度高、摩擦系数低、耐磨性强以及表面化学性能稳定等优异的机械及摩擦学性能,这使其在硬质合金工模具领域具有广阔的应用前景.本文采用热丝化学气相沉积法(hot filament chemical vapor deposition,HFC...     

Mechanism and prediction of failure of diamond films deposited on various substrates by HFCVD

Diamond films were deposited on the WC-Co cemented carbide and Si3N4 ceramic cutting tool substrates by hot-filament-assisted chemical vapour deposition. The adherence property of diamond films was estimated using the critical load (Pcr) in the indentation test. The adhesive strength of diamond films is related to the intermediate layer between the film and the substrate. Poor adhesion of diamond films to polished cemented carbide substrate is owing to the formation of graphite phase in the interface. The adhesion of diamond films deposited on acid etched cemented carbide substrate is improved, and the peeling-off of the films often happens in the loosen layer of WC particles where the cobalt element is nearly removed. The diamond films' adhesion to cemented carbide substrate whose surface layer is decarbonizated is strengthened dramatically because WC phase forms by reaction between the deposited carbon and tungsten in the surface layer of substrates during the deposition of diamond, which results in chemical combination in the film-substrate interface. The adhesion of diamond films to silicon nitride substrate is the firmest due to the formation of chemical combination of the SiC intermediate layer in the interfaces. In the piston-turning application, the diamond-coated Si3N4 ceramic and the cemented carbide cutting tools usually fail in the form of collapsing of edge and cracking or flaking respectively. They have no built-up edge(BUE) as long as coating is intact.As it wears through, BUE develops and the cutting force on it increases 1 - 3 times than that prior to failure. This can predict the failure of diamond-coated cutting tools.     

直流电弧等离子体喷射在金刚石膜制备和产业化中的应用

综述了北京科技大学在直流电弧等离子体喷射CVD金刚石膜沉积系统研制和改进及大面积高质量(包括光学级)金刚石自支撑膜沉积的研究进展和产业化状况.用同样技术研发出了可用于复杂形状硬质合金工具金刚石膜涂层工具批量生产的强电流直流伸展电弧等离子体CVD金刚石膜涂层系统,讨论了利用该设备研发金刚石膜涂层硬质合金工具及其现场切削试验的结果.     

Adhesion analysis and dry machining performance of CVD diamond coatings deposited on surface modified WC-Co turning inserts

This paper investigates the effects of different surface pretreatments on the adhesion and performance of CVD diamond coated WC-Co turning inserts for the dry machining of high silicon aluminum alloys. Different interfacial characteristics between the diamond coatings and the modified WC-Co substrate were obtained by the use of two different chemical etchings and a CrN/Cr interlayer, with the aim to produce an adherent diamond coating by increasing the interlocking effect of the diamond film, and halting the catalytic effect of the cobalt present on the cemented carbide tool. A systematic study is analyzed in terms of the initial cutting tool surface modifications, the deposition and characterization of microcrystalline diamond coatings deposited by HFCVD synthesis, the estimation of the resulting diamond adhesion by Rockwell indentations and Raman spectroscopy, and finally, the evaluation of the dry machining performance of the diamond coated tools on A390 aluminum alloys. The experiments show that chemical etching methods exceed the effect of the CrN/Cr interlayer in increasing the diamond coating adhesion under dry cutting operations. This work provided new insights about optimizing the surface characteristics of cemented carbides to produce adherent diamond coatings in the dry cutting manufacturing chain of high silicon aluminum alloys.     

微晶/纳米金刚石复合涂层的沉积与表征

采用偏压增强热丝CVD(HFCVD)法,通过引入惰性气体Ar,在经过甲醇新预处理方法处理后的硬质合金衬底表面成功沉积了微晶/纳米金刚石复合涂层。对金刚石复合涂层的表面形貌、成分、表面粗糙度进行了分析和研究。研究结果表明:新的预处理方法能够提高金刚石薄膜与衬底之间的附着强度。Ar的引入使得金刚石薄膜二次形核率更高,颗粒也更加细小,纳米金刚石复合涂层不但具有高的附着强度,而且具有非常低的表面粗糙度。对于拓展纳米金刚石涂层在精密加工领域中的应用具有一定的作用。     

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。     

化学预处理对微型钻头沉积类金刚石薄膜附着力的影响

在刀具上沉积类金刚石(DLC)薄膜的关键技术问题是如何提高DLC薄膜的附着力,以发挥DLC薄膜在刀具涂层领域的优势。本文通过对微型钻头表面进行不同的化学预处理后利用射频等离子体化学气相沉法沉积DLC薄膜,对影响膜基附着力的内在规律进行了探讨。结果表明:采用简单酸碱腐蚀(先后使用NaOH溶液和HNO3溶液进行腐蚀)对DLC薄膜附着力的提高有一定作用,而综合腐蚀(首先使用酸碱腐蚀,然后使用Murakami试剂腐蚀)的效果更佳;此外,使用Murakami试剂腐蚀时间过长(超过6 min)会影响钻头本体的机械强度。实验结果对于DLC薄膜作为微型钻头涂层的应用具有很好的指导意义。     

Enhancing the adhesion of diamond films on cobalt-cemented tungsten carbide substrate using tungsten particles via MPCVD system

To increase the adhesion of diamond films and avoid the negative effects of using cobalt, previous treatments have employed tungsten particles to cover the surface of the 6 wt.% cobalt-cemented tungsten carbide (WC-Co) substrate. The surface of the tungsten particles is transformed into W₂C and WC, which attracts and traps carbon. Through the process of nucleation, the carbon forms around the tungsten particles, thereby satisfying the conditions necessary for the formation of diamond film. Using Raman spectroscopy, we determined that diamond films of good quality with excellent adhesive properties and a hardness level as high as 27.78 GPa could be produced following pretreatment with 2.0 μm tungsten particles. Rockwell indentation tests indicate that addition of tungsten particles promotes the interfacial adhesion of diamond films with WC-Co substrates. We determined that using smaller tungsten particles decreased the number of gaps and cavities on the surface of the substrate, thereby enhancing the adhesion of the diamond film.     

Diamond-coated cutting tools for biomedical applications

Diamond coatings are attractive for cutting processes due to their high-hardness, low-friction coefficient; excellent wear resistance, and chemical inertness. The application of diamond coatings on cemented, tungsten carbide (WC-Co) burs has been the subject of much attention in recent years as a method to improve cutting performance and tool life. WC-Co burs containing 6% Co and 94% WC substrate, with an average grain size of 1–3 μm, were used in this study. To improve the adhesion between diamond and WC substrates, it is necessary to etch away the surface Co and prepare the surface for subsequent diamond growth. Hot filament chemical vapor deposition (HFCVD), with a modified vertical filament arrangement, has been used for the deposition of diamond films. Diamond film quality and purity has been characterized using scanning electron microscopy (SEM) and micro-Raman spectroscopy. The performance of diamond-coated WC-Co burs, uncoated WC-Co burs, and diamond-embedded (sintered) burs have been compared by drilling a series of holes into various materials such as human teeth, borosilicate glass, and acrylic teeth. Flank wear has been used to assess the wear rates of the burs when machining biomedical materials such as those just described. This paper was presented at the 2nd International Surface Engineering Congress sponsored by ASM International, on September 15–17, 2003, in Indianapolis, Indiana, and appears on pp. 273–82 of the Proceedings.     

Improvement in adhesion of diamond film on Cu substrate with an inlay structured interlayer

Diamond films were fabricated by using a two-step process on copper substrates in this study. The first step involved electroplating a chromium (Cr)–diamond composite interlayer on copper substrate and in the second step continuous diamond film was deposited on top using the hot-filament chemical vapor deposition (HFCVD) method. The interfacial characteristics was investigated by indentation tests and the thin film surface morphology, phase structure and residual stress analyzed by scanning electron microscopy (SEM), X ray diffraction (XRD) and Raman spectroscopy. The results show that the diamond particles are deeply imbedded in the chromium layer and the amorphous Cr in the composite interlayer was carburized to Cr₃C₂ during the CVD process. Low residual stress was detected in the diamond film and good adhesive strength between film and substrate was obtained due to the diamond particles anchored deep in the Cr₃C₂ matrix. Concentric cracks but no delaminated areas and radial cracks were observed on the periphery of the indentation at indentation load of 441 N.