阶梯型复合刀具CVD金刚石涂层制备工艺及应用研究

针对加工阶梯孔类的阶梯型复合刀具,采用热丝辅助化学气相沉积技术(HFCVD),通过超声辅助酸碱两步预处理法,并且采用钽丝上下两层平行布置的沉积装置,调节生长参数,研究了YG6硬质合金阶梯型复合刀具的金刚石涂层制备技术.为了研究涂层性能,以含少量石棉的复合纤维刹车片作为加工对象,分别对比实验了金刚石涂层和未涂层刀具的钻削性能.结果表明:相对传统单层热丝沉积工艺,采用双层热丝布置方式,在涂层过程中能使切削刃各个部分的温度保持平衡稳定,使得阶梯复合刀具每个切削刃都能均匀地涂上一层金刚石薄膜.采用该方法沉积的金刚石涂层阶梯复合刀具在钻削过程中具有良好的切削性能及附着强度,特别是在高速加工中金刚石涂层阶梯复合刀具在轴向钻削力及扭矩方面都小于未涂层刀具,金刚石涂层阶梯复合刀具在钻削刹车片阶梯复合孔加工中具有显著的优势.     

金刚石薄膜涂层刀具的破损机理研究

切削过程中金刚石薄膜从基体表面的破损剥落是金刚石薄膜涂层刀具的一种主要损坏形式.本文通过实验研究了金刚石薄膜涂层刀具的破损机理及刀具表面状态、切削用量对其损坏形式的影响.研究结果表明,较大的切削用量、机械冲击、交变切削载荷及积屑瘤频繁脱落等是导致金刚石薄膜涂层刀具破损剥落的主要原因.金刚石薄膜的破损剥落起始于薄膜与基体之间及薄膜底面金刚石晶粒之间的原始微小间隙缺陷,这些原始微小间隙缺陷是在沉积金刚石薄膜时,由于成核密度较低等原因而形成的.金刚石薄膜剥落时薄膜的断裂主要沿晶界发生.     

金刚石薄膜在硬质合金基体上的生长及附着强度研究

硬质合金是制作金刚石薄膜涂层刀具的重要基体材料,金刚石薄膜在硬质合金基体上的成核、生长及界面特征直接影响其附着强度.本文通过扫描电镜、X射线衍射分析、X射线光电子谱(XPS)及断续切削实验,研究了硬质合金基体含Co量对金刚石薄膜成核、生长及附着强度的影响.研究结果表明,经酸洗处理后,硬质合金基体含Co量对金刚石薄膜成核、生长没有太大影响.但对其附着强度有很大影响.含Co量越高,附着强度越低.酸腐蚀去Co处理后基体表面变得疏松、不连续非金刚石碳界面的存在及热膨胀系数较大是含Co量较高时,附着强度下降的主要原因.     

金刚石涂层的纳米压痕力学性能研究

用HFCVD法在硬质合金刀具上制备了CVD金刚石涂层,利用纳米压痕仪研究了CVD金刚石涂层的硬度和弹性模量等力学性能.结果表明,反应室气压、衬底温度、反应气体中CH4含量、沉积时间等参数改变了CVD金刚石膜中sp2成分含量、晶界数量及晶界上缺陷,从而影响CVD金刚石涂层的纳米硬度和弹性模量.较高或较低的衬底温度都会导致硬质合金刀具上CVD金刚石涂层的纳米硬度、弹性模量降低;随着反应室气压、反应气体中CH4含量的增加,硬质合金刀具上CVD金刚石涂层的纳米硬度、弹性模量降低;沉积时间低于6 h时,沉积时间对硬质合金刀具上CVD金刚石涂层的纳米硬度、弹性模量影响显著,沉积时间超过6 h后,沉积时间对硬质合金刀具上CVD金刚石涂层的纳米硬度、弹性模量逐渐趋向稳定.     

渗硼并两步处理硬质合金微晶金刚石涂层工具研究

研究了固体粉末渗硼并碱酸两步处理预处理硬质合金基体的表面组织、形貌、粗糙度,并在处理过的硬质合金基体上,用强电流直流伸展电弧等离子体CVD法沉积微晶金刚石薄膜涂层.进一步的涂层质量表征,附着力测试及切削实验研究结果表明,这种涂层质量高、附着力好(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优于无涂层硬质合金工具.在加工ZAlSi12合金时,微晶金刚石涂层车刀片、铣刀片的切削寿命是无涂层车刀片、铣刀片切削寿命的32倍和26倍.     

微/纳米金刚石复合涂层刀具的制备及切削试验

利用化学气相沉积法在硬质合金基体上制备微/纳米金刚石复合涂层,采用扫描电镜、Raman光谱仪、洛氏硬度计、微粒喷浆试验仪对涂层进行微结构与性能表征,同时进行切削试验.结果表明:涂层表面晶粒细小,颗粒尺寸达到纳米级,涂层纯度高,膜/基结合力好,耐磨性高.切削试验结果显示:微/纳米金刚石复合涂层刀具切削加工工件的表面粗糙度比硬质合金刀具小,其表面粗糙度平均值为0.931μm;从后刀面磨损量结果看出微/纳米金刚石复合涂层刀具使用寿命长;从前、后刀面磨损形貌看出金刚石复合涂层结合力好,耐磨性高.     

离子轰击增强金刚石膜与Si衬底结合力的进一步研究

由于金刚石与Si有较大的表面能差,利用化学气相沉积(CVD)制备金刚石膜时,金刚石在镜面光滑的Si表面上成核困难,而负衬底偏压能够增强金刚石在镜面光滑Si表面上的成核,表明金刚石核与Si表面的结合力也得到增强.本文分析衬底负偏压引起的离子轰击对Si表面产生的影响之后,基于离子轰击使得Si衬底表面产生了微缺陷(凹坑)增大了金刚石膜与Si衬底结合的面积,理论研究了离子轰击对金刚石膜与Si衬底结合力的影响.     

MPCVD法纳米金刚石膜的制备及分析

利用MPCVD方法在玻璃基片上成功的制备了非常光滑、致密均匀的纳米金刚石膜.沉积工艺分为两步:成核,CH4/H2=3;;生长,O2/CH4/H2=0.3:3:100;沉积过程中保持工作压力为4.0kPa,衬底温度500℃.拉曼、透射电镜、红外光谱、表面轮廓仪等的测试表明:膜层由纳米级金刚石晶粒组成,最大晶粒尺寸小于100nm,成核密度大于1011/cm2.成核面晶粒的点阵常数较大,表明存在较多缺陷,表面粗糙度小于2nm,在可见光区完全透明,红外光学性能接近金刚石单晶理论值.     

负衬底偏压热灯丝CVD金刚石膜成核的研究

本文利用扫描电子显微镜和原子力显微镜研究了Si(100)衬底上热灯丝金刚石膜成核过程.在-240V和250mA下,在镜面抛光的Si(100)衬底上金刚石最大成核密度超过了1010cm-2.研究表明,负衬底偏压增强成核主要是发射电子和离子轰击的结果.     

[100]定向织构生长金刚石薄膜的红外光学性能研究

采用微波等离子增强化学气相沉积法在(100)镜面抛光的硅片衬底上实现了金刚石薄片[100]定向织构生长.并用扫描电子显微镜、拉曼散射和傅立叶红外光谱仪分析测试了不同工艺得到的金刚石薄片的表面形貌、组成结构和红外性能.结果表明:负偏压辅助定向成核和氢的等离子刻蚀不仅促进了金刚石薄膜的定向织构生长,而且还能刻蚀成核期的非金刚石成分.从而提高了金刚石薄片的红外光透过特性.     

金刚石膜在Si(100)衬底上的选择沉积

采用自行设计的微波等离子体化学气相沉积系统,利用铜网作为模板实现了在Si(100)衬底上金刚石膜的选择沉积.用场发射扫描电子显微镜(SEM)、Raman散射谱对样品进行了表征与分析.并与同样生长条件下未采用模板时得到的金刚石样品进行了比较.结果发现,采用模板后,金刚石膜的成核密度和质量都得到很大提高.     

在预涂陶瓷过渡层的多谱段ZnS衬底上沉积金刚石膜的探索研究

本文采用真空电子束蒸镀技术在多谱段ZnS衬底上沉积了适合金刚石膜沉积的致密陶瓷过渡层,并利用微波等离子体CVD金刚石膜低温沉积技术进行了金刚石膜沉积研究.发现在陶瓷过渡层上的金刚石形核极其困难,其原因可能是陶瓷涂层在沉积过程中龟裂导致ZnS蒸汽扩散逸出干扰金刚石形核所致.本文采用诱导形核技术在过渡层/ZnS试样表面观察到极高密度(1010/cm2)的金刚石形核,并对金刚石/过渡层/ZnS试样的红外透过特性进行了评价.     

Systematic study of various stages during the growth process of diamond-like carbon film by atomic force microscopy

The diamond like carbon (DLC) films have been grown by radio frequency plasma enhanced chemical vapor deposition (RF-PECVD) in methane-argon plasma. In PECVD, the plasma sheath potential drop arising due to argon plasma was utilized to grow the DLC film on silicon (100) substrate at low temperature without using any external negative bias voltage. The growth process of the DLC film has been studied completely starting from nucleation to continuous film by atomic force microscopy. It was seen that the DLC film nucleates around surface defects on the substrate and that the film growth occurs by both adatom deposition and coalescence between nucleated islands. Raman spectrum confirms that the DLC film nucleates excessively in sp² hybridized state and that during the growth process the fraction of sp³ CH_x (x = 1 − 3) increases which leads to the amorphous nature of the film. Long range uniformity of the film was identified using scanning electron microscope.     

Investigation of Pretreated Silicon Wafers for CVD Growth of Diamond Film

Difference between lattice constants of silicon (Si) and diamond is approximately 52%. Therefore Si_1—xC_x which has a lattice constant between two materials should be formed on Si substrate to be diamond nucleation sites and reduce the stress between the diamond film and Si substrate. Si wafers with carbonization and dc-biasing pretreatment were prepared in a microwave plasma chemical vapor deposition (CVD) system, then they were investigated by Raman spectroscopy, Photoluminescence (PL), chemical etching and scanning electron microscope (SEM) to study the pretreatment effect. This was achieved by studying a series of samples pretreated by carbonization and dc-biasing.     

加氮对直流电弧等离子体喷射金刚石膜生长、形貌和质量的影响

利用直流等离子体喷射化学气相沉积法制备掺氮的金刚石厚膜.本文研究了在甲烷/氩气/氢气中加入氮气对金刚石膜生长、形貌和质量的影响.反应气体的比例由质量流量计控制,在固定氢气(5000sccm)、氩气(3000sccm)、甲烷(100sccm)流量的情况下改变氮气的流量,即反应气体中氮原子和碳原子的变化比例(N/ C比)范围是从0.06到0.68.同时金刚石膜在固定的腔体压力(4kPa)和衬底温度(800℃)下生长.金刚石膜用扫描电镜(SEM)、拉曼谱和X射线衍射表征.结果表明,氮气在反应气体中的大量加入对直流等离子体喷射制备金刚石膜的形貌、生长速率、晶体取向、成核密度等有非常显著的影响.     

High-density silicon and silicon nitride cones

High-density cone-shaped silicon and silicon nitride have been synthesized on Si(1 0 0) substrates via plasma-assisted hot-filament chemical vapor deposition using a gas mixture of nitrogen, hydrogen and methane. Aligned silicon cones containing 3–10 at% C and N have been formed with less than 1 h growth. Further growth can lead to the increase of cone size and density, as well as to the formation of polycrystalline silicon nitride films on the tip and surface. The formation of these materials is thought to be due to the remodification of Si substrates under the effect of plasma and active C and N species. Different nucleation and growth styles were obtained under different growth conditions and reactive gas mixtures.