天然金刚石形成透明硼皮金刚石的研究

 本文采用离子注入法，对天然金刚石表面进行少量渗硼，形成透明硼皮金刚石。经NP-1型X光电子能谱仪（XPS）表面测试，证明注入硼后的金刚石表面硼原子和碳原子形成了结合键。又经热失重分析（TGA）表明，用B₂O₃和硼作离子源进行注入，均能使金刚石的抗氧化温度得到提高，但用硼注入得到的“硼皮”金刚石抗氧化性更好些。用四种不同能量进行注硼时，都能使金刚石的抗氧化性得到几乎相同程度的提高，与注入的深度无关。     

高能氮离子注入人造金刚石的热稳定性

 叙述了在GLZ-100E工业离子注入机上采用20~60 keV氮离子及氮分子离子注入人造金刚石晶体的实验研究。XPS分析表明，注入离子在人造金刚石颗粒表面形成了一层较为稳定的含氮混合物层。高温差热分析（DTA）的实验表明，经氮离子束处理的金刚石，其氧化起始温度T（onset）由原来的730 ℃左右提高到800 ℃以上，且随着氮注入剂量的增加而增加，氧化速度也随之变缓；差热分析还表明，随着温度的升高，金刚石首先转化为石墨（DTA曲线上表现为吸热），然后氧化燃烧生成CO₂（放热），而注入离子能量的增加，氧化温度的提高幅度略有下降。离子注入还使其高温石墨化性能显著改善。     

金属包裹体的变化及对人造金刚石强度的影响

 当温度超过1 000 ℃时，人造金刚石中的金属触媒包裹体，在形态、结构和成份上都将发生改变，并且这种变化会在金刚石晶格内造成尺寸更大的缺陷区域，因此在表面氧化不起决定性作用的情况下，金属触媒包裹体的这种变化，就成了导致金刚石强度下降的最直接的原因。我们对在氩气保护下、不同温度处理的一系列人造金刚石样品进行了强度测量，并用SEM、X射线衍射及光学显微镜等手段观测了金刚石断裂表面上的包裹体及其形态变化。我们的实验结果证实了上述结论。我们还发现，金属触媒包裹体的存在极大地影响着金刚石的热稳定性，它们使金刚石在1 000 ℃左右即可向石墨转化。     

B离子注入引起的金刚石薄膜体积膨胀现象

离子注入是获得金刚石N型或P型导电材料的有效途径之一。然而,离子注入对金刚石的晶格结构有破坏作用,造成金刚石薄膜体积的膨胀。本文对B离子注入合成Ib型金刚石薄膜后体积膨胀现象进行了研究,分析了引起体积膨胀的可能因素及原因。     

多次冲击石墨合成聚晶金刚石的实验研究

 利用高能炸药爆轰产物驱动金属飞片，碰撞“硬”回收包套以输入平面冲击波，在24~37 GPa的压力范围内，对纯石墨进行1~4次的冲击压缩实验，合成出了纯度很高、形貌良好的立方型聚晶金刚石。随着冲击次数的增加，金刚石的转化率和粒度有增大的趋势。但是，当金刚石粒度较大时（约100 μm以上），如果冲击温度较低（约1 000 K以下），同时冲击压力又较高（约20 GPa以上），金刚石颗粒就容易被冲击波破碎。     

微波ECR全方位离子注入制备类金刚石碳膜的结构及摩擦学性能研究

利用微波ECR全方位离子注入技术，在单晶硅（100）衬底上制备类金刚石薄膜.分析结果表明，所制备的类金刚石碳膜具有典型的类金刚石结构特征，薄膜均匀、致密，表面粗糙度小，摩擦系数小.其中，薄膜的结构和性能与氢流量比关系密切，随氢流量比的增加，薄膜的沉积速率减小，表面粗糙度降低，且生成sp³键更加趋向于金刚石结构，表面能 更低，从而使摩擦系数大幅降低. 关键词： 全方位离子注入 类金刚石碳膜 拉曼光谱 摩擦磨损     

IRS400型材料发射率测试装置的研制

为了准确评估红外材料和涂层的隐身性能,研制了一套IRS400型材料发射率测试装置,主要用于温度范围（50～400）℃,光谱范围（3～5）m和（8～12）m的固体不透明材料和涂层定向发射率测量。给出IRS400型材料发射率测试装置的技术指标,阐述其工作原理,IRS400的光学系统采用全反射式设计,探测器选用钽酸锂热释电探测器,采用50 ℃～1 000 ℃黑体辐射源标准装置对黑体发射率B（1,2）进行标定。通过解决标定和环境温度补偿等关键技术,确保发射率测量不确定度小于2%(k=2)。     

氧化镓的同步辐射研究

 利用金刚石对顶砧（DAC）高压装置产生高压，使用体积比为16∶3∶1的甲醇、乙醇和水混合液作为传压介质，通过原位高压同步辐射技术对氧化镓的高压行为进行了研究（0～42.5 GPa）。实验发现在室温下13.3 GPa压力附近，单斜结构的氧化镓发生了结构相变，变成三角结构。相变后镓离子由原来同时位于由氧离子围成的四面体和八面体的中心位置变成只位于八面体的中心位置。卸压后的X射线衍射谱表明，氧化镓又恢复为单斜结构，该相变为可逆相变。     

FeMn粉末触媒对合成金刚石的影响

 利用FeMn粉末触媒在国产六面顶压机上进行了合成金刚石单晶的实验,研究了高温高压条件下（5.7 GPa、1 550 ℃）,石墨-FeMn粉末触媒体系中金刚石单晶的生长特性。通过光学成像显微镜观测表明：合成出的金刚石单晶呈浅黄色,晶形完整,且都是八面体,晶体里含有白色物质,粒度集中在0.3~0.5 mm;通过扫描电镜观测了晶体的表面形貌,表面有熔坑;通过穆斯堡尔谱,发现粉末触媒里主要是FeMn合金和独立状态的Fe,金刚石内部主要是Fe和Fe₃C;利用X射线荧光光谱,检测出样品里有Fe和Mn元素。     

含氮类金刚石薄膜的紫外辐照研究

用射频等离子体方法在玻璃基底上制备的类金刚石（DLC）薄膜,采用离子注入法掺氮,并对掺氮DLC薄膜紫外（UV）辐照前后的性能变化进行了研究。研究结果表明：随氮离子注入剂量及UV辐照时间的增加,位于2 930cm-1附近的SP3C-H吸收峰明显变小,而位于1 580cm-1附近的SP2C-H吸收峰则明显增强,薄膜的电阻率明显呈下降趋势;随UV辐照时间的增加,位于1 078cm-1附近的Si-O-Si键数量及位于786cm-1附近的Si-C键数量明显增加。即氮离子注入和UV辐照明显改变了DLC薄膜的结构与特性。     

Boron distribution in the subsurface region of heavily doped IIb type diamond

For the first time investigations of the boron distribution in the subsurface region of HPHT boron-doped diamond that is promising for applications in electronics were carried out by X-ray photoelectron (XPS) and Raman spectroscopy. It was found from XPS data that the boron content decreased gradually more than one order of magnitude in depth of surface. The first-principle calculations have shown that the Raman polarizability in the crossed polarization configuration should increase considerably with boron doping. The Raman spectra from as-grown and polished surfaces of heavily boron-doped diamond are discussed in the context of theoretical results.     

多晶金刚石烧结中晶粒表面石墨化的实验研究

 利用X射线微区衍射，X射线光电子谱（XPS）及激光拉曼光谱等分析，对高温高压下以金刚石微粉为原料的多晶金刚石烧结过程中，金刚石晶粒表面石墨化现象进行了考察。结果表明，虽经历了烧结过程，但在没有掺杂剂作用的区域内，没有发现金刚石晶粒表面的石墨化。晶粒表面石墨化的高峰期，处于掺杂剂刚开始液化，但尚未饱和充填金刚石晶粒间空隙的烧结初期阶段，随着液相掺杂剂的饱和充填作用，金刚石晶粒表面的石墨消失，并最终完成多晶金刚石的烧结。     

硼掺入量对含硼金刚石单晶热稳定性的影响

 在铁基触媒原材料中添加不同含量的六方氮化硼,采用粉末冶金方法制备片状触媒,在六面顶压机上合成出含硼金刚石单晶。用体视显微镜对金刚石单晶的结构、形貌进行观察,并用电子探针（EPMA）和波谱仪（WDS）分析了金刚石（111）晶面的硼含量,发现金刚石表面有硼元素存在,且其含量随着触媒中掺硼量的增加而变化。在测定了含硼金刚石单晶的静压强度的基础上,采用冲击韧性测定仪和差热分析仪对不同掺硼量触媒合成出的金刚石单晶在空气中的热稳定性进行了系统的对比研究。结果表明,触媒掺硼量对金刚石的机械强度和热稳定性有重要影响,随着掺硼量的变化,其机械强度和热稳定性均存在一个最佳值。     

The effect of boron ion implantation and annealing on the microstructure and electrical characteristics of the diamond films

Diamond films were doped by boron ion-implantation with the energy of 120 keV. The implantation dose ranged from 10¹⁴ to 10¹⁷ cm⁻². After the implantation, the diamond films were annealed at different temperatures (600–750°C) for different times (2–15 min). Scanning Electronic Microscope, Raman and Secondary Ion Mass-spectrum were used to investigate the effect of boron ion implantation and annealing on the microstructure of the diamond films. The electrical resistivities of the diamond films were also measured. It was found that the best dose of boron ion-implantation into the diamond film was around 10¹⁶ cm⁻². The appropriate annealing temperature and time was 700°C and 2–5 min, respectively. After implantation, the resistivities were reduced to 0.1 Ω cm (almost nine orders lower than the unimplanted diamond films). These results show that boron ion implantation can be an effective way to fabricate P-type diamond films.     

Synthesis and characterizations of boron and nitrogen co-doped high pressure and high temperature large single-crystal diamonds with increased mobility

We synthesized and investigated the boron-doped and boron/nitrogen co-doped large single-crystal diamonds grown under high pressure and high temperature (HPHT) conditions (5.9 GPa and 1290℃). The optical and electrical properties and surface characterization of the synthetic diamonds were observed and studied. Incorporation of nitrogen significantly changed the growth trace on surface of boron-containing diamonds. X-ray photoelectron spectroscopy (XPS) measurements showed good evident that nitrogen atoms successfully incorporate into the boron-rich diamond lattice and bond with carbon atoms. Raman spectra showed differences on the as-grown surfaces and interior between boron-doped and boron/nitrogen co-doped diamonds. Fourier transform infrared spectroscopy (FTIR) measurements indicated that the nitrogen incorporation significantly decreases the boron acceptor concentration in diamonds. Hall measurements at room temperature showed that the carriers concentration of the co-doped diamonds decreases, and the mobility increases obviously. The highest hole mobility of sample BNDD-1 reached 980 cm²·V^-1·s^-1, possible reasons were discussed in the paper.     

铁基触媒中碳化硼含量对含硼金刚石单晶表观活化能的影响

通过在铁基触媒中添加适量的碳化硼,制备出了具有不同硼含量的含硼金刚石单晶。利用差热分析仪,测量了含硼金刚石单晶的差热和热重。采用Kissinger方法,计算了含硼金刚石单晶在加热过程中发生氧化反应的表观活化能,对比分析掺硼量对含硼金刚石单晶热稳定性的影响。结果表明:差热和热重测量值与表观活化能计算值的变化规律基本一致;随着掺硼量的增加,含硼金刚石单晶的热稳定性先提高后降低,剧烈氧化时表观活化能随着掺硼量的增加而减小。     

掺杂立方氮化硼对金刚石聚晶致密化和显微结构的影响

 以小于0.5 μm的金刚石和氮化硼（以下简称cBN）微粉为原料,在6.0 GPa和1 450～1 480 ℃保温30 min的工艺条件下,成功地烧结出晶粒尺寸小于1 μm、以WC/Co硬质合金为衬底的金刚石聚晶。研究了cBN掺杂对金刚石基质密实化和显微结构的影响。研究表明,cBN可以有效地抑制金刚石异常长大。细晶而且致密的金刚石聚晶有优异的力学性能。     

Synergistic influences of titanium,boron, and oxygen on large-size single-crystal diamond growth at high pressure and high temperature

The synergistic influences of boron, oxygen, and titanium on growing large single-crystal diamonds are studied using different concentrations of B₂O₃ in a solvent-carbon system under 5.5 GPa-5.7 GPa and 1300 ℃-1500 ℃. It is found that the boron atoms are difficult to enter into the crystal when boron and oxygen impurities are doped using B₂O₃ without the addition of Ti atoms. However, high boron content is achieved in the doped diamonds that were synthesized with the addition of Ti. Additionally, boron-oxygen complexes are found on the surface of the crystal, and oxygen-related impurities appear in the crystal interior when Ti atoms are added into the FeNi-C system. The results show that the introduction of Ti atoms into the synthesis cavity can effectively control the number of boron atoms and the number of oxygen atoms in the crystal. This has important scientific significance not only for understanding the synergistic influence of boron, oxygen, and titanium atoms on the growth of diamond in the earth, but also for preparing the high-concentration boron or oxygen containing semiconductor diamond technologies.