纳米金属功能材料研究进展

纳米金属材料是一类重要的激光惯性约束聚变和强辐射源靶材料。通过靶材料微观结构的调控，将其特征尺寸降低到纳米量级，已成为该研究领域的一种新型研究手段。针对目前ICF和强辐射源物理研究的目标和需求，本单位在纳米金属功能材料研究方向开展了一些研究工作，取得了初步的研究成果，主要有：     

强激光辐照下纳米晶体铜薄膜层裂破坏的实验研究

采用强激光辐照加载技术和激光速度干涉(VISAR)测试技术，对纳米晶体铜薄膜的层裂特性进行实验测量和分析.基于VISAR实测的自由面速度波形，计算得到纳米晶体铜薄膜在超高拉伸应变率下的层裂强度高达3 GPa，明显高于多晶铜的层裂强度, 其原因归咎于纳米晶体材料中存在大量晶界阻碍了位错运动.     

采用真空热压技术制备纳米金属钨块体材料

 采用真空热压技术,在570 ℃和1 GPa的条件下成功制备具有单相α-W结构、平均晶粒尺寸为34 nm、尺寸为Φ10 mm×1 mm的难熔金属钨纳米块体材料,其密度为理论密度的88.8%,显微硬度为4.8 GPa。纳米金属钨的密度和显微硬度随热压温度、热压压强和热压时间增大而升高。     

ICF靶材料和靶制备技术研究进展

 主要介绍了中国工程物理研究院ICF靶材料科学与靶制备技术在材料研究、靶丸制备技术、薄膜制备技术、精密微工艺及靶参数测量等方面的主要研究进展。在靶材料研究方面,近年相继研制成功全氘代聚苯乙烯（D-PS）有机材料、微靶掺杂和激光吸收与X射线转换金属纳米或团簇材料;探索了新型有机气凝胶储氢材料,开展了金属小团簇理论研究和纳米金属复合材料的研究工作。在靶制备技术与工艺方面,完成了PS单层、双层和三层塑料空心微球的研制工作;利用低温等离子体聚合涂层技术,建立了微球表面沉积纯CH薄膜以及金属掺杂CH薄膜的工艺和技术;在玻璃微球充氩技术研究中,开展了原子力扫描显微镜对玻璃球壳钻孔工艺研究以及粒子辐照改性充气技术研究,等等。     

高性能ZnO纳米块体材料的制备及其拉曼光谱学特征

利用六面顶高压设备制备了高密度、低脆性、纳米级的ZnO块体材料，用MDI/JADE5 X射线衍射仪(Cu靶)和XL30S-FEG场发射扫描电子显微镜对高压样品的相组成、晶粒尺寸及微观形貌进行了表征.利用E55+FRA106/5傅里叶变换激光拉曼光谱仪通过ZnO块体样品位于50—500cm^-1之内的拉曼光谱, 研究了极性半导体纳米材料的拉曼光谱学特征.发现在极性半导体ZnO纳米块体材料中，没有出现明显的尺寸限制效应. 关键词： ZnO纳米块体 拉曼光谱 尺寸限制效应     

纳米晶Cu薄带的单辊法制备及结构分析

 采用单辊法制备出纳米晶Cu薄带，利用X射线衍射对纳米晶Cu薄带的结构进行分析，并研究了工艺参数对结构的影响。实验发现：纳米晶Cu薄带的平均晶粒度为65.17～121.8 nm，辊轮转速越快，喷铸压力越小，保护气压越大，保护气体越冷，薄带的晶粒尺寸越小；纳米晶内部均存在晶格畸变和晶胞参数的涨落，说明采用单辊法制备纯金属薄带会在材料内部产生不同程度的晶格扭曲，Cu带处于非稳定状态；所有样品均发生(200) 晶面择优取向，原因可能与单辊法的快淬工艺有关。     

强激光辐照下纳米晶体铜薄膜层裂破坏的实验研究

采用强激光辐照加载技术和激光速度干涉(VISAR)测试技术,对纳米晶体铜薄膜的层裂特性进行实验测量和分析.基于VISAR实测的自由面速度波形,计算得到纳米晶体铜薄膜在超高拉伸应变率下的层裂强度高达3 GPa,明显高于多晶铜的层裂强度, 其原因归咎于纳米晶体材料中存在大量晶界阻碍了位错运动. 关键词： 纳米晶体铜薄膜 层裂 激光辐照     

激光熔敷镍石墨烯立方氮化硼涂层的耐磨性能

在AISI 4140基体上采用预置材料激光熔敷的方法制备了镍石墨烯立方氮化硼(Ni-Graphene-CBN)复合材料涂层。X射线衍射(XRD)和Raman测试证明了石墨烯和CBN存在于所制备的涂层材料中。扫描电镜(SEM)图片给出了所制备的复合材料涂层的表面和断面形貌。进行了复合材料涂层的纳米机械性能和耐磨性的测试。测试结果表明:随着CBN含量的增加,复合涂层的硬度及弹性模量相应提高,分别由4.3 GPa提高到6.2 GPa和101 GPa提高到140 GPa; 同时其耐磨性也有明显改善,6% CBN含量的涂层摩擦系数由基体材料的0.2降低到0.15,最大磨损量降到基体磨损量的一半。     

影响纳米Cu固体材料性能的工艺参数研究

 采用正交试验方法，通过XRD，MHV2000型显微硬度计（数显）和基于浮力原理等测试手段研究了压制压力、保压时间、退火温度和退火时间对自悬浮定向流－冷压法制备纳米Cu固体材料性能（晶粒大小、密度及显微硬度）的影响。结果表明：对晶粒度而言，退火温度是显著性影响因素，同时表明纳米Cu固体具有较好的热稳定性；对密度而言，压制压力是显著性影响因素；对显微硬度而言，退火时间是显著性影响因素。     

0.5Ba(Ti0.8Zr0.2)O3-0.5(Ba0.7Ca0.3)TiO3压电薄膜的摩擦、磨损性能

具有准同型相界组分的0.5Ba(Ti_0.8Zr_0.2)O₃-0.5(Ba_0.7Ca_0.3)TiO₃ (BZT-0.5BCT)陶瓷, 表现出优异的铁电、压电性能, 作为一种具有潜在应用前景的无铅压电材料得到广泛关注. 本文采用溶胶-凝胶方法在Si(100)基底上制备了BZT-0.5BCT压电薄膜. 使用原子力显微镜和扫描电子显微镜测量得到样品的形貌图, 形貌图表明该方法制备的无铅压电薄膜表面光滑, 晶粒大小均匀、呈半球形, 直径为80–100 nm, 厚度为1.7 μm, 膜的内部有气孔.摩擦力实验表明, 压电薄膜样品与硅针尖之间存在静电力的作用, 导致其摩擦力远大于硅针尖与SiO₂之间的摩擦力, 但是两者的摩擦系数基本相同.划痕实验表明, BZT-0.5BC薄膜具有很强的法向承载能力, 但是切向抗磨损能力差, 样品的平均弹性模量为23.64 GPa± 5 GPa, 其硬度为2.7–4 GPa, 两者均略低于压电陶瓷Pb(Zr, Ti)O₃材料的体态值. 关键词： BZT-BCT薄膜 纳米摩擦力 纳米压痕 纳米划痕     

A different approach to fabricate nanocrystalline LTB:Cu pellets with thermoluminescence response

In this study, lithium-tetraborate (LTB) was synthesized by three methods of high-temperature solid state, wet and combustion reactions. Copper was added to pure LTB by solution assisted method, to improve the thermoluminescence (TL) properties. The pellets of LTB were produced using pressing and sintering operations at 850 °C. The synthesized LTB pellets, exposed to the gamma radiation of ⁶⁰Co source in the dose range of 5–20Gy and glow curves as well as dose–response diagrams were obtained. Ultimately, the effects of different factors on TL behaviors like dopant, crystallite size and particle morphologies were studied. The results show that between pure samples, LTB which synthesized by combustion method has higher TL sensitivity than those of other methods. However, it was seen a weak glow peak for 5Gy, due to the nanocrystalline structure of LTB. This property led to decrease TL intensity at low-doses and postponed saturation at high-doses. Fading of this sample was also less than others and has relatively better reproducibility. Among LTB:Cu pellets which synthesized by the wet reaction showed the higher TL response than others due to the creation of more traps and luminescence centers and had promising properties in the case of dose response linearity and fading.     

纳米Cu固体材料的X射线衍射与正电子湮没研究

 采用自悬浮-冷压法，在不同压力下制得纳米Cu固体材料并对其在不同温度和保温时间下进行退火，利用X射线衍射(XRD)和正电子湮没寿命谱(PAS)分析对材料的结构和微观缺陷进行了表征。XRD分析表明，压制而得的样品晶粒度为20 nm，低于300 ℃退火3 h后并未发现晶粒显著长大；PAS分析表明，压制后的样品缺陷主要为单空位和空位团，大空隙很少，随着退火温度的升高和退火时间的延长，单空位通过扩散结合成空位团，大空隙也在温度较高时分解为空位团，导致空位团的含量增加，而单空位和大空隙的含量降低。     

Strain rate sensitivity of ultra-fine and nanocrystaline metals and alloys

The mechanical behavior of metals and alloys is strongly related to grain size. In particular, the grain refining leads to the increase in yield strength in the ultra-fine grain (<1 μm) and nanocrystalline (<100 nm) regimes.Instrumented nanoindentation measurements allow a rapid evaluation of mechanical properties of materials, and the possibility to perform tests in a very wide range of loads. The strain rate sensitivity of ultra-fine and nanocrystalline metals can be derived by changing loading rates. The present paper presents the results on the strain rate sensitivity of ultra-fine grain metals produced by equa-channel angular pressing and nanocrystalline materials produced via electrodeposition. The results were obtained by systematic experiments performed at different loading rates (3, 30 and 300 mN/s) showing broad ranges of variations for the investigated metals. Also, the strain rate sensitivity of the studied materials was derived from the load vs. depth curves.     

固结压强对纳米PbF2的相变和离子电导率的影响

 用惰性气体蒸发-真空原位固结法制备了直径为10 mm、厚度为1～2 mm的具有清洁界面的纳米PbF₂块体材料,原位固结压强为0.3～1.8 GPa。采用X射线衍射和复阻抗谱方法,研究了固结压强对纳米PbF₂物相组成、晶粒度和离子电导率的影响。结果表明,相同压强下,纳米β-PbF₂比粗晶β-PbF₂更易于向α-PbF₂转化;随着压强增大,样品中低电导率的α-PbF₂相不断增加,导致离子电导率下降。压强引起的连续相变使晶粒度缓慢长大。由于晶粒细小,纳米α-PbF₂的离子电导率比粗晶α-PbF₂提高约一个数量级,与粗晶β-PbF₂相当。     

Effects of N2 addition on nanocrystalline diamond films by HFCVD in Ar/CH4 gas mixture

Nanocrystalline diamond (NCD) films were grown on silicon substrates by hot filament chemical vapor deposition in Ar/N₂/CH₄ gas mixtures. The effects of seeding process prior to deposition, the total gas pressure, and concentration of nitrogen on the grain size, morphology and bonding nature in HFCVD technique were investigated. The results indicated that a low total gas pressure is favorable for nanosized diamond crystallites. Films micrograph obtained from scanning electron microscopy showed diamond nanograins elongated with the addition of nitrogen in the plasma. Crystal structure investigations were carried out by X-ray diffraction measurements for deposited films. An increase in the size of crystallite is also observed from XRD measurements in NCD film when nitrogen was added in plasma. From Raman spectra, it was observed that the relative intensity of G peak increases indicating more graphite content after nitrogen added in the plasma. The effects of the nitrogen incorporation in nanocrystalline films in HFCVD are discussed.     

Modulation of residual stress in diamond like carbon films with incorporation of nanocrystalline gold

Residual stress modulation in the diamond-like carbon coatings with incorporation of gold nanoparticles was studied critically. The films were deposited on glass and Si (1 0 0) substrates by using capacitatively coupled plasma chemical vapor deposition. Stresses in the films were determined from the broadening of the optical absorption tail and were found to decrease from 2.3 GPa to 0.48 GPa with increasing gold content (2-7 at.% Au) in the DLC matrix. Gold incorporation also made the films harder than the corresponding DLC coatings. Modulation of stress with nanocrystalline gold content in the DLC matrix was related to the relative amount of sp²/sp³ content in the DLC films.     

Mechanical properties of nanocrystalline copper under thermal load

The material properties of nanocrystallines are known to generally have a strong dependence on their nanoscale morphology, such as the grain size. The Hall-Petch effect states that the mechanical strength of nanocrystalline materials can vary substantially for a wide range of grain sizes; this is attributed to the competition between intergranular and intragranular deformations. We employed classical molecular dynamics simulations to investigate the morphology-dependent mechanical properties of nanocrystalline copper. The degradation of material properties under thermal load was investigated during fast strain rate deformation, particularly for the grain size. Our simulation results showed that the thermal load on the nanocrystalline materials alters the grain-size behavior of the mechanical properties.     

High Pressure effects on electrical resistivity and dielectric properties of nanocrystalline SnO2

Nanocrystalline tin oxide (SnO₂) was prepared by chemical precipitation method with different grain sizes. The X-ray diffraction studies showed the structural stability of nanocrystalline SnO₂ under high-pressure. Electrical and dielectric properties were studied on these samples using complex impedance spectroscopy under different hydrostatic pressures. Electrical resistivity and dielectric studies showed a transition in nanocrystalline SnO₂ when it was subjected to high-pressure. The transition pressures obtained from both the resistivity and dielectric measurements agree with each other. The transition pressures were found to increase considerably with the decrease in grain size. Dielectric constant was found to decrease with the reduction of grain size. In order to find whether the transition with pressure is structure- related or not, Raman spectroscopy was done at normal temperature and pressure (NTP) and as a function of pressure at room temperature. Raman modes at NTP showed lines which correspond to tetragonal rutile structure of SnO₂. In situ high-pressure Raman measurements were carried out up to 3.38 GPa. No structural change was found with pressure.