ECR plasma assisted deposition of zinc nanowires

Deposits of one dimensional nanowires of zinc with diameters of 90-120 nm have been obtained by means of dc sputtering within an electron cyclotron resonance plasma reactor. The sputtering has been made effective by using a negatively biased cylindrical target. The structure of the nanocrystalline wires deposited on glass substrates were investigated with scanning electron microscopy, transmission electron microscopy and scanning tunneling microscopy. STM revealed that the structure of the one dimensional nanowires are ensemble of nanoclusters and nanowires with diameter of 4-5 nm. The crystalline nature of the metallic nanowires was studied with X-ray and electron diffraction analysis. The native oxide present on the metallic wires was revealed by photoluminescent spectroscopy. Theoretical modeling has been used to explain the possible mechanisms operative inside the plasma which lead into deposition of zinc on the substrate starting from the precursor species.     

基于单一气源的PECVD方法制备SiC薄膜及其微观结构研究

为制备出满足惯性约束聚变（ICF）实验要求的SiC薄膜,本文采用等离子体增强化学气相沉积（PECVD）法,以四甲基硅（TMS）作为唯一反应气源,在不同工作压强下制备SiC薄膜。利用扫描电子显微镜、表面轮廓仪、原子力显微镜、精密电子天平、X射线光电子能谱、傅里叶变换红外光谱对薄膜进行表征与分析。结果表明：SiC薄膜的成分与工作压强密切相关,随着工作压强的增加,薄膜中Si含量整体呈下降趋势;随着工作压强的增加,薄膜沉积速率先增大后减少,密度先减小后增大;与其他制备工艺相比,采用单一气源制备SiC薄膜,其表面粗糙度极低（1.25～1.85 nm）,薄膜粗糙度随工作压强的增加呈先增大后减小的趋势。     

Effect of Low-Frequency Power on Etching Characteristics of 6H-SiC in C_4F_8/Ar Dual-Frequency Capacitively Coupled Plasma

Dry etching of 6H silicon carbide(6H-SiC)wafers in a C_4Fs/Ar dual-frequency capacitively coupled plasma(DF-CCP)was investigated.Atomic force microscopy(AFM)and X-ray photoelectron spectroscopy(XPS)were used to measure the SiC surface structure and compositions,respectively.Optical emission spectroscopy(OES)was used to measure the relative concentration of F radicals in the plasma.It was found that the roughness of the etched SiC surface and the etching rate are directly related to the power of low-frequency(LF)source.At lower LF power,a smaller surface roughness and a lower etching rate are obtained due to weak bombardment of low energy ions on the SiC wafers.At higher LF power the etching rate can be efficiently increased,but the surface roughness increases too.Compared with other plasma dry etching methods,the DF-CCP can effectively inhibit C_xF_y films'deposition,and reduce surface residues.     

Ion beam synthesis and doping of photonic nanostructures

Optically-active silica nanowires are produced by metal-induced growth on silicon substrates using ion-implantation, with two different strategies employed for their fabrication. The first is based on Er implantation of nanowires produced by a thin-film Pd catalyst layer, and the second employing implanted Er as both the catalyst and dopant. The luminescence properties of the resulting Er-doped silica nanowires are reported and compared with similarly implanted fused silica samples. Comparison shows that the luminescence lifetime of Er is increased by incorporation within the nanowires due to a reduction in the density of available optical states in these structures. Additional details of the synthesis, structure and properties of these functionalised nanowires are also presented.     

Relation between etching profile and voltage–current shape of sintered SiC etching by atmospheric pressure plasma

Sintered silicon carbide (SiC) was etched by a dielectric barrier discharge source. A high voltage bipolar pulse was used with helium gas for the plasma generation. One stable filament plasma was generated and could be used for SiC etching. As the processing gas (NF₃) mixing rate increased, the width and depth of the etching profile became narrower and deeper. The differentiated V–Q Lissajous method was used for measuring the capacitances (C_eq) of the electrode after the plasma turned on. The width of the etching profile was proportional to C_eq. As the current peak value I_smx of the substrate current increased, the volume removal rate of SiC increased. The etch depth was proportional to the ratio of I_smx to C_eq. Additionally, because of the different characteristics of the plasma disks on SiC substrate by the voltage polarity, the etching profile was unstable. However, in high NF₃ mixing process, the etching profile became stable and deeper.     

Ion beam induced amorphization and recrystallization of Si/SiC/Si layer systems

Epitaxial, buried silicon carbide (SiC) layers have been fabricated in (100) and (111) silicon by ion beam synthesis (IBS). In order to study the ion beam induced epitaxial crystallization (IBIEC) of buried SiC layers, the resulting Si/SiC/Si layer systems were amorphized using 2 MeV Si²⁺ ion irradiation at 300 K. An unexpected high critical dose for the amorphization of the buried layers is observed. Buried, amorphous SiC layers were irradiated with 800 keV Si⁺ ions at 320 and 600°C, respectively, in order to achieve ion beam induced epitaxial crystallisation. It is demonstrated that IBIEC works well on buried layers and results in epitaxial recrystallization at considerably lower target temperatures than necessary for thermal annealing. The IBIEC process starts from both SiC/Si interfaces and may be accompanied by heterogenous nucleation of poly-SiC as well as interfacial layer-by-layer amorphization, depending on irradiation conditions. The structure of the recrystallized regions in dependence of dose, dose rate, temperature and crystal orientation is presented by means of TEM investigations.     

Electronic structure of In_2O_3 nanowires synthesized at low temperature

In₂O₃ nanowires with uniform morphology and single crystalline structure were synthesized at low temperature of 400℃⁴50℃using InSb as the precursor via VLS mechanism.The nanowires have uniform diameter of about 40 nm and are up to tens of micrometres in length and grew along the[100]direction as established by high resolution electron microscopy.The electronic and local structures of ln203 nanowires,compared to that of In203 powder,have been studied with X-ray absorption fine structure（XAFS） at In K-edge and O K-edge.The XAFS results reveal the stronger In-O bonding in In₂O₃ nanowires compared to bulk In₂O₃.     

Influence of nitrogen ion implantation energies on surface chemical bonding structure and mechanical properties of nitrogen-implanted silicon carbide ceramics

Nitrogen ions were implanted into silicon carbide ceramics (N⁺-implanted SiC) at different ions energies. The surface chemical bonding structure of N⁺-implanted SiC ceramics were investigated by using X-ray photoelectron spectroscopy (XPS). The hardness of N⁺-implanted SiC ceramics was measured using nano-indenter, and the friction and wear properties of the N⁺-implanted SiC/SiC tribopairs were studied using ball-on-disk type tribo-meter in water lubrication. The wear tracks were observed using non-contact surface profilometer and scanning electron microscope (SEM). The results showed that the surface roughness of N⁺-implanted SiC ceramic was higher than that of SiC ceramic, and some chemical bonds such as Si–N, C–C, CN and C–N bonds were formed in N⁺-implanted layer besides Si–C bonds. In comparison of SiC ceramic’s hardness, the hardness of N⁺-implanted SiC ceramics at 30 and 50 keV was higher while that at 65 keV was lower. Under water lubrication, the friction coefficient and the specific wear rates for the N⁺-implanted SiC/SiC tribopairs were all lower than those of the SiC/SiC tribopairs, and displayed the lowest values at 50 keV. According to XPS analysis, it was concluded that the high wear resistance and low friction coefficient for the N⁺-implanted SiC/SiC tribopairs were attributed to the formation of carbon rich composite on the surface of N⁺-implanted SiC ceramics.     

Fracture strength estimation of SiC block for IS process

The Japan Atomic Energy Agency has been conducting R&D on thermochemical water-splitting Iodine–Sulfur (IS) process for hydrogen production to meet massive demand in the future hydrogen economy. A concept of sulfuric acid decomposer was developed featuring a heat exchanger block made of SiC. Recent activity has focused on the reliability assessment of SiC block. Although knowing the strength of SiC block is important for the reliability assessment, it is difficult to evaluate a large-scale ceramics structure without destructive test. In this study, a novel approach for strength estimation of SiC structure was proposed. Since accurate strength estimation of individual ceramics structure is difficult, a prediction method of minimum strength in the structure of the same design was proposed based on effective volume theory and optimized Weibull modulus. Optimum value of the Weibull modulus was determined for estimating the lowest strength. The strength estimation line was developed by using the determined modulus. The validity of the line was verified by destructive test of SiC block model, which is small-scale model of the SiC block. The fracture strength of small-scale model satisfied the predicted strength.     

Deuterium retention in SiC coated graphite by D2+ implantation

The doped graphite tiles bolted to the active cooling heat sink, made of GBST1308 (1% B₄C, 2.5% Si, 7.5% Ti) coated with SiC, are now being used as the only plasma facing material (PFM) for the EAST device since the campaign of 2008. From the plasma density and fueling point of view, it is important to study thoroughly the hydrogen isotope retention in this kind of SiC-coated doped graphite. D₂⁺ implantations into the SiC coated doped graphite were performed at Shizuoka University. The chemical states of Si and C were studied by means of X-ray photoelectron spectroscopy (XPS), and the thermal desorption behavior of deuterium was analyzed by thermal desorption spectroscopy (TDS). It was found that deuterium was trapped by both C and Si in the SiC coatings. In the previous studies, Oya et al. reported the deuterium retention behavior in polycrystalline β-SiC. In this paper, difference of retention behavior in β-SiC and SiC coating will be also discussed.     

用于ICF的非晶SiC微球制备及微观结构研究

以四甲基硅烷、反式二丁烯和氢气为工作气源,采用化学气相沉积-高温热解法成功制备了壁厚约21μm的非晶SiC微球。利用能量色散X射线光谱仪、X射线光电子能谱仪、X射线衍射仪、Raman光谱仪、扫描电子显微镜、白光干涉仪和X射线照相机对SiC微球的化学成分、结晶状态、表面形貌与粗糙度以及密度与球形度等进行了测量和分析。结果表明:在无氧环境下,通过450~900℃的高温热解及致密化可将在聚α甲基苯乙烯芯轴上沉积的掺硅碳氢聚合物涂层转变成致密的SiC微球。SiC微球呈非晶态,其C/Si原子比约为1.3,主要含有C—Si键和C=C键,微观结构呈无规则状且颗粒分布均匀,密度、球形度和壁厚均匀性分别为2.62 g/cm~3、99.8%和96.8%。     

FCM燃料堆内行为模拟及结构设计研究

The thermal mechanical performance of the fully ceramics microencapsulated fuel (FCM) with different non-fuel part size was simulated using two-dimensional characteristic unit. When the fissile loading meet the requirements of the reactor core, the stress condition of SiC matrix and SiC layers were investigated for FCM pellets with different structures. Non-fuel parts and SiC layers suffered relative lower stress by optimizing FCM pellet structure and adjusting distance between different TRISO particles. The stress distribution of matrix, non-fuel part and SiC layer was discussed for the FCM pellets with non-fuel part size from 100 μm to 500 μm. The results indicate that, the maximum hoop stress of the matrix and SiC layer increased with the increasing of non-fuel part size, while the non-fuel parts exhibited crosscurrent. Non-fuel parts and SiC layer possessed lower stress when the non-fuel part was 400 μm. The stress of non-fuel part was about 400 MPa, and the maximum hoop stress of the SiC layers were about 200 MPa. The failure probability was 2.5×10-4. The structure integrity was maintained for the pellets with 400 μm non-fuel part, at the same time the failure probability SiC layer was low. Structural optimization is the basis for the application of FCM pellet.     

SiC/SiC composite fabricated with carbon nanotube interface layer and a novel precursor LPVCS

Continuous SiC fiber reinforced SiC matrix composites (SiC/SiC) have been studied as promising candidate materials for nuclear applications. Three-dimensional SiC/SiC composite was fabricated via polymer impregnation and pyrolysis (PIP) process using carbon nanotubes (CNTs) as the interface layer and LPVCS as the polymer precursor. The microstructural evolution of the fiber/matrix interface was studied. The porosity, mechanical properties, thermal and electrical conductivities of the SiC/SiC composite were investigated. The results indicated that the high densification efficiency of the liquid precursor LPVCS resulted in a low porosity of the SiC/SiC composite. The SiC/SiC composite exhibited non-brittle fracture behavior, however, bending strength and fracture toughness of the composite were relatively low because of the absence of CNTs as the interface layer. The thermal and electrical conductivities of the SiC/SiC composite were low enough to meet the requirements desired for flow channel insert (FCI) applications.     

FCM燃料堆内行为模拟及结构设计研究

本文采用二维特征模型模拟不同无燃料区厚度全陶瓷微封装弥散（FCM）燃料的热力学行为，在保证堆芯装载要求的条件下，研究不同结构FCM燃料SiC基体和包覆燃料颗粒SiC层的应力状态。通过优化无燃料区厚度，调整TRISO颗粒间的间距，保证无燃料区和SiC层同时具有较低的应力水平。分析了无燃料区厚度为100 ~ 500 μm时基体SiC、无燃料区以及SiC层的应力分布，结果表明，基体SiC和SiC层最大应力随无燃料区厚度增大而增大，而无燃料区的最大应力则随其厚度增大而降低。当无燃料区厚度为400 μm时，无燃料区和SiC层均处于较低的应力状态，无燃料区SiC基体应力约为400 MPa，而SiC层的最大环向应力约为200 MPa，其失效概率约为2.5×10-4。因此，当无燃料区厚度为400 μm时，FCM燃料既能维持芯块结构完整，又能保证SiC层具有较低的失效概率。结构优化为FCM燃料的应用提供了基础。      

HTGR包覆燃料颗粒碳化硅层细晶化研究

高温气冷堆(HTGR)是能适应未来能源市场的第四代先进核反应堆堆型之一,其固有安全性的第一道保障是使用的TRISO型包覆燃料颗粒。在TRISO型燃料颗粒4层包覆结构中,SiC包覆层是承受包覆燃料颗粒内压和阻挡裂变产物释放的关键层,制备高质量SiC包覆层是核燃料领域中的重大问题和关键技术之一。本文介绍高温气冷堆燃料颗粒的基本结构,详述制备SiC包覆层的流化床-化学气相沉积过程,提出SiC层细晶化这一研究方向,并系统阐述包覆燃料颗粒SiC包覆层细晶化的优势。在细晶化SiC材料制备方法方面,系统分析SiC粉体、陶瓷、薄膜和厚膜材料的研究现状,并结合本实验室前期研究成果提出制备细晶SiC包覆层的可行制备策略。     

1972 National Symposium on Atomic Energy,Tokyo, Japan

Strength and Young's modulus of pyrolytic silicon carbide (SiC) were measured. The specimens were the ringed SiC which were taken from TRISO coated fuel particles for High Temperature Gas-cooled Reactors (HTGR). Four kinds of unirradiated specimens and the two of irradiated ones were prepared for the measurement. The SiC coating layer consisting of columnar structure with large crystal grains (about 5 μm) was stronger than the SiC of laminar structure with small grains (less than 1μm). The mean strength of the former SiC was larger than 1,700 MN/m², while that of the latter SiC, less than 1,600 MN/m^s. The SiC with low density (3.14 g/cm³) was the weakest among the present specimens. By irradiation of fission recoil, the mean strength of the SiC of columnar structure with large grains almost unchanged, but that of the SiC of laminar structure with small grains increased about 14%, of which irradiation dose was about 20 times larger than that for the former specimen. As for Young's modulus, the values ranged between 324 and 381 GN/m² and no significant dependence of the modulus on microstructure of the SiC and irradiation was recognized.     

Effect of 10 MW/m2 plasma exposure on W-SiC/SiC dual layer tiles

W-SiC/SiC dual layer tile has many advantages as a high heat flux component (HHFC) material for fusion, in theory. However, due to insufficient data known, its high potentiality and near term availability has not been well recognized. This work provides the recent materials R&D status and the first plasma exposure test result from the world largest helical device, large helical device of National Institute for Fusion Science in Japan. Tungsten armor with SiC/SiC substrate layer survived during the LHD plasma exposure with 10 MW/m² maximum heat load for the 5.3-s operation cycle. The macro and microstructure evolution, including crack and pore formation, was analyzed and an excellent high heat load resistance was demonstrated.     

Interaction of Ruthenium Tetroxide with Stainless Steel

Research and development (R&;D) on the selection of molybdenum first wall during FY1975–1976 are described. The JT-60 machine parameters are plasma current of 2.7 MA, toroidal magnetic field of 4.5 T, duration time of 5 to 10 s and additional heating power of 20 to 30 MW. From the viewpoint of first wall design, these parameters are more stringent in JT-60 than in medium size tokamaks. Therefore, R&;D on selection of material and structure of the JT-60 first wall was carried out. Initially, comparison between candidate materials were made regarding material, thermal, mechanical and vacuum properties. Molybdenum, pyrolytic graphite (PyG) and CVD-Sic coated graphite (SiC/C) were primary candidate materials. Of these three materials, full-sized trial productions of the first wall were made. High heat load tests with electron beam were carried out to compare thermal shock and thermal cycle properties. Test conditions were heat fluxes of 350 to 1,000 W/cm², duration of 10 s and cycle numbers from 10 to 320. From the test results, many cracks and “crater-like” damage were observed on the surfaces of PyG and SiC/C, but no damage was observed on the Mo surface. Following evaluation of all properties including these results, Mo was selected as primary first wall material for JT-60. Moreover, a trial production of Mo honeycomb structure was done. However, the honeycomb structure was not applied because of the expensive fabrication cost. After the operation of JT-60, the first wall materials (limiter, armor plates and magnetic limiter plate) were changed to graphite in FY1987 in order to reduce severe plasma contamination.     

The ARIES-AT advanced tokamak,Advanced technology fusion power plant

The ARIES-AT study was initiated to assess the potential of high-performance tokamak plasmas together with advanced technology in a fusion power plant and to identifying physics and technology areas with the highest leverage for achieving attractive and competitive fusion power in order to guide fusion R&D. The 1000-MWe ARIES-AT design has a major radius of 5.2 m, a minor radius of 1.3 m, a toroidal β of 9.2% (β_N = 5.4) and an on-axis field of 5.6 T. The plasma current is 13 MA and the current-drive power is 35 MW. The ARIES-AT design uses the same physics basis as ARIES-RS, a reversed-shear plasma. A distinct difference between ARIES-RS and ARIES-AT plasmas is the higher plasma elongation of ARIES-AT (κ_x = 2.2) which is the result of a “thinner” blanket leading to a large increase in plasma β to 9.2% (compared to 5% for ARIES-RS) with only a slightly higher β_N. ARIES-AT blanket is a simple, low-pressure design consisting of SiC composite boxes with a SiC insert for flow distribution that does not carry any structural load. The breeding coolant (Pb–17Li) enters the fusion core from the bottom, and cools the first wall while traveling in the poloidal direction to the top of the blanket module. The coolant then returns through the blanket channel at a low speed and is superheated to ∼1100 °C. As most of the fusion power is deposited directly into the breeding coolant, this method leads to a high coolant outlet temperature while keeping the temperature of the SiC structure as well as interface between SiC structure and Pb–17Li to about 1000 °C. This blanket is well matched to an advanced Brayton power cycle, leading to an overall thermal efficiency of ∼59%. The very low afterheat in SiC composites results in exceptional safety and waste disposal characteristics. All of the fusion core components qualify for shallow land burial under U.S. regulations (furthermore, ∼90% of components qualify as Class-A waste, the lowest level). The ARIES-AT study shows that the combination of advanced tokamak modes and advanced technology leads to an attractive fusion power plant with excellent safety and environmental characteristics and with a cost of electricity (4.7 ¢/kWh), which is competitive with those projected for other sources of energy.     

Ag diffusion in cubic silicon carbide

The diffusion of Ag impurities in bulk 3C-SiC is studied using ab initio methods based on density functional theory. This work is motivated by the desire to reduce transport of radioactive Ag isotopes through the SiC boundary layer in the Tristructural-Isotropic (TRISO) fuel pellet, which is a significant concern for the Very High Temperature Reactor (VHTR) nuclear reactor concept. The structure and stability of charged Ag and Ag-vacancy clusters in SiC are calculated. Relevant intrinsic SiC defect energies are also determined. The most stable state for the Ag impurity in SiC is found to be a Ag atom substituting on the Si sub-lattice and bound to a C vacancy. Bulk diffusion coefficients are estimated for different impurity states and values are all found to have very high activation energy. The impurity state with the lowest activation energy for diffusion is found to be the Ag interstitial, with an activation energy of approximately 7.9 eV. The high activation energies for Ag diffusion in bulk 3C-SiC cause Ag transport to be very slow in the bulk and suggests that observed Ag transport in this material is due to an alternative mechanism (e.g., grain boundary diffusion).