The effect of a nitrogen-rich surface layer on the sub-surface deuterium (hydrogen) concentration distribution in titanium

Deuterium and nitrogen depth profiles in Ti with modified surfaces have been measured with Auger electron spectroscopy, secondary ion mass spectroscopy, and D(³He,p)⁴He nuclear reaction analysis. Nitrogen-rich surfaces layers of varying thicknesses were created on Ti by exposure to N₂ gas at 650°C. Deuterium loading was performed by exposure to 1 Torr of D₂ gas at 500°C. The deuterium distribution was influenced by nitrogen in the near-surface regions of all samples. Specifically, deuterium solubility was suppressed in surface regions of high (greater than 1%) nitrogen concentration. The deuterium solubility also remained low within the first few microns, well beyond the region of high nitrogen concentration. This effect is attributed to internal elastic stresses imposed by the non-deuterium absorbing nitrogen-rich layer on the Ti. These stresses prohibit the volume expansion associated with deuterium absorption. We estimate stresses on the order of 3–4 GPa are required to suppress the deuterium solubility to the values observed. The deuterium absorption kinetics were observed to depend systematically on the thickness of the nitrogen-rich layer. This is consistent with limited solubility near the surface or a surface poisoning effect influencing the overall deuterium diffusion from the gas phase into the Ti bulk.     

Depth profiling of D implanted into Ti at different temperatures

Depth proliles of 6.6 keV D⁺ implanted into titanium in the temperature range between 140 K and 500 K have been studied using the D(³He, α) H nuclear reaction.

At 140 K the trapped amount is close to 100% at low doses and reaches saturation at about 2 × 10¹⁸D/cm², whereas at room temperature no saturation could be reached up to 2 × 10¹⁹ D/cm². At higher temperatures the amount decreases until no deuterium could be detected in the surface layer above 500 K.

The depth profiles are strongly dependent on temperature. At 140 K the deuterium is found in a surface layer of about 2000 Å with a maximum ratio of deuterium to metal atoms of 2.5. At room temperature a hydride layer of TiD^1.8, forms. The thickness of the hydride layer depends on deuterium dose and extends to 1.5 μm at 2 × 10¹⁹ D/cm². At higher temperatures the atom concentrations are lower and the deuterium seems to diffuse deeply into the bulk.

These results are discussed in terms of diffusion of deuterium i n Ti and titanium hydride.     

The influence of the implantation temperature on the generation of dislocations in antimony-implanted and annealed silicon

We report the first observation of non-equilibrium redistribution effects during laser treatment of a binary system having equilibrium segregation coefficient, k₀, much greater than unity. Polycrystalline aluminium samples implanted with 30 keV Sb⁺ ions to a dose of 1.7 × 10¹⁷ ions/cm² were irradiated with single pulses (7 ns FWHM) from a Nd: glass laser operating in TEM₀₀ mode. The peak energy density (at the centre of the laser spot) varied from 2.0 to 5.7 J/cm². A detailed liquid phase diffusion analysis, explicitly incorporating rapid melt front motion and interfacial segregation, is performed to fit the Sb depth profiles measured with a nuclear microprobe. An effective distribution coefficient k = 1 (as compared to equilibrium value of k₀～7) is obtained in agreement with the theoretical limiting value for large melt front velocities.     

ERD studies of D-ion depth distributions after implantation into some pure metals and alloys

This paper presents a report on experimental results of depth distributions of deuterium ions implanted with 25 keV energy at a fluence interval of (1.2–2.3) × 10²² m⁻² into samples of pure metals (Cu, Ti, Zr, V, Pd) and diluted Pd alloys (Pd-Ag, Pd-Pt, Pd-Ru, Pd-Rh). The post-treatment depth distributions of deuterium and hydrogen atoms were measured within a few hours after implantation with the use of elastic recoil detection (ERD) analysis. After three months the measurements were repeated. The comparison of the obtained results in both series of studies allowed us to make an important observation of the desorption rates of implanted deuterium atoms from pure metals and diluted Pd alloys. The maximum measured concentrations of deuterium atoms in pure Zr and Ti foils with relatively small desorption rate of deuterium atoms within three months after implantation were observed. Also a very high spreading of deuterium atom distributions was observed in all the measured pure metals and alloys. It can be explained by the large diffusion coefficients of deuterium and extremely fast kinetics.     

Deuterium accumulation in an assembly of nickel foils irradiated by high-temperature deuterium plasma

The accumulation of deuterium in an assembly of nickel foils by the pulsed irradiation of a deuterium plasma is studied. It is established that implanted deuterium is transferred to a much greater depth than that corresponding to the projective range of deuterium plasma ions with a maximum velocity of 10⁸ cm/s. The maximum concentration (up to 4 at % deuterium) is observed in the second Ni foil. The observed phenomenon can be explained by the action of shock waves and concomitant stresses on the transport and redistribution of deuterium to greater depths.     

Hydrogen isotopic replacement and microstructure evolution in zirconium deuteride implanted by 150 keV protons

Zirconium tritiated(ZrT_x) is an alternative target material for deuteron–triton(D-T) reaction neutron generator. The isotopic replacement and microstructure evolution induced by hydrogen isotope implantation could significantly affect the performance of the target film. In this work, the zirconium deuteride film deposited on Mo/Si substrate was implanted by 150 ke V protons with fluence from 1×10~(16) to 1×10~(18) protons/cm~2. After implantation, the depth profiles of retained hydrogen(H) and deuterium(D) in these target films were analyzed by elastic recoil detection analysis(ERDA), and time of flight-secondary ion mass spectrometry(To F-SIMS). Additionally, the microstructure evolution was also observed by x-ray diffraction(XRD) and scanning electron microscope(SEM). The D concentration in the Zr Dx film decreased versus the proton implantation fluence. An analytical model was proposed to describe the hydrogen isotopic trapping and exchange as functions of incident protons fluence. Additionally, the XRD analysis revealed that no new phase was formed after proton implantation. Furthermore, circular flakings were observed on the ZrD_x surface from SEM images at fluence up to 1×10~(18) protons/cm~2, and this surface morphology was considered to associate with the hydrogen atoms congregation in Mo/Si boundary.     

Experimental investigation of the energy and depth dependence of flux peaking

The yield of helium ions backscattered from Yb implanted in silicon crystals has been studied as a function of the angle between the incident beam direction and various symmetry axes of the silicon crystal. The depth of the implanted Yb has been varied by using different implantation energies, and the analyzing beam energy has been varied from 0.5 to 2 MeV in an effort to obtain information about the energy and depth dependence of the flux-peaking phenomenon. The results are compared with those of Andersen and coworkers. We have observed the oscillation with depth of the flux in the center of a channel predicted by Van Vliet.     

稠密氘气物态方程研究

 用二级轻气炮作为加载手段,通过瞬态辐射高温计对样品氘的冲击压缩层的光谱辐射亮度历史进行测量,测得氘气中冲击波速度和冲击温度,并用离解电离平衡方程从理论上分析了冲击压缩下稠密气体的组分,理论计算的Hugoniot曲线及冲击温度和实验结果吻合。     

Depth concentrations of deuterium ions implanted into some pure metals and alloys

Pure metals (Cu, Ti, Zr, V, Pd) and diluted Pd alloys (Pd-Ag, Pd-Pt, Pd-Ru, Pd-Rh) were implanted by 25-keV deuterium ions at fluences in the range (1.2–2.3) × 10²² m⁻². The post-treatment depth distributions of deuterium ions were measured 10 days and three months after the implantation by using Elastic Recoil Detection Analysis (ERDA) and Rutherford Backscattering (RBS). Comparison of the obtained results allowed us to make conclusions about relative stability of deuterium and hydrogen gases in pure metals and diluted Pd alloys. Very high diffusion rates of implanted deuterium ions in V and Pd pure metals and Pd alloys were observed. Small-angle X-ray scattering revealed formation of nanosized defects in implanted corundum and titanium.     

The oxidation characteristics of nitrogen-implanted silicon

The trapping of 5 keV deuterium in ～ 165 and ～ 4000 nm thick BeO films grown by thermal oxidation on Be substrates was investigated at different temperatures using the D(³He,H)⁴He nuclear reaction. The ratio of implanted D to BeO molecules obtained at saturation is 0.24 to 0.34. The D migrates from its end of range location and distributes itself uniformly in the BeO film. With increasing implant temperature the BeO layer flakes from the Be substrate. The distribution of D in BeO films at high concentrations is not consistent with diffusivity measurements at low concentrations of T in BeO.     

Angular distribution of desorbing/permeating deuterium from modified Pd(1 1 1) surfaces

The angular distribution of desorbing deuterium molecules was investigated for the clean Pd(1 1 1) surface and for modified Pd(1 1 1) surfaces, either pre-covered with 0.2 ML potassium or with an ultra-thin V₂O₃ surface oxide. The palladium sample was part of a permeation source and the angular distribution was measured by lateral displacement of the sample in front of a differentially pumped flux detector. For the clean surface at 523 K, the angular distribution is close to a cosine distribution, but changes to a cos^1.9Θ distribution at 700 K. Potassium on the surface alters the angular distribution to a cos³Θ function at 523 K. The ultra-thin vanadium oxide layer on the Pd(1 1 1) surface has no significant influence on the angular distribution of deuterium desorption. The experimental results were compared with existing data of the energy dependent sticking coefficient and the energy distribution of the desorption flux as measured by time-of-flight spectroscopy. This made it possible to get information on the applicability of detailed balance and normal energy scaling.     

Tomographic study of the three-dimensional distribution of a high-fluence implant in a polymer

6 Li⁺ ions were implanted into PMMA at high flux up to fluences of 1×10¹⁵ cm^-2 under angles of 0° to 70° towards the surface normal. The Li depth distributions were determined by means of neutron depth profiling, and compared with theoretical simulations. The three-dimensional Li distribution was reconstructed from the one-dimensional depth profiles by means of a tomographic technique. It turned out that the measured Li depth distributions can be described by a superposition of Gaussian and exponential functions. This points at considerable Li mobility during or after the ion implantation, with trapping in unsaturable traps in the ion-irradiated region which roughly follow the electronic energy transfer distribution. The Li redistribution is more pronounced along the track direction than transversely to it. The normalized Li distributions in various implantation directions were fed into our tomographic program to reconstruct the three-dimensional distribution of the deposited lithium. As expected, the lithium preferentially distributes along the ion tracks. This work is another hint that mobility of implanted ions in solids does not proceed isotropically, but is strongly influenced by the radiation-damage distributions. Received: 11 May 1998 / Accepted: 9 September 1998 / Published online: 24 February 1999     

Numerical approach for depth profiling with GE‐XRF

The atomic percentage of implanted particles on the sample surface was estimated from the peak position of angle dependency of the experimental grazing exit X‐ray fluorescence (GE‐XRF) intensity profile. An algorithm for constructing three‐parametric Gaussian‐type depth profiles of atoms implanted in a substrate was developed. The position of the maximum and its value of the implanted particles distribution as well as a dispersion of that distribution were considered in the calculations. The model was applied to the intensity of the As Kα line emitted from As atoms implanted in a Si wafer. The least‐square method was used to minimize the overall difference between experimental and calculated GE‐XRF intensity. Optimum parameters of the particle distribution were determined in this procedure. Using that profile, the depth dependencies of effective real and imaginary parts of atomic scattering factor and complex index of refraction of the sample material were evaluated. Copyright © 2006 John Wiley & Sons, Ltd.     

Experimental verification of a zero order desorption model: D2 on Ni(110)

The rate of desorption of deuterium from the low temperature (α) state on Ni(110) follows nearly zero order kinetics. Simultaneous measurements of intensities and profiles of half-order diffraction beams and changes in work function during isothermal desorptionof D₂, have shown that the zero order region is associated with the presence of islands of the (1 × 2) phase which act as reservoirs of deuterium. These results are discussed in terms of a recent model for zero order desorption which requires the presence of 3 deuterium surface phases in equilibrium. The activation energy for desorption of the α-state is 67 ± 6 kJ mol⁻¹.     

Investigation of the ETA-BETA II plasma edge by surface analysis of collector probes

To investigate the ion flux escaping from the plasma and the impurity flux released by the wall, collector probes made of graphite, silicon and titanium have been exposed to the deuterium plasma confined in the toroidal device ETA BETA II. The damages on the collector surfaces have been surveyed by a scanning electron microscopy (SEM) apparatus. The deuterium and impurity retention have been measured by elastic recoil detection (ERD) and Rutherford backscattering spectroscopy (RBS) techniques respectively. The implantation build-up has been investigated as a function of the exposure time. The deuterium dose in graphite saturates after a few discharges, whereas the metal impurities exhibit a linear increase in time. The deuterium flux and its radial dependence, inferred from the implanted concentrations, have been compared with those measured by Langmuir probes. Metal impurities have been identified and their relative abundances have been compared with the material wall composition. The impurity flux is found consistent with the global content in the plasma derived by spectroscopic measurements. The deuterium dose measured in different samples has been related to the backscattering coefficient of the materials. Finally, to investigate the damage on sample probes facing the plasma particle flow, erosion probes made of vitreous graphite with silver implanted at a fixed depth have been exposed to the plasma and the thickness change after exposure recovered.     

Antimony implanted silicon: A comparison between the total implanted concentration profile and the donor concentration profile

Abstract

The total concentration profiles of various doses of antimony, implanted into silicon at 100 keV, have been determined by a new technique, using Kr⁺ ions to detect selectively the antimony (as Sb-M X-rays) at the expense of the silicon. Since most of these X-rays arise from only a few tens of Angstroms below the surface of the silicon, this allows the X-ray generation to be used in conjunction with an anodic stripping technique to obtain the antimony depth distribution. These profiles are compared with others, obtained by measuring the donor concentration as a function of depth, using standard Hall effect and conductivity measurements. A significant difference between these profiles was observed, which is thought to be due to the suppression of electrical activity which occurs as the result of lattice damage. Confirmatory evidence is presented in the form of electron microscope observations of the implanted region at various depths below the silicon surface.     

硅离子注入层的电场调制反射光谱

结合剥层技术,对略高于临界剂量的P⁺注入p-Si层,进行了电解液电场调制反射(以下简称EER)光谱研究,对非均匀的结构无序材料的光学测量,提出采用“特效波长”的建议,硅的这一波长是E₁,E₁+△₁能区的349O?(hω≈3.55eV),c-Si和α-Si对3490?光波的吸收系数均等于10⁶cm^-1,将((△R)/R)_3.55ev按深度x的分布同无序度的 关键词：     

Laser and Thermal Modification of Silver–Ion Implanted Glasses

We investigate sodium–calcium silicate glasses implanted with 60 keV Ag⁺ ions with a dose of 3·10¹⁶ cm^–2 at an ion current density of 10 A/cm². As a result of the ion implantation, a composite layer with silver nanoparticles is synthesized in the region near the surface. However, this layer is characterized by high nonuniformity in the size distribution of these particles over the depth of the layer. Subsequent pulsed laser irradiation in combination with equilibrium heat treatment makes it possible to modify this composite layer, improving the uniformity in the size distribution of the nanoparticles. This is particularly promising for the improvement of the technology of obtaining nonlinear optical materials. To control the parameters of the layers obtained we suggest a method based on an analysis of the optical reflection and transmission spectra measured on the side of the implanted and opposite surfaces of glass samples.     

基于温度梯度的ICF冷冻靶均化技术研究

惯性约束聚变(ICF)冷冻靶中氘氘(D2)、氘氚(DT)等燃料冰层在靶丸中的分布由靶丸所处的温度场决定。在氘氘冷冻靶中,垂直温度梯度引起的气-液界面张力梯度可以抵消重力作用,使氘氘液体在靶丸内均匀分布;然后在氘氘的三相点附近缓慢降温,可以实现燃料冰层的均化。 在氘氘冷冻靶均化实验系统上,采用温度梯度结合制冷速率与制冷过程控制的方法,实现了1 mm直径、30 m壁厚的辉光放电聚合物(GDP)靶丸中氘氘冰层的均化,对背光阴影图像中亮环位置进行分析表明: 氘氘冰层的平均厚度为185.56 m,均匀度为80.2%,模数-功率谱曲线中模数2~100对应的内表面粗糙度为2.26 m。     

基于温度梯度的ICF冷冻靶均化技术研究

惯性约束聚变(ICF)冷冻靶中氘氘(D2)、氘氚(DT)等燃料冰层在靶丸中的分布由靶丸所处的温度场决定。在氘氘冷冻靶中,垂直温度梯度引起的气-液界面张力梯度可以抵消重力作用,使氘氘液体在靶丸内均匀分布;然后在氘氘的三相点附近缓慢降温,可以实现燃料冰层的均化。在氘氘冷冻靶均化实验系统上,采用温度梯度结合制冷速率与制冷过程控制的方法,实现了1mm直径、30μm壁厚的辉光放电聚合物(GDP)靶丸中氘氘冰层的均化,对背光阴影图像中亮环位置进行分析表明:氘氘冰层的平均厚度为185.56μm,均匀度为80.2%,模数-功率谱曲线中模数2~100对应的内表面粗糙度为2.26μm。