北京大学4.5 MV静电加速器核反应分析系统

为满足对聚变堆面向等离子体材料中氘氚滞留问题的研究,北京大学4.5 MV静电加速器在原束线基础上新增核反应分析系统,该系统使用能量0.8～3.6 MeV的H⁺、D⁺、³He⁺和⁴He⁺粒子束流,可对核反应微分截面和样品中元素浓度的深度分布进行测量分析。本文对核反应分析原理、核反应分析系统的设备布局和实验方法进行了讨论,并以D(³He,p)⁴He核反应为例,分析了微分截面计算和样品中氘元素浓度深度分布的数据结果,其深度分辨小于1.5 μm,实验误差约为7.5%。     

Thin-layer activation of hip-joint prostheses for tribological tests

Thin-layer activation as a method of measuring wear has been applied in a tribological study of artificial hip joints made from CoCrMo forged alloy. The activation of CoCrMo alloy using protons, deuterons, ³He, and -particles has been studied systematically. Excitation functions are reported for the reactions ⁵⁹Co(d, p)⁶⁰Co and ¹⁰⁰Mo(, n)¹⁰³Ru.     

Depth profiling study on the migration of tritium in titanium induced by deuterium-ion bombardment

A thin titanium layer with uniformly absorbed tritium (T/Ti ˜1.0) was bombarded by 390 keV D₃⁺ ions (130 keV per deuteron). Bombardment was performed at low (111 K) and room temperatures up to fluences of 5.9 × 10¹⁸ D/cm² and 3.0 × 10¹⁸ D/cm², respectively. Depth profiles of tritium up to a depth of 0.8 mg/cm² (˜1.8 μm) were measured and the change of the profile with fluence was investigated by means of the T(d, )n nuclear reaction. At both of the temperatures, a dip was formed on the depth profile of tritium at the depth around the projected range, indicating that the deuteron bombardment induced the migration of tritium against the concentration gradient. At the low temperature, the dip showed a gradual growth with fluence and saturation of the growth at the higher fluences, which could not be described by the existing model for isotope mixing. The spectrum of protons from the D(d, p)T reaction obtained in the same measurement suggested that the release of deuterium suddenly started at the final stage of the present bombardment. The dip formed at room temperature was larger than that at the low temperature. The migration of tritium induced by the bombardment is discussed on the basis of the experimental results obtained.     

Depth-profiling of beryllium on graphite with ion beams

The surface layer of beryllium-coated graphite was analysed by backscattering and nuclear reaction methods using a 2.5 MeV accelerator. For the Be analysis the nuclear reactions ⁹Be(p, d)⁸Be, ⁹Be(p, )⁶Li, ⁹Be(d, p)¹⁰Be, ⁹Be(d, t)⁸Be, ⁹Be(d, )⁷Li and ⁹Be(³He, p)¹¹B are compared with backscattering of ⁴He⁺ and protons. For the analysis of carbon, which provides complementary information to the depth profiling of Be, and for the analysis of oxygen, which is the third element of importance in the system, elastic backscattering of ⁴He⁺ and protons is applied. It turns out that the backscattering analysis with protons of 1.3 MeV presents the best compromise for a quick and straightforward measurement of all three elements. The other methods have their merits for a more detailed analysis.     

The aging of zirconium tritides: A transmission electron microscopy study

Young Zr tritides were investigated for aging times up to about 6 months' using analytical transmission electron microscopy. No isotopic differences between hydrides and tritides were seen as far as precipitation morphology and structures are concerned. Also, no low-temperature phase transitions were observed in the tritides γ and δ. ³He generated by tritium decay was found to precipitate in very small bubbles (1–2 nm in diameter and densities of about 5×10²³ m⁻³) which were first clearly visible after approximately 24 days of aging. In addition to the ³He bubbles, interstitial loop damage was observed. Acoustic emission techniques applied to 5 and 6 months old Zr-T samples did not reveal any above background acoustic activity.     

氚衰变对氚化钛结构影响的XRD分析

氚自然衰变生成3He,3He的聚集会引起贮氚材料物理和化学性质的明显变化。本文以氚化钛为研究对象,运用XRD研究其晶体结构在贮存初期的演化规律,对氦在氚化钛贮存初期的时效行为进行了研究。结果表明:氚化钛特征峰的宽化是由氚衰变生成的3He累积所引起,氚化钛晶体结构保持fcc结构不变。     

Investigations of lattice location and mobility of carbon in GaAs using the channeling technique

In order to get information about the lattice location and the mobility of ¹²C in GaAs wafers, the channeling technique in combination with nuclear reaction analysis (NRA) is a powerful method. The targets were implanted with ¹²C ions (2.6 × 10¹³−2.6 × 10¹⁵cm⁻²) at energies between 60 and 3000 keV. This corresponds to implantation depths of about 0.1 to 3 μm. Using the nuclear reaction ¹²C(d, p)¹³C a depth distribution of the implanted carbon is obtained. The relationship between the concentration of ¹⁴C in random and along the 100 and 110 axial directions gives information about the substitutional lattice location of carbon within the GaAs crystal. In addition, we measured lattice defect depth distributions with a 1.5 MeV ⁴He⁺ beam before and after thermal annealing at temperatures up to 600°C.     

Sputtering yield and residual vacuum influence during titanium implantation into iron

Ti implantation into iron-based alloys is known to improve tribological properties (low friction and wear) by formation of an amorphous Fe-Ti-C surface layer due to the interaction of the carbonaceous molecules in the residual vacuum with the surface during implantation. To state precisely the conditions of this amorphous-layer formation, thin evaporated iron targets were implanted with 110 keV Ti ions at room temperature with fluences ranging from 6 × 10¹⁶ to 3 × 10¹⁷ Ti/cm² and at different residual pressures. Samples were analysed using backscattering spectrometry with 5.7 MeV ⁴He ions to obtain titanium profiles and to follow the evolution of sputtering yield versus fluence and residual vacuum pressure, and also for determining the amount of carbon and oxygen incorporated on the Ti-implanted surface as a function of fluence and pressure. Theoretical calculations of sputtering and high-fluence Ti distributions were performed and compared to experimental data. The importance of the reactions that occur between the implanted surface and the residual gases in the vacuum during implantation (C and O competition) is discussed.     

D+注入Li4SiO4的表面化学状态及其热解吸行为

锂陶瓷氚增殖剂的氢同位素行为是聚变堆固态产氚包层关心的重要课题。本文将3 keV D⁺注入Li₄SiO₄,采用X射线光电子能谱在线分析注氘前后材料表面的化学状态,同时采用热解吸谱（TDS）实验技术,研究注氘后Li₄SiO₄中氢同位素的热解吸行为。实验结果表明：D⁺注入会改变Li₄SiO₄表面的化学环境,产生多种辐照缺陷和化学键合状态;氘滞留量和热解行为受注氘时样品的温度影响较大,可在一定程度上预测产氚包层中氚的滞留行为。     

脉冲离子束作用下金属氚化物氦释放测量技术研究

为认识脉冲离子束作用下金属氚化物的氦释放行为,建立了脉冲离子束作用下金属氚化物氦释放测量系统。利用标准体积气体取样装置,采用气体反扩散法,对系统的容积比、灵敏度进行了实验标定。在此基础上,发展了脉冲离子束作用下金属氚化物氦释放的测量技术,开展了脉冲离子束作用下金属氚化物氦释放实验研究。结果显示,单次脉冲离子束作用下金属氚化物的氦释放呈脉冲式,释放量最大可达10~(13)个原子以上。     

Ion implantation doping and electrical conductivity enhancement of C60 films

Pristine C₆₀ films sublimed onto sheet mica were implanted with 20 keV K⁺ ions and I⁺ ions at doses of 1.0 × 10¹⁶/cm², 3.0 × 10¹⁶/cm² and 5.0 × 10¹⁶/cm², and with 20 keV Ar⁺ ions at a dose of 5.0 × 10¹⁶/cm². The distributions of dopants were studied using Rutherford backscattering spectrometry (RBS). The temperature dependence of sheet resistivity of the films was investigated applying a four-probe system. It was proposed that the conductivity enhancement of K⁺ implanted C₆₀ films was due to the implanted ions in the films, while for I⁺ implanted C₆₀ films, both implanted I⁺ ions and irradiation effects of the ions contributed to the enhancement of conductivity.     

Effects of ion implantation on poly(dimethylsilylene-co-methylphenylsilylene)

The effects of ion implantation on the electrical and structural properties of poly(dimethylsilylene-co-methylphenylsilylene), (DMMPS) thin films have been investigated. Ionic species of krypton, arsenic, fluorine, chlorine, and sulfur were implanted at energies ranging from 35 to 200 keV and with doses of up to 1 × 10¹⁶ ion cm². The conductivity of the polymer increased upon implantation reaching a maximum value of 9.6 × 10⁻⁶ (Ω cm)⁻¹ for the case of arsenic ion at a dose of 1 × 10¹⁶ ion cm² and energy of 100 keV. The results showed that ion implantation induced conduction in DMMPS was primarily due to structural modifications of the material brought about by the, energetic ions. Infrared analysis and Auger electron spectroscopy showed evidence for the formation of a silicon carbide-like structure upon implantation.     

氖中微量组分气相色谱测量分析方法与验证

为测量聚变堆固态氚增殖剂堆内辐照氚增殖剂的产氚速率，除用常规电离室之外，本研究建立了Ne载气的高精度气相色谱在线检测分析方法，通过测量产氚回路中的氦产生量，验证系统中产生的氚量，从而为聚变堆固态包层产氚包层增殖剂材料辐照产氚性能提供一种新的产氚速率测量验证方法。本工作通过研制含有三个检测器、五个色谱柱的气相色谱分析系统，建立了Ne中微量⁴He、H₂及杂质组分的色谱检测分析方法，并完成了实时在线检测的验证实验。结果表明，研发的色谱分析系统可实现高纯Ne中4He、H₂及杂质组分的检测分析，H₂、⁴He检测限可分别达到1.0×10^-6、5.9×10^-6，各组分含量及峰面积的相对标准偏差(sr)均小于5.0%(n=6)，线性相关系数(r²)均大于0.99，说明检测方法重复性好。根据Ne中多组分气体的在线检测验证实验可知，单时段和多时段内的测量重复性均较好，可为辐照产氚考核系统中的产氚速率验证提供分析手段，进而为正式入堆得到辐照数据和氚衡算提供技术支持。     

Nonlinearity of pulse height of recoil helium in 3Heproportional counters

The pulse height distribution in ³He proportional counters has been investigated to accurately quantify the response function to be used in fast neutron spectroscopy. The measurements were performed as a function of the operating voltage, the counting gas mixture, and the incident neutron energy. The special emphasis of this study has been put on the nonlinearity of the pulse height of a recoil helium induced by the ³He(n,n)³He reaction. A distinct deviation of 14% at maximum to lower energies was found in the position of the recoil edge with the energy axis calibrated by the full energy peaks of the ³He(n,p)T reaction produced with neutrons of thermal energy and 2.413 MeV. It was confirmed that the nonlinear effects, such as an initial recombination and a space-charge effect, take place more significantly in the energy loss process of a recoil helium because of its higher linear energy transfer (LET) in the filling gas compared to that of a proton and triton pair emitted from the ³ He(n,p)T reaction. The deviation becomes larger with an increase of the average LET in the gas mixture. The experimental results suggested that the nonlinear effect caused by a higher LET recoil helium is inevitable for the filling gas, even if the operating voltage is changed to an acceptable range     

Effect of forming gas anneals on the photoluminescence from nanocrystalline silicon formed by Si implantation into SiO2 matrix

The blue region of the room temperature photoluminescence spectrum from Si nanocrystallites formed in SiO₂ by Si⁺ ion implantation has been observed for the first time after annealing in a forming gas (10% H₂ + 90% N₂) ambient. Thermally grown SiO₂ on Si substrates were implanted with a dose of 2 × 10¹⁷ Si⁺ cm⁻² at energies of 200 keV and 400 keV. For reference purposes, quartz silica was implanted also with the same dose of 200 keV Si⁺ ions. The implanted samples were annealed in nitrogen and forming gas at 900°C for 3 to 180 min. Both the SiO₂ and quartz samples exhibited luminescence at about 380 nm which was weak, but detectable, before annealing. During extended anneals in forming gas, the intensity increased by a factor of about 2 above that recorded after a nitrogen anneal but the peak position was unchanged. The intensity was greater in samples annealed in forming gas which is due to the additional hydrogen. It would seem that this blue luminescence originates from new luminescent centres in the matrix caused by the Si⁺ ion implantation.     

PdY合金管束的氢渗透性能

PdY合金膜因其具有良好的透氢性能与机械性能,有望应用于聚变堆氢同位素纯化工艺。基于PdY合金膜的服役参数及氚安全要求,有必要研究在低氢压下PdY合金膜的氢同位素渗透特性,为后续设计氢同位素纯化组件提供数据支撑。本工作基于直管外压式PdY扩散器,研究了低氢压(<50 kPa)、工作温度为350～450℃条件下,厚度为80μm的PdY合金薄膜管的氢渗透速率与膜两侧压力、工作温度的关系。结果表明,低氢压下,PdY合金膜的氢渗透规律符合■,且压力指数n等于0.9,渗透速率控制机制主要表现为表面过程控速;提高工作温度使得合金膜的渗透通量增大,且温度对扩散过程的影响更大,使渗透过程更加趋于表面控速。此外,计算了该工作温度范围下的渗透系数,并通过阿伦尼乌斯公式推导求得渗透活化能约为24.54 kJ/mol,渗透常数Φ₀为5.86×10^-6 mol/(m·s·kPa^0.9)。低氢压下,该厚度膜的渗透系数可由5.86×10^-6e~(-24.54/(RT)) mol/(m·s·kPa^0.9...     

Characterization of silicon oxynitride films using ion beam analysis techniques

Heavy-ion elastic recoil detection analysis (HIERDA) is the ideal technique for quantitative analysis of silicon oxynitride films on silicon because of its unique ability to measure simultaneously all elements of interest (i.e., H, C, N, O and Si), thereby permitting key parameters such as the O/N-ratio to be determined in a single measurement. However, high-energy accelerators suitable for such HIERDA measurements are becoming much less readily available. Hence, the present paper investigates and calibrates an alternative IBA technique for simultaneous O, N and C analysis – namely, the use of (d,p) and (d,) nuclear reactions. Under optimum analysis conditions (850 keV deuterons and 150° detector angle), the Si background level sets a lower detection limit of 1×10¹⁶ nitrogen atoms/cm² and 3×10¹⁵ oxygen atoms/cm². H analysis is carried out separately, using low-energy ERDA and a 2 MeV ⁴He beam. Absolute cross-sections have been obtained for each of the (d,p) and (d,) groups. Comparison with data in the recent Handbook of Modern Ion Beam Materials Analysis shows reasonable agreement (10–15%) for the (d,p) reactions on oxygen and carbon. However, in the case of nitrogen, the measured cross-section values are 70% larger than the Handbook data. Several silicon oxynitride samples have been analyzed, first at UWO using 850 keV deuterons, and subsequently at ANU using HIERDA and a 200 MeV Au beam. The resulting O/N-ratios agree to within 10%. The relative importance of radiation damage effects is briefly discussed.     

Deuterium implantation in graphite

A study has been made of deuterium ion implantation in polycrystalline graphite over the temperature range 100 K to 450 K. Deuterium depth profiles are obtained using a method based on observing the energy spectra of the tritons and protons from D-D reactions initiated with a 200 keV probing deuteron beam. In marked contrast to the low adsorption for gaseous hydrogen previously reported, graphite is found here to retain large concentrations of implanted deuterium with atomic loadings exceeding unity in the deeper regions of a cold target. The amount of deuterium retained continues to decrease with increasing temperature until at 150°C the retention has fallen to approximately half that at −160°C. No evidence is found for a layer of surface deuterium of the type seen in metals such as copper. Scanning electron micrographs of irradiated areas show no observable surface deformation for doses of up to 2.4 × 10¹⁹ deuterons/cm².     

Analysis of sapphire implanted with different elements using artificial neural networks

Five elements (Ti, Fe, Co, Er and Au) were implanted in sapphire to fluences between 8×10¹³ and 5×10¹⁷ at/cm², and energies between 200 and 800 keV. We used Rutherford backscattering to determine the dose and depth of the implanted elements. The data analysis is performed using an artificial neural network (ANN). Here we report a generalisation of previous works where ANNs were successfully applied for specific implantations such as Er in sapphire and Ge in Si. We have now developed a code that it is able to analyse data from implantations of any element with Z between 18 and 83 into sapphire. Although this problem is considerably more complex than single-system ANNs, the ANN developed produced excellent results when applied to experimental data. We discuss the reliability of the ANN and its applicability to the analysis of large batches of implanted samples.     

The cross section for the K(n,p)Ar reaction between 14.2 and 17.2 MeV

Activation techniques have been used to measure the cross section for the ⁴¹K(n,p)⁴¹Ar reaction between 14.2 and 17.2 MeV. Neutrons were produced by the ³H(d,n)⁴He reaction, and the mixed-power method was used to measure the neutron flux through the ²⁷Al(n,)²⁴Na reaction. The activated samples were counted for the 1294 keV, 1.827 h γ-activity of ⁴¹Ar and the 1369 keV, 15.03 h γ-activity of ²⁴Na using a 16% Ge(Li) detector and a 4096-channel analyzer. The cross sections for the ⁴¹K(n,p)⁴¹Ar reaction using the mixed-power method were found to be 53 ± 3 mbarn at 14.2 ± 0.2 MeV, 47 ± 3 mbarn at 15.2 ± 0.2 MeV, 41 ± 3 mbarn at 16.2 ± 0.2 MeV and 36 ± 4 mbarn at 17.2 ± 0.2 MeV. The associated-particle method was also used for measuring the neutron flux in order to check the mixed-powder result at 14.2 MeV. The average cross section for three associated-particle runs at 14.2 MeV was found to be 50 ± 3 mbarn which, within experimental error, agrees with the mixed-powder value.