惯性约束聚变靶材中间体氘代乙醛的合成与表征

氘代乙醛（ＣＤ３ＣＤＯ）是合成惯性约束聚变（ＩＣＦ）固体靶材料氘代聚苯乙烯（ＤＰＳ）的重要中间体之一。以电石（ＣａＣ２）及重水（Ｄ２Ｏ）为原料,经多步液－固,气－液化学反应,合成氘经达９９．２％,的氘代乙醛,介绍了氘代乙醛的合成工艺及其氘代率的表征方法,并对主要合成工艺参数等进行了探讨。     

低能氘离子束轰击固体靶产生的远程D-D核聚变现象研究

利用强流低能氘离子束轰击由吸氢金属形成的氘自吸收靶，研究固体内Ｄ－Ｄ聚变反应规律。并通过对实验测得的Ｄ－Ｄ聚变伴随粒子能谱，探索Ｄ－Ｄ聚变反应与靶材料结构的相关性。同时，利用氘团簇离子（ｄ＾＋３）氘核（ｄ＾＋）束轰击吸氘固体，研究固体内Ｄ－Ｄ聚变反应的特性。实验中观测到了伴随离子能谱中介于质子峰（３ＭｅＶ）和氚峰（１ＭｅＶ）之间的一个宽峰。结果分析表明，该峰是由固体靶内超出离子射程几倍至十几倍处发     

辛酸-1-13C的合成与分析

将以溴代正庚烷为原料合成的格氏试剂溴化正庚基镁与Ｂａ＾１３ＣＯ３和浓Ｈ２ＳＯ４作用产生的＾１３ＣＯ２进行羧化反应，通过水解，提纯，制得辛酸－１－＾１３Ｃ，产率可达９０％－９３％，用薄层层析对其进行了定性分析，利用ＭＳ、ＩＲ、＾１Ｈ－ＮＭＲ和＾１３Ｃ－ＮＭＲ对其进行了结构分析和测定＾１３Ｃ丰度（８９．５％），并按口服药物的质量要求，用ＩＣＰ－ＡＥＳ和ＡＦＳ方法对有关金属元素进行了定量测定。     

氘在钛中的扩散行为

对以氘化钛形式吸附在金属钛中的氘的扩散行为进行了研究。样品经电子束加温至３４３℃，用＾４Ｈｅ－Ｄ前向反冲方法测量氘化钛分解后氘在钛表面和内部的浓度分布。由扩散方程求得吸附的氘化钛样品中氘的扩散系数和表面复合系数，并与通过向钛中注入氘的方法得到的结果进行了比较。     

流通式氘化铀床室温回收氘的研究

研究了氢气经过流通式氘化铀床,利用气－固相之间的同位素交换反应回收床中的氘。用质谱分析测定交换过程中床内流出气体的各组分（Ｈ２,ＨＤ与Ｄ２）的体积百分含量。此外,还观察了床的入口氢气压力和床的温度对气－固交换反应的影响。结果表明：在优化条件下,从氘化铀床室温回收９８％的氘,而氘的同位素纯度不低于６０％是可能的。     

氘化钛中氘扩散和表面复合行为研究

用核反应分析（ＮＲＡ）、前向反冲分析法（ＥＲＤ）、背散射谱法（ＲＢＳ）等离子束分析方法研究了ＴｉＤｘ／Ｍｏ样品中氘的行为。结果表明，在以化学形式存在的ＴｉＤｘ／Ｍｏ样品中氘均匀分布。在ＴｉＤ１．５／Ｍｏ膜表面存在一层２６ｎｍ的氧化层，氧含量为１．４×１０１７ｃｍ－２。达到氘化钛大量明显分解温度（３４３℃）时，氘在氘化钛中扩散系数为２．３×１０－８ｃｍ２／ｓ，表面复合系数为１．９×１０－２７ｃｍ４／ｓ。扩散系数与温度呈指数关系Ｄ＝Ｄ０ｅ－Ｅ／ｋＴ。随着表面氧含量的增加，氘在氘化钛表面复合系数逐渐减小。在ＴｉＤ１．５／Ｍｏ样品表面镀上一层约８０ｎｍ的铜膜后，复合系数增大。     

氘标色氨酸和氘标川芎哚的合成研究

以色氨酸和氘水及色氨酸和氯化氘两种交换反应合成氘标色氨酸,其产率分别为９５％和９２％．氘标总丰度分别为９６．２％和９８．５％。以色氨酸和氘水反应合成的氘标色氨酸为原料,经环化,氧化脱羧及水解等反应合成氘标川芎哚,产率为１１．６％,氘标总丰度约为９０５,结果表明,合成的氘标川芎哚满足药物代谢研究的需要。     

北京大学6MV串列静电加速器的运行及其应用

北京大学６ＭＶ串列静电加速器上建成４条束流输运线，加速＾１Ｈ，＾１２Ｃ，＾１６Ｏ，＾１９Ｆ，＾３５Ｃｌ，＾７９Ｂｒ等离子，并开展物理实验研究。首次利用Ｄ（＾１２Ｃ，ｐ）＾１３Ｃ核反应建立起高灵敏度的氘分析法；利用共振核反应＾１Ｈ（＾１９Ｆ，αγ）＾１６Ｏ分析材料中氢的深度分布；用重离子背散射分析超导材料ＹＢａ２Ｃｕ３Ｏ７－ｘ；用３５ＭｅＶ＾３５Ｃｌ和４５ＭｅＶ＾７９Ｂｒ的弹性前冲分析不同材料中的轻     

^14C标记农药杀螟松和马拉硫磷的制备

以Ｂａ＾１４ＣＯ３为起始原料制得＾１４ＣＨ３ＯＨ，然后和＾１４ＣＨ３ＯＨ与ＰＳＣｌ３在碱性条件下反应，再加入甲基砂基苯酚，在甲基异丁酮溶剂体系下制得＾１４Ｃ－刹螟松，放化纯度〉９５％，放射性比活度为１８８．７ＢＭｑ／ｍｏｌ，＾１４ＣＨ２ＯＨ与Ｐ２Ｓ５合成的中间体，加顺丁烯酸二乙酯在甲苯溶剂体系中反应制成＾１４Ｃ－马拉硫磷，放化纯度〉９５％，放射性比活度为１５６．４ＭＢｑ／ｍｏｌ。     

氘在Ti-32Mo-5Nb合金中的行为

利用质子增强背散射和Ｘ射线衍射等方法,对氘在β相相的Ｔｉ－３２Ｍｏ－５Ｎｂ合金中的深度分布及Ｔｉ３２－Ｍｏ－５Ｎｂ合金吸氘前后的相结构等进行了分析研究。结果表明：该合金在低温阶段的吸氘速率明显现于纯钛,平均氘钛原子 ２．５,其中一部分氘与合金中的钛生成ＴｉＤ１．９７１,另一部分氘则固溶在Ｔｉ－３２Ｍｏ－５Ｎｂ合金中。     

钛膜表面氧化层对吸氘性能的影响

利用金属氢化物热力学和动力学参数测试系统对表面具有氧化层的钛膜进行了恒温吸氘和变温吸氘实验。结果表明：试样恒温吸氘时。吸氘速率随氧化层厚度的增加而变慢，达到吸氘平衡的时间也变长；试样变温吸氘时，在相同的升温速率和相同的初始氘气压力下，吸氘温度随氧化层厚度的增加而升高，表明钛膜表面氧化层具有一定的阻氘性能。     

超轻水中氘含量的气相色谱分析

通过实验研究建立了测定超轻水中氘含量的气相色谱分析方法。用金属镁在500℃高温下将超轻水分解为气体,然后在常温下以高纯H2为载气,5A分子筛作为色谱柱,进行超轻水中氘含量的检测。用金属镁法分解水样,避免了传统铀法可能带来的放射性危害,且同位素效应远小于金属锌法。采用色谱在常温下检测氢气中氘的含量,也克服了普遍采用液氮低温法操作复杂,且H2、HD和D2的校正因子难以测定的缺点。研究结果表明,以极低重水标准样绘制的HD峰面积与对应氘含量的标准曲线能反向延长到天然丰度以下,能用于不同氘含量的超轻水样品检测。该分析方法精密度高,同一样品经多次分解进样,检测的相对标准偏差5%,在3个添加水平下的回收率为96.6%～99.9%,合成相对不确定度为0.166。测量结果精密度和准确度较高,完全能满足超轻水生产过程中氘含量定量分析的要求。     

钛膜中氘氚浓度的弹性反冲法测量

研究采用弹性反冲探测(ERD)方法测量钛膜中氘、氚的浓度。实验所用Ti膜用磁控溅射法制备，膜厚小于100nm，以石英玻璃（SiO₂）为底衬，Ti膜加镀了1层Ni保护膜，以防Ti膜氧化和增强Ti膜吸氢。以6.0MeVO粒子作为入射粒子，在30°方向上探测反冲粒子，在此实验条件下，O粒子对D、T的碰撞截面为卢瑟福截面。对两个样品用ERD方法测量钛膜中的D、T含量，获得了D、T的面密度。测量结果表明，采用如上方法测量Ti膜中D、T浓度的误差小于7％。     

冷冻靶的环境热辐射屏蔽技术研究

通过建立三维柱腔冷冻靶计算模型,研究了外界环境辐射对间接驱动冷冻靶靶丸及燃料冰层温度场的影响。考虑柱腔内部激光入射孔（LEH）膜透光率对柱腔内靶丸和冰层温度场分布的影响,利用COMSOL软件对柱腔冷冻靶温度场进行了数值模拟计算。研究结果表明：受外界辐射影响,靶丸表面温度场呈两极热、赤道冷分布;LEH膜透光率越大,靶丸外表面温差和冰层内表面温差越大。当LEH膜透光率小于1%时,冰层内表面最大温差低于0.1 mK,可满足冰层均化和保持的要求。实验中,通过在LEH膜上镀不同厚度的铝层调控其透光率,并选择LEH膜镀铝层厚度为35 nm的冷冻靶开展了氘氘冷冻均化实验。结果表明：当LEH膜上的镀铝层厚度为35 nm时,冰层的保持能力得到大幅提升。从X射线相衬图像可知,冰层的厚度均匀性约为80.2%,粗糙度约为1.65 μm,平均厚度约为50.5 μm。     

侧线反馈对H2/HD/D2低温精馏分离的影响

为研究带侧线反馈的低温精馏氢同位素分离规律性,建立了带侧线反馈的低温精馏氢同位素分离计算方法,并以H2/HD/D2体系进行了计算分析.计算结果表明,侧线反馈对分离性能影响显著,再沸器中以D2为主,氘丰度可达到0.90,而无侧线反馈情况下,再沸器中以HD为主,氘丰度不超过0.50;有侧线反馈条件下,系统运行约40 h HD向D2的转化达到峰值,而在无侧线情况下,HD浓缩在40 h已达到饱和;当侧线采出比为1时,脱氘率最高.     

Changes to the reflectance of Be mirrors due to deuterium plasmas contaminated with oxygen

The reflectance of Be mirrors due to impact by ions from a deuterium plasma has been studied under several bombardment conditions. Analysis of the resulting surface films has been performed using various diagnostic techniques, with the conclusion that the primary factor leading to the decrease in reflectance following bombardment with energetic ions is the conversion of the surface oxide layer, composed of BeO, to the hydroxide, Be(OD)₂, with a corresponding increase in the optical extinction coefficient. The increase in the thickness of the layer is also important. Modifications to the surface layer are thought to involve a balance between the ion-induced diffusion of Be atoms to the surface where they may react with incident D and O atoms, and physical and chemical sputtering processes. For incident ion energies less than ∼50 eV, chemical reactions leading to disoxidation of the oxide-hydroxide film dominate, while keV-range ions (primarily D, but with some O impurities) lead to the formation of hydroxide, and an increase in the surface layer thickness.     

Exposure of Equal-Channel Angular Extruded Tungsten to Deuterium Plasma

Surface morphology and deuterium retention in ultrafine-grained tungsten fabricated by equal-channel angular pressing(ECAP) have been examined after exposure to a low energy,high-flux deuterium(D) plasma at fluences of 3×10~(24) D/m~2 and 1×10~(25) D/m~2 in a temperature range of 100 ℃-150 ℃.The methods used were scanning electron microscopy(SEM) and thermal desorption spectroscopy(TDS).Sparse and small blisters(~0.1 μm) were observed by SEM after D plasma irradiation on every irradiated surface;yet they did not exhibit significant structure or plasma fluence dependence.Larger blisters or protrusions appeared after subsequent TDS heating up to 1000 ℃.The TDS results showed a single D desorption peak at ~220℃ for all samples and the D retention increased with increasing numbers of extrusion passes,i.e.,the decrease of grain sizes.The increased D retention in this low temperature range should be attributed to the faster diffusion of D along the larger volume fraction of grain boundaries introduced by ECAP.     

Deuterium Retention and Physical Sputtering of Low Activation Ferritic Steel

Low activation materials have to be developed toward fusion demonstration reactors. Ferritic steel, vanadium alloy and SiC/SiC composite are candidate materials of the first wall, vacuum vessel and blanket components, respectively. Although changes of mechanical-thermal properties owing to neutron irradiation have been investigated so far, there is little data for the plasma material interactions, such as fuel hydrogen retention and erosion. In the present study, deuterium retention and physical sputtering of low activation ferritic steel, F82H, were investigated by using deuterium ion irradiation apparatus. After a ferritic steel sample was irradiated by 1.7 keV D^ ions, the weight loss was measured to obtain the physical sputtering yield. The sputtering yield was 0.04, comparable to that of stainless steel. In order to obtain the retained amount of deuterium, technique of thermal desorption spectroscopy (TDS) was employed to the irradiated sample. The retained deuterium desorbed at temperature ranging from 450 K to 700 K, in the forms of DHO, D2, D2O and hydrocarbons. Hence, the deuterium retained can be reduced by baking with a relatively low temperature. The fiuence dependence of retained amount of deuterium was measured by changing the ion fiuence. In the ferritic steel without mechanical polish, the retained amount was large even when the fluence was low. In such a case, a large amount of deuterium was trapped in the surface oxide layer containing O and C. When the fluence was large, the thickness of surface oxide layer was reduced by the ion sputtering, and then the retained amount in the oxide layer decreased. In the case of a high fluence, the retained amount of deuterium became comparable to that of ferritic steel with mechanical polish or SS 316 L, and one order of magnitude smaller than that of graphite. When the ferritic steel is used, it is required to remove the surface oxide layer for reduction of fuel hydrogen retention. Ferritic steel sample was exposed to the environment of JFT-2M tokamak in JAERI and after that the deuterium retention was examined. The result was roughly the same as the case of deuterium ion irradiation experiment.     

Study on Vibrational Distribution of D2 Molecules in Edge Plasmas

The molecules‘s behavior in edge plasma is very important in understanding the phenomena near plasma-facing materials. In this paper, various processes of deuterium molecules are discussed and most recent data are applied in the evaluation of molecules‘ vibrational excitation. For the excitation of the molecules to triplet states, complete sets of vibrationally-resolved cross sections are not available from the literatures. Semi-classical Gryzinski method is used to calculate these cross sections and rate coefficients. Finally, The vibrational distribution of deuterium molecules is calculated by applying a quasi-steady state model for the balance of the vibrational populations. The dependence on the plasma parameters is discussed.     

A method for thickness determination of thin films of amalgamable metals by total-reflection X-ray fluorescence

A method for thickness determination of thin amalgamable metallic films by total-reflection X-ray fluorescence (TXRF) is presented. The peak’s intensity in TXRF spectra are directly related to the surface density of the sample, i.e. to its thickness in a homogeneous film. Performing a traditional TXRF analysis on a thin film of an amalgamated metal, and determining the relative peak intensity of a specific metal line, the layer thickness can be precisely obtained. In the case of gold thickness determination, mercury and gold peaks overlap, hence we have developed a general data processing scheme to achieve the most precise results.