直拉单晶硅中洁净区形成后铜沉淀行为的研究

本文研究了直拉单晶硅中形成洁净区后过渡族金属杂质铜的沉淀行为. 样品经过高低高三步常规热处理形成洁净区后, 在不同温度下引入杂质铜, 然后对样品分别进行普通热处理和快速热处理, 通过腐蚀和光学显微镜研究发现, 在700 ℃引入铜杂质后经过普通热处理和快速热处理都不会破坏洁净区, 在900 ℃和1100 ℃引入铜杂质后经过普通热处理不会破坏洁净区, 而经过快速热处理会破坏洁净区. 研究表明, 快速热处理可以使硅片体内产生大量的空位, 空位的外扩散是破坏洁净区的主要原因. 关键词： 直拉单晶硅 铜沉淀 洁净区     

点缺陷对硼掺杂直拉硅单晶p/p~+外延片中铜沉淀的影响

系统研究了点缺陷对晶体硅中氧沉淀生成的影响,及点缺陷和氧沉淀对重掺硼直拉硅单晶p/p⁺外延片中铜沉淀的影响.样品先在不同的气氛下进行1250℃/60 s快速热处理,随后在750℃/8 h+1050℃/16 h常规热处理过程中引入铜沾污.通过腐蚀结合光学显微镜研究发现,以O₂作为保护气氛时,p⁺衬底中的沉淀密度较小,以Ar和N₂作为保护气氛时,重掺硼p⁺衬底中生成了高密度的沉淀,且在上述所有样品的外延层中均无缺陷生成.研究认为,以O₂作为保护气时引入的自间隙硅原子（Si_I）可以抑制沉淀的形成,而以Ar和N₂作为保护气氛时引入的空位则会促进沉淀的生成,这是导致此差异的主要原因.另外,研究还发现,p/p⁺外延结构能很好地吸除硅片中的铜杂质,从而保持了外延层的洁净.     

ICP-AES测定基体沉淀分离后的硫酸铜中10种微量元素

研究了应用硫氰酸铵与铜离子加热生成硫氰酸亚铜沉淀而分离出铜基体,用ICP-AES同时测定硫酸铜样品中As、Cd、Co、Cr、Fe、Mg、Mn、Ni、Pb、Zn的方法.该方法检出限为0.001-0.11μg/mL,加标回收率为88.6%-100.9%,RSD小于2%.本方法快速简便,应用于硫酸铜的测定,结果令人满意.     

多晶硅中的氧碳行为及其对太阳电池转换效率的影响

认识及控制多晶硅中杂质行为对于实现低成本、高效率多晶硅太阳电池有着重要的意义.利用红外光谱技术研究了定向凝固多晶硅锭中不同部位材料热处理前后的氧浓度、碳浓度变化,结合少子寿命、光电转换效率、内量子效率等电池性能,探索不同含量的氧、碳杂质对电池性能影响的物理机制.提出一种考虑碳影响的氧沉淀生长模型,并模拟了热处理后氧沉淀的尺寸分布和数量.研究发现,碳除了使利用硅锭顶部材料制备得到的电池转换效率降低外,还是决定氧沉淀作用的重要因素.由于碳含量多造成中部材料氧沉淀的尺寸大、数量多,引起缺陷,增加复合,而碳在底部 关键词： 氧 碳 太阳电池 转换效率     

单晶硅片中的位错在快速热处理过程中的滑移

研究了单晶硅片中维氏压痕诱生的位错在不同气氛下高温快速热处理中的滑移行为.研究表明: 在快速热处理时, 位错在压痕残余应力的弛豫过程中能发生快速滑移; 当快速热处理温度高于1100℃时, 在氮气氛下处理的硅片比在氩气氛下处理的硅片有更小的位错滑移距离. 我们认为这是由于氮气氛下的高温快速热处理在压痕处注入的氮原子钉扎了位错, 增加了位错的临界滑移应力, 从而在相当程度上抑制了位错的滑移. 可以推断氮气氛下的高温快速热处理注入的氮原子增强了硅片的机械强度. 关键词： 快速热处理 位错滑移 机械性能 单晶硅     

绿黄色磷灰石热处理紫外可见光谱研究

绿蓝色磷灰石因其颜色和"帕拉伊巴"绿蓝色碧玺相似而为消费者所熟知。为了验证此种磷灰石颜色是否经过人工处理,将不同颜色的磷灰石样品分别置于空气气氛下进行400~800℃的热处理。结果表明绿黄色磷灰石经过650℃的热处理就可产生绿蓝色。根据热处理过程中样品的X射线粉末衍射数据,在热处理过程中并未发生相变。为了进一步研究热处理过程中样品颜色的变化行为和实验参数对热处理效果的影响,将绿黄色磷灰石样品分别置于空气和还原气氛下进行300~800℃的对比热处理实验。结果显示不同气氛下样品颜色的变化行为十分相似。因此这也表明绿黄色磷灰石颜色的改变和元素价态的变化没有直接关联。室温下样品的紫外可见吸收光谱(200~800 nm)主要表现在蓝紫区强烈吸收,红橙区有一宽缓的吸收带(620~720 nm),黄绿区透过,出现了515, 528, 578, 739和747 nm等一系列吸收峰。随着热处理温度的升高,样品在可见光范围内的吸收系数大幅降低颜色变浅,吸收截止边逐渐蓝移导致样品逐渐呈现蓝色。与此同时,随着温度升高至400℃, 620~720 nm吸收带中最强吸收峰位置会发生蓝移导致样品的黄色调减弱。当温度达到800℃时,样品褪色, 620~720 nm吸收带消失,但515, 528, 578, 739和747 nm等一系列吸收峰仍然存在。因此绿黄色磷灰石在热处理过程中颜色的变化主要和吸收截止边以及620~720 nm吸收带的变化有关。     

银对氧化亚铜电学性质的影响

为了阐明杂质对半导体一系列物理性质影响的机构,必须研究杂质在半导体材料中的扩散过程。在本工作中进行了银对氧化亚铜电学性质影响的研究。银是在10^-4mmHg的真空中、600—1000℃温度范围内各不同温度下用扩散方法引入氧化亚铜中去的。我们测量了所有样品的电导温度由线(温度从20—-150℃)。结果表明:在600℃和800℃之下引入氧化亚铜中去的银引起新的局部能级,相应的激活能是0.45—0.48eV。对於在1000℃之下进行银扩散所得氧化亚铜样品却没有观察到新的能级,激活能仍是原来不含银的情况下的0.30eV。测量霍尔系数的结果表明,上述具有不同激活能的样品均为空穴型。上述实验结果可以解释为在600℃及800℃进入氧化亚铜的银转变成为AgO,在氧化亚铜内形成一受主杂质(AgO)^-(即产生0.45—0.48eV能级的杂质)。而在1000℃进入氧化亚铜样品的银将占据铜的空格点,即转变为Ag₂O;这对氧化亚铜的电学性质不会起什么影响,因此观察到的仍是原来氧的能级。     

高温热处理a面AlN表面形貌演变机理

非极性a面AlN(a-AlN)能够从根本上解决极性AlN引起的量子限制斯塔克效应问题,是提升AlGaN发光器件效率的有效途径。但是,非极性AlN生长面临更大的挑战,目前难以实现低缺陷密度、高平整表面的非极性a-AlN。高温热处理是一种提高AlN质量的有效方法,但在热处理过程中,非极性a-AlN的表面形貌演变的物理机理尚不明确,直接影响了a-AlN表面改善与质量提升。本研究通过对a-AlN薄膜在不同条件下进行高温热处理,对样品的表面形貌演变过程进行了表征与分析,并结合第一性原理计算,揭示了高温热处理对非极性a-AlN表面的影响及其物理机理。结果表明,在高温热处理过程中Al、N原子更趋向于从a面与m面分解,而在c面吸附,使得a-AlN样品表面在高温热处理过程中出现了沿c轴方向的高取向性条纹原子台阶形貌,进而提高a-AlN材料质量。本研究为实现高质量非极性a-AlN材料及紫外发光器件提供了重要基础。     

直拉硅单晶中原生氧沉淀的透射电镜研究

利用透射电镜对掺氮(NCZ) 和普通 (CZ) 直拉硅单晶中的原生氧沉淀进行研究. 研究表明，在NCZ样品中，有高密度的粒径为5nm的氧沉淀生成，而在CZ样品中，没有观察到这种氧沉淀. 初步认为，这种细小的氧沉淀是以650℃低温下形成的N-O复合体为核心在随后的冷却过程中形成. 关键词： 直拉硅 透射电镜 氧沉淀     

钼丝中含氧和氮所引起的内耗峰

一、引言 如所周知,钼中含有微量的杂质(氧、氮和碳)就会大大地降低它的韧性。Olds和Rengstorff曾经系统地研究了氧、氮和碳对铸钼的韧性的影响,结果指出:极少量的氧就会使铸钼变脆,例如1—2×10~(-6)的氧含量(重量比)对室温的韧性已有一定的影响,氮虽然并不象氧那样有害,但它比碳严重一些。关于微量杂质使钼变脆的原因虽然还未有确切的了解,但是一般认为:杂质的沉淀是使钼变脆的主导原因。杂质的沉淀又往往与热处理有密切的联系,因为热处理基本上就是一种控制原子扩散速率的过程。     

Structure,impurity composition,and photoluminescence of mechanically polished layers of single-crystal silicon

The introduction of optically active defects (such as atomic clusters, dislocations, precipitates) into a silicon single crystal using irradiation, plastic deformation, or heat treatment has been considered a possible approach to the design of silicon-based light-emitting structures in the near infrared region. Defects were introduced into silicon plates by traditional mechanical polishing. The changes in the defect structure and the impurity composition of damaged silicon layers during thermal annealing (TA) of a crystal were examined using transmission electronic microscopy and x-ray fluorescence. Optical properties of the defects were studied at 77 K using photoluminescence (PL) in the near infrared region. It has been shown that the defects generated by mechanical polishing transform into dislocations and dislocation loops and that SiO₂ precipitates also form as a result of annealing at temperatures of 850 to 1000°C. Depending on the annealing temperature, either oxide precipitates or dislocations decorated by copper atoms, which are gettered from the crystal bulk, make the predominant contribution to PL spectra.     

Out-diffusion and precipitation of copper in silicon: An electrostatic model

Concentrations of mobile interstitial copper and precipitated copper in silicon were studied after a high temperature intentional contamination and quench to room temperature. It was found that below a critical contamination the copper predominantly diffuses out to the surface, while for higher initial copper concentrations it mainly precipitates in the bulk. The critical copper contamination equals the acceptor concentration plus 10(16) cm (-3). This behavior can be explained by the electrostatic interaction between the positively charged interstitial copper and the forming copper precipitates.     

Pulsed nanosecond annealing of magnesium-implanted silicon

Single-crystalline silicon is implanted by magnesium ions at room temperature and then subjected to pulsed ion-beam annealing. The surface morphology, crystallinity, and optical properties of the implanted silicon are studied before and after annealing. It is shown that ion implantation makes a near-surface layer of silicon about 0.1 m thick amorphous. Pulsed nanosecond ion-beam annealing results in silicon recrystallization and the formation of crystalline magnesium silicide precipitates. Optimal values of the implantation dose and pulse energy density for the formation of magnesium silicide precipitates in the near-surface layer of silicon are found.     

Influence of annealing on the concentration profiles of boron implantations in silicon

The influence of annealing on the concentration profiles of boron implanted into silicon with does of 10¹⁴ ions/cm² up to 10¹⁶ ions/cm² and an energy of 70 keV was studied. The concentration profiles were measured with Secondary Ion Mass Spectrometry (SIMS). The broadening of the concentration profiles during annealing can be described as a superposition of effects resulting from a relatively immobile and a mobile boron fraction. The properties of the immobile boron fraction were studied by measuring the influence of a boron implantation on the distribution of a homogeneous boron background dope. From these experiments it was concluded that the immobile boron fraction consists of boron precipitates. The properties of the mobile fraction were studied from concentration profiles that were obtained after annealing during different periods at the same temperature. It was found that during the initial stage of the annealing process a fast broadening of the profile occurs; this was assumed to be due to an interstitial type boron diffusion. After prolonged annealing the much slower substitutional type diffusion prevails, due to trapping of the interstitial boron atoms by vacancies. The reliability of the SIMS method, as applied to profile measurements, was checked for the high boron doses used in this investigation. Excessive boron precipitates, obtained after annealing of a high dose, such as 10¹⁶ ions/cm² at about 1000°C, appear to give some increase of the ion yield.     

Effect of nitriding time on secondary recrystallization behaviors and magnetic properties of grain-oriented electrical steel

The effect on secondary recrystallization behaviors and magnetic properties of grain-oriented electrical steel of nitriding time from 0 to 240 s in the acquired-inhibitor method has been studied. It was found that the volume fraction of nitride precipitates increased with increasing nitriding time. However, the average diameter of the nitride precipitates decreased with increasing nitriding time. Two kinds of nitride precipitates were found to have formed after primary recrystallization annealing. A fine rod-shaped precipitate was found to be Si₃N₄ and and a coarse, lozenge-shaped precipitate was MnSiN₂. Moreover, primary grain size decreased with increasing nitriding time due to retarding of the grain growth by precipitates. After secondary recrystallization annealing, the specimen that was nitrided for 30 s obtained the largest volume fraction of abnormal growth grains and largest area percentage of Goss grains. Conversely, specimens that were nitrided more or less than 30 s demonstrated poor secondary recrystallization and obtained low area percentage of Goss grains. Furthermore, the optimum nitriding time to obtain the best magnetic properties was 30 s. In addition, the optimum nitrogen content was 150 ppm.     

Microstructure evolution of zircaloy-4 during Ne ion irradiation and annealing: An in situ TEM investigation

The microstructural evolution of zircaloy-4 was studied, including the amorphization and recrystallization of Zr（Fe, Cr）2 precipitates, and the density of dislocations under in situ Ne ion irradiation and post annealing. The results show that irradiation at a relatively high temperature and dose induces the formation of nanocrystals in pre-amorphized Zr（Fe, Cr）2 precipitates. The recrystallized nanocrystals also have the structure of hcp-Zr（Fe, Cr）2. The formation of the nanocrystals is thought to be the consequence of competition between atomistic disordering and the recrystallization of precipitates under ion irradiation. The free energy of the nanocrystal is lower than that of the amorphous state, which is another reason for the recrystallization of the precipitates. With increased annealing temperature, the density of the nanocrystals is increased. The dislocation density sharply decreases with the increase in the annealing temperature, and its size increases.     

Study of precipitation in NaCl:Pb2+ by light scattering and ultramicroscopy

The formation and dissolution behaviour of precipitates in NaCl : Pb²⁺ single crystals is studied by light scattering and ultramicroscopy. Measurements of Rayleigh ratio together with ultramicroscopic observations during isochronal annealing indicate the presence of two types of precipitates in as-grown crystals. Isochronal annealing after suitable thermal and thermomechanical treatments shows that precipitates of first type (I) which form and dissolve at lower temperatures, are due to homogeneous nucleation. Precipitates of the second category (II) which form and dissolve at higher temperatures are aligned along crystallographic directions and have their origin in stress-assisted processes. Isothermal annealing has been used to study the dissolution kinetics of the precipitated fraction, and it is found that the kinetics is of first order. The enthalpy of solution is determined from a study of the temperature dependence of the kinetic rate constant, in conjunction with available information on the migration energy of Pb²⁺ in NaCl. The enthalpy so deduced is in good agreement with the value as usually obtained from the concentration dependence of the dissolution temperature.     

Precipitation in solution-treated aluminium–4 wt% copper under cyclic strain

Solution-treated Al–4 wt% Cu was strain-cycled at ambient temperature and above, and the precipitation and deformation behaviours investigated by TEM. Anomalously rapid growth of precipitates appears to have been facilitated by a vacancy super-saturation generated by cyclic strain and the presence of continually refreshed dislocation density to provide heterogeneous nucleation sites. Crystallographic texture appears to be responsible for latent hardening in specimens tested at room temperature. Increasing temperatures lead to a gradual hardening throughout life due to precipitation. Specimens machined at 45° from the rolling direction, which exhibit rapid precipitation hardening, show greater texture hardening due to increased axial stress required to cut precipitates in specimens. In the temperature range 100–200°C, precipitation of Θ″ is suppressed by cyclic strain, and precipitation of Θ′ promoted. The rapid growth of precipitates generated by cyclic strain operates with diminishing effect at higher temperatures due to faster recovery of non-equilibrium vacancy concentrations. Θ′ precipitates generated under cyclic strain are smaller and more finely dispersed than those produced via quench-ageing due to heterogeneous nucleation on dislocations and possess a low aspect ratio and rounded edges of the broad faces caused by the introduction of ledges into the growing precipitates by dislocation cutting. Frequency effects indicate that dislocation action is responsible for the observed reduction in aspect ratio. Accelerated formation of grain-boundary precipitates appears partially responsible for rapid inter-granular fatigue failure at elevated temperatures, resulting in coexistent fatigue striations and ductile dimples on the fracture surface.     

氢气区熔硅单晶氢致缺陷的研究

本文应用X射线透射截面形貌技术研究了氢气区熔硅单晶中氢致缺陷与热处理温度的关系。根据早期氢致缺陷的X射线形貌图衍衬分析,指出氢沉淀周围晶格受到压缩性应变,并简单阐述了硅氢键断裂与氢致缺陷形成过程。 关键词：