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A nanocrystalline fcc phase via devitrification of a Ni36Fe32Ta7Si8B17 amorphous alloy Ni36Fe32Ta7Si8B17非晶合金反硝化制备纳米晶fcc相
Pub Date : 1999-09-01 DOI: 10.1016/S0965-9773(99)00363-3
P Rizzi , M Baricco , G Riontino , L Battezzati

Various multicomponent alloys containing Ni-Fe-Si-B and refractory metals have been rapidly solidifed in order to check their tendency to produce glassy phases and their devitrification behaviour has been studied. Among these a Ni36Fe32Ta7Si8B17 alloy presents primary crystallization with production of fcc nanocrystals embedded in the glassy matrix. The kinetics of the transformation is determined at 530 °C showing that it consists in two steps: fast nucleation and growth of nanocrystals plus homogenization of the remaining matrix with crystal coarsening. Evidence based on TEM observations, XRD patterns and DSC experiments, are reported in favour of a homogeneous mechanism of nucleation. Faceting of nanocrystals is observed for the first time in such transformations and is attributed to a stress effect on the particles.

本文对含Ni-Fe-Si-B和难熔金属的多种多组分合金进行了快速凝固,以检验其产生玻璃相的倾向,并对其反晶化行为进行了研究。其中Ni36Fe32Ta7Si8B17合金呈现一次晶化,并产生嵌套在玻璃基体中的fcc纳米晶。在530℃时测定了相变动力学,表明相变包括两个步骤:纳米晶体的快速成核和生长以及剩余基体的均匀化和晶体粗化。基于TEM、XRD和DSC实验的证据表明,其成核机制是均匀的。在这种转变中首次观察到纳米晶体的面状,并归因于对颗粒的应力效应。
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引用次数: 3
Hysteretic magnetisation curves in the granular Cu100-xCox system Cu100-xCox颗粒体系的磁滞曲线
Pub Date : 1999-09-01 DOI: 10.1016/S0965-9773(99)00364-5
P Allia , M Coisson , P Tiberto , F Vinai

The magnetic hysteresis properties of granular Cu100-xCox alloys (x = 5 to 20) containing nanometric Co particles, prepared under different quenching conditions and submitted to various anneals, have been measured at room temperature. Major loops (vertex field 1 × 104 Oe) and minor loops (vertex field between 1 × 102 and 9 × 103 Oe) were measured by vibrating-sample magnetometry. The features of major loops were analysed in terms of sample composition and structural state; the dependence of remanence and coercivity of minor loops on vertex field has been analysed in detail. A novel graphical representation method, particularly suitable for describing the details of the narrow hysteresis loops observed in granular systems has been proposed and checked.

在室温条件下,测量了不同淬火条件下制备的含纳米Co颗粒Cu100-xCox合金(x = 5 ~ 20)的磁滞特性。用振动样品磁强计测量了大环(顶点场为1 × 104 Oe)和小环(顶点场为1 × 102 ~ 9 × 103 Oe)。从样品组成和结构状态等方面分析了主要环的特征;详细分析了小环的剩余力和矫顽力与顶点场的关系。提出并验证了一种新的图形表示方法,特别适合描述颗粒系统中观察到的窄磁滞回线的细节。
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引用次数: 4
Nitrogen sorption tests, SEM-windowless EDS and XRD analysis of mechanically alloyed nanocrystalline getter materials 机械合金化纳米晶吸气剂材料的氮吸附试验、sem -无窗EDS和XRD分析
Pub Date : 1999-09-01 DOI: 10.1016/S0965-9773(99)00372-4
G. Valdrè , D. Zacchini , R. Berti , A. Costa , A. Alessandrini , P. Zucchetti , U. Valdrè

Gas absorbing materials (getters) find several applications in modern vacuum technology; in particular to maintain required vacuum levels in evacuated and sealed enclosures. The gas absorbing properties of these getters depend on the physico-chemical nature of their surfaces. The aim of this work is to study the absorption properties of commercial Zr-based alloys (non-evaporable getters) after mechanical alloying by means of a high vacuum planetary ball milling equipped with an in-situ compaction facility. The main aim was to refine the grain size and to develop particular defect structures to enhance the getter properties. The results have shown an improvement of the specific pumping speed of the ball milled commercial Zr-Zr(V,Fe)2 alloy with respect to the starting microcrystalline material. In particular, under our experimental conditions, the specific pumping speed vs absorbed gas curve presents a maximum after 2 hours of milling; prolonged milling reduced the pumping speed of the alloyed material. This behaviour is explained in terms of two opposing simultaneous chemical and structural effects.

吸气材料在现代真空技术中有多种应用;特别是在真空和密封外壳中保持所需的真空水平。这些吸附剂的气体吸收性能取决于其表面的物理化学性质。本工作的目的是研究商业zr基合金(不可蒸发吸收剂)在机械合金化后的吸收性能,采用高真空行星球磨配备原位压实设备。主要目的是细化晶粒尺寸和发展特定的缺陷结构,以提高吸气剂的性能。结果表明,球磨后的Zr-Zr(V,Fe)2合金的比抽速相对于初始微晶材料有所提高。特别是在我们的实验条件下,在铣削2小时后,比抽速与吸收气体的曲线达到最大值;长时间铣削降低了合金材料的抽运速度。这种行为可以用同时发生的两种相反的化学和结构效应来解释。
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引用次数: 21
Magnetic behaviour during the first crystallisation stages in Co-B amorphous alloys: a test of the exchange penetration through interfaces Co-B非晶合金第一次结晶阶段的磁性行为:通过界面交换渗透的测试
Pub Date : 1999-09-01 DOI: 10.1016/S0965-9773(99)00367-0
A Hernando , A González , C Ballesteros , A Zern , D Fiorani , F Lucari , F D’Orazio

Two amorphous compositions of the Co-B system, which present quite different magnetic behaviour, have been studied in the as-cast state and after low temperature annealings. The Co80B20 amorphous alloy submitted to thermal treatments undergoes a primary crystallisation which transforms the material into a two phase system composed of nanocrystals of cobalt embedded in a Co-B amorphous matrix. The role of the cobalt grains on the magnetisation processes and the coercive field is analysed for temperature ranging from 77 to 300 K. It is found that the hardening effect of the grains diminishes on increasing the temperature. The large crystalline anisotropy of the Co grains as well as the magnetic state of the grain boundary which transmits the exchange interaction, are mainly responsible for the observed behaviour.

在铸态和低温退火条件下,研究了Co-B体系中两种具有完全不同磁性的非晶态组分。热处理后的Co80B20非晶态合金经历一次晶化,将材料转变为嵌套在Co-B非晶态基体中的钴纳米晶组成的两相体系。在77 ~ 300 K的温度范围内,分析了钴晶粒对磁化过程和矫顽力场的影响。结果表明,随着温度的升高,晶粒的硬化作用减弱。Co晶粒的大的晶体各向异性以及传递交换相互作用的晶界磁态是观察到的行为的主要原因。
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引用次数: 3
Structural, mechanical and magnetic properties of nanostructured FeAl alloys during disordering and thermal recovery 纳米FeAl合金在无序和热恢复过程中的结构、力学和磁性能
Pub Date : 1999-09-01 DOI: 10.1016/S0965-9773(99)00357-8
X. Amils , J. Nogués , S. Suriñach , J.S. Muñoz , L. Lutterotti , S. Gialanella , M.D. Baró

The microstructural, mechanical and magnetic properties of the ball milled and annealed Fe-40Al at% B2 alloys have been studied. The disordering process is characterized by an alloy hardening and a para-ferromagnetic transition, which depend mainly on the grain refinement and the creation of antisite defects. The reordering process shows a continuous softening of the nanocrystalline alloy and the recovery of the paramagnetic state, which is essentially governed by the annihilation of antisite defects. The correlation between the microstructural, mechanical and magnetic properties make magnetic measurements a suitable, non-destructive, tool to study the microstructural and mechanical state of FeAl nanocrystalline alloys.

研究了Fe-40Al球磨和退火后的% B2合金的显微组织、力学性能和磁性能。失序过程的特征是合金硬化和准铁磁转变,这主要取决于晶粒细化和反位缺陷的产生。重排序过程显示出纳米晶合金的持续软化和顺磁状态的恢复,这主要是由反位缺陷的湮灭控制的。显微组织、力学性能和磁性能之间的相关性使磁测量成为研究FeAl纳米晶合金显微组织和力学状态的一种合适的、非破坏性的工具。
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引用次数: 25
Microstructure and magnetic properties of iron-aluminum multilayers 铁铝多层膜的微观结构和磁性能
Pub Date : 1999-09-01 DOI: 10.1016/S0965-9773(99)00366-9
M Carbucicchio , C Grazzi , M Rateo , G Ruggiero , G Turilli

Thin film multilayers, constituted by ten Fe/Al bilayers with Fe thickness in the range 15 ÷ 30 Å and constant Al thickness of 20 Å, have been obtained by electron beam evaporation in ultra high vacuum. Sample characterization was performed using transmission electron microscopy, surface Mössbauer spectroscopy and alternating gradient force magnetometry. For iron thickness ≥ 20 Å the periodicity of multilayers is maintained, while for 15 Å the periodicity is almost completely lost and fine particles showing a superparamagnetic behavior begin to form. In all samples the magnetization is laying in the film plane, and, moreover, it shows an easy and hard direction at 90°. The magnetic behavior is typical of poly-domain systems.

采用超高真空电子束蒸发法制备了10层Fe/Al双层膜,Fe厚度为15 ~ 30 Å, Al厚度为20 ~ Å。采用透射电子显微镜、表面Mössbauer光谱和交变梯度力磁强计对样品进行表征。当铁厚度≥20 Å时,多层膜的周期性保持不变,而当铁厚度≥15 Å时,多层膜的周期性几乎完全丧失,并开始形成具有超顺磁性的细颗粒。在所有样品中,磁化均分布在薄膜平面上,且呈现出90°的易、硬方向。磁性行为是多畴体系的典型特征。
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引用次数: 5
Transmission electron microscopy investigation of SnO2 thin films for sensor devices 传感器用SnO2薄膜的透射电镜研究
Pub Date : 1999-09-01 DOI: 10.1016/S0965-9773(99)00371-2
A.M Serventi , D.G Rickerby , M.C Horrillo , R.G Saint-Jacques , J Gutiérrez

Tin oxide thin films, deposited on alumina or silicon, are commonly employed as sensors of pollutant gases in the atmosphere. The response of these materials in gas sensing applications depends on the microstructural and morphological characteristics of the film, which are dependent on the specific production process and deposition conditions. Sensor sensitivity and selectivity can be improved by doping the oxide layer with small quantities of Pt. Tin oxide films were deposited on polycrystalline alumina substrates by reactive r.f. magnetron sputtering at different values of the substrate temperature during the process. Transmission electron microscopy was employed to investigate the microstructure of the samples, before and after Pt doping. The TEM results are discussed in relation to the behavior of the films in sensing applications.

沉积在氧化铝或硅上的氧化锡薄膜通常用作大气中污染气体的传感器。这些材料在气敏应用中的响应取决于薄膜的微观结构和形态特征,而这些特征又取决于特定的生产工艺和沉积条件。通过在氧化层中掺杂少量的铂,可以提高传感器的灵敏度和选择性。在不同的衬底温度下,通过反应磁控溅射在多晶氧化铝衬底上沉积了氧化锡薄膜。采用透射电镜观察了Pt掺杂前后样品的微观结构。讨论了TEM结果与薄膜在传感应用中的行为的关系。
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引用次数: 12
Metastable phase nucleation in irradiated metallic alloys 辐照金属合金的亚稳相成核
Pub Date : 1999-09-01 DOI: 10.1016/S0965-9773(99)00362-1
Paolo M. Ossi , Rosanna Pastorelli

Phase nucleation in irradiated metallic alloys is studied by the atomistic Segregation-Charge Transfer (SCT) model, taking into account that when bombardment conditions favour the development of dense collision cascades the system explores kinetic and thermodynamic regions conventionally not accessible. Locally non-equilibrium compositional and charge density profiles evolve at the interface between a cascade and the crystalline matrix, driven by the interface enrichment of one of the film constituents. Charge relaxation to (meta)stable equilibrium is simulated by Charge Transfer Reactions (CTR), each involving a couple of dissimilar atoms of the initial alloy. Both the amount of energy needed in a single CTR and the local strain undergone by the target as a consequence of ion formation are calculated. Considering a set of nineteen alloys which are reported to be amorphized and seventeen ones which remain crystalline under ion bombardment, for both structure stability parameters threshold values are found, which allow to separate crystalline from vitrified alloys.

考虑到当轰击条件有利于密集碰撞级联的发展时,系统探索了通常无法进入的动力学和热力学区域,通过原子分离-电荷转移(SCT)模型研究了辐照金属合金中的相成核。局部非平衡的成分和电荷密度分布在级联和晶体基质之间的界面上演化,这是由其中一种薄膜成分的界面富集所驱动的。通过电荷转移反应(CTR)模拟电荷弛豫到(元)稳定平衡,每个反应都涉及一对不同的初始合金原子。计算了单个CTR所需的能量和靶由于离子形成而产生的局部应变。考虑到19种非晶化合金和17种在离子轰击下保持结晶的合金,找到了两种结构稳定性参数的阈值,可以将结晶与玻璃化合金分开。
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引用次数: 2
Study of the phase separation in amorphous silicon oxycarbide glasses under heat treatment 热处理下非晶碳化硅玻璃的相分离研究
Pub Date : 1999-09-01 DOI: 10.1016/S0965-9773(99)00360-8
H. Brequel , J. Parmentier , G.D. Sorar , L. Schiffini , S. Enzo

The structural evolution of three silicon oxycarbide glasses was studied by X-ray diffraction (XRD) as a function of the pyrolysis temperature. Three compositions were prepared by the sol-gel method and pyrolysed at 1000°C under atmosphere of Ar. The black glasses obtained correspond respectively to i) silicon oxycarbide network with excess of C, ii) stoichiometric SiCxO2(1-x) where x = 0.3, and iii) silicon oxycarbide network with deficiency of C, i.e. with excess of Si. At this stage of the treatment, the samples are made up of a single and amorphous phase. A phase separation occurs after further pyrolysis in the high temperature range 1200–1500°C, leading to the formation of nanocrystalline β-SiC and amorphous SiO2. We used a cubic silica structure factor to model the component due to amorphous silica. This enabled us to apply the Rietveld method to all patterns and to obtain a satisfactory fit of the experimental data. From these refinements, the amount of each phase (crystalline or amorphous) can be determined, based on the assumption that the electron density of the model agrees with the actual amorphous phase. A comparison is also made with results from chemical analysis and 29Si Magic Angle Spinning NMR found in the litterature. Concerning the crystalline component β-SiC, its average crystallite size and microstrain were also evaluated. The evolution of the phase separation was then reported versus the pyrolysis temperature and seems to suggest a nucleation-and-growth mechanism.

利用x射线衍射(XRD)研究了三种碳化硅玻璃的结构随热解温度的变化规律。采用溶胶-凝胶法制备了3种组合物,在1000℃氩气下进行热解。得到的黑色玻璃分别对应于i)过量C的碳化硅网络,ii)化学计量SiCxO2(1-x),其中x = 0.3, iii)缺乏C的碳化硅网络,即过量Si。在处理的这个阶段,样品由单一和非晶相组成。在1200 ~ 1500℃高温范围内进一步热解后发生相分离,形成纳米晶β-SiC和无定形SiO2。我们使用立方二氧化硅结构因子来模拟由于无定形二氧化硅而产生的成分。这使我们能够将Rietveld方法应用于所有模式,并获得了令人满意的实验数据拟合。基于模型的电子密度与实际的非晶态相一致的假设,通过这些改进,可以确定每个相(结晶或非晶态)的数量。并与文献中发现的化学分析结果和29Si魔角自旋核磁共振结果进行了比较。对结晶组分β-SiC的平均晶粒尺寸和微应变进行了评价。然后报告了相分离随热解温度的演变,似乎表明了一种成核和生长机制。
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引用次数: 46
Effects of atomic diffusion processes in Co-Cu multilayer granular films Co-Cu多层颗粒膜中原子扩散过程的影响
Pub Date : 1999-09-01 DOI: 10.1016/S0965-9773(99)00365-7
D Bisero , G Bordin , M Minelli , F Ronconi , F Spizzo , A Baraldi , S Lizzit , G Paolucci , L Pareti , G Turilli

Co-Cu multilayer granular films deposited onto SiO2/Si substrates have been submitted to thermal treatments in scanning mode. Their magnetisation, resistance and magnetoresistance have been studied after applying two different heating rates. The analysis of experimental data points out that only with the lower heating rate the properties of the films are strongly modified. In this case, indeed, XPS measurements show the presence of interdiffusion between atomic species of the substrate and metallic species inside the film. XPS data are presented to show the modifications in composition and chemical environment produced by thermal treatments.

将Co-Cu多层颗粒膜沉积在SiO2/Si衬底上,并在扫描模式下进行热处理。采用两种不同的加热速率对其磁化、电阻和磁阻进行了研究。实验数据分析表明,只有在较低的加热速率下,薄膜的性能才会发生明显的变化。在这种情况下,XPS测量确实显示了衬底的原子种类和薄膜内的金属种类之间相互扩散的存在。XPS数据显示了热处理后的成分和化学环境的变化。
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引用次数: 1
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Nanostructured Materials
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