Crystallization behaviour of Fe−(Nb,Cu)−Si−B metallic glasses

The crystallization behaviour and Curie temperatures of Fe?(Nb,Cu)?Si?B metallic glasses were studied by means of differential scanning calorimetry (DSC), thermomagnetic gravimetry (TMG) and X-ray diffraction. The agreement between the DSC and TMG results was complete. For all Fe?Si?B amorphous alloys, two-peak crystallization was observed with the primary crystallization of α-Fe(Si) followed by eutectic crystallisation. The effects of Cu and Nb additions on the crystallization behaviour and on the activation energies for each stage of the crystallization process of Fe?Si?B glass were investigated.     

Fe基非晶和纳米晶合金晶化及电化学腐蚀行为

应用单辊甩带法制备非晶态Fe78Si13B9和Fe73.5Si13.5B9Nb3Cu1薄带,并以非晶晶化退火法制备出纳米晶Fe73.5Si13.5B9Nb3Cu1薄带.利用X射线衍射(XRD)仪和示差扫描量热计(DSC)对该非晶薄带的非晶特性及其晶化过程进行了研究.并用电化学极化曲线的方法和电化学阻抗技术研究了非晶态Fe78Si13B9和纳米晶Fe73.5Si13.5B9Nb3Cu1合金在1mol/LNaOH溶液里的电化学腐蚀行为,用SEM对极化测试后的试样形貌进行了观察;同时还研究了不同的热处理温度对材料结构及在1mol/LNaOH溶液里耐腐蚀性能的影响.结果表明,该非晶薄带的晶化过程分为两步;纳米晶比非晶合金的耐腐蚀性要好;且随着热处理温度的升高,非晶和纳米晶的耐腐蚀性能都得到提高.     

Thermal induced structural and magnetic transformations in Fe73.5−xCex=0,3,5,7Si13.5B9Nb3Cu1 amorphous alloy

Structural and magnetic properties of amorphous and partly crystallized Fe_73.5?xCe_x=0,3,5,7Si_13.5B₉Nb₃Cu₁ alloys, were analysed in the temperature ranging from RT to 800 °C with scanning calorimetry and magnetometry. The Fe(Si) and Fe(B) structures were identified and characterised with set of crystallization temperatures and activation energies. Also, Curie temperatures for amorphous and for crystalline structures were determined and analysed as functions of Ce content.     

纳米掺铁二氧化钛的sol-gel法制备与表征(Ⅰ)热重红外联用分析掺铁二氧化钛凝胶的热分解和晶化特性

本文通过热分析、红外联用和Ｘ射线衍射分析了不同煅烧温度下的纳米掺铁二氧化钛样品,研究了ｓｏｌ－ｇｅｌ方法制备的纯二氧化钛和掺铁二氧化钛干凝胶的热分解和晶化过程,结果表明,干凝胶有较为明显的两个阶段的热分解。在实验上得到的二氧化钛干凝胶粉为无定形,无定形二氧化钛加热晶化过程是一个持续的过程,没有明显的晶化温度。     

Thermodynamic analysis and purifying an amorphous phase of frozen crystallization centers

The possibility of dissolving frozen crystallization centers in amorphous alloys of the Fe–B system is considered by means of thermodynamic calculations. This can in turn improve the thermal stability of an amorphous alloy. The effect isothermal annealing has on the thermal stability of multicomponent amorphous alloys based on iron is investigated via the highly sensitive dilatometric technique, measurements of microsolidity, and electron microscopic investigations. The annealing temperature is determined empirically on the basis of the theses of the thermodynamic theory of the high temperature stability of multicomponent amorphous alloys, according to which there exists a range of temperatures that is characterized by a negative difference between the chemical potentials of phases in a heterogeneous amorphous matrix–frozen crystallization centers system. The thermodynamic condition of the possible dissolution of frozen crystallization centers is thus met. It is shown that introducing regimes of thermal processing allows us to expand the ranges of the thermal stability of iron-based amorphous alloys by 20–40 K through purifying an amorphous matrix of frozen crystallization centers. This conclusion is proved via electron microscopic investigations.     

超声波合成磁性4A沸石分子筛

为了解决微细粉末状沸石产品应用中与所处理溶液难以分离的问题, 在传统水热合成法合成4A沸石的晶化原料液中, 加入磁性Fe3O4微粒, 经过70 ℃, 功率为100 W的超声波晶化6 h, 合成了一系列Fe3O4含量不同的磁性4A沸石,并对其进行了XRD、SEM、IR、TG/DTA、EDX、磁化率及吸附性能等表征测试. 结果表明, 磁性4A沸石具有良好的磁稳定性, 其磁化率随Fe3O4含量的增加而增大; 磁性4A沸石对水中氟离子和六价铬的吸附与纯4A沸石性能相同, 其吸附速率可以用拟二级动力学方程来描述.     

Experimental study of Fe–C–O based system above 1,000 °C

The paper deals with the study of phase transformation temperatures of the model Fe–C–O based metallic alloys in the high temperature region (above 1,000 °C). Six model alloys with graded carbon and oxygen content were prepared and studied. Temperatures of phase transitions were obtained using DTA method (differential thermal analysis). The Setaram SETSYS 18? (TG/DTA/DSC/TMA) modular experimental system was used for measurements. Influence of composition change (carbon and oxygen content) on shift of phase transformation temperatures is investigated in this paper. New original data (phase transformation temperatures) were obtained in this study. Controlled heating of the alloys was conducted at the rates of 2, 4, 7, 10, 15 and 20 °C min^?1. Comparison of the obtained experimental data with the data presented in the literature was also carried out. It follows from comparison of the obtained results with the data accessible in the literature that a lack of experimental data exists, and these available data significantly differ.     

化学镀镍-高磷合金晶化行为的现场XRD研究

从柠檬酸-酒石酸-乳酸-EDTA混合体系中得到含P 12％(质量比)的化学镀高磷Ni-P合金，其差热曲线显示，在350和420 ℃出现两个放热过程.现场XRD分析结果显示，镀层在300 ℃以下保持非晶态结构，在320 ℃之后开始晶化，首先析出介稳的Ni5P2和Ni12P5相，在360 ℃后开始有稳定的Ni3P和Ni相的衍射峰出现， 400 ℃以上只有Ni3P和Ni相. 325 ℃恒温时，镀层在4 min内保持非晶态的衍射特征，随即析出Ni5P2和Ni12P5相, 并在2 h内基本保持不变. 350 ℃恒温时，析出的Ni5P2和Ni12P5介稳相只存在40 min.实验结果表明, DTA曲线上350 ℃的放热峰不仅有非晶相转变为介稳相的过程，也包含部分介稳相转化为稳定相的过程.     

Thermal analysis and longtime stability of amorphous Co100−xBx alloys

Crystallization behaviour of amorphous Co_100?xB_x alloys (17 <x ≤ 40) has been investigated by differential thermal analysis (DTA) and dynamic temperature X-ray diffraction (DTXD) methods in the freshly prepared state and at a period of about eight years after preparation. The crystallization temperatures lie in the range 670 K–760 K. An average decrease of about 1.25 K/year over a period of eight years has been observed to take place in the crystallization temperatures of these materials. The value of heat of crystallization (ΔH _cr) and activation energy lie in the range 2.3 kJ/g-at – 5.9 kJ/g-at and 2.1 eV – 2.4 eV, respectively. The phases obtained at crystallization temperatures during DTXD analysis have been discussed.     

The effect of Nb and Ni addition on crystallization behavior of amorphous–nanocrystalline Fe–Cr–B–Si alloys

The crystallization behavior of amorphous Fe–Cr–B–Si alloys in the presence of Ni and Nb elements was the goal of this study. In this regard, four different amorphous–nanocrystalline Fe₄₀Cr₂₀Si₁₅B₁₅M₁₀ (M=Fe, Nb, Ni, Ni_0.5Nb_0.5) alloys were prepared using mechanical alloying technique up to 20 h. Based on the achieved results, in contrast to Fe₅₀Cr₂₀Si₁₅B₁₅ alloy, the amorphous phase can be successfully prepared in the presence of Ni and Nb in composition. Although the crystallization mechanism of prepared amorphous phase in different alloys was the same, the Fe₄₀Cr₂₀Si₁₅B₁₅Nb₁₀ alloy showed higher thermal stability in comparison with other samples. The crystallization activation energy of this amorphous alloy was estimated about 410 kJ mol^?1 which was much higher than Fe₄₀Cr₂₀Si₁₅B₁₅Ni₁₀ (195.5 kJ mol^?1) and Fe₄₀Cr₂₀Si₁₅B₁₅Ni₅Nb₅ (360 kJ mol^?1) samples. The calculated values of Avrami exponent (1.5 < n < 2.2) indicated that the crystallization process in different alloying systems is the same and to be governed by a three-dimensional diffusion-controlled growth.     

Ni-P非晶合金催化剂的制备、结构和性能

超细非晶态合金ＭＰ或ＭＢ(Ｍ=Ｎｉ,Ｃｏ,Ｆｅ)的高比表面和结构不规整性使其表现出催化加氢的高活性和选择性,有可能成为新型石油化工加氢催化剂[1-3].其制备主要有物理和化学两类方法[3-5].从提高催化活性角度,化学还原法是最为优越的方法.ＮｉＢ催化活性明显高于ＮｉＰ...     

Crystallization of Co75-xFexGe15B10 amorphous alloys

The crystallization behavior of Co_75-xFe_xGe₁₅B₁₀ (x=3.0, 4.6 and 6.0) amorphous alloys was monitored by differential thermal analysis and thermo-mechanical analysis. The crystallization process of the melt spun ribbons was interrupted at 450, 525, 650, 800 and 900°C and their microstructures were investigated by X-ray diffractometry. It was observed that the crystallization occurs in a sequential mode attributed to the formation of different types of precipitates. It was shown that the crystallization products change as a function of Fe content. After full crystallization, GeFe, Co₃B, FeGe₂ and Co₂Ge compounds were found as well as a Co rich solid solution. This revised version was published online in August 2006 with corrections to the Cover Date.     

Thermal decomposition of PTFE in the presence of silicon,calcium silicide,ferrosilicon and iron

Simultaneous TG/DTA has been used to study the thermal decomposition of binary compositions containing polytetrafluoroethene (PTFE) with silicon (Si), calcium silicide (CaSi₂), ferrosilicon (FeSi) or iron (Fe) powders. In nitrogen and under dynamic heating program the thermal decomposition of Si/PTFE and CaSi₂/PTFE is an exothermic process. The other two compositions decompose endothermically. In each case the decomposition reactions show first-order kinetics but only iron does not change considerably the kinetics of PTFE depolymerization. The constants of the decomposition rate at 850 K for silicon containing reducers are about four times higher than those of PTFE and Fe/PTFE. This revised version was published online in July 2006 with corrections to the Cover Date.     

Formation and Crystallization of Fe(III) Hydroxides. Influence of precipitation temperature and the nature of the starting Fe(III) salt on Fe(III) hydroxide crystallization in alkaline medium

It is shown that amorphous precipitates of Fe(III) hydroxides are composed of two phases, namely weakly magnetic primary particles and ferrimagnetic fine-grained particles. The relative proportion of the two phases, the type of phase transitions and the rate of amorphous precipitate crystallization during the ageing process are determined by the precipitation temperature. The crystallization of Fe(III) hydroxides during the ageing in mother liquors occurs by the “oriented growth” mechanism.     

Combination of electrochemical hydrogenation and Mössbauer spectroscopy as a tool to show the radiation effect of energetic heavy ions in Fe–Zr amorphous alloys

Radiation effects of energetic heavy ion irradiation in Fe–Zr amorphous alloys were investigated by the help of Mössbauer spectroscopy, X-ray diffraction and electrolytical hydrogenation. The electrolytical hydrogenation of non-irradiated and irradiated samples was carried out by a unique cathodic potential (−1000 mV versus SHE). The combination of electrolytical hydrogenation and Mössbauer analysis gives a very sensitive method for detecting structural changes of these amorphous alloys. It was found that the structural changes in the amorphous state, which are undetectable without hydrogenation by Mössbauer spectroscopy, modify the localization and the concentration of introduced hydrogen, and are reflected in a significant change of magnetic hyperfine interaction. The results can be associated with structural changes due to the effect of energetic heavy ion irradiation.     

Determination of boron in amorphous and nanostructured soft magnetic alloys,ribbons and layered materials by ICP atomic emission spectrometry

Optimum conditions for the accurate determination of B in amorphous or nanocrystalline soft magnetic Fe and Co base alloys (ribbons), boride coated powders and other materials by ICP atomic emission spectrometry are worked out. The spectral interferences of the 3 most prominent B emission lines caused by the matrix elements Fe, Co and Ni and the enhancement of the B blank values by a memory effect are investigated. Using a well-suited line fitted to the sample matrix and a special measuring regime including frequent recalibrations by an external standard, the total error of the analytical method could be reduced to 0.02% at B contents of 1 to 5% (w/w).     

Determination of boron in amorphous and nanostructured soft magnetic alloys, ribbons and layered materials by ICP atomic emission spectrometry

Optimum conditions for the accurate determination of B in amorphous or nanocrystalline soft magnetic Fe and Co base alloys (ribbons), boride coated powders and other materials by ICP atomic emission spectrometry are worked out. The spectral interferences of the 3 most prominent B emission lines caused by the matrix elements Fe, Co and Ni and the enhancement of the B blank values by a memory effect are investigated. Using a well-suited line fitted to the sample matrix and a special measuring regime including frequent recalibrations by an external standard, the total error of the analytical method could be reduced to 0.02% at B contents of 1 to 5% (w/w).     

Application of TMA and DTA for study of the crystallization behaviour of SiO2 in the thermal transformation of kaolinite

TMA/DTMA with DTA studies on the thermal changes of kaolinite were performed with special emphasis on the crystallization behaviour of amorphous SiO₂. The results of four different physical techniques (semiquantitative XRD, DTA, TMA and DTMA) were clearly in good agreement with the fact that the 1420°C exotherm in DTA is due to silica crystallization.Thanks to Dr. B. K. Sarkor, Director of the Institute for his kind permission to publish the paper and to Mr. D. K. Ahosh for his needful suggestions.     

Sol‐Gel‐Process in the Ammono‐System – a Novel Access to Silicon Based Nitrides

Controlled coammonolysis of elementalkylamides in aprotic organic solvents at low temperatures have been shown to result in the formation of polyazanes. The synthetic procedure developed may be addressed as “sol‐gel‐route in the ammono system”. Pyrolysis of these novel polymer precursors gave access to multinary nitrides. For the model systems Si(NHMe)₄/B(NMe₂)₃, Si(NHMe)₄/Ti(NMe₂)₄, and Si(NHMe)₄/Ta(NMe₂)₅ polymeric boro‐, titano and tantalosilazanes were obtained. Pyrolysis in ammonia at 1000 °C yielded amorphous silicon boron nitride, silicon titanium nitride and silicon tantalum nitride powders; further heating of the nitride powders at 1500 °C in nitrogen atmosphere led to the formation of partly crystalline composites of α‐Si₃N₄ and amorphous silicon boron nitride for the Si/B/N system, a composite of finely dispersed TiN and amorphous silicon titanium nitride for the Si/Ti/N system, and crystalline TaN and amorphous silicon nitride for the Si/Ta/N system. Furthermore, the structure and pyrolysis chemistry of the polymeric intermediates, as well as the morphology of the pyrolysis products, were studied by NMR, MAS‐NMR, FT‐IR, DTA‐TG‐MS, XRD, SEM, EDX and elemental analyses.