Atom probe tomography study of the decomposition of a bulk metallic glass

The microstructural evolution of a Pd₄₀Ni₄₀P₂₀ bulk metallic glass that was isothermally annealed at 260 °C for 14 h, and then aged at 340 °C for times up to 1280 min has been studied. Differential scanning calorimetry (DSC) curves of the aged samples show an endothermic peak at approximately 370 °C in addition to the ubiquitous glass transition. The endothermic peak appears after 20 min aging and disappears after 320 min aging. The corresponding X-ray diffraction (XRD) data show no Bragg peaks that could indicate the formation of a crystalline phase. Near-atomic-resolution atom probe tomography (APT) was used to study changes in the atomic spatial distributions as a function of aging time. The chemical environment around each of the atomic species, and the tendencies for solute clustering and chemical short range ordering, were determined from statistical analysis of the APT data. Clustering and possible phase separation are identified by APT after only 20 min aging at 340 °C, which correlates with the appearance of the peak in the DSC signal. Crystallization is apparent in the APT and XRD data after aging for 320 min. The study suggests that the amorphous Pd₄₀Ni₄₀P₂₀ annealed at a temperature 40 °C above T_g phase separates into two or more amorphous phases. The endothermic peak in the DSC trace is produced by the dissolution of the phase separation.     

Primary crystallization in Al-rich metallic glasses at unusually low temperatures

The initial stage of the primary crystallization reaction and the glass transition of the marginal metallic glass Al₈₉Y₆Fe₅ were investigated by conventional differential scanning calorimetry (DSC) and modulated differential scanning calorimetry (MDSC), microcalorimetry, X-ray diffraction (XRD) and transmission electron microscopy. A sharp onset of the primary crystallization was found by microcalorimetry and XRD studies at temperatures which were 120 °C below the primary crystallization peak observed in conventional DSC. A systematic MDSC study of annealed samples revealed a wide spectrum of glass transition onsets, which show a strong dependence on the annealing conditions. In addition, the glass transition onsets can be linked to the initial stage of the primary crystallization. The spectrum of glass transition onsets observed is discussed with respect to the occurrence of phase separation preceding the nucleation and growth of dendritic aluminium nanocrystals.     

Preparation, thermal stability, and magnetic properties of Fe---Co---Zr---Mo---W---B bulk metallic glass

A bulk metallic glass (BMG) cylinder of Fe₆₀Co₈Zr₁₀Mo₅W₂B₁₅ with a diameter of 1.5 mm was prepared by copper mould casting of industrial raw materials. The amorphous state and the crystallization behavior were investigated by X-ray diffraction (XRD). The thermal stability parameters, such as glass transition temperature (T_g), crystallization temperature (T_x), supercooled liquid region (ΔT_x) between T_g and T_x, and reduced glass transition temperature T_rg (T_g/T_m) were measured by differential scanning calorimetry (DSC) to be 891, 950, 59 K, and 0.62, respectively. The crystallization process took place through a single stage, and involved crystallization of the phases -Fe, ZrFe₂, Fe₃B, MoB₂, Mo₂FeB₂, and an unknown phase, as determined by X-ray analysis of the sample annealed for 1.5 ks at 1023 K, 50 K above the DSC peak temperature of crystallization. Mössbauer spectroscopy was studied for this alloy. The spectra exhibit a broadened and asymmetric doublet-like structure that indicated paramagnetic behavior and a fully amorphous structure. -Fe was found in the amorphous matrix for a cylinder with a diameter of 2.5 mm. The success of synthesis of the Fe-based bulk metallic glass from industrial materials is important for the future progress in research and practical application of new bulk metallic glasses.     

高强高韧Mg60Cu16Ni10Nd14块体非晶合金的研究

采用铜模铸造法制备了直径为5mm的Mg60Cu16Ni10Nd14块体非晶合金,利用扫描电镜(SEM)、透射电镜(TEM)X射线衍射(XRD)和差示扫描量热仪(DSC)研究了其组织、相结构和热稳定性。结果表明:合金为完全的非晶结构,且出现了相分离;玻璃转变温度Tg、晶化温度Tx分别为431和488K,过冷液相区△Tx为57K,表明该合金具有较大的玻璃形成能力。压缩试验表明:合金的压缩断裂强度为653MPa,断口出现的大量韧窝是合金塑性变形量达到2.5%的主要原因。     

Cu50 Zr42 Al8块体金属玻璃的组织和力学性能

采用悬浮熔炼-铜模吸铸法制备了Cu50Zr42Al8块体金属玻璃,研究了其楔形试样的组织演变.随着熔体凝固过程中冷却速度的变化,楔形试样中存在表面全非晶区,中心晶体区以及二者之间的过渡区域,并确定Cu50Zr42Al8块体金属玻璃临界尺寸为4.8 mm.分别考察了φ4 mm铸态完全非晶棒和φ5 mm非晶复合棒的力学性能.φ4 mm非晶棒的压缩断裂强度,弹性应变和塑性应变分别为2260 MPa,2.0%,0.4%,几乎没有塑性变形.而φ5 mm铸态非晶复合棒的屈服强度、断裂强度分别为1670MPa、1849 MPa,弹性应变和塑性应变分别为1.6%和1.9%.非晶基体中存在的马氏体相CuZr和正交晶相Cu10Zr7的竞争影响了非晶复合棒的最终力学行为.     

Zr43Cu50Al7块体非晶合金的结构弛豫和晶化研究

在不同加热速率下应用差示扫描量热法(DSC)研究了Zr43Cu50Al7块体非晶合金的结构弛豫现象和晶化行为,得到了满意的晶化曲线.由晶化曲线得到弛豫峰与玻璃转变温度(Tg)、晶化起始温度(Tx)和晶化峰温度(Tp).Zr43Cu50Al7非晶合金的过冷液相区ΔTx达76.2 K,具有较强的玻璃形成能力.对所得到的弛豫峰作了初步的研究,并运用Kissinger法和Deloy法分别计算出玻璃转变激活能Eg、晶化起始激活能Ec、晶化峰的激活能Ep和晶化阶段激活能Ex.结果表明Zr43Cu50Al7块体非晶合金具有良好的热稳定性.     

Cu74Ni12—xSnxP14合金的非晶形成趋势

用X射线衍射(XRD)和差动扫描量热(DSC)法研究了Sn对液态淬火Cu_(74)Ni_(12-x)Sn_xP_(14)合金非晶形成能力的影响,并从动力学和结构化学方面进行了分析,结果表明,适量添加Sn可使合金非晶形成能力得到改善,在x=2—6at-％Sn的成分范围内得到完全非晶组织。     

微量添加Fe元素对CuZrAl块体金属玻璃的结构和力学性能的影响(英文)

使用水淬法制备含微量Fe元素的CuZrAl块体金属玻璃。使用X射线衍射(XRD)检测其结构;采用DSC研究Fe元素的添加对块体金属玻璃热稳定性的影响,微量添加Fe元素显著拓宽了过冷液相区。Cu44Zr48Al7Fe块体金属玻璃的塑性应变约为1.5%。使用透射电子显微镜(TEM)观察其微观结构,结果发现,添加1%～2%Fe(摩尔分数)的CuZrAl合金中出现了相分离的富CuZr非晶相。     

过冷液态Zr48Cu36Ag8Al8块体非晶合金的相分离及组织演变

本文通过x射线衍射(XRD)、差示扫描量热法(DSC)和透射电子显微镜(TEM)研究了退火温度对Zr₄₈Cu₃₆Ag₈Al₈金属玻璃微观结构演化的影响。结果表明,快速凝固获得的样品为典型的非晶态结构。当样品在703K保温20分钟时,均一的非晶基体相分离成两种非晶合金,即,发生相分离。由于相分离结构与非晶基体在等温退火过程是竞争的关系,这个结构很容易向晶化态进行转变,形成AlZr₂ AlAg₃相。Zr₄₈Cu₃₆Ag₈Al₈金属玻璃的微观结构在过冷液相区等温退火过程中经历了的局部结构转变,相分离以及纳米晶转变,这个过程意味着Zr₄₈Cu₃₆Ag₈Al₈金属玻璃的微观结构对退火温度十分敏感。此外,相分离的形成可以加速纳米晶的形成。     

Structure relaxation and crystallization of Al83Ni10Ce7 metallic glass

Structure relaxation and crystallization of Al₈₃Ni₁₀Ce₇ metallic glass were studied by different scanning calorimetry (DSC) and X-ray diffraction (XRD). According to the DSC scan, it is interesting to find that the second exothermic peak changes with pre-annealing temperatures (below glass transition temperature), suggesting a change in the amorphous structure upon relaxation. Continuous heating crystallization and isothermal crystallization exhibit different crystallization mechanism of the present alloy. fcc-Al and a metastable phase precipitate simultaneously in the first stage crystallization during continuous heating; however, only a metastable phase precipitates during isothermal annealing below glass transition temperature (T_g).     

Na2O含量对BaO-SrO-Nb2O5-B2O3-SiO2系玻璃陶瓷微结构和性能的影响

采用熔融法制备NaO-BaO-SrO-Nb2Os-B2O3-SiO2玻璃陶瓷.借助DSC、XRD、SEM和电学性能测试研究不同含量的Na2O对其相组成、显微结构、介电性能、体积电阻率及击穿强度的影响.结果表明随着Na2O含量(摩尔分数)的增加,玻璃转变温度(Tg)和第一析晶放热峰(Tg1)温度逐渐降低,而第二析晶放热峰温度(Tg2)呈先降低后升高再降低的变化.经(800℃,3h)+(900℃,3h)热处理后,未添加Na2O的样品析出单相四方钨青铜结构的Ba0.5Sr0.5Nb2O6,而添加5%Na2O(摩尔分数)的样品变为单相Ba0.25Sr0.75Nb2O6.当Na2O为10%时,样品的主晶相仍为Ba0.25Sr0.75Nb2O6,但析出NaSr1.2Ba0.8Nb5O15和Na2Ba2Si2O7相;继续增加Na2O量到15%时,样品的晶相种类不变而衍射峰强度有所增强.样品的介电常数随Na2O含量的增加呈“N”字形变化,样品的体积电阻率和击穿强度随Na2O含量的增加而降低,未添加Na2O试样的击穿强度最大为1500kWcm,其储能密度达3J/cm3.     

非晶态铝合金晶化过程的形核与长大行为研究

制备了一种具有较宽过冷液态温度范围（△T=17K）的非晶态Al85Ni5Y8Co2（原子分数）合金。利用差热分析、电阻测量及高分辨电镜监测了合金化动力学过程。结果表明，在非晶态铝合金的退火过程中纳米Al粒子的形核与长大过程是可分离的，即首先发生淬态Al晶核的长大，之后在过冷液态温区发生高密度纳米Al粒子的形核，最终是Al晶核 的长大过程。     

Formation and crystallization of Zr-Ni-Ti metallic glass

The metallic Zr65 Ni25 Ti10 (mole fraction, ％) glass has been fabricated by a single roller melt-spinning method. The glass forming ability(GFA) and thermal stability of the Zr65 Ni25 Ti10 melt-spun ribbons were investigated by using X-ray diffraction(XRD) and differential scanning calorimetry(DSC) in the mode of continuous heating. It is shown that the reduced glass transition temperature (Trg) is 0. 506 and the supercooled liquid region (△Tx) is 30 K. Two exothermic peaks were observed in the DSC curves of the as-quenched ribbon, which indicates that the crystallization process undergoes two different stages. The phase transformation during the isothermal annealing was investigated by X-ray diffraction(XRD) and transmission electronic microscope(TEM). It is observed that the metastable FCC Zr2 Ni(Fd3m, a= 12.27 A) precipitated while annealing in the suppercooled region(615 K) and the stable BCT Zr2Ni(I4/mcm, a= 6.499 A, c= 5.270 A) precipitated while annealing at higher temperature(673 K or 723 K). The crystallines are on nanoscale, with grain size of 15-30 nm. The reason for the precipitation of the different structural Zr2 Ni from the glassy matrix under different annealing conditions was discussed based on the concept of multi-component chemical short range order(MCSRO).     

The origin of a two-stage endothermic reaction in Zr36Ti24Be40 metallic glass

The origin of a two-stage endothermic reaction in Zr₃₆Ti₂₄Be₄₀ metallic glass was investigated by differential scanning calorimetry (DSC), thermo-mechanical analyzer (TMA) and high resolution transmission electron microscopy (HREM). HREM image of a specimen heated to 420°C under a constant applied tensile stress of 3 MPa showed the formation of medium-range-ordered clusters 1 nm to 2 nm in size. This phenomenon is attributed to strain-induced deformation. This suggests that the formation of clusters may be an appropriate interpretation of the additional endothermic heat in the supercooled liquid region.     

Fe-Si-B非晶条带加热时的晶化过程及对性能的影响

通过使用差热分析（DSC）,X衍射仪（XRD）,物性测量仪（PPMS）和透射电镜（SEM）等设备对进口商用Fe-Si-B非晶条带的结构及性能进行了详细检测和分析。条带晶化过程中没有明显的玻璃转变吸热过程,且会发生二次晶化。随着晶化程度的增加,晶化衍射斑会越来越明显,磁性能基本无变化,但是韧性降低,脆性增加。     

Zr60Al15Ni25大块非晶合金的无序程度对晶化动力学的影响

采用高分辨率电镀观测铸态Zr60Al15Ni25的微观结构。X-射线分析表明,铸态Zr60Al15Ni25合金为非晶态,而通过高分辨电镜发现非晶合金中存在大量的短程有序区。实验发现,非晶合金的无序程度与相对应的母合金铸锭的凝固组织密切相关。通过差示扫描量热法研究非晶合金在线性加热和等温条件下的晶化动力学。结果表明：非晶合金的晶化是预先存在的短程有序区作为晶核长大开始的三维扩散控制的过程。Zr60Al15Ni25块体非晶合金的无序程度对其晶化动力学具有明显的影响,即无序程度越大,非晶合金的晶化越迟缓。     

电脉冲孕育处理对Zr基块体非晶热稳定性及退火晶化的影响

通过先对Zr55Ni5Al10Cu30合金熔体施加脉冲电流处理,再利用非真空吸铸法制备出Zr55Ni5Al10Cu30块体非晶合金的方式,研究了电脉冲孕育处理对非晶热稳定性及退火晶化的影响。差分扫描量热(DSC)及X射线衍射(XRD)分析结果表明:经电脉冲孕育处理后Zr55Ni5Al10Cu30块体非晶合金的玻璃转变温度上升,晶化温度降低,过冷液相区变窄,同时玻璃转变激活能和晶化激活能有所减少。电脉冲孕育处理没有改变Zr55Ni5Al10Cu30块体非晶合金退火晶化相演变过程,但提高了非晶退火晶化率。电脉冲孕育处理对Zr55Ni5Al10Cu30块体非晶合金的晶化起到了促进作用。     

Ni-Based Metallic Glass Composites Containing Cu-Rich Crystalline Nanospheres

In this work, a quaternary Ni–Cu–Nb–Ta system has been designed to obtain composite microstructure with spherical crystalline Cu-rich particles embedded in amorphous Ni-rich matrix. The alloy samples were prepared by using singleroller melting-spinning method. The microstructure and thermal properties of the as-quenched alloy samples were characterized by X-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, and differential scanning calorimetry. It shows that the spherical crystalline Cu-rich particles are embedded in the amorphous Ni-rich matrix. The average size of the Cu-rich particles is strongly dependent upon the Cu content. The effect of the alloy composition on the behavior of liquid–liquid phase separation and microstructure evolution was discussed. The phase formation in the Ni-based metallic glass matrix composite was analyzed.     

氢对锆基块状非晶玻璃转变及晶化动力学的影响

利用非等温差热扫描量热分析方法及Kissinger方程，研究了H原子对Zr-Ti-Cu-Ni-Be块状非晶合金玻璃转变和晶化的激活能影响。结果表明，H能够提高玻璃转变温度和晶化温度，增加玻璃转变和晶化激活能；引起晶化不同阶段热焓减少；并且充入H能降低玻璃转变温度和晶化温度对加热速度的依赖程度。     

Zr-Ti-Cu-Ni-Be大块非晶合金等温晶化过程相分离研究

利用差示扫描量热法(DSC)和透射电镜(TEM)对Zr41.2Ti13.8Cu12.5Ni10Be22.5(at％)大块非晶合金的等温晶化过程和析出相进行了研究。结果表明，大块非晶合金在等温晶化过程中表现出多阶段相析出行为，并且在不同的晶化阶段，析出相也有所不同。在第1个晶化阶段，析出相主要是体心四方(b.c．t)结构的Zr2Cu相；而在晶化的第2个阶段，晶化相主要为简单六方结构的ZrBe2相。从一定程度上证实了Zr41.2Ti13.8Cu12.5Ni10Be22.5大块非晶合金在发生晶化时会形成富Zr区和富Be区，即有相分离的趋势。XRD测试的结果也证实了非晶合金在发生完全晶化时，主要的晶化产物为Zr2Cu和ZrBe2相。