小角X射线散射法对GH4096高温合金中γ'相的尺寸分布分析

通过物理化学相分析的方式,电解提取了5种冷却速率下生产的GH4096高温合金在高温蠕变前、后的γ'析出相,并制样以后进行小角X射线散射(SAXS)分析,得到了γ'析出相的尺寸分布,辅以扫描电子显微镜(SEM)手段,比较了5种冷却速率对γ'相析出的影响以及经高温蠕变后γ'相所发生的变化。研究结果表明:不同的固溶冷却速率对γ'析出相的尺寸分布存在影响。较慢的冷却速率使得γ'析出相在较小过冷度时长大,而在较大过冷度时又大量析出,各个尺寸段的γ'析出相质量分数分布相对平均,没有含量特别高的某一段。较快的冷却速率,析出的γ'相尺寸相对较小,且尺寸较为接近。绝大部分γ'相都分布在10～96 nm之间。经过高温蠕变以后,不同冷却速率下制备试样的γ'相平均尺寸和尺寸中位数不同程度地变大。经高温蠕变后,γ'析出相的尺寸分布也发生了一些变化。冷却速率相近的3个试样经过高温蠕变过程后,60～96 nm尺寸范围段的γ'析出相质量分数显著大于其他段,而36～60 nm尺寸范围段的γ'析出相显著减少。冷却速率最快和冷却速率最慢的试样经过高温蠕变后,200～300 nm尺寸范围段的γ'析出相质量分数都较大幅度增加,但发生减少的尺寸范围段不一样。SAXS法得到的数据有统计性意义和趋势性,未来结合图像法的定量结果相互印证可以展现更好的γ'相形貌,助力材料研究。     

X射线小角散射法测量纳米粉末的粒度分布

在常规高分辨X射线衍射仪上应用小角散射法测量了ZnO、ZrO2、Fe和Al2O3纳米粉末的粒度分布。测量结果与专用X射线小角散射仪器的测量结果一致，并经TEM分析验证。证明在常规高分辨X射线衍射仪上应用小角散射法测量纳米粉末的粒度是可行的。与采用四狭缝系统或Kratky狭缝系统的专用小角散射仪相比，该方法的特点是操作简单，成本较低，易于推广。目前此法可测量1～300nm范围的粉末粒度。     

X光小角散射,分割分布函数法测定超细粉末的粒度组成

本文基于圆球粒子系散射方程,将粒度范围分割成区间,各区间的粒度分布近似取同一值,积分方程转化为线性方程组。用小角测角仪,在固定角测定散射强度,由方程组求解出1～300nm范围内的粒度组成。还对相干效应和湿度影响等问题作了若干探讨。     

电感耦合等离子体原子发射光谱法测定钢铁及合金中析出相组成成分的研究

通过电感耦合等离子体原子发射光谱法(ICP-AES)测定了钢铁及合金析出相中Fe,Ni,Cr,Co,Mo,V,Ti,Mn,Al,Zr,W,Nb共12种组成成分。对仪器测量条件如功率、雾化器压力、进样量、积分时间进行了优化,对基体效应的影响、分析谱线的光谱干扰及其校正以及析出相的溶解条件进行了研究。通过调整电解量及试液稀释体积,控制试液中各元素的浓度在10 mg/mL以内,同时采用内标法有效地消除了基体干扰;通过选择合适的分析谱线,使各待测元素在测定范围内无明显光谱重叠干扰。主量元素对微痕量元素测定的背景干     

GH903合金中析出物的相分析

本文介绍了Incoloy 903(GH903)合金中析出物的类型和X-射线衍射的标准d值,制定了该合金析出物的提取和定量相分析方法.讨论了该合金的相分析结果.     

HGH104合金中析出相的研究

本文通过对本合金中四种不同热处理状态下的析出相进行了定性和定量分析试验,选择出提取高温合金中析出相的最佳电解制度。     

X-射线荧光光谱法分析中镍基高温合金中16种元素

用PANalytical MagiX Pro顺序型X射线荧光光谱仪,多系列镍基高温合金光谱标准样品拟合成一套校准曲线的方法,测定多种牌号镍基高温合金中的Al,Si,P,Ti,Ce,V,Cr,Mn,Fe,Co,W,Cu,Ta,Zr,Nb,Mo16种元素.采用SuperQ高级定量分析软件提供的数学模型对各元素的谱线干扰及基体效应进行校正,方法具有准确可靠、稳定性好、速度快等优点.     

K4208高温合金中析出相的表征

K4208高温合金中W、Mo含量比较高,通常会形成碳化物和金属间相。为了对K4208高温合金中析出相做定性定量分析,通过实验选择了合适的电解条件:电解液为10g/L氯化锂-40g/L磺基水杨酸-5%(V/V)甘油甲醇溶液,电流密度为0.04~0.06A/cm²,电解温度为0~-5℃。采用电解萃取方法将析出相从合金基体中分离,研究了析出相的分离方法,将碳化物溶解,得到了单独新相。通过X射线衍射(XRD)测定了析出相的点阵常数,用X射线小角散射法测定析出相的粒度分布。采用扫描电镜(SEM)研究了析出相的形貌和元素组成,用电感耦合等离子体原子发射光谱法(ICP-AES)测定了析出相中各元素含量及析出相总量。结果表明:电解条件对析出相的萃取量影响明显,K4208高温合金中有新相、γ′、M₆C和M₁₂C这4种析出相。新相的稳定性比较高,不溶于6%(V/V)H₂SO₄-20%(V/V)H₂O₂溶液和20%(V/V)HCl乙醇溶液,在50%(V/V)H₂SO₄中部分溶解。M₆C和M₁₂C相呈块状,粒径相对较小,混合相的平均粒径为170.7nm;新相呈片状,颗粒粗大,平均粒径为216.6nm。     

K4208高温合金中析出相的表征

K4208高温合金中W、Mo含量比较高,通常会形成碳化物和金属间相。为了对K4208高温合金中析出相做定性定量分析,通过实验选择了合适的电解条件:电解液为10g/L氯化锂-40g/L磺基水杨酸-5%(V/V)甘油甲醇溶液,电流密度为0.04～0.06A/cm²,电解温度为0～-5℃。采用电解萃取方法将析出相从合金基体中分离,研究了析出相的分离方法,将碳化物溶解,得到了单独新相。通过X射线衍射(XRD)测定了析出相的点阵常数,用X射线小角散射法测定析出相的粒度分布。采用扫描电镜(SEM)研究了析出相的形貌和元素组成,用电感耦合等离子体原子发射光谱法(ICP-AES)测定了析出相中各元素含量及析出相总量。结果表明:电解条件对析出相的萃取量影响明显,K4208高温合金中有新相、γ′、M₆C和M₁₂C这4种析出相。新相的稳定性比较高,不溶于6%(V/V)H₂SO₄-20%(V/V)H₂O₂溶液和20%(V/V)HCl乙醇溶液,在50%(V/V...     

新型Ni-Cr-Co基高温合金长期时效后的相分析

采用物理化学相分析技术研究了一种新型Ni Cr Co基高温合金长期时效后的析出相γ′(+η),M23C6,MC和M6C(+μ)的相组成,分析了时效温度和时效时间对析出相含量的影响,并用X射线小角散射(SAXS)分析了γ′(+η)相在不同粒度间隔的质量分布。     

Double structural hardening in an AlLiCuMg alloy studied by anomalous small angle X-ray scattering

The sequence of precipitation at low temperatures (T < 150°C) in industrial AlLiCuMg alloys (2091 family) has been given as the superposition of the occurring in the binary AlLi (α → α + δ′ Al₃Li) and of that occurring in the pseudobinary AlCuMg (α → α + GPB → α + S′). Although the final state has been ascertained by TEM observations, no direct proof of the Guinier Preston Baragaskii (GPB) zones has been given. By small (medium) angle X-ray scattering and a comparison of the binary, ternary and quaternary alloys in the same aging conditions, the existence of GPB zones is proved and the superposition confirmed. Moreover anomalous scattering, by labeling Cu atoms, determines the nature of GPB zones and the sequence of (CuMg) precipitation.     

X-射线荧光光谱法测定中、低合金钢中的12个元素

用X射线荧光光谱仪,测定中,低合金钢中Si,Mn,P,S,Cr,Ni,Cu,V,Ti,Mo,As等12个化学元素.给出了各元素的干扰校正系数和基体效应校正系数.方法准确,灵敏,稳定性好,速度快.     

Determination of dispersoid size distributions in Inconel MA 754 by small-angle X-ray scattering

The dispersoid size frequency distribution and volume fraction of the nickel based oxide dispersion strengthened alloy Inconel MA 754 have been determined using small-angle X-ray scattering (SAXS). Two methods of determining dispersoid size distributions from the SAXS spectra are utilized. One method involves a calculation of log-normal distribution parameters from the integrated intensity, forward scattering and the Porod radius. A second method employs an integral transform of the data to calculate the size distribution. Dispersoid size distributions from the transform method exhibit close agreement with histograms obtained from thin foil transmission electron microscopy. Measurement of dispersoid volume fractions from the integrated intensity, coupled with dispersoid size frequency distributions allow a calculation of the average planar separation distance of the dispersoids. The results for two heats of MA 754 lead to predicted dislocation creep strengths which are in reasonable agreement with short time creep data at 1000 and 1093°C. The effect of the presence of mixed aluminum-yttrium oxides in MA 754 is considered.     

Evaluation of microstructural changes in alloy 713 LC by neutron small angle scattering and analytical electron microscopy

Small angle neutron scattering (SANS) studies in combination with transmission electron microscopy (TEM) were performed on the cast nickel base superalloy Alloy 713 LC and on a Hf-modified version of the same alloy. With the aid of the TEM results the profile of the scattering curves was correlated with the M₂₃C₆ carbide and the γ′ precipitates. A coarsening of the γ′ precipitates with increasing creep deformation to a larger plate-like shape was observed. The small axis of these precipitates averaged over the grains was parallel to the stress axis. The γ′precipitates start to become anisotropic even in the primary stage of creep. In the vicinity of the fracture surface the volume fraction of the cavities and microcracks caused by creep deformation was 10⁻³ to 10⁻² The influence of the cavities was indicated by the smaller anisotropy factor measured near the fracture surface in comparison to the rest of the cylindrical part of the specimen. The variation of the anisotropy factor as determined by the SANS-method may be used to nondestructively measure the accumulated damage in the material. formerly at Oak Ridge National Laboratory, Oak Ridge, TN     

A study of the mechanism of hardness change of Al-Zn-Mg alloy during retrogression reaging treatments by small angle X-ray scattering (SAXS)

In this work, the changes in hardness of Al-Zn-Mg alloy during retrogression and reaging (RRA) treatments were detected and the mechanism of the hardness change was studied by Small Angle X-ray Scattering (SAXS). It was discovered that the hardness changes during RRA treatments are as follows. (1) Hardness decreases at the beginning of retrogression, achieves a minimum value at 90 seconds, and then increases and achieves the second maximum value at 6 minutes, and finally decreases simply. (2) Hardness of the reaged sample is higher than that of the retrogressed sample. The following conclusions were drawn from the experimental results of SAXS. (1) The drop in hardness for short retrogression time is attributed to the decrease of volume fraction of the precipitates and the growth of the particles; the drop in hardness with increasing retrogression time after the second maximum of hardness achieved is attributed to coarsening of the particles. 2. The increase in hardness during reaging is due to the occurrence of new precipitates and the increase of volume fraction of the precipitates.     

中小型热轧等边角钢的开发与工艺改进

利用钢球料生产线，开发中小型号等边角钢，进行工艺改进，投产少、见效快。     

钢中硅系夹杂物粒度的原位统计分布分析

研究了钢中硅系夹杂物的颗粒尺寸测定的原位统计分布新方法。结合定量金相和扫描电镜多种物理分析手段,探讨了原位火花光谱中元素硅的异常光谱信号与硅夹杂物的颗粒数量、尺寸之间的相关性,发现钢中单位面积内尺寸大于3μm的夹杂物颗粒个数对异常火花相对频数影响较大,异常平均强度占总体平均强度的比例也与大于3μm的硅系夹杂物的平均粒径密切相关,由此建立了相应的数学模型来计算钢中较大颗粒硅系夹杂物的数量、平均粒径和最大平均粒径。将方法应用于多种钢样品中硅系夹杂物颗粒的状态分析,所得结果与定量金相分析结果具有良好的对应关系。