Research data for: Origin of age softening in the refractory high-entropy alloys

This dataset contains the raw data used in the study on the "Origin of Age Softening in Refractory High-Entropy Alloys". It includes the 3D FIB/SEM dataset, nanoindentation datasets, Correlative SEM/EDX/EBSD dataset, APT dataset, STEM-EDX datasets, STEM-EELS dataset, and the TKD dataset.Description of the data and file structureThe raw data were collected using a series of advanced microscopy techniques and a nanoindenter from Ti-V-Nb-Ta high-entropy alloys. Details on the materials and the data acquisition parameters can be found in the paper "Origin of Age Softening in Refractory High-Entropy Alloys" by J. Liu et al. in Science Advances.Datasets include:<br>1. '3D FIB-SEM'Image stack.raw: This is a stack of two-dimensional scanning electron microscopy (SEM) images acquired by serially sectionning using a focused ion beam (FIB). The data can be accessed using commercial software Avizo or the open-source ImageJ software.Voxel size.txt: This file includes the voxel size information for the image stack.2. 'Nanoindentation'<br>This folder contains the raw nanoindentation datasets from the four samples studied in the research. NanoSuite was used to extract the values of modulus and hardness.TiVNbTa_Wisc_700C_1day.mss: Nanoindentation data from the TiVNbTa sample after 1-day aging at 700°C.TiVNbTa_Wisc_700C_5days.mss: Nanoindentation data from the TiVNbTa sample after 5 days of aging at 700°C.TiVNbTa_Wisc_700C_40days.mss: Nanoindentation data from the TiVNbTa sample after 40 days of aging at 700°C.TiVNbTa_Wisc_homogenised.mss: Nanoindentation data from the homogenized TiVNbTa sample.3. 'APT'<br>This folder contains the raw atom probe tomography (APT) data used to analyze the chemical composition at atomic resolution from the selected samples in the study. AP Suite was used to analyze and visualize the datasets.#1.HITS: Raw atom probe tomography data from the matrix of the Ti-V-Nb-Ta sample after 1-day aging at 700°C.#2.HITS to #6.HITS: Additional raw atom probe tomography datasets following the same description as #1.HITS.#7.HITS and #8.HITS: Raw atom probe tomography data from the matrix of the Ti-V-Nb-Ta sample after 40-day aging at 700°C.Precipitate.HITS: Raw atom probe tomography data containing a precipitate in the Ti-V-Nb-Ta sample after 40-day aging at 700°C.4. 'STEM-EDX'<br>This folder contains the raw data of the energy-dispersive X-ray (EDX) line scan used for the chemical analysis of the Ti-V-Nb-Ta sample after 40-day aging at 700°C. Aztec version 4.2 was used to interpret and extract the quantification line scan.TiVNbTa_40dayProject 1data: This folder includes the raw EDX data.reports: This folder includes two line scanning data in CSV format.Project 1.oip: This is the shortcut to use Aztec to open.5. 'STEM-EELS'<br>This folder contains the energy electron loss spectroscopy (EELS) data used to analyze the chemical composition and oxidation states of specific elements in the TiVNbTa sample after 40-day aging at 700°C. Digital Micrograph can be used to open and analyze the .dm3 file.Core loss O reconstructed with 3 components.dm3: This is the aligned EELS map.GB precipitate.msa: This is the EELS spectrum extracted from a precipitate at the grain boundary in the EELS map.intragrainular precipitate.msa: This is the EELS spectrum extracted from a precipitate in the metal matrix in the EELS map.matrix.msa: This is the EELS spectrum extracted from the metal matrix in the EELS map.6. 'TKD'<br>This folder contains the on-axis transmission Kikuchi diffraction (TKD) data used to interpret the crystallographic orientation of nanoscale features in the Ti-V-Nb-Ta sample after 40-day aging at 700°C. The .ctf files can be accessed using the Oxford Instruments Channel 5 software or the open-source Matlab codes at https://mtex-toolbox.github.io/.On_axis_5nm_1p5nA.ctf: TKD data from the TiVNbTa sample aged at 700°C for 40 days.7. 'SEM-EDX-EBSD'<br>This folder contains co-located energy-dispersive X-ray (EDX) chemical and electron backscatter diffraction (EBSD) orientation mapping from the selected samples, showing the chemical and crystallographic orientation information. Aztec version 4.2 was used to interpret the data and extract the maps.TiVNbTa_40dayProject 1data: This folder includes the raw EDX and EBSD data.Project 1.oip: This is the shortcut to use Aztec to open.TiVNbTa_homogenisedProject 1data: This folder includes the raw EDX and EBSD data.Project 1.oip: This is the shortcut to use Aztec to open.Methods3D FIB/SEM data were acquired with the Zeiss Crossbeam 540 dual-beam instrument.APT data were obtained using a CAMECA LEAP 5000XR instrument.SEM-EDX-EBSD data were collected using the Oxford Instruments XmaxN 150 EDX detector, and the Oxford Instruments Nordlys Max EBSD detector on a Zeiss Crossbeam 540 dual-beam instrument.STEM-EDX data were obtained with a Jeol JEM-3000F STEM equipped with an Oxford Instruments EDX detector.STEM-EELS data were collected on a Cs-corrected JEOL ARM 200F. .TKD data were acquired using a Zeiss Merlin FEG-SEM system equipped with a Bruker e-flash high-resolution EBSD detector and an OPTIMUSTM TKD head.Nanoindentation data were collected using an Agilent G200 nanoindenter with a Berkovich diamond indenter.

本数据集包含了题为《难熔高熵合金时效软化起源》的研究中所使用的原始实验数据，涵盖三维聚焦离子束/扫描电子显微镜（3D FIB/SEM）数据集、纳米压痕数据集、关联式扫描电子显微镜/能量色散X射线光谱/电子背散射衍射（SEM/EDX/EBSD）数据集、原子探针断层扫描（APT）数据集、扫描透射电子显微镜-能量色散X射线光谱（STEM-EDX）数据集、扫描透射电子显微镜-电子能量损失谱（STEM-EELS）数据集以及透射菊池衍射（TKD）数据集。

**数据与文件结构说明**
本研究的原始数据通过一系列先进显微表征技术及纳米压痕仪，针对Ti-V-Nb-Ta高熵合金采集得到。关于实验材料与数据采集参数的详细信息，请参阅J. Liu等人发表于《Science Advances》的论文《Origin of Age Softening in Refractory High-Entropy Alloys》。

数据集具体包含以下内容：
1. '3D FIB-SEM'
- `Image stack.raw`：通过聚焦离子束（FIB）逐层切割获取的二维扫描电子显微镜（SEM）图像堆叠文件，可通过商用软件Avizo或开源软件ImageJ读取。
- `Voxel size.txt`：包含该图像堆叠的体素尺寸信息。
2. 'Nanoindentation'
该文件夹包含本研究中4个测试样品的原始纳米压痕数据集，使用NanoSuite软件提取模量与硬度数值。
- `TiVNbTa_Wisc_700C_1day.mss`：TiVNbTa样品在700℃时效1天后的纳米压痕数据。
- `TiVNbTa_Wisc_700C_5days.mss`：TiVNbTa样品在700℃时效5天后的纳米压痕数据。
- `TiVNbTa_Wisc_700C_40days.mss`：TiVNbTa样品在700℃时效40天后的纳米压痕数据。
- `TiVNbTa_Wisc_homogenised.mss`：均质化处理后的TiVNbTa样品的纳米压痕数据。
3. 'APT'
该文件夹包含用于原子级分辨率化学组分分析的原始原子探针断层扫描（APT）数据，使用AP Suite软件进行数据分析与可视化。
- `#1.HITS`：Ti-V-Nb-Ta样品在700℃时效1天后基体的原始原子探针断层扫描数据。
- `#2.HITS`至`#6.HITS`：与`#1.HITS`描述一致的额外原始原子探针断层扫描数据集。
- `#7.HITS`与`#8.HITS`：Ti-V-Nb-Ta样品在700℃时效40天后基体的原始原子探针断层扫描数据。
- `Precipitate.HITS`：Ti-V-Nb-Ta样品在700℃时效40天后包含析出相的原始原子探针断层扫描数据。
4. 'STEM-EDX'
该文件夹包含用于分析700℃时效40天后Ti-V-Nb-Ta样品化学组分的原始能量色散X射线光谱（EDX）线扫数据，使用Aztec 4.2版本软件进行数据解析与定量线扫结果提取。
- `TiVNbTa_40dayProject 1data`：包含原始EDX数据的文件夹。
- `reports`：包含两份CSV格式的线扫数据文件夹。
- `Project 1.oip`：用于通过Aztec软件打开的快捷方式。
5. 'STEM-EELS'
该文件夹包含用于分析700℃时效40天后TiVNbTa样品中特定元素化学组分与氧化态的电子能量损失谱（EELS）数据，可使用Digital Micrograph软件打开并分析`.dm3`格式文件。
- `Core loss O reconstructed with 3 components.dm3`：经过对齐处理的EELS面扫数据。
- `GB precipitate.msa`：从EELS面扫数据中晶界析出相提取得到的EELS谱图。
- `intragrainular precipitate.msa`：从EELS面扫数据中晶内析出相提取得到的EELS谱图。
- `matrix.msa`：从EELS面扫数据中金属基体提取得到的EELS谱图。
6. 'TKD'
该文件夹包含用于解析700℃时效40天后Ti-V-Nb-Ta样品中纳米尺度结构晶体取向的轴上透射菊池衍射（TKD）数据，`.ctf`格式文件可通过牛津仪器Channel 5软件或开源Matlab代码（https://mtex-toolbox.github.io/）读取。
- `On_axis_5nm_1p5nA.ctf`：TiVNbTa样品在700℃时效40天后的TKD数据。
7. 'SEM-EDX-EBSD'
该文件夹包含针对选定样品的同步能量色散X射线光谱（EDX）化学表征与电子背散射衍射（EBSD）取向成像数据，可同时呈现化学组分与晶体取向信息，使用Aztec 4.2版本软件进行数据解析与图像提取。
- `TiVNbTa_40dayProject 1data`：包含原始EDX与EBSD数据的文件夹，配套快捷方式为`Project 1.oip`。
- `TiVNbTa_homogenisedProject 1data`：包含均质化处理样品的原始EDX与EBSD数据的文件夹，配套快捷方式为`Project 1.oip`。

**实验方法说明**
- 3D FIB/SEM数据通过Zeiss Crossbeam 540双束仪器采集。
- APT数据通过CAMECA LEAP 5000XR仪器获取。
- SEM-EDX-EBSD数据通过搭载牛津仪器XmaxN 150 EDX探测器与Nordlys Max EBSD探测器的Zeiss Crossbeam 540双束仪器采集。
- STEM-EDX数据通过搭载牛津仪器EDX探测器的Jeol JEM-3000F扫描透射电子显微镜获取。
- STEM-EELS数据在Cs校正型JEOL ARM 200F仪器上采集。
- TKD数据通过搭载Bruker e-flash高分辨率EBSD探测器与OPTIMUSTM TKD探头的Zeiss Merlin FEG-SEM系统采集。
- 纳米压痕数据通过搭载贝氏金刚石压头的Agilent G200纳米压痕仪采集。