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 structure

The 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:
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'
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'
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'
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_40day
• • Project 1
  • • data: 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'
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'
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'
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_40day
• • Project 1
  • • data: This folder includes the raw EDX and EBSD data.
    • Project 1.oip: This is the shortcut to use Aztec to open.
  • TiVNbTa_homogenised
  • • Project 1
    • • data: This folder includes the raw EDX and EBSD data.
      • Project 1.oip: This is the shortcut to use Aztec to open.

Methods

• 3D 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.