(Sandia National Laboratories) Multimodal datasets of materials are rich sources of information which can be leveraged for expedited discovery of process-structure-property relationships and for designing materials with specific structures and/or properties. Here, we provide a multimodal dataset of magnetron sputter-deposited molybdenum (Mo) thin films, which are used in a variety of industries including high temperature applications, photovoltaics, and microelectronics. A process space consisting of 27 unique combinations of sputter power and Argon (Ar) deposition pressure was explored. We include an extensive set of eight experimental characterization modalities for each unique power/pressure combination: X-ray diffraction, scanning electron microscopy, residual stress, resistivity, atomic force microscopy, rutherford backscattering, nanoindentation, and transmission electron microscopy with automated crystal orientation mapping data. We also include simulated experiments over an expanded set of powers, pressures and working distances to capture process data in addition to this experimental structure and property data. We acknowledge the Laboratory Directed Research and Development program for providing funding for this study. This work was performed, in part, at the Center for Integrated Nanotechnologies, an Office of Science User Facility operated for the U.S. Department of Energy (DOE) Office of Science.
Sputter deposited Mo thin films: multimodal characterization of residual stress, resistivity, crystallinity, and surface morphology
# Sputter-Deposited Mo Thin Films: Multimodal Characterization of Structure, Surface Morphology, Density, Residual Stress, Electrical Resistivity, and Mechanical Response
—
language:
– en
datacard_version: “1.0”
dataset_id: “OSTI:2311620”
name: “Sputter-Deposited Mo Thin Films (27-condition multimodal characterization dataset)”
tags:
– project:genesis
– type:dataset
– science:materials
– risk:general
– keywords:magnetron-sputter-deposition
– keywords:molybdenum
– keywords:thin-films
– keywords:multimodal
– keywords:xrd
– keywords:sem
– keywords:afm
– keywords:rbs
– keywords:nanoindentation
– keywords:residual-stress
– keywords:resistivity
license: “unknown”
# license_name:
# license_link:
authors:
– name: “Matias Kalaswad”
affiliation: “Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States)”
orcid: “”
– name: “Joyce Olsen Custer”
affiliation: “Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States)”
orcid: “”
– name: “Sadhvikas Jayachandra Addamane”
affiliation: “Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States)”
orcid: “”
– name: “Ryan Muhammad Khan”
affiliation: “Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States)”
orcid: “”
– name: “Luis Jose Jauregui”
affiliation: “Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States)”
orcid: “”
– name: “Tomas Farley Babuska”
affiliation: “Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States)”
orcid: “”
– name: “Amelia A. Henriksen”
affiliation: “Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States)”
orcid: “”
– name: “Frank William DelRio”
affiliation: “Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States)”
orcid: “”
– name: “Remi Philippe Michel Dingreville”
affiliation: “Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States)”
orcid: “”
– name: “B. L. Boyce”
affiliation: “Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States)”
orcid: “”
– name: “David P. Adams”
affiliation: “Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States)”
orcid: “”
sponsor_orgs:
– “USDOE Laboratory Directed Research and Development (LDRD) Program”
– “USDOE National Nuclear Security Administration (NNSA)”
– “USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities (SUF)”
research_orgs:
– “Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States)”
dataset_type: “MD”
description: |
Multimodal experimental dataset for magnetron sputter-deposited molybdenum (Mo) thin films exploring
process–structure–property relationships across a controlled process space.
**Process space**
– Direct-current magnetron sputter power: 100 W, 500 W, 750 W
– Argon deposition pressure: 2, 3, 5, 8, 11, 14, 17, 20, 23 mTorr
– 27 unique power/pressure combinations
– Three nominally identical films per condition (81 films total)
**Included modalities (raw measurements)**
– X-ray diffraction (XRD): five \(\theta\)–\(2\theta\) scans per film (Rigaku Smart Lab II, Cu K\(\alpha\))
– Scanning electron microscopy (SEM): three images per film (0°, 6°, 12° tilt), Thermo Fisher Magellan 400
– Atomic force microscopy (AFM): three 1 \(\mu\)m scans for one film per condition, plus exported height-coordinate ASCII
– Rutherford backscattering spectrometry (RBS): one spectrum for one film per condition (2.0 MeV He, 165° detector)
– Film stress: wafer curvature pre/post deposition and ~two weeks post deposition; stress via Stoney’s equation
– Sheet resistance: six 4-point-probe measurements per wafer; resistivity computed using thickness
– Nanoindentation: 25 load–displacement curves for one film per condition (Hysitron TI980, Berkovich)
**Scale**
– 2072 measurements across scalar, 2D linescan, and 3D imaging modalities
– 1889 additional derived quantities (e.g., hardness, modulus, resistivity, density, RMS roughness)
**Limitations / notes**
– AFM, RBS, and nanoindentation were collected for one film per unique process condition (not all 3 replicates).
– Some SEM images may include small drift (reported \(\le\)100 nm) and operator-set brightness.
– Oxygen contamination was noted for two 100 W films at high pressure (20 and 23 mTorr) based on SIMNRA fits; Ar not detected to within experimental limits (suggested <1 at.%).
issue_date: "2023-04-24"
report_number: "SAND–2023-05488J"
contact_name: "David P. Adams"
contact_email: "dpadams@sandia.gov"
# Data Access Information
access_url: "https://www.osti.gov/servlets/purl/2311620"
repository: "OSTI"
repository_url: "https://www.osti.gov/biblio/2311620"
file_format: "CSV, RAS, TIF, TXT"
data_size: "unknown"
# Security Classification and Sensitivity
classification: "U"
marking: "UUR"
distribution_statement: "Approved for public release; distribution is unlimited."
export_control: "none"
sensitivity_level: "public"
—
## Overview
This dataset accompanies the journal article:
Kalaswad, M. et al., “Sputter-Deposited Mo Thin Films: Multimodal Characterization of Structure, Surface Morphology, Density, Residual Stress, Electrical Resistivity, and Mechanical Response,” *Integrating Materials and Manufacturing Innovation*, 12(2) (2023). DOI: 10.1007/s40192-023-00297-4.
Mo thin films were deposited by DC magnetron sputtering on oxidized Si(100) substrates in a controlled matrix of power and argon pressure conditions and characterized using multiple complementary measurement modalities.
## Data Structure
### File Organization
The article describes summary CSV files plus per-film folders organized by deposition condition and film. A representative structure is:
dataset/ ├── deposition_process_parameters.csv ├── sheet_resistance_resistivity_thickness.csv ├── film_stress_measurements.csv ├── films/ │ ├── P{power}_mTorr{pressure}/ │ │ ├── film_1/ │ │ │ ├── xrd/.ras │ │ │ ├── sem/.tif │ │ │ ├── afm/.tif # one film per condition │ │ │ ├── afm/heights/.txt # one film per condition │ │ │ ├── rbs/.txt # one film per condition │ │ │ └── nanoindent/.txt # one film per condition (25 curves) │ │ ├── film_2/ │ │ └── film_3/
### Data Format
– **Primary formats**: CSV, TXT, RAS, TIF
– **Instances**: Mo thin film samples deposited under a specific (power, Ar pressure) condition, with replicated films (3 per condition)
– **Counts**: 81 films; 27 conditions; repeated measurements per film for several modalities (e.g., 5 XRD scans per film)
## Variables
| Variable Name | Type | Unit | Description | Range/Values |
|—|—:|—|—|—|
| sputter_power | categorical/int | W | DC magnetron sputter power setpoint | 100, 500, 750 |
| ar_pressure | categorical/float | mTorr | Argon working pressure setpoint | 2, 3, 5, 8, 11, 14, 17, 20, 23 |
| film_thickness | float | nm | Profilometer step-height thickness (ride-along sample) | ~188–275 (examples in paper) |
| xrd_intensity | array | a.u. | Diffractogram intensity vs \(2\theta\) | \(2\theta\) range ~60° (per paper) |
| sem_image | image | — | SEM micrographs of surface morphology | HFW 1.5 µm |
| afm_height_map | image/array | nm | AFM topographic height map + exported ASCII \(z\) | 1 µm scans, 512×512 px |
| rbs_spectrum | array | counts | Backscattering yield vs energy/channel | He 2.0 MeV |
| biaxial_stress | float | MPa | Film stress from wafer curvature (Stoney) | compressive to tensile (~1.3 GPa shown) |
| sheet_resistance | float | \(\Omega/\square\) | 4-point probe sheet resistance | varies with condition |
| resistivity | float | \(\Omega\cdot\)cm | Derived: sheet resistance × thickness | varies with condition |
| indentation_load_displacement | array | \(\mu\)N vs nm | Nanoindentation load–displacement curves | max load 600–1000 µN |
| hardness | float | (as-reported) | Derived via Oliver–Pharr | varies with condition |
| reduced_modulus | float | (as-reported) | Derived via Oliver–Pharr | varies with condition |
| rms_roughness | float | nm | AFM-derived RMS roughness | ~0.25–4 nm (reported) |
| density | float | atoms/cm\(^3\) | Derived from SIMNRA areal density / thickness | up to ~bulk Mo (reported) |
## Usage Guidelines
### Access and Citation
– **Paper DOI**: 10.1007/s40192-023-00297-4
– **OSTI landing page**: https://www.osti.gov/biblio/2311620
– **Referenced MDF dataset DOI**: 10.18126/IO99-LDJ2
### Licensing Terms
License is **unknown** from the provided documents. Confirm license terms at the authoritative repository record(s) before reuse/redistribution.
## Provenance
– **Version**: 1.0 (as described in the article)
– **Release Date**: 2023-04-24
– **Change Log**: Not provided
## Datasheet for Dataset
### Motivation
– **Purpose**: Support multimodal analysis of Mo thin film process–structure–property relationships and enable materials informatics/ML studies.
– **Creators**: Sandia National Laboratories authors listed above.
– **Funding**: DOE LDRD; DOE Office of Science User Facility (CINT); NNSA contract DE-NA0003525.
### Composition
– **Instances**: Individual Mo thin films on oxidized Si(100) substrates, with multiple measurement modalities.
– **Instance Count**: 81 films (3 replicates × 27 conditions).
– **Missing Data**: AFM/RBS/nanoindentation only for one film per condition.
– **Confidentiality**: Public-release marking (UUR); no PII described.
### Collection Process
– **Acquisition**: XRD, SEM, AFM, RBS, wafer curvature stress, 4-point probe electrical measurements, nanoindentation.
– **Sampling**: Full grid of (power, pressure) with replicate depositions per grid point.
– **Timeframe**: Not specified.
– **Ethical Review**: Not applicable / not stated.
### Preprocessing/Cleaning/Labeling
– AFM plane-fit/flatten; RMS roughness computed from central subregions.
– RBS modeled with SIMNRA; density derived from areal density and thickness.
– Stress computed via Stoney’s equation.
– Resistivity computed from sheet resistance and thickness.
– Hardness/modulus computed via Oliver–Pharr.
### Uses
– **Prior Uses**: Published as a data descriptor article in 2023.
– **Intended Uses**: Cross-modal correlation, ML feature extraction, model validation, reference dataset.
– **Unsuitable Uses**: Analyses requiring all modalities for all three replicates without additional data collection.
### Distribution
– **Distribution Method**: Public access via OSTI (and referenced MDF DOI in the paper).
– **Distribution Date**: 2023-04-24
– **License**: unknown
– **Restrictions**: None stated
### Maintenance
– **Maintainer**: Not specified; corresponding author contact provided.
– **Contact**: dpadams@sandia.gov
– **Updates**: Not stated.
## Related Resources
– OSTI record: https://www.osti.gov/biblio/2311620
– Paper DOI: https://doi.org/10.1007/s40192-023-00297-4
– MDF DOI (cited): https://doi.org/10.18126/IO99-LDJ2
## Contact Information
– **Name**: David P. Adams
– **Email**: dpadams@sandia.gov
– **Organization**: Sandia National Laboratories
## Compliance
### OSTI Requirements
– [x] Public OSTI record exists (OSTI:2311620)
– [ ] E-Link 2 metadata compliance not evaluated here
– [ ] Export control review status not provided here
– [ ] Data management plan not provided here
