# README — Supplementary Data of the Dissertation "Characterization of Coated Particles from Mechano-Fusion"

## General Remark ##
This dataset is the Supplementary accompanying the cumulative dissertation "Characterization of Coated Particles from Mechano-Fusion". It contains the additional research data referred to in the dissertation (e.g., "see Supplementary"): pristine particle characterization, calculations, an example experimental protocol, atomic force microscopy (AFM) data as well as micro-computed tomography (micro-CT) and nano-CT image data of mechano-fusion (MF) coated particles. The research data of the publications included in the dissertation (Papers A–E) are published separately together with the respective publications.

**Characterization of Coated Particles from Mechano-Fusion**  
*(German: Charakterisierung von beschichteten Partikeln aus dem Mechano-Fusion-Prozess)*

Dissertation to attain the academic degree of Doktor-Ingenieur (Dr.-Ing.), submitted to the Faculty of Mechanical, Process and Energy Engineering, Technische Universität Bergakademie Freiberg.

Author:  
Judith Miriam Seyffer (née Friebel)

Reviewers:  
Prof. Dr.-Ing. Urs Alexander Peuker, TU Bergakademie Freiberg  
Prof. Dr. rer. nat. Alfred Weber, TU Clausthal

Abstract:
*The dry particle coating process of mechano-fusion (MF) is of interest for a variety of applications, ranging from pharmaceuticals to battery materials. In this work, MF was used to produce hetero-aggregate type coated particles. Dense, discrete and homogeneous monolayer coatings were formed for the particle system consisting of spherical alumina host particles and spherical polystyrene guest particles over a wide parameter space of the available MF device. Increasing the processing intensity, mainly by increasing the rotational speed, led to guest particle deformation and even comminution. The hetero-aggregate microstructure was investigated from different perspectives. Correlating a hetero-aggregate microstructural property (specific surface area) with the macroscopic property of flowability revealed distinct structure–property groups, detailing the influence of MF process parameters. Dry laser diffraction provided information beyond the apparent hetero-aggregate particle size, e.g., on the guest particle aggregation and deformation state. Insight into the 3D structure and morphology of the coating, as well as the guest particle connectivity, was gained through micro-computed tomography (micro-CT), by computing, e.g., coating thickness and guest particle distances. Atomic force microscopy allowed for the guest particle-discrete quantification of deformation. The analyses via micro-CT were extended to a model battery particle system, which exhibited continuous coatings. Since the observed hetero-aggregate structures are not specific to MF, the characterization workflows are transferable to other particle systems and dry coating processes.*

Publications included in the dissertation:

- **Paper A:** J. M. Seyffer, N. Stefenelli, L. Ditscherlein & U. A. Peuker (2026). Guest particle deformation and powder flow behavior in mechano-fusion: Linking microscopic structure to macroscopic performance. *Powder Technology*, 469, 121853.
- **Paper B:** J. M. Seyffer, R. Mitra & U. A. Peuker (2026). Particle size analysis and beyond – laser diffraction and derived information regarding structures of mechano-fusion coated particles. *Advanced Powder Technology*, 37(9), 105387.
- **Paper C:** J. M. Friebel, R. Ditscherlein, L. Ditscherlein & U. A. Peuker (2024). Three-Dimensional Characterization of Dry Particle Coating Structures Originating from the Mechano-fusion Process. *Microscopy and Microanalysis*, 30(2), 179–191.
- **Paper D:** P. Gräfensteiner, J. Friebel, L. Ditscherlein, O. Furat, U. A. Peuker & V. Schmidt (2024). An AFM-based approach for quantification of guest particle deformation during mechano-fusion. *Powder Technology*, 434, 119293.
- **Paper E:** P. Rieder, P. Gräfensteiner, J. M. Seyffer, T. Kirstein, N. Brachhold, C. G. Aneziris, V. Schmidt & U. A. Peuker (2026). Analyzing the 3D morphology of particle systems coated by mechano-fusion using micro-CT image data. Under review in *Particuology*.

The work was carried out within the Priority Programme SPP 2289 funded by the Deutsche Forschungsgemeinschaft (DFG).

DOI of this dataset: https://doi.org/10.25532/OPARA-1561  
License: Creative Commons Attribution 4.0 International (CC BY 4.0)

Contact:

Technische Universität Bergakademie Freiberg  
Institute of Mechanical Process Engineering and Mineral Processing  
Agricolastraße 1  
D-09599 Freiberg  
Germany


## Relation of the Data to the Dissertation ##

The following table lists, for each zip archive, the chapters, figures, tables and equations of the dissertation that the data corresponds to. Chapter numbers refer to the numbering in the dissertation (Chapter 7 contains the reprinted Papers A–E, the Appendix is numbered A–D).

| Archive | Content | Chapter | Figures / Tables / Equations |
|---|---|---|---|
| `Experimental-protocol.zip` | Example of the spreadsheet-based protocol of an MF experiment with the Picobond AMS | 2.5.2 Operation of the Picobond | – |
| `Calculations.zip` | Particle–particle interaction (Hamaker constant, Tabor parameter, JKR force, Chen-NJCEP model) and regime map | 2.3.1, 2.3.2, 2.4.4, 4.5.2, Appendix A | Figures 2.7, 2.11, 4.15, A.1; Equations 2.8, 2.10, 2.13, 2.15–2.22, 2.24–2.26 |
| `Particle-systems.zip` | Characterization of the pristine particle systems (BET, bulk density, particle density, PSD, SEM, TGA) and manufacturer data sheets | 3 Particle Systems | Table 3.1 |
| `AFM-data.zip` | AFM topographies for roughness determination and force-distance (FD) spectroscopy for adhesion force determination | 4.5.2, Appendix D.6, D.7 | Figures 4.12, 4.13, 4.14, 4.15, D.7; Table D.1 |
| `micro-CT-data.zip` | Micro-CT image data of the mixed guest particle system (PMMA MH60-FD host, alumina DAW-03 and PS SX-350H guests) | 1, 3, 6 Conclusion and Outlook | Figures 1.1 (middle particle), 6.2 |
| `nano-CT-data.zip` | Nano-CT image data of a coated particle of the scaled down particle system (alumina DAW-05 host, PMMA MP-2801 guests) | 3, 4.4.2 | Figure 4.10 |


## Dataset Overview ##

Most archives contain their own `README.md` file with detailed information on devices, acquisition parameters and data processing.

### Experimental-protocol.zip

`Example-Picobond-Protocol.xlsx` is an example of the comprehensive spreadsheet-based protocol that was filled in for each MF experiment with the Picobond AMS (Hosokawa Alpine AG, Augsburg, Germany). Its data sheets provide the metadata for the digital data archiving (see Chapter 5 Research Data Management).

### Calculations.zip

`Particle-Particle-Interaction.xlsx` contains the determination of the mixed Hamaker constant, the interfacial energy and the Tabor parameter, the JKR adhesion force and the adhesion force according to the Chen-NJCEP model for the main particle system (alumina DAW-45 host, PS SX-350H guest). `Regime-Map.xlsx` contains the combined experimental data (process parameters, energy input, granular Bond number and Stokes deformation number), the calculation of the granular Bond number and the regime map data extracted from the original publication of Khala et al. (2023).

### Particle-systems.zip

Characterization data of the pristine host and guest particles: BET specific surface area (`BET`), bulk density (`Bulk-density`), particle density by gas pycnometry (`Density`), particle size distributions by laser diffraction (`PSD`), SEM images (`SEM`), thermogravimetric analysis (`TGA`) and the manufacturer data sheets (`Data-sheets`). The measurement files contain the measurement parameters and method-specific settings. The devices are listed in the corresponding README file. BET and laser diffraction data of alumina DAW-45 and PS SX-350H are published in separate repositories: https://doi.org/10.25532/OPARA-933 (BET) and https://doi.org/10.25532/OPARA-1283 (laser diffraction).

### AFM-data.zip

All measurements were performed with the AFM XE-100 (Park Systems, Gwacheon, Korea). Acquisition parameters and processing steps are described in the corresponding README file.

- `Roughness` contains contact mode topography images of six uncoated alumina particle surfaces and six coated particle surfaces. `Raw-data` holds the original images (.tiff), `Processed-data` the flattened, binned and artifact-corrected topographies as xyz text files (Gwyddion export) with preview images, and `Results-roughness-script` the results of the moving segment roughness computation. **Important:** the images `230726024001.tiff` and `230726035002.tiff` are wrongly scaled in their metadata. The image dimension of 512 px × 512 px corresponds to 20 µm × 20 µm and **not** 10 µm × 10 µm (see corresponding README file). The processed files with `_cr` in their name are cropped sections of these images.
- `FD-measurements` contains force-distance spectroscopy data acquired with a colloidal probe (PS SX-350H particle, 3.5 µm diameter, attached to a tipless cantilever) on alumina host particles. Each of the six measurements in `Raw-data` consists of 256 FD curves on a 5 µm × 5 µm grid (one text file per curve with Z scan, Z detector and force) and an `_info.txt` file with the x-y positions of the measurement points. `Particle-images` contains images of the measured particles and `Results-FD-script` the adhesion forces computed with the Matlab script collection, individually and combined (after excluding irregular measurement).

### micro-CT-data.zip

Micro-CT scan of MF coated particles of the mixed guest particle system, acquired with a Zeiss Xradia 510 VERSA (Carl Zeiss Microscopy GmbH, Oberkochen, Germany) at a pixel size of 0.4099 µm. Acquisition, reconstruction and segmentation parameters are given in the corresponding README file.

- `Raw-reconstructed-images` contains the reconstructed image stack (947 slices, 944 px × 974 px, 16-bit TIFF) and `Header.txt` with the acquisition parameters.
- `Segmented-images` contains 12 coated particles (`Particle 01` to `Particle 12`) that were manually cropped from the reconstructed data and segmented with ilastik. For each particle, the three phases are provided as separate image stacks (`Alumina Guest`, `Host`, `PS Guest`, TIFF).
- `Results-particle-properties` contains the 12 coated particle subfolders with the .csv files containing the particle properties of each labeled object obtained with MorphoLibJ `Analyze Regions 3D` in ImageJ (e.g., volume, surface area, sphericity, centroid and fitted ellipsoid).
- `Overview-recon.PNG` and `3D-Viewer.PNG` are preview images of the reconstructed data.

### nano-CT-data.zip

Nano-CT scan of a single coated particle of the scaled down particle system, acquired with a Zeiss Xradia 810 ULTRA (Carl Zeiss Microscopy GmbH, Oberkochen, Germany) in high resolution mode at a pixel size of 16 nm. Acquisition, preprocessing, segmentation and coating thickness analysis are described in the corresponding README file.

- `Raw-reconstructed-images` contains the reconstructed image stack (930 slices, 16-bit TIFF).
- `Segmented-images` contains the segmented guest particle coating (`Guest-coating`) and host particle (`Host-particle`), 451 slices each.
- `Filtered-by-thickness` contains the guest particle coating after the optional thickness filtering in Dragonfly.


## Dataset Structure ##

The dataset is provided as six zip archives which have the following folder structure:

```
Experimental-protocol.zip
└── Example-Picobond-Protocol.xlsx

Calculations.zip
├── README.md
├── Particle-Particle-Interaction.xlsx
└── Regime-Map.xlsx

Particle-systems.zip
├── README.md
├── BET/
│   ├── Alumina-DAW03-BET.XLS
│   ├── Alumina-DAW05-BET.XLS
│   ├── PMMA-MH60FD-BET.XLS
│   └── PMMA-MP2801-BET.XLS
├── Bulk-density/
│   └── Bulk-density.xlsx
├── Data-sheets/
│   ├── Alumina-Denka.pdf
│   ├── PMMA-MH60FD-CoatingProducts.pdf
│   ├── PMMA_MH-Series-CoatingProducts.pdf
│   ├── PS-PMMA-SokenChemical-Kowa.pdf
│   └── PTFE-Goodfellow-6-9mu.pdf
├── Density/
│   ├── Alumina-DAW45-Density.XLS
│   └── Polystyrene-SX350H-Density.XLS
├── PSD/
│   ├── Alumina-DAW03-PSD.csv
│   ├── Alumina-DAW05-PSD.csv
│   ├── PMMA-MH60FD-PSD.csv
│   └── PTFE-Goodfellow-PSD.csv
├── SEM/                                  (4 .TIF images per particle system)
│   ├── Alumina-DAW05/
│   ├── Alumina-DAW45/
│   ├── PMMA-MH60FD/
│   ├── PMMA-MP2801/
│   ├── PS-SX350H/
│   └── PTFE-Goodfellow/
└── TGA/
    ├── Alumina-DAW45-TGA.txt
    └── PS-SX350H-TGA.txt

AFM-data.zip
├── README.md
├── FD-measurements/
│   ├── Particle-images/                  (5 .tif images)
│   ├── Raw-data/
│   │   ├── 251214001/
│   │   │   ├── 251214001_001.txt ... 251214001_256.txt
│   │   │   └── 251214001_info.txt
│   │   ├── 251214002/
│   │   ├── 251214003/
│   │   ├── 251214004/
│   │   ├── 251214005/
│   │   └── 251214022/
│   └── Results-FD-script/
│       ├── <measurement>_no_smoothing.xlsx   (6 files)
│       └── Combined-results.xlsx
└── Roughness/
    ├── Raw-data/
    │   ├── Alumina/                      (6 .tiff images)
    │   └── Coated-particle/              (3 .tiff images)
    │       └── README.md
    ├── Processed-data/
    │   ├── Alumina/                      (6 × _xyz.txt + _preview.PNG)
    │   └── Coated-particle/              (6 × _xyz.txt + _preview.PNG)
    └── Results-roughness-script/
        ├── Alumina/                      (6 .xlsx files)
        ├── Coated-particle/              (6 .xlsx files)
        └── Combined-results-Rq.xlsx

micro-CT-data.zip
├── README.md
├── 3D-Viewer.PNG
├── Overview-recon.PNG
├── Raw-reconstructed-images/
│   ├── 0001.tiff ... 0947.tiff
│   └── Header.txt
├── Segmented-images/
│   ├── Particle 01/
│   │   ├── Alumina Guest 01/             (cropped_particle_01_Object Predictions_000.tiff ...)
│   │   ├── Host 01/
│   │   └── PS Guest 01/
│   ├── Particle 02/
│   ├── ...
│   └── Particle 12/
└── Results-particle-properties/
    ├── Particle 01/
    │   ├── Alumina Guest 01.csv
    │   ├── Host 01.csv
    │   └── PS Guest 01.csv
    ├── Particle 02/
    ├── ...
    └── Particle 12/    

nano-CT-data.zip
├── README.md
├── Raw-reconstructed-images/
│   └── 2023_11_20_PB_010_HResZer160s901Reconstruction0001.tiff ... 0930.tiff
├── Segmented-images/
│   ├── Guest-coating/                    (Guest-coating0000.tif ... Guest-coating0450.tif)
│   └── Host-particle/                    (Host-particle0000.tif ... Host-particle0450.tif)
└── Filtered-by-thickness/                (Guest-coating-filtered0000.tif ... Guest-coating-filtered0450.tif)
```