Research activities of the

Plasmachemistry Research Group

 Reseach areas related to thermal
plasma processing
- Synthesis of fine particles from nanometer size to
micrometer one
- Modification of particle morphology
(acicular  spherical, solid  hollow, core-shell
structures, e.g. nm size magnetic iron core with graphite
shell)
- Waste processing: decomposition of hazardous wastes,
extraction of precious components
- Coatings by atmospheric plasma spraying
- Plasma sintering (SPS)
 Available plasma units
• TEKNA PL 35 system: Radiofrequency Inductively coupled
thermal plasma torch having max. 35 kW power
• Transferred and non-transferred arc plasma units up to 30 kW
power
• Shultzer-Metco plasma spraying system
• Spark Plasma Sintering machine (FCT GmbH)
 Particle synthesis and
modification of the morphology
Powders Spheroidization
• Ferrites • Al2O3
• SiC • TiO2
• Si3N4 • Hollow SiO2
• TiB2
• LaB6
• ZrC Shell – core structure
• Alumo-silicate • Carbon coated magnetic
• Mg-Ti alloys for H2 particle
storage • ZrO2 coated ferrites
• Fullerene • Metal dots coated particles
• Graphene for catalysts
• Particle functionalization
Characterization of nanoparticles
• Chemical composition analysis
– ICP-OES
– ICP-MS
– XRF
• Morphological analysis
– LD-Particle Size Analyzer
– SEM, TEM AFM image of
– AFM carbon black
nanoparticles
Characterization of nanoparticles
• Surface properties
– Surface area & porosity
(Quantachrome Autosorb 1C)
– Zeta potential
– XPS (ESCA)
• Phase composition
– XRD
• Chemical bonds
– FT-IR
– Raman
 Sintered bulk materials
• Si3N4 composites: • Al2O3 composites:
– Ferrite – CaSO4
– MLG
– CNT – SiC
– MLG – Si3N4
– ZrO2 fibre – CNT
– ferrit
• SiC composites:
• HAP composites
– Si3N4
– CNT
– Ti – MLG
– MLG • Glass ceramics
• Ferrites
• ZrO2
 Surface coating techniques

• Plasma spraying • Film deposition

– Ferrite coating – DLC coatings
– ZrO2
– SiC
– Si3N4
– HAP
 Surface modification
1. Atmospheric and low pressure plasmas (RF, DBD,
PIII)
2. Ion bombardment
• Polymer surfaces • Inorganic surfaces
– Plastics – CNT
– Textiles – Graphene
Improve: – Metals
– Wear resistance Improve:
– Adhesion – Wear resistance
– Bioactivity – Hidrophilization
– Functionalization
Surface treatment by low temperature plasma: PIII

Gas inlet

UHV
chamber
(120 l ) RF RF
matching generator

Turbomolecular
pump

High voltage Fore vacuum

pulser pump

Plasma immersion ion implantation (PIII, PI3)

plasma source ion implantation (PSII)
plasma-based ion implantation (PBII)
and deposition (D) variants
 PIII equipment and typical process conditions

RF plasma: N2 or He, etc. (4N5 purity),

27.13 MHz (Dressler, Germany)
150 W
flow rate = 25 cm3 (STP)/min
pressure  510-1 Pa
Pulser: ANSTO (Australia)
f = 65  218 Hz
t = 5 μs
Conditions: U = 1530 kV
F = 1 31017 cm-2
FR = 371013 cm-2 s-1
 Polymers treated, surface analytical methods applied
and properties studied

Polymers: UHMWPE, PA, PC, PET, PTFE…

Methods:
XPS: surface composition, chemical bonding
Raman: molecular structure
Nanomechanical tests: hardness, modulus, roughness,
resistance to scratch & wear
Wettability:surface free energy, polar and dispersive
components
Electrical conductivity: changes in electric resistance
Colorimetry: lightness, colourfulness
 Applications of PI3 treatment

 Nitridation (metals, polymers)

 Metal ion implantation (Ti, Al, Sb, C)

 PIIID implantation-deponation (DLC, ta-C, MoS2-Ti)

 RPIIID reactive implantation (TiN, AlN)

 PIII low energy: Si-doping (5-20 nm)

Hip joint prostheses

• Stainless steel, titanium alloy

• Ultra high molecular weight
polyethylene

Tribological properties of the

combination of these materials
need improvements.
 Selected results by PIII

N9

Raman Intensity [a.u.]

N8
N7

N6

UHMWPE/N PIII: Volume loss PTFE/N PIII: Wettability can be N5

can decrease from 35 to 15 mm3 decreased or increased
N4

N3

N2
N1
Untreated

800 1000 1200 1400 1600 1800 2000

-1
Raman shift [cm ]

Wear resistance and lifetime of hip joint PET/He PIII: a-C:H forms
prostheses can be increased
 Surface treatment by atmospheric low temperature
plasma: DBD
12000
300
9000
200
6000

Current [mA]
Voltage [V]
3000 100

0
0
-3000
-100
-6000

-9000 -200

-12000 -300
0 25 50 75 100 125 150 175 200 225 250
Time [μs]

Scheme of DBD reactor Curves of voltage and current

Advantages:
• no vacuum is needed
• small contact times
• continuous, in-line technology

Diffuse coplanar surface barrier discharge

(DCSBD)
 Surface analysis by XPS
• X-ray Photoelectron Spectroscopy (ESCA)
• For any vacuum compatible condensed matter
• Sampling depth: 5 -15 nm
• Depth-profiling by in situ etching
• Qualitative analysis for all elements
except H and He
• Quantitative analysis with a few relative % error
• Chemical state & chemical structure
 X-ray
Electron
Photoelectron
energy Spectrometer
analyzer

Electron
Ion detector Data
gun acquisition
X-ray I
and
gun processing
Sample B.E.

lock
UHV
system
 XPS MultiQuant - Quantification
models
The XPS intensity data
sensitively reflect the
sample geometry: in all
Homogeneous Oxide-Layer
cases a geometry model
is applied

Layers-on-Plane Layers-on-Sphere Layers-on-Cylinder Layers-on-Polyhedron

Islands-on-Plane Islands-on-Sphere Islands-on-Cylinder Islands-on-Polyhedron

MTA Természettudományi Kutatóközpont (MTA TTK)
Anyag és Környezetkémiai Kutatóintézet (AKI)

MTA Research Centre for Natural Sciences

Research Institute of Materials and Environmental Chemistry
Plasmachemistry Research Group

Website: ttk.mta.hu

Contact person: Károly Zoltán (karoly.zoltan@ttk.mta.hu)