General research meeting
October 4th 2012
SCRiPTS – General Research Meeting – October 4th 2011
Program
 Introduction
 Overview tasks
 Good laboratory practice
 Scientific overview – PhD and master thesis
 Conferences 2013
 Coming up
SCRiPTS – General Research Meeting – October 4th 2011
Introduction: SCRiPTS
2 professors + 1 emiritus professor
3 post-docs (Petra, Els, Pieter )
14 PhD students
2012: 6 Master students
SCRiPTS – General Research Meeting – October 4th 2011
Overview tasks
Clean room
Glenn
Calibration pipettes
Koen
Orders
Kenny, Katrien
TGA-DTA
Els, Kenny
XRD
Jonas (Films)
Koen (Powders)
AFM
Danny, Petra
TEM
Katrien H
Optional: Glenn, Katrien
DK, Pieter, Jonathan D.
FIB-SEM
Katrien H
Glenn
Kenny
Ink-jet printers
Jonas
Contact angle
Petra
Lab responsible
Katrien
Waste
Jonathan D.
Literature
Klaartje
Furnace room
Glenn
Kenny
Jonas
Microwave
Jonathan W, Mieke M
Calibration pH meter,
balance
Heleen
SCRiPTS – General Research Meeting – October 4th 2011
General things
 research meetings
 lab needs to be tidy – offices as well!!!
SCRiPTS – General Research Meeting – October 4th 2011
Good laboratory practice
 Safety goggles and lab coat
 label flasks – samples
 Fill in lab book
 Fill in log book at the different equipment sites
 Communicate!!!! (good AND bad - correct)
SCRiPTS – General Research Meeting – October 4th 2011
Working in the lab
 Everybody has his/her own lab desk, keep this clean!! After use of a fume hood,
clean up (= remove syringes, syringe wrapping paper, pipet points, paper...). It is nicer
if you can start your experiments in a clean fume hood!
 Waste in the correct containers
 Every product has its place in the lab. After use, put it back in the right place.
When solvent are used in smaller container (generally brown flasks), then these
should be labelled properly. There are labels available in the lab. If there does not
exist a label for your solvent, let me know.
 Empty product bottles are placed at the container of contaminated glass in the lab,
the yellow labels stay on the bottle!!! The bottles will be scanned out and removed.
 In general, it is not allowed to keep solutions in the lab desk, only solid products
(powders, tapes...) can be stored there. The solution can be in a leaking tray on the lab
desk (-> proper labelling).
SCRiPTS – General Research Meeting – October 4th 2011
Working in the lab
 A general cleaning day will be held once a month. This is a good time to go
through your solutions (precursors or suspensions), powders, tapes... to see whether
it is still necessary to keep those samples. There is no need to store precursor
solutions for 6 months, if you will make each time a new one...
 If there is any problem concerning the lab (dirty, broken equipment, waste
contamination...), please contact the responsible persons, your supervisor or me.
SCRiPTS – General Research Meeting – October 4th 2011
Literature
After every conference
Abstract, title, authors, date and place
Every paper
DOI
Final version
 check-up every 4 months
2011 is finalized
2012 coming up!
SCRiPTS – General Research Meeting – October 4th 2011
Scientific overview
 Coated Conductors
 Y1Ba2Cu3O7-δ superconductors
 Pinning centra: Ta2O3 - BaZrO3
 DFT approach
 TiO2 and BaTiO3
 TCO materials
 Thermo-electric materials
 Luminescent materials for large area applications
 Low k-materials
 CRC – Concrete research
 Catalysts
SCRiPTS – General Research Meeting – October 4th 2011
COATED CONDUCTORS
JONAS FEYS, BRAM, PIETER, GLENN, SANDER, KATRIEN, JONATHAN DE ROO
SCRiPTS – General Research Meeting – October 4th 2011
Ink-jet printing of water-based YBCO inks
Preparation of the ink: use of soluble salts in water + NTA and TEA
Important parameters for printing: surface tension and viscosity
𝜐𝑟𝜌
𝜐 2 𝑟𝜌
𝑊𝑒
𝑅𝑒 =
, 𝑊𝑒 =
, 𝑂ℎ =
=
𝜂
𝜎
𝑅𝑒
𝜂
𝜎𝜌𝑟
8
𝑑𝑐𝑜𝑛 = 𝑑0 3
tan
𝜃𝑒𝑞𝑚
𝜃𝑒𝑞𝑚
3 + tan2
2
2
dcon (theor)= 168 µm
dcon (exp)= 120 - 160 µm
0.25 cm
13
Ink-jet patterning of water-based YBCO inks
Goal
Narrow
High
Flat surface
φ orifice
µm
line width
µm
9
40
22
90
30
200
Ink-jet patterning of water-based YBCO inks
Problems that can occur :
 Satellite drops
 Splashing
 Bulging
 Coffee-Ring Effect
Optimization of ink and printing parameters
Flux pinning in High Temperature Superconductors
 Enhancement of the (RE)Ba2Cu3O7
superconducting properties
 Pinning centres: BaZrO3, (Y,Gd)2O3,
Ta2O5 and HfO2 nanostructures
 JC peaks in all angles of the applied
field and an overall systematic
increase in JC
 Ex-situ addition
 Ink-jet printing
SCRiPTS – General Research Meeting – October 4th 2011
BaZrO3
HfO2
Ta2O5
YBCO
Ba2+
O2Zr4+
•
•
•
Solvothermal
 Aqueous
 MP
•
Microwave
 Aqueous
 MP
•
Heating-up
 Organic
•
Solvothermal
•
Hot Injection

BnOH

Ta(OEt)5

HfCl4

Oleic acid
Microwave

Octadecene

3 hours ><
3days
Stabilization in
water

Dopamine
•
•
Low yield

Optimization!
Hot Injection

YBCO
acetates

Oleic acid

Octadecene

NaOH
•
Steric stabilization
•
Gel formation
•
Ligand exchange!
•
Optimisation
SCRiPTS – General Research Meeting – October 4th 2011
Development of new buffer layers for
coated conductors
SrTiO3
• Preparation of water-based inks
• Optimizing IJP parameters
• Optimizing microstructural properties
YBiO3
• Analysis of YBiO3 thin film stability
• Deposition of YBiO3 on buffered metal-tape
• Optimization thermal processing
SCRiPTS – General Research Meeting – October 4th 2011
TITANATES
PETRA, MELIS, JONAS BILLIET, MIEKE, JONATHAN WATTÉ
SCRiPTS – General Research Meeting – October 4th 2011
Ink-Jet Printing of Photocatalytically Active TiO2 Thin Films from
Aqueous Precursor Solutions and Nanoparticle Containing Suspensions
Aqueous TiO2 solutions, stable > 6 months
Ti-precursor : alkoxides
Conc. Ti4+: 0.4-0.5 M
very sensitive to hydrolysis
(precursor solutions containing <15 % organics)
Complexing agents: citric acid, triethanolamine
η: 4.3-5.6 cp, pH: 5-9
Bottom-up synthesis of TiO2 particles : Ø < 500 nm,
mass load = >15%, H2O
Improvement photocatalytic activity, Reduce sintering
temperature
Conc. Ti4+: 0.4, H2O ≥ 70 vol%, Fast hydrolysis
increasing viscosity (better jettability)
Complexing agents: ethylenediaminetetraacetic acid,
TEA, tetraethylammonium hydroxide
Microwave synthesis at 100°C-140°C for 10-20 min
16
Volume (%)
14
Ti-E µw at 140C-10min
12
Ti-E
10
Ti-E+EG
8
Ti-E after 3 months
6
Ti-E after washing
4
(a)
2
0
-0.02
1
glass
10
100
Size (d.nm)
Ti-CA
ln C/C0
-0.07
Ti-TEA
DB
-0.12
-0.17
-0.22
0
100
200
300
400
500
Time (min)
Arin, M., P. Lommens, et al. J. Eur.Cer. Soc.(2011) 31(6):
Arin M. et al. 2012 Nanotechnology (2012) 23 165603
1067-1074
SCRiPTS – General Research Meeting – October 4th 2011
Low temperature deposition of photocatalytic TiO2 layers on polymers
• Microwave-assisted hydrothermal synthesis on prepared Ti-precursors
> 90% crystallinity, > 90% yield
Proof-of-concept
• Deposition on polymers (PMMA, Kapton)
• Incorporation of buffer layers or chemical linkers
=> amorphous silica layers
=> silane coupling reagents
• Characterization: durability, photocatalytic properties, transparency…
SCRiPTS – General Research Meeting – October 4th 2011
Mesoporous titania architectures with incorporated
noble metal nanoparticles:
A highly active photocatalyst.
• Mesoporous titania with Au nanoparticles

– ‘trap and degrade’ of pesticides
 Mesoporous titania
 High
area
Mesoporous titania with
Pt specific
nanoparticles
 Water
splitting


Anatase phase
gold nanoparticles

1-3 nm diameter
Ordening of TiO2 nanocristals into
mesoporous structures
3 different TiO2
nanocrystals
Mesoporous ordening
by block-copolymers
Decoration of TiO2 with Pt
H2O
Photocatalytic reaction
O2
+
H2
TCO MATERIALS
KENNY, NICOLAS
SCRiPTS – General Research Meeting – October 4th 2011
Ink jet printing of Al-doped ZnO coatings
Scope of research:
•
Ink jet printing of AZO thin films and patterns on glass and PET substrates
with excellent optical and electrical properties
•
•
Development of inks containing stabilised ions & AZO nanoparticles
Studying the influence of the dopant concentration on the opto-electrical
properties
SCRiPTS – General Research Meeting – October 4th 2011
Inkjet printing of transparent conductive films and
patterns for display applications
• Conductive films serve as the electrode material to distribute the needed
power for the display
• ITO (Indium-tin oxide) normally used but too scarce (too expensive)
•AZO (Aluminum doped zinc oxide) is a candidate to replace ITO
More abundant (=cheaper)
Properties can compete with ITO
• Inkjet printing:
 to minimize material waste
Patterns without a time consuming etching process
THERMO – ELECTRIC MATERIALS
KOEN
SCRiPTS – General Research Meeting – October 4th 2011
Thermoelectric Materials
• Thermal gradient
results in potential
difference
• Heat - electricity
conversion applications
• SrTiO3 as n-type
thermoelectric material
• Nanostructuring to
improve the device’s
efficiency
Nanostructuring Approach
Enhancement of the thermoelectric conversion efficiency in
nanostructured material compared to bulk material
– Impregnation of SrTiO3 precursor into mesoporous template
materials (mesoporous silica and carbon)
– Densification of SrTiO3 – silica composite and/or mesoporous SrTiO3
yielding bulk nanostructured SrTiO3
– Study of thermoelectric effect of different samples
Impregnation
precursor
Template removal
(optional)
SrTiO3 – silica
composite
e.g.
MCM-48
Densification and testing of both composite and
“mesoporous” SrTiO3
LUMINESCENT MATERIALS
HELEEN, NIELS
Patterned remote phosphors by inkjet printing
phosphor
particle
matrix
• matrix development
• printing of commercial phosphor particles
• printing of home-made phosphor particles
blue LED
+ yellow phosphor
+ red phosphor
SCRiPTS – General Research Meeting – October 4th 2011
fosforbaantjes
verstrooiingsmatrix
schermpixels
blauwe
led
golfgeleider
•
•
•
•
Synthesis of YAG:Ce
Creating those particles by different techniques
=> Finding the best synthesis
Controlling the size of the particles
Optimisation of the properties of the created
YAG:Ce (QE, photostability,…)
LOW-K MATERIALS
FREDERIK
CRC RESEARCH
MIEKE, ELENI, JORIS
SCRiPTS – General Research Meeting – October 4th 2011
Completely Recyclable Concrete (CRC)
Mieke De Schepper & Eleni Arvaniti
Study of the hydration process
What is the effect of cement fineness?
What is the effect of cement composition?
Hydration stopped by
• freeze drying
• solvent exchange
Dissolution of
clinker minerals
Analysis by
• TG
• XRD/Rietveld
• Isothermal calorimetry
Formation of hydration products
Thermodynamic modelling
of experimental results
• Dissolution: empirical approach by
Parrot and Killoh (1984)
• Formation: by Gibbs free energy
minimization program GEMS
Heat release
Completely recyclable concrete (CRC)
Eleni Arvaniti
Objective
Study the effect of elements like Cl-, SO42-, on burnability of CRC. It may be
positive or negative depending on the concentration
Thermodynamic model to study the effect of small concentrations of chloride or
sulfate in the clinker composition, on the phase composition of reaction products,
under various curing conditions
Procedure
Starting point: CRC composition that
fulfills all OPC requirements
Test: different concentrations of CaCl2 or
CaSO4 are inserted into the clinker each
time
Burning clinker: in different temperatures
1050, 1150, 1250, 1350, 1450 oC
Heating rate: 10oC/min
Remaining time in each temperature: 1h
Output: phase composition of clinker in
each temperature. Check properties of
produced cement
Instrumentation - Software
TG
XRD/Rietveld analysis
High temperature furnace (BLF)
Scanning Electron Microscopy
FactSage 6.2 software (?)
Thermodynamic modeling
Difficulties:
- find the appropriate software
- database not available for cement
- missing thermodynamic data
INK-JET PRINTING OF POLYMERS
LARA
Lara Misseeuw
Inkjet printing of optical polymers
Aim:
Synthesize miniaturized polymer optical sensors/waveguides
through inkjet printing
Colaboration between:
S4
PBM
Prof Dubruel
S3
SCRiPTs
Prof Van Driessche
IMEC
Synthesize polymer
solutions
• MMA + Fluoro
• MMA + PEGMA
Printing of the
polymer solutions in
a defined pattern
Check if the produced
pattern will satisfy
Characterization
• Molecular weight
• Purity
Characterization
• Rheology
• Resolution
Characterization
• Transparency
• Refractive index
Conferences 2013
 Suggestions can be made
MRS
E-MRS
Electroceramics
Sol-gel conference Madrid
 EUCAS 2013
 NNNC 13
 Serbia - conference
 Abstracts! Deadline!
 FOF – FWO funding
SCRiPTS – General Research Meeting – October 4th 2011
Coming up !!!
 3 IWT defences
Jonathan W, Koen, Heleen
 3 PhD defences end 2012- beginning 2013
Danny, Frederik, Melis
SCRiPTS – General Research Meeting – October 4th 2011
Issues
-Viscoscity for limited amounts of liquids
- Plate to plate geometry
- Measuring oxygen in furnace
- Sensor??? Now min 10 ppm – 1 ppm
- furnace
- YBCO, dry furnace, thermostatic closet
SCRiPTS – General Research Meeting – October 4th 2011