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SCRiPTS – General Research Meeting – October 4th 2011
General research meetingOctober 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
Clean room Glenn Calibration pipettes Koen
Orders Kenny, Katrien TGA-DTA Els, Kenny
XRD Jonas (Films)Koen (Powders)
AFM Danny, Petra
TEM Katrien HOptional: Glenn, Katrien DK, Pieter, Jonathan D.
FIB-SEM Katrien HGlennKenny
Ink-jet printers Jonas Contact angle Petra
Lab responsible Katrien Waste Jonathan D.
Literature Klaartje Furnace room GlennKennyJonas
Microwave Jonathan W, Mieke M Calibration pH meter, balance
Heleen
Overview tasks
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
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).
Working in the lab
SCRiPTS – General Research Meeting – October 4th 2011
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.
Working in the lab
SCRiPTS – General Research Meeting – October 4th 2011
Literature
After every conferenceAbstract, title, authors, date and place
Every paperDOI Final version
check-up every 4 months2011 is finalized2012 coming up!
SCRiPTS – General Research Meeting – October 4th 2011
Scientific overview Coated Conductors
Y1Ba2Cu3O7-δ superconductorsPinning 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 CONDUCTORSJONAS FEYS, BRAM, PIETER, GLENN, SANDER, KATRIEN, JONATHAN DE ROO
13
Ink-jet printing of water-based YBCO inksPreparation of the ink: use of soluble salts in water + NTA and TEA
Important parameters for printing: surface tension and viscosity
𝑅𝑒= 𝜐𝑟𝜌𝜂 ,𝑊𝑒= 𝜐2𝑟𝜌𝜎 ,𝑂ℎ = ξ𝑊𝑒𝑅𝑒 = 𝜂ඥ𝜎𝜌𝑟
𝑑𝑐𝑜𝑛 = 𝑑0ඩ 8tan𝜃𝑒𝑞𝑚2 ൬3+ tan2 𝜃𝑒𝑞𝑚2 ൰
3
dcon (theor)= 168 µm
dcon (exp)= 120 - 160 µm
0.25 cm
Ink-jet patterning of water-based YBCO inks
φ orificeµm
line widthµm
9 40
22 90
30 200
Narrow
Goal High
Flat surface
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
SCRiPTS – General Research Meeting – October 4th 2011
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
Flux pinning in High Temperature Superconductors
SCRiPTS – General Research Meeting – October 4th 2011
• Solvothermal Aqueous MP
• Microwave Aqueous MP
• Heating-up Organic
BaZrO3 HfO2 Ta2O5
• Solvothermal
BnOH
HfCl4
• Microwave
3 hours >< 3days
• Stabilization in water
Dopamine
• Hot Injection
Ta(OEt)5
Oleic acid
Octadecene
• Low yield
Optimization!
• Steric stabilization
• Ligand exchange!
YBCO
• Hot Injection
YBCO acetates
Oleic acid
Octadecene
NaOH
• Gel formation
• Optimisation
Ba2+
O2-
Zr4+
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
TITANATESPETRA, MELIS, JONAS BILLIET, MIEKE, JONATHAN WATTÉ
SCRiPTS – General Research Meeting – October 4th 2011
Aqueous TiO2 solutions, stable > 6 monthsTi-precursor : alkoxidesConc. Ti4+: 0.4-0.5 Mvery sensitive to hydrolysis (precursor solutions containing <15 % organics)Complexing agents: citric acid, triethanolamineη: 4.3-5.6 cp, pH: 5-9
Arin, M., P. Lommens, et al. J. Eur.Cer. Soc.(2011) 31(6): 1067-1074
Bottom-up synthesis of TiO2 particles : Ø < 500 nm, mass load = >15%, H2OImprovement photocatalytic activity, Reduce sintering temperatureConc. Ti4+: 0.4, H2O ≥ 70 vol%, Fast hydrolysisincreasing viscosity (better jettability)Complexing agents: ethylenediaminetetraacetic acid,
TEA, tetraethylammonium hydroxideMicrowave synthesis at 100°C-140°C for 10-20 min
0
2
4
6
8
10
12
14
16
1 10 100Vo
lum
e (%
)Size (d.nm)
Ti-E
Ti-E+EG
Ti-E after 3 months
Ti-E after washing
Ti-E µw at 140C-10min
-0.22
-0.17
-0.12
-0.07
-0.02
0 100 200 300 400 500
ln C
/C0
Time (min)
glass
Ti-CA
Ti-TEA
DB
(a)
Arin M. et al. 2012 Nanotechnology (2012) 23 165603
Ink-Jet Printing of Photocatalytically Active TiO2 Thin Films from Aqueous Precursor Solutions and Nanoparticle Containing Suspensions
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% yieldProof-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…
• Mesoporous titania with Au nanoparticles– ‘trap and degrade’ of pesticides
Mesoporous titania architectures with incorporated noble metal nanoparticles:
A highly active photocatalyst.
Mesoporous titania with Pt nanoparticles Water splitting
Mesoporous titania High specific area 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
Photocatalytic reaction
H2O O2 + H2
SCRiPTS – General Research Meeting – October 4th 2011
TCO MATERIALSKENNY, NICOLAS
SCRiPTS – General Research Meeting – October 4th 2011
Ink jet printing of Al-doped ZnO coatingsScope 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
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 ITOMore abundant (=cheaper)Properties can compete with ITO
• Inkjet printing: to minimize material wastePatterns without a time consuming etching process
SCRiPTS – General Research Meeting – October 4th 2011
THERMO – ELECTRIC MATERIALSKOEN
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 ApproachEnhancement 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
MCM-48
SrTiO3 – silica composite
Impregnation precursor
Template removal (optional)
Densification and testing of both composite and “mesoporous” SrTiO3
e.g.
LUMINESCENT MATERIALSHELEEN, NIELS
SCRiPTS – General Research Meeting – October 4th 2011
phosphorparticle
matrix
Patterned remote phosphors by inkjet printing
blue LED
+ yellow phosphor
+ red phosphor
• matrix development• printing of commercial phosphor particles• printing of home-made phosphor particles
• 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,…)
schermpixels
blauwe led
golfgeleider
fosforbaantjes verstrooiingsmatrix
LOW-K MATERIALSFREDERIK
SCRiPTS – General Research Meeting – October 4th 2011
CRC RESEARCHMIEKE, ELENI, JORIS
Formation of hydration products
Completely Recyclable Concrete (CRC)
Study of the hydration processWhat is the effect of cement fineness?
What is the effect of cement composition?
Hydration stopped by• freeze drying• solvent exchange
Analysis by• TG• XRD/Rietveld• Isothermal calorimetry
Dissolution of clinker minerals
Mieke De Schepper & Eleni Arvaniti
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
Procedure
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
Objective
Starting point: CRC composition that fulfills all OPC requirementsTest: different concentrations of CaCl2 or CaSO4 are inserted into the clinker each timeBurning clinker: in different temperatures 1050, 1150, 1250, 1350, 1450 oCHeating rate: 10oC/minRemaining time in each temperature: 1hOutput: phase composition of clinker in each temperature. Check properties of produced cement
Instrumentation - Software
TGXRD/Rietveld analysisHigh temperature furnace (BLF)Scanning Electron MicroscopyFactSage 6.2 software (?)Thermodynamic modelingDifficulties: - find the appropriate software - database not available for cement- missing thermodynamic data
INK-JET PRINTING OF POLYMERSLARA
Lara Misseeuw
Inkjet printing of optical polymersAim: Synthesize miniaturized polymer optical sensors/waveguides
through inkjet printing
Colaboration between:
S4PBM
Prof Dubruel
S3SCRiPTs
Prof Van DriesscheIMEC
Synthesize polymer solutions• MMA + Fluoro• MMA + PEGMA
Characterization• Molecular weight• Purity
Printing of the polymer solutions in a defined pattern
Characterization• Rheology• Resolution
Check if the produced pattern will satisfy
Characterization• Transparency• Refractive index
SCRiPTS – General Research Meeting – October 4th 2011
Conferences 2013 Suggestions can be made
MRSE-MRSElectroceramicsSol-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 2013Danny, 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
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