scripts – general research meeting – october 4th 2011 general research meeting october 4th 2012

SCRiPTS – General Research Meeting – October 4th 2011

General research meetingOctober 4th 2012


Program

Introduction Overview tasks Good laboratory practice Scientific overview – PhD and master thesis Conferences 2013 Coming up


Introduction: SCRiPTS

2 professors + 1 emiritus professor 3 post-docs (Petra, Els, Pieter ) 14 PhD students 2012: 6 Master students


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


General things

research meetings lab needs to be tidy – offices as well!!!


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)


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


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


Literature

After every conferenceAbstract, title, authors, date and place

Every paperDOI Final version

check-up every 4 months2011 is finalized2012 coming up!


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


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


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


• 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+


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


TITANATESPETRA, MELIS, JONAS BILLIET, MIEKE, JONATHAN WATTÉ


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


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


TCO MATERIALSKENNY, NICOLAS


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


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


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


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


Conferences 2013 Suggestions can be made

MRSE-MRSElectroceramicsSol-gel conference Madrid EUCAS 2013 NNNC 13 Serbia - conference Abstracts! Deadline!

FOF – FWO funding


Coming up !!!

3 IWT defences Jonathan W, Koen, Heleen

3 PhD defences end 2012- beginning 2013Danny, Frederik, Melis


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 general research meeting october 4th 2012

Documents

lab book

lab dirty

general cleaning day

lab desk proper labelling

lab coat label flasks

good time

clean fume hood

materials crc