Molecules,

Materials and Dr. Nuria Oliva-Jorge

Measurements 2 18th January 2022
Lab Briefing
 Lab materials and expectations

Review of core concepts

Lab specifics
Lab Briefing •
•
General Information
Detailed Objectives
Contents • Ideas to explore
• Materials and Methods
• Safety

Reporting your findings

Sign up
Handouts
 Expectations

Pre-lab Write-up in lab notebook Report

Describes procedure in detail in lab notebook Written in ACS Biomaterials Science

Answer questions in handouts (individual) Good record-keeping practice and Engineering Letters format
Due 21/01 @5pm (Groups A-C) Submit scan/photo by EOD Due 22/02/2022 @23:59
Due 28/01 @5pm (Groups E-F)
 JANUARY/FEBRUARY 2022
Monday Tuesday Wednesday Thursday Friday Saturday Sunday
18 19 20 21 22 23
Intro Lecture Prelabs G.A-C
due @5pm

24 25 26 27 28 29 30
Lab G.A-C Prelabs G.D-F
Write–up (EOD) due @5pm

31 1 2 3 4 5 6
Lab G.D-F
Write–up (EOD)

7 8 9 10 11 12 13
14 15 16 17 18 19 20
21 22
Report due
@11:59PM
What is nano?
Nanoscience and nanotechnology are the fields of study
dealing with materials which have at least one dimension
on the order of 1-100 nm (1x10-9 m).

Nanoscience is studying materials and devices to

understand and manipulate their basic properties.

Nanotechnology is using nanoscience to reliably produce

devices that could be used for a specific application.
Nanoparticle Colorants

• 4th century Roman glass cage cup

• Trace amounts of gold and silver nanoparticles
• Red when light from behind, green when lit
from in front
• Nanoparticles of ~70 nm embedded in the
glass cause surface plasmon resonance
Applications for Nanoparticles

Copper & silicon

nanoparticles
Quantum Dots

Semiconductor nanocrystals Applications:

that exhibit quantum size
effects in their optical and
electronic properties

Finely tuned, size-dependent optical properties

Cotta, MA. CS Appl. Nano Mater. 2020, 3, 6, 4920–4924

Cd/Se Quantum Dots
Explore the synthesis and properties of nano-scale Cd/Se Quantum Dots
• How do we make Quantum Dots?
• Seed solutions of cadmium and selenium
• Cd and Se form clusters that quickly grow larger,
typically into spheres
• Growth controlled using surfactants

• What new properties do they have?

• Size-dependent luminescence
• Behave following particle-in-a-box model
(larger boxes – smaller energy gaps)
• Used for imaging, color displays, sensors
Jablonski diagrams and luminescence
Vibrational states

Excited State

𝐸=h ∙ 𝜈

𝑐
𝜆=
𝜈
Energy

Ground State

https://www.chemguide.co.uk/analysis/uvvisible/theory.html
 Absorbance measurement
Transmission, T = I/I0 Absorbance, A = -log10(T)

Beer-Lambert Law 𝑨=𝜺∙ 𝒍 ∙𝒄

Absorbance Transmittance
0 100%
ε Molar Absorption Coefficient (M-1cm-1)
1 10% l Optical path length (cm)
2 1%
c Concentration (M)
3 0.1%
4 0.01%
5 0.001%

https://www.edinst.com/blog/the-beer-lambert-law/##targetText=The%20Beer%2DLambert%20law%20states,calculated%20by%20measuring%20its%20absorbance.
 Absorbance vs fluorescence measurement

https://www.chromedia.org/chromedia?waxtrapp=mkqjtbEsHiemBpdmBlIEcCArB&subNav=cczbdbEsHiemBpdmBlIEcCArBP
Excitons in QDs
Electron + pairing hole = exciton

Need of surfactant to observe

excitons, mechanism unknown
 Trap states in QDs
Electron + pairing hole = exciton

• Trap-state broad emission

• Significantly red-shifted,
dependent on size
• Poorly understood, thought to
originate in surface defects.
• Luminescence dominates
Making QDs
 Synthetize two batches of Cd/Se
QDs
•With/without oleylamine
•Note colours under UV light

Objectives
Record spectrophotometric
data

• UV-Vis absorbance spectra

• Fluorescence excitation/emission
spectra
Materials
Chemicals Equipment

• 1-Octadecene • A balance
• 10 ml graduated cylinder
• Trioctylphosphine
• 25 ml round bottom flasks
• Oleic Acid • Heating mantles

• Selenium, powder • Thermometer

• 10 ml syringe
• Cadmium acetate dehydrate
• 1 ml glass pipette
• Oleylamine (procedure 2 only) • 10 small glass vials
• UV-Vis and fluorescence spectrometer

Note you do not have to make the cadmium seed solution, your GTA will prepare it before class.
Safety
Cadmium Acetate Hydrate Trioctylphosphine

Selenium
Oleylamine

Octadecene
Other hazards
• Always wear gloves, protective clothing and safety goggles.
• Perform syntheses in well-ventilated fume hood.
• Dispose of waste in adequate containers.

Octadecene @130C and 165C Always use gloves, lab coat and goggles
Procedure

Procedure 1 Procedure 2

±
Questions for Pre-lab assignment
 What is a quantum dot?

 How does the colour of the CdSe QDs change with increasing reaction times? Can you explain the

phenomenon using the particle-in-a-box model?

 Why do the QDs not precipitate from solution?

 If the reaction continues for a long time, i.e., the quantum dots grow increasingly large, how do their optical

properties evolve accordingly?

 Why are the QDs emission peaks very broad?

 The emission peaks and their corresponding absorption peaks do not appear at exactly the same

wavelength. In fact, the QDs absorb more energy than they emit. Where does the extra energy dissipate?

Explain using a diagram.

Good record-keeping practices
Proper notebook page
Written as the work is performed
Dated and signed by author
Each section has a clear, descriptive
heading
The writing is legible and
grammatically correct
Active voice in first person: “I
added the two ingredients…”
Errors: Do Not write over; cross,
and write above
What to write with…
No pencils.* Erasers are a definite
no-no!
No aqueous-based pens (e.g., most
felt-tips).
Best bet for general use: black,
ballpoint pen.
No white-out!! Just strike through,
explain and initial errors.
About the notebook…
Notebooks have to last 23 years
after patent issue.
Notebook should be bound. No
spiral notebooks! No loose-leaf!
Page layout easy to graph, date,
sign, etc.
Table of contents
What goes in the notebook?
• Plans
• Realities (deviations from the plan)
• Observations
• Sketches and photographs
• “Links” to instrument logbooks and data on disks
• Ideas: a notebook is a repository of creativity
• E-mails from collaborators (tape or paste them in)
• Graphs (tape of paste them in)
• Summaries of papers you have read
• Hints and tips you may get from science friends
Checklist

 Black, ballpoint pen used?

 Legible handwriting?
 Entries signed/dated (13 October 2002 better than 13/10/02)
 Clear headings saying what this page is about?
 Written in first person? Complete sentences?
 Is the researcher correctly “thinking in the notebook”—i.e., ideas and plans and
observations integrated and written down.
 Is the notebook stored safely when not in use?
Report Guidelines

Report written in ACS Biomaterials Science and Should include:

Engineering Letters format

Restricted to 6 double-spaced Word-processed Introductory material

pages (or 2500 words) Outline of the experiments
Max 3-4 figures Results – presentation and description
Brief abstract of less than 100 words Concluding remarks
Continuous narrative, no section headings Supplementary material not allowed
Report Expectations

Content
Format (30%) Extra Points
(70%)
Follows Guidelines? Necessary background
• Word/page limit information?
• Figure limit • i.e. particle-in-a-box model
Estimate QD particle size using
• No subheadings • Figures support text?
emission wavelengths
• See QD student procedure
Written skills All lab experiments covered?
• Good use of English • Procedures
• Scientific language
• Results

Data presentation? Discussion of Results

•Axes labelled? Legend? • Objective description of data
•Figure captions? • Why data looks the way it look? How
•Figures referenced in the text? do you explain it with theory?
Any questions?
Course Leader: Course Technician:
Dr. Nuria Oliva-Jorge Joel Eustaquio
n.oliva-jorge@imperial.ac.uk j.eustaquio@imperial.ac.uk
SMUH U301A, White City Campus
Labs: RCS1 108
GTAs:
Groups GTA 1 GTA 2 GTA 3
A&D Brenna Parke Joseph Hansen-Shearer Angelos Vrynas
b.parke20@imperial.ac.uk joseph.hansen-shearer18@imperial.ac.uk a.vrynas19@imperial.ac.uk
B&E Joana Salvado Correia Joseph Hansen-Shearer Jacob Lee
j.correia@imperial.ac.uk joseph.hansen-shearer18@imperial.ac.uk j.lee19@imperial.ac.uk
C&F Joana Salvado Correia Jacob Lee Angelos Vrynas
j.correia@imperial.ac.uk j.lee19@imperial.ac.uk a.vrynas19@imperial.ac.uk