Federal University of Santa Catarina

Mechanical Engineering Department

Materials Engineering Undergraduation Course

Centre for Advanced Nanotechnology - University of Toronto

Internship report II

(Period: 09/05/2014 to 15/08/2014)

Student: Brian Martins Ilkiw

Enrollment number: 12101140

Supervisor: Bin Bin Li

__________________________

We agree with the content on this internship report.

Toronto, Canada, 2014.

2

Centre for Advanced Nanotechnology

Department of Materials Science & Engineering

Faculty of Applied Science & Engineering

University of Toronto

Haultain Building

170 College Street

M5S 3E4

Toronto, Ontario, Canada

+1 (416) 978-4556

www.utoronto.ca/~ecan

3

Acknowledgment

To Centre for Advanced Nanotechnology and University of Toronto

for the work opportunity;

To Centre for International Experience of University of Toronto and

Canadian Bureau for International Education CBIE for managing my internship

and turning it possible;

To National Council for Scientific and Technological Development

CNPq for the sponsorship and support;

To my supervisor, Bin Bin Li, for all support, knowledge and

attention spent on me during my research;

To Professor Ph.D. Harry E. Ruda, director of the Centre for Advanced

Nanotechnology, for the trust and working opportunity;

To Prof. Paulo Wendhausen and Ing. Pablo Junges for the attention,

comprehension and support during my research;

To Bojan Miljkovic, Christina Souza, Julie Riou, Camille Hudin and others

researchers or students for the partnership and mutual aid.

4

Summary 1. Introduction........................................................................................................ 5

2. Wastewater treatment ..................................................................................... 6

3. Preparation ......................................................................................................... 7

3.1. Cleaning and etching steps ....................................................................... 7

3.2. Powder preparation ..................................................................................... 8

3.3. Solution preparation .................................................................................... 8

4. Spin Coating ...................................................................................................... 9

5. Doping ............................................................................................................... 10

5.1. Antimony ...................................................................................................... 10

6. Analysis ............................................................................................................ 11

6.1. Microscopic analysis ................................................................................. 12

6.2. Cyclic voltammetry analysis ................................................................... 12

7. Nickel influence .............................................................................................. 13

8. PVB influence .................................................................................................. 16

9. Lanthanum influence ..................................................................................... 17

10. Iridium influence ............................................................................................. 19

11. Conclusion ....................................................................................................... 23

12. References ....................................................................................................... 24

Annex A About Centre for Advanced Technology ....................................... 25

Appendix A Samples description ................................................................... 26

Appendix B Activities timetable ..................................................................... 29

5

1. Introduction

This report refers to activities realized from May 9 to August 12, 2014 at

Centre of Advanced Technology of University of Toronto, located in Toronto,

Canada, as a mandatory part of Science without Borders program. The student

was part of a research that aims produces anodes for phenol oxidation of

wastewaters. He was in charge to search about, study, prepare and

characterize Antimony doped Tin oxide nanostructured films on Titanium foil

substrate by spin coating deposition technique. Co-doping with Nickel, Polyvinyl

butyral, Lanthanum and Iridium were also largely discussed by the student.

6

2. Wastewater treatment

A plenty of industries produce wastewater as a result of their industrial

process and chemical reactions. Not only inorganic materials, such as acids,

bases, heavy metals or salts, but also organic components are often present in

industrial wastewater [1]. In order to turn this water into non-polluted water,

several treatment methods can be applied. For the inorganic wastewater the

treatment can be separated in two steps, being the primary treatment

coagulating sedimentation, floatation, neutralization, oxidation or reduction, and

the secondary treatment filtration, activated carbon adsorption, chelation and

membrane separation. After those treatments the constituent of chemical

oxygen demand must de decomposed and the water reaching effluent

standards [2].

Figure 1 Inorganic wastewater flow diagram [2].

Indeed the organic wastewater treatment is quite distinct. In the primary

stage occurs the process of coagulation, sedimentation, floatation and

neutralization. After that, at the second stage there are the oxidation of organic

compounds and some biological treatment. And finally, at the third stage the

filtration, activated carbon adsorption and membrane separation take place [2].

Figure 2 Organic wastewater flow diagram [2].

7

Those methods can vary depending on the kind of chemicals presents in

each wastewater. That report focuses on chemical oxidation that is located on

the second stage of the organic treatment.

This chemical oxidation occurs due to anodes, in our case Ti/SnO2,

which oxidizes phenol. Phenolic substances are extremely toxic; moreover they

are non-biodegradable [3]. In order to give an environmental friendly destination

to these aromatic compounded wastewaters, this electrochemical oxidation

method is used, as the main reagent, the electrode, is environmental clean.

There are several types of anodes proper for this application: Pt, Ti/IrO2,

Ti/RuO2, Ti/PbO2, DSA, but the Ti/SnO2 anode was chosen for this study since

previous studies show that this anode give a higher current efficiency, provide

an almost complete total organic carbon (TOC) elimination [1] and have others

important film characteristics as small size, high sensitivity, good stability, fast

response and recovery speed [4]. The SnO2 nanofilm can also be applied to

others functions, for instance gas sensing.

3. Preparation

The used process is based on previous studies and results. The

students main role was to improve this technique and develop nanofilms with a

higher standard.

The preparation starts cutting the titanium foil substrate (3.5 x 3.5 cm)

with 0.13 mm of thickness. After that, in order to clean it and remove the TiO2

present on the titaniums surface, the following steps are done.

3.1. Cleaning and etching steps

Cleaning steps:

5 minutes immersed in acetone at 80C;

10 minutes immersed in acetone in an ultrasonic cleaner at room

temperature;

5 minutes immersed in isopropyl alcohol at 80C;

5 minutes immersed in deionized water at 80C.

8

Etching steps:

25 minutes immersed in 18% HCl solution at 80C;

Wash with deionized water and dry with airflow.

Figure 3 A. Non-etched substrate. B. Etched substrate

3.2. Powder preparation

In order to guarantee the best properties and complete dissolution of tin

in ethanol, before preparing the used solutions, we dissolve SnCl2 anhydrous

crystalline, 99% min, in a closed beaker with ethanol and simultaneously stir

with a magnetic bar at 500 RPM and heat at 55C until it gets totally dissolved.

After that, the beaker is opened, and the solution kept stirring and heating until

the solution is totally dried and SnOxCly powder is formed.

3.3. Solution preparation

Making a solution has some different aspects depending on which

substances are present. It is usual to do a 25ml solution, which is enough to

until 6 samples. The preparation starts putting 25 ml of anhydrous ethyl alcohol

(ethanol) and a weighed amount of intended substances in a small beaker. The

beaker is closed and putted to stir by a magnetic bar at 300 RPM and

simultaneously heated by a hot plate at 60C during at least 1 hour. After the

solute is totally dissolved the solution is cooled down by air.

A B

9

4. Spin Coating

Since the growing interest in wastewater treatment by electrochemical

methods, several methods were studied and developed, such as direct

oxidation on electrode surface, indirect oxidation and electro-Fenton reactions

through hydroxyl radicals. For these methods, the main component is the anode

used, and the metal oxide anodes are the most used, e.g. Ti/PbO2, Ti/SnO2-

Sb2O5, Ti/RuO5, and Ti/IrO2 [5].

For this anode preparation the most widely used are thermal

decomposition, electro-deposition, spray pyrolysis, sol-gel mechanism,

sputtering, spin-coating technique, chemical vapor deposition and electron

beam evaporation [5].

The chosen method was spin-coating followed by a thermal

decomposition, as the spin coating provides a uniform distribution of the

elements, characteristic which was not present in only thermal deposed

samples. Comparing with other similar process (dip-coating), samples made by

spin-coating technique have a better defined crystal form, a smoother and more

compact surface [5]. Furthermore, electrochemical deposition technique has

been simultaneously tested by another researcher and results could be

compared [6].

The equipment used for this technique was an SCS Spincoater model

P6700 (figure 4), that consists in a rotatory plate where the sample is fixed. The

process is basically simple, and consists in fixing the sample at the plate by

suction, then with a syringe collect around 0.7 ml of the selected solution and

drop it uniformly on the titanium substrate, as it creates a thin layer of solution.

After that the spincoater is covered and turned on. As soon as it is turned on,

the rotatory plate goes to a frequency of rotation of 750 revolutions per minute

(RPM). After 25 seconds the angular velocity increases until reaches 2000 RPM

in 50 seconds, when the rotation remains constant for more 60 seconds, and

then it decreases until stops, totaling a 125 seconds process. This procedure

forces the solution to spread by centrifugal forces.

10

Figure 4 Spincoater

Subsequently, thermal decomposition takes place. The sample is placed

on a ceramic plate and in a furnace at 100C during 10 minutes for evaporation

of the solvent. After that the sample is transferred to a furnace at 500C where it

stays for more 10 minutes for annealing. Following, the sample is cooled down

by air. When cooled, the first layer is ready, so this process is repeated as many

times as the number of required layers. Usually it is made 4 layers like this

process plus a distinct last layer, which have a slowly annealing. This process

starts at 100C where the temperature remains constant for 10 minutes, then

slowly increases until 500C, where it stays for 30 minutes, when the furnace is

shut down and the sample takes overnight for cooling down.

5. Doping

5.1. Antimony

Each semiconductor has an intrinsic energy gap, which is the requested

energy to transition from the valence band to the conduction band. Smaller the

gap, easier to an electron goes from a band to another, which means higher

conductivity.

A pure tin oxide is classified as an n-type semiconductor; with a band gap

of around 3.7 eV, it is not favorable for electron transference in electrochemical

11

oxidation. However adding certain dopants to tin oxide, it is possible to reduce

the band gab, consequently increasing the conductivity. Furthermore, it also can

increase electrochemical activity [7]. As tin and antimony have close atomic

number (50; 51), similar electronegativity (1.96; 2.05 Pauling scale) and same

atomic radius (140 pm), an antimony doping can occur on the tetragonal rutile

SnO2 structure (figure 5).

Figure 5 Rutile tetragonal structure [11]

At first time, Sb2O3 was used for doping solution; however this oxide

seemed has low solubility in alcohol. As a first try, small amount of hydrochloric

acid was added in order to reduce the solutions pH and consequently raises

the solubility. As this try had low efficiency, using SbCl3 was cogitated. As a

result, the antimony trichloride easily dissolved and fulfilled doping

requirements.

Based on previous studies, a solution with a Sb concentration of 5 weight

% relative to Sn was used in all experiments. In order to further improve some

electrodes characteristics, some co-doping with Nickel, Polyvinyl butyral (PVB),

Lanthanum and Iridium were also experienced.

6. Analysis

With the samples deposition done, we proceed to some experiments and

analysis to have a complete understanding about samples properties and

morphology.

12

6.1. Microscopic analysis

In order to analyze the samples surface, a scanning electron microscope

(SEM) is used. The microscope used in our analysis was a Hitachi S-5200 ultra

high-resolution field emission SEM, which scans the sample with a focused

beam of high-energy electrons. These electrons interact with samples atoms

and produce three kinds of signal: backscattered electrons, X-rays, and

secondary electrons (which are the mostly used in our analysis). Secondary

electrons are detected and produce an image of the samples surface. With this

image, which can reaches nanoscales with a good resolution, we can note if the

surface is rough, smooth, or if there is cracks, holes, bubbles, dots and the

morphology in general.

To make sure that the elements amounts that we dissolve in our solution

were the same as the amount that were deposed in the sample, we do an

energy-dispersive X-ray spectroscopy (EDS) analysis that gives information

about the chemical composition of the film. That analysis produces a spectrum

with set of peaks, where each one represents a unique element. Once this

analysis is done we can realize the composition and exact amount of each

element present in the nanofilm.

6.2. Cyclic voltammetry analysis

In order to know and understand the samples behavior to

electrochemical reactions, a Cyclic Voltametry experiment is applied. A three-

electrode arrangement and a potentiostat Princeton Applied Research model

263A are used. The system follows the American polarity convention, so

positive current is cathodic and occurs when reduction takes place at working

electrode; and negative current is anodic and occurs when oxidation takes

place at working electrode.

Several tests were applied, where a potential is applied between the

reference and working electrode, and the equipment measures the current and

plots a graph current versus potential. The reference electrode (RE) is an

Ag/AgCl electrode, the working electrode (WE) is the Titanium substrate with

the nanofilm, and the counter electrode (CE) is a Platinum wire. The potential is

13

applied between 0mV and 4000mV and the scan rate between 25mV/s and

200mV/s.

Figure 6 - Electrodes

To measure the electron-transfer rate, efficiency and systems

reversibility the electrodes are immersed in an equimolar solution of potassium

ferro/ferri-cyanide in 1M of NaOH.

To measure the overpotential for O2 evolution, the electrode electroactivity

and lifetime the electrodes are immersed in an aqueous solution of 1M of

H2SO4, and 100 cycles are applied.

7. Nickel influence

Besides the antimony doping, nickel co-doping was tested to increase

electrical properties, stability and morphology. The amount of nickel was varied

to realize its behavior according with different percentages. Figure 7 shows the

influence of nickel on the films morphology. The first image shows some cracks

at surface. Those cracks cannot be seen at the second image, where was

added some amount of nickel. The film with nickel also seems smoother than

the one without nickel.

14

Figure 7 A. Sb doped Sn without Ni. B. Sb doped Sn with 2.5 weight % relative to Sn.

To better understand the influence of nickel amount, five samples were

compared on Cyclic Voltammograms.

Sample SnOx (g)

SbCl2 (g)

NiCl2 (g)

Sb/Sn weight %

Ni/Sn weight %

B15 = Ni0 2 0.1 0 5 0

B25 = Ni2.5 2 0.1 0.05 5 2.5

B29 = Ni5 2 0.1 0.1 5 5

B23 = Ni7.5 2 0.1 0.15 5 7.5

B21 = Ni10 2 0.1 0.2 5 10 Table 1 Elements amount per sample [8].

As it is shown in figure 8, although the oxygen evolution peak remains

almost the same for all 5 samples (~2100mV), as more nickel is added, lower is

the current density. That means that films with higher amounts of nickel have a

lower electrochemical activity.

0 1000 2000 3000 4000

200

0

-200

-400

-600

-800

-1000

-1200

-1400

i (m

A/c

m2)

E (mV vs. Ag/AgCl)

Ni0

Ni2,5

Ni5

Ni7,5

Ni10

Figure 8 - Voltammetric behaviour of antimony-doped tin oxide anode with different amount of Nickel [8].

15

Cyclic voltammetric experiments in potassium ferro/ferri-cyanide solution

were also performed. The results of each one of the five samples at different

scan rates are shown in figure 9.

-200 0 200 400 600 800

10

5

0

-5

-10

i (m

A/c

m2

)

E (mV vs.Ag/AgCl)

200 mV/s

100 mV/s

50 mV/s

25 mV/s

(a) Ni0

-200 0 200 400 600 800

4

3

2

1

0

-1

-2

-3

-4

i (m

A/c

m2

)

E (mV vs. Ag/AgCl)

200 mV/s

100 mV/s

50 mV/s

25 mV/s

(b) Ni2,5

-1000 -500 0 500 1000 1500

3

2

1

0

-1

i (m

A/c

m2

)

E (mV vs. Ag/AgCl)

200 mV/s

100 mV/s

50 mV/s

25 mV/s

(c) Ni5

-1000 -500 0 500 1000 1500

4

2

0

-2

-4

-6i (m

A/c

m2

)

E (mV vs. Ag/AgCl)

200 mV/s

100 mV/s

50 mV/s

25 mV/s

(d) Ni7,5

-500 0 500 1000 1500

4

2

0

-2

-4

-6

-8

-10

-12

i (m

A/c

m2

)

E (mV vs. Ag/AgCl)

200 mV/s

100 mV/s

50 mV/s

25 mV/s

(e) Ni10

Figure 9 - Cyclic voltammograms obtained in 10mM [Fe(CN)6]3-

/[Fe(CN)6]4-

and 0.1M NaOH solution at different scanning rates (200 mV/s, 100 mV/s, 50 mV/s and 25 mV/s) for different

amount of nickel in the coating solution [8].

In Ni0 and Ni2.5 we can see a reduction peak and an oxidation peak,

meaning that the reaction is reversible. However in Ni5, Ni7.5 and Ni10 we can

see a weak or no oxidation peak. Another important point to be noticed is that

the difference peak potential is higher for Ni2.5 than for Ni0.

In image 10, we can see that all five samples resisted after 100 cycles.

16

0 1000 2000 3000 4000

20

0

-20

-40

-60

-80

-100i (m

A/c

m2)

E (mV vs. Ag/AgCl)

10cycles

20 cycles

30 cycles

40 cycles

50 cycles

60 cycles

70 cycles

80 cycles

90 cycles

100 cycles

(a) Ni0

0 1000 2000 3000 4000

10

0

-10

-20

-30

-40

-50

i (m

A/c

m2

)

E (mV vs. Ag/AgCl)

10 cycles

20 cycles

30 cycles

40 cycles

50 cycles

60 cycles

70 cycles

80 cycles

90 cycles

100 cycles

(b) Ni2,5

0 1000 2000 3000 4000

0

-2

-4

-6

-8

i (m

A/c

m2)

E (mV vs. Ag/AgCl)

10 cycles

20 cycles

30 cycles

40 cycles

50 cycles

60 cycles

70 cycles

80 cycles

90 cycles

100 cycles

(c) Ni5

0 1000 2000 3000 4000

0

-5

-10

-15

-20

-25

i (m

A/c

m2

)

E (mV vs. Ag/AgCl)

10 cycles

20 cycles

30 cycles

40 cycles

50 cycles

60 cycles

70 cycles

80 cycles

90 cycles

100 cycles

(d) Ni7,5

0 1000 2000 3000 4000

2

0

-2

-4

-6

-8

-10

-12

-14

i (m

A/c

m2

)

E (mV vs. Ag/AgCl)

10 cycles

20 cycles

30 cycles

40 cycles

50 cycles

60 cycles

70 cycles

80 cycles

90 cycles

100 cycles

(e) Ni10

Figure 10 - Voltammetric behaviour of antimony-doped tin oxide anode with different amounts

of Nickel after each 10 cycles, until 100 cycles [8].

8. PVB influence

Another try for co-doping was the Polyvinyl butyral (PVB), a polymer that

is supposed to improve the nanofilm morphology. As it is shown in figure 11,

adding PVB to the coating solution brought a great improve in terms of

morphology, since there is few cracks in the film with PVB.

17

Figure 11 SEM image of A. Sb doped Sn anode without PVB. B. Sb doped Sn anode with PVB.

On the other hand, when the cyclic voltametry was done, we can easily

realize that adding PVB we also reduce significantly the conductivity of the

electrode.

0 1000 2000 3000 4000

0

-400

-800

-1200

i (m

A/c

m2

)

E (mV vs. Ag/AgCl)

Sn-Sb-Ni-PVB

Sn-Sb-Ni

9. Lanthanum influence

Based in some references [7], using lanthanum as a co-doping element

would improve the efficiency of electrochemical degradation of organic

compounds, in other words it would increase the amount of phenol removed

from wastewater by the electrode.

The spincoating deposed sample made had a following composition,

obtained by EDS.

Figure 12 - Cyclic voltammogram comparing the influence of PVB.

18

Figure 13 A. EDS analysis for sample with La (B16). B. SEM image of sample with La (B16).

Analyzing the Cyclic Voltammogram for stability, we can realize that the

electrode with lanthanum not even lasted for 10 cycles (figure 14).

0 1000 2000 3000 40002

0

-2

-4

-6

-8

-10

-12

-14

i (m

A/c

m2

)

E (mV vs. Ag/AgCl)

Sn - 3,1% Sb - 6% La (B16) 1 cycle

10 cycles

Figure 14 - Cyclic voltammogram showing the behavior of B16 after 10 cycles.

This behavior can be due to too high amount of lanthanum present on

the nanofilm. Further tests with other amounts of lanthanum could not be

performed due to lack of time and because others elements were giving more

substantial results.

19

10. Iridium influence

According to some previous studies [9], iridium (IV) oxide, used as a

nanofilm, has a high stability and activity during the oxygen evolution reaction.

Indeed, it has been used in IrO2-based dimensionally stable anode (DSA) for

wastewater treatment.

As a first step a 2 layers-anode was prepared in a regular titanium foil

substrate. The coating solution was done by 0.2g of Dihydrogen hexachloro-

idrate (IV) hydrate (H2IrCl6 xH2O) in 5ml of 2-propanol (Iso-Propyl alcohol). By

cyclic voltammetric analysis we got the graph in figure 15.

0 1000 2000 3000 4000

0

-400

-800

-1200

-1600

i (m

A/c

m2

)

E (mV)

B32

10 cycles

20 cycles

30 cycles

100 cycles

Figure 15 - Cyclic voltammogram of B32 showing its behavior during 100 cycles.

The sample B25 (5 layers of SnOx (2g) + SbCl (0.1g) + NiCl (0.05g))

was the best sample we had so far, according to cyclic voltammograms (figure

16), galvanostatic oxidation experiment, determination of Chemical Oxygen

Demand (COD) and current efficiency made by another student in the

laboratory. If we compare B25 with B32, we can see that Iridium quietly

increases the current density; however it also has a lower oxygen evolution

potential, i.e. the oxygen evolution potential of B32 is around 1500mV, while on

B25 this value is around 2000mV.

20

0 1000 2000 3000 400010

0

-10

-20

-30

-40

-50

i (m

A/c

m2

)

E (mV vs. Ag/AgCl)

10 cycles

20 cycles

30 cycles

40 cycles

50 cycles

60 cycles

70 cycles

80 cycles

90 cycles

100 cycles

(b) Ni2,5

Figure 16 - Cyclic voltammogram of B25 showing its behavior during 100 cycles [8].

Aiming to join the high oxygen evolution potential of nickel-antimony

doped tin oxide with the high current density that iridium allows, a sample using

iridium as an interlayer between the titanium foil and Ni-Sb-Sn layers was done.

According to Comminellis [10], an IrO2 interlayer can be the solution for

the problem of low stability under anodic polarization that Ti/SnO2-SbCl3

anodes have. The high anodic stability and isomorphous structure with TiO2 and

SnO2 that IrO2 have would increase the anodes service life [10].

The cyclic voltammogram of B33 (2 bottom layers of IrO2 and 5 top

layers of nickel, antimony and tin oxide) can be seem in figure 17.

-200 0 200 400 600 8006

3

0

-3

-6

i (m

A/c

m2

)

E (mV)

200mV/s

100mV/s

50mV/s

25mV/s

B33

0 1000 2000 3000 4000

0

-400

-800

-1200

i (m

A/c

m2

)

E (mV)

B33

10 cycles

20 cycles

30 cycles

100 cycles

Figure 17 A. Cyclic voltammogram of B33 on Ferri/Ferro solution. B. Cyclic voltammogram of B33 showing its behavior during 100 cycles.

21

We can see that there are reduction and oxidation peaks, the current

density remained high and the lifetime is still good also. Nevertheless, the

oxygen evolution potential is being lowered by iridium influence.

In order to get rid of Iridium influence on oxygen evolution point,

remaining just the chemical stability that this element brings, samples with 2

iridium layers plus 8 Ni-Sb-Sn layers on top (B35), and 2 iridium layers plus 18

Ni-Sb-Sn layers on top (B36) were made keeping the same amount of iridium

and nickel, antimony and tin in each solution as previous samples. SEM images

and EDS analysis of B35 are shown in figure 18.

Element Weight% Atomic%

O K 38.53 81.44

Ti K 1.97 1.39

Ni K 1.11 0.64

Sn L 53.55 15.26

Sb L 4.15 1.15

Ir M 0.69 0.12

Totals 100.00

Figure 18 - EDS analysis and SEM image of B35

Can be noticed that even after 8 layers of Ni-Sb-Sn, there are still some iridium

and titanium on the surface of the anode. Cyclic voltammograms of B35 and

B36 are shown in figure 19.

22

-200 0 200 400 600 800

6

4

2

0

-2

-4

-6i (m

A/c

m2

)

E (mV)

200mVs

100mVs

50mVs

25mVs

B35

-200 0 200 400 600 800

6

4

2

0

-2

-4

-6

i (m

A/c

m2

)

E (mV)

200mV/s

100mV/s

50mV/s

25mV/s

0 1000 2000 3000 4000

0

-400

-800

-1200

-1600

i (m

A/c

m2)

E (mV)

B35

10 cycles

20 cycles

30 cycles

100 cycles

0 1000 2000 3000 4000

0

-200

-400

-600

-800

i (m

A/c

m2

)

E (mV)

B36

10 cycles

20 cycles

30 cycles

100 cycles

Figure 19 A. Cyclic voltammograms of B35 in Ferri/Ferro solution. B. Cyclic voltammograms of B35 during 100 cycles. C. Cyclic voltammograms of B36 in Ferri/Ferro solution. D. Cyclic

voltammograms of B36 during 100 cycles.

As it is demonstrated in the graphs, by adding 18 layers of tin oxide on

top of the iridium layers, it was possible to get rid of the influence of iridium on

oxygen evolution point, as on B36 it is almost 2000mV. On the other hand, it

made that the current density went down, as well as the stability. Further

experiment as galvanostatic oxidation, determination of COD, current efficiency

and actual phenol oxidation should be done to find out which sample is more

efficient and practicable. Samples have been sent to industry to practical

experiments.

A

B

C

D

23

11. Conclusion

This research aimed to prepare and characterize antimony doped tin

oxide nanostructured film by spin coating deposition. Several Sb doped SnO2

nanofilms were done with different concentrations and variations, as adding co-

doping elements as nickel, PVB, lanthanum and iridium.

With the support of various studies, searches, references and

experiments, we had noted that the amount of nickel as a co-doping strongly

influences the films morphology, reducing the quantity of cracks. It also seems

to improve materials stability, increasing its lifetime. However with amounts of

nickel equal or above 5 weight % relative to tin, it gets a reduction in terms of

chemical reaction, decreasing the anodes efficiency.

In experiments that were tried to co-dope with PVB, it became clear that

this polymer brings a great morphology improvement, but it leads in a drastic

reduction in the electrodes conductivity.

When co-doping with lanthanum was experienced, with the assumption

that it would upgrade electrodes electrical properties, it was realized that it

result in an extensive worsening of lifetime. It may be due of a too high amount

of lanthanum that was deposed on the substrate. Experiments with less

percentage of lanthanum may give more expressive results.

Even with the short period of time and amount of iridium that was

available for experiments, that was the element which the bests nanofilms were

done with. Using iridium as an interlayer brought a formidable stability and

conductivity for the anode. Further experiments have to be done, in order to

know ideal proportions and number of layers to have a better combination of

properties of tin, antimony, nickel and iridium. Some samples produced with

iridium as an interlayer were sent to industry to be tested in phenol oxidation

and to have evaluated their effectiveness.

24

12. References

[1] Ch. Comminellis and A. Nerini, Anodic oxidation of phenol in the presence of

NaCl for wastewater treatment J. Appl. Electro-chem. 25 (1995) 23-28.

[2] Waste Water Treatment Systems, [Accessed on August 1, 2014], Available at

http://www.nomura-nms.co.jp/english/product/02_01_09.html

[3] WANG Jian-gong, LI Xue-min, Electrochemical treatment of wastewater

containing chlorophenols using boron-doped diamond film electrodes, 2 J. Cent.

South Univ. (2012) 19: 1946-1952

[4] Wenfeng Shen, Properties of SnO2 based gas-sensing thin films prepared by

ink-jet printing, Sensors and Actuators B 166-167 (2012) 110-116

[5] Hao Xu, Wei Yan and Cheng Li Tang, A novel method to prepare metal oxide

electrode: Spin-coating with termal decomposition, Chinese Chemical Letters

22 (2011) 354-357.

[6] Hudin, Camille, Preparation and characterization of doped SnO2 film by

electrochemical deposition, Polytech Nantes / Centre for Advanced

Nanotechnology.

[7] Haiqind Xu, Ai-Ping Li, Qi Qi, Wei Jiang, and Yue-Ming Sun, Electrochemical

degradation of phenol on the La and Ru doped Ti/SnO2-Sb electrodes, Korean

J. Chem. Eng., 29(9), 1178-1186 (2012).

[8] Riou, Julie, Electrochemical characterization and treatment of organic

pollutants with mixed metal oxide anodes, ENSICAEN / Centre for Advanced

Nanotechnology.

[9] Stphane Fierro, and Christos Comninellis, Kinetic study of formic acid

oxidation on Ti/IrO2 electrodes prepared using the spin coating deposition

technique, Electrochimica Acta 55 (2010) 7067-7073.

[10] Carmem L.P.S. Zanta, Pierre-Alan Michaud, Christos Comninellis, Adalgisa

R. de Andrade, and Julien. F.C. Boodts, Electrochemical oxidation of p-

cholorophenol on SnO2-Sb2O5 based anodes for wastewater treatment, Journal

of Applied Electrochemistry 33: 1211-1215, 2003.

[11] Rutile Unit Cell, [Accessed on August 4, 2014], Available at

http://en.wikipedia.org/wiki/Rutile#mediaviewer/File:Rutile-unit-cell-3D-balls.png

25

Annex A About Centre for Advanced Technology

Canada's first centre for nanotechnology research, formed in September

1997 under the name The Energenius Centre for Advanced Nanotechnology

(ECAN) as a result of a generous donation fromEnergenius Inc., a Canadian

company dedicated to advancing nanotechnology research. As CAN's founding

member and supporter of the Energenius Chair in Advanced Nanotechnology

held by Professor Harry Ruda, Energenius entered into a strong partnership

with CAN in promoting the commercialization and spin-off of nanotechnology

advances to CAN and to the global market.

Strong industrial support, a team of world-leading research scientists and

state-of-the-art tools place CAN at the forefront for developing the key enabling

technologies, nanoelectronic and nanophotonic applications, in which

nanotechnology will make its first major impact - information technologies,

advanced manufacturing and advanced materials and processes.

CAN's mission:

o To provide visionary leadership in creating a solid, dynamic, multidisciplinary research and development infrastructure for Canada.

o To establish critical mass of principal investigators and facilities to enable us to perform internationally competitive research.

o To promote economic development in Ontario and in Canada, and to contribute to the training of highly-qualified personnel for careers in nanotechnology.

26

Appendix A Samples description

Sa

mp.

Con

c.

SnO

x [g

]

Con

c.

Sb2O

3 [g

]

Con

c.

SbC

l2 (

g)

Con

c.

NiC

l2.6

H2

0

(g)

Con

c.

LaC

l2

(g)

Con

c.

PVB

[g]

IrC

l6 (

g)H

CL

(mL)

IPA

volu

me

(mL)

Ethy

l

Vol

ume

(mL)

Tem

p

anne

al

(C

)

Tim

e

anne

al

(min

s)

Not

esSp

ingC

oati

ngED

X

Ato

mic

%SE

MO

bs

B1

2.00

00.

300

0.20

00.

500

500

30S

olu

tio

n w

as m

ad

e a

lread

y.

Etc

hin

g: 30 m

in

B2

2.00

00.

300

0.20

00.

500

500

30S

olu

tio

n w

as m

ad

e a

lread

y.

Etc

hin

g: 30 m

in

B3

2.00

00.

300

0.20

00.

500

500

30S

olu

tio

n w

as m

ad

e a

lread

y.

Etc

hin

g: 50 m

in (

2n

d t

ime u

sin

g)

20K

V, S

n, S

b, N

i.

no

t v

ery

un

ifo

rmS

am

e a

s B

1 a

nd

B2

B4

2.00

00.

108

0.00

00.

500

500

30S

olu

tio

n w

as m

ad

e a

lread

y.

Etc

hin

g: 50 m

in (

2n

d t

ime u

sin

g)

20K

V, S

n, S

b.

go

od

mo

rph

olo

gy

B5

1.00

00.

100

0.10

00.

250

5050

030

Etc

hin

g 3

0 m

in. S

olu

tio

n s

till n

ot

tota

lly

dis

olv

ed

20K

V, 40m

, T

i-36, S

n-

2.6

, S

b-0

.6, N

i-0

Bad

mo

rph

olo

gy

So

luti

on

mad

e w

ith

ou

t H

Cl.

B6

1.00

00.

100

0.10

00.

100

0.25

040

500

30

Etc

hin

g 3

0 m

in. S

olu

tio

n s

till n

ot

tota

lly

dis

olv

ed

20K

V, 40m

, T

i-6, S

n-1

6,

Sb

-0, N

i-2.2

no

t g

oo

d m

orp

ho

log

y,

Sb

2O

3 n

ot

dis

ov

ed

an

d

can

be s

een

.

So

luti

on

mad

e w

ith

ou

t H

Cl. S

bC

l

inste

ad

of

Sb

2O

3

B7

1.00

00.

100

0.10

00.

250

0.20

025

500

30

Etc

hin

g 2

0 m

in (

1st

tim

e).

So

luti

on

alm

ost

tota

lly

dis

olv

ed

Sp

in c

oati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

1 (

last

lay

er)

20K

V, 40m

, T

i-14, S

n-

32, S

b-1

.3, N

i-1

go

od

mo

rph

olo

gy

wit

h

so

me c

racks.

Fir

st

tim

e u

sin

g H

Cl to

dis

olv

e

Sb

2O

3. 5 lay

ers

of

co

ati

ng

B8

1.00

00.

100

0.10

00.

250

0.20

025

500

30

Etc

hin

g 2

0 m

in (

1st

tim

e).

So

luti

on

alm

ost

tota

lly

dis

olv

ed

Sp

in c

oati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 7

tim

es p

lus P

rog

ram

1 (

last

lay

er)

10K

V, 40m

, T

i-0.5

, S

n-

15, S

b-3

.1, N

i-2.6

, O

-78

go

od

mo

rph

olo

gy

wit

h

so

me c

racks.

Rep

eat

B7, h

ow

ev

er

8 lay

ers

of

co

ati

ng

.

B9

2.00

00.

100

0.00

00.

000

0.00

00.

200

2550

0p

rogr

am

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

30K

V, 1

,

Ti-

22

.3,

Sn-

4.1

, Sb

-0.3

, O

-72

.6

Th

e p

rog

ram

fo

r th

e last

lay

er

was

ch

an

ged

, slo

w h

eati

ng

. (p

rog

ram

2)

B10

2.00

00.

000

0.20

00.

000

0.00

00.

000

2550

0p

rogr

am

2

Sp

in c

oati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

30K

V, 40

, T

i-3

4.6

, Sn

-

5.4

, Ni-

0.6

, O-5

8.7

May

be s

olu

tio

n v

ery

thin

, n

ot

co

ver

well

Pro

gra

m 2

.

B11

2.00

00.

000

0.00

00.

200

0.00

00.

000

2550

0p

rogr

am

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

15K

V, 6

,

Ti-

14

.6,

Sn-

17

.2,

La-

0,

O-6

7.5

Pro

gra

m 2

B12

2.00

00.

100

0.10

00.

000

0.00

00.

200

2550

0p

rogr

am

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

B9 p

lus N

i-0.1

g

B13

2.00

00.

100

0.20

00.

000

0.00

00.

200

2550

0p

rogr

am

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

B10 p

lus S

b-0

.1g

an

d H

Cl-

0.2

ml

B14

2.00

00.

100

0.00

00.

400

0.00

00.

200

2550

0p

rogr

am

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

B11 p

lus S

b-0

.1g

, L

a-0

.2g

an

d H

Cl-

0.2

ml

No

t g

oo

d s

am

ple

s (

may

be t

o m

uch

etc

hin

g)

Sp

in c

oati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

1 (

last

lay

er)

Sp

in c

oati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

1 (

last

lay

er)

Prog

ram

1-A

nnel

: 25C

- t

o 10

0C f

or 1

0min

s, u

sing

40

min

s in

crea

to

500C

for

30

min

s, t

urn

off

the

pow

er a

nd c

oolin

g do

wn

natr

uly.

Tak

e ou

t th

e sa

mpl

e on

nex

t da

y.

Spin

gCo

atin

g Sn

-Sb

-O2

on

Ti f

oil

Subs

trat

e: T

i Foi

l-1

0.03

2mm

(0.

0013

in)

thic

k, f

rom

Alf

aSea

r; T

i Foi

l-2:

0.1

27m

m /

0.0

05",

fro

m M

cMas

ter-

Car

r.

Sp

in c

oati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

1 (

last

lay

er)

30K

V

on

ly S

n, n

o S

b.

Bad

mo

rph

olo

gy

27

B

152

.00

00

.10

00

.00

00

.00

00

.00

00

.00

025

50

0p

rogr

am

2

Sp

in c

oati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

Sb

Cl3

dis

so

lved

very

easy

.

B16

2.0

00

0.0

00

0.1

00

0.0

00

0.2

00

0.0

00

0.0

00

10

50

0p

rogr

am

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

B15 p

lus L

a-0

.2g

B17

2.0

00

0.0

00

0.1

00

0.1

00

0.0

00

0.0

00

0.0

00

10

50

0p

rogr

am

2

Sp

in c

oati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

B15 p

lus N

i-0.1

g

B18

2.0

00

0.0

00

0.1

00

0.1

00

0.2

00

0.0

00

0.0

00

10

50

0p

rogr

am

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

So

luti

on

mad

e a

dd

ing

B16 t

o B

17

B19

2.0

00

0.1

00

0.1

00

25

50

0p

rogr

am

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

Sam

e s

olu

tio

n a

s B

15, p

lus N

i;

Sam

e s

olu

tio

n a

s B

12 b

ut

Sb

Cl2

inste

ad

of

Sb

2O

3

B20

0.8

00

0.0

40

0.0

40

0.0

80

10

50

0p

rogr

am

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

B19 p

lus P

VB

B21

2.0

00

0.1

00

0.2

00

25

50

0p

rogr

am

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

B22

2.0

00

0.1

00

0.2

00

0.2

00

25

50

0p

rogr

am

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

do

no

t d

isso

lve (

PV

B)

/ sp

in-

co

ati

ng

no

t d

on

e

B23

2.0

00

0.1

00

0.1

50

25

50

0p

rogr

am

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

B21 c

on

du

cti

vit

y w

as b

ad

, so

pu

t

less N

i

B24

2.0

00

0.1

00

0.1

50

0.2

00

25

50

0p

rogr

am

2

Sp

in c

oati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

PV

B n

ot

dis

so

lved

/ p

rob

ab

ly

reach

ed

Gla

ss T

ran

sit

ion

Tem

pera

ture

~70C

/ s

pin

-co

ati

ng

no

t d

on

e

B25

2.0

00

0.1

00

0.0

50

25

50

0p

rogr

am

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

Ni-0

less N

i

B26

2.0

00

0.1

00

0.0

40

25

50

0p

rogr

am

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

La-0

less L

a (

1,2

%)

28

B2

72

.00

00

.05

00

.05

025

50

0p

rog

ram

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

B25 w

ith

less a

nto

mo

ny

B2

82

.00

00

.05

00

.05

025

50

0p

rog

ram

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

B25 w

ith

less a

nto

mo

ny

an

d m

ore

La.

B2

92

.00

00

.10

00

.10

025

50

0p

rog

ram

2

Sp

in c

oati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

B19 r

ep

eate

d -

dif

fere

nt

so

luti

on

B3

02

.00

00

.10

00

.10

025

50

0p

rog

ram

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

B19 e

letr

od

ep

osit

ion

befo

re

sp

inco

ati

ng

B3

12

.00

00

.10

00

.10

025

50

0p

rog

ram

2

Sp

in c

oati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

B29 r

ep

eate

d -

sam

e s

olu

tio

n

B3

20

.20

05

.00

05

00

pro

gra

m 2

Sp

in c

oati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

just

Ir w

ith

IP

A

B3

3

(fir

st 2

laye

rs)

0.2

00

5.0

00

50

0p

rog

ram

2

Sp

in c

oati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 2

tim

es.

firs

t 2 lay

ers

ju

st

Ir.

B3

3 (

last

5 la

yers

)

2.0

00

0.1

00

0.0

50

25

50

0p

rog

ram

2

Sp

in c

oati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

5 lay

ers

aft

er

the f

irst

2 lay

ers

of

Ir.

Sam

e r

eceip

t as B

25

B3

4

(fir

st 2

laye

rs)

0.2

00

5.0

00

50

0p

rog

ram

2

Sp

in c

oati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 2

tim

es.

firs

t 2 lay

ers

ju

st

Ir.

B3

4 (

last

5 la

yers

)

2.0

00

0.1

00

0.0

25

25

50

0p

rog

ram

2

Sp

in c

oati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 4

tim

es p

lus P

rog

ram

2 (

last

lay

er)

5 lay

ers

aft

er

the f

irst

2 lay

ers

of

Ir.

B33 b

ut

wit

h h

alf

NiC

l.

B3

5

(fir

st 2

laye

rs)

0.2

00

5.0

00

50

0p

rog

ram

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 2

tim

es.

firs

t 2 lay

ers

ju

st

Ir.

B3

5 (

last

8 la

yers

)

2.0

00

0.1

00

0.0

50

25

50

0p

rog

ram

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 7

tim

es p

lus P

rog

ram

2 (

last

lay

er)

8 lay

ers

aft

er

the f

irst

2 lay

ers

of

Ir.

Sam

e s

olu

tio

n a

s B

33

B3

6

(fir

st 2

laye

rs)

0.2

00

5.0

00

50

0p

rog

ram

2S

pin

co

ati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 2

tim

es.

firs

t 2 lay

ers

ju

st

Ir.

B3

6 (

last

18

laye

rs)

2.0

00

0.1

00

0.0

50

25

50

0p

rog

ram

2

Sp

in c

oati

ng

, d

ried

du

rin

g 1

0 m

inu

tes a

t

100C

+500C

du

rin

g 1

0 m

in. R

ep

eate

d 1

7

tim

es p

lus P

rog

ram

2 (

last

lay

er)

18 lay

ers

aft

er

the f

irst

2 lay

ers

of

Ir. S

am

e s

olu

tio

n a

s B

33

29

Appendix B Activities timetable

Timetable

Activity Week

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15

Safety training

Learning activities and experiments

Making samples

Researching

SEM, EDS analysis

Voltammetric analysis

Brian Martins Ilkiw Centre for Advanced Nanotechnology

Supervisor: Bin Bin Li 2014 Summer Research - University of Toronto