Internship Report:

Fundamental characterization and

application of porous carbons

From 29th May to 20th August 2017 at Okayama University

Lejeune Eglantine,

MAT 3, Polytech Grenoble

Year 2016/2017

Tome Principal et

Annexes

1

Table of content:

Special thanks ............................................................................................................................. 2

Introduction: ................................................................................................................................ 3

I. Internship presentation ................................................................................................... 3

II. Devices used for fundamental characterization ........................................................... 4

1) Raman spectroscopy ......................................................................................................... 4

2) TG DTA .............................................................................................................................. 5

3) XRD ................................................................................................................................... 6

4) Gas Adsorption .................................................................................................................. 6

5) Identification test, example of fundamental characterization ............................................ 8

III. Studying of structural effects to the specific reaction of metal complex adsorbed on

porous carbons ........................................................................................................................... 8

1) Fundamental characterization of W10 and W15 ............................................................... 9

2) Study the effect of pore geometry and/or surface chemistry ........................................... 11

IV. Feedbacks of internship ................................................................................................ 13

Conclusion: ................................................................................................................................ 13

Glossary: .................................................................................................................................... 14

Bibliography: ............................................................................................................................. 14

Picture’s origins ........................................................................................................................ 15

Annexes : ................................................................................................................................... 16

2

Special thanks

I would like to thanks all the people who help me during this internship and contributed

in my internship success and to lead me for enjoy my travel in Japan.

I want to thanks my professor, Professor Ohkubo who helped me so much before and

during my internship; who spent a lot of time to help me to understand my subject, and

has been understanding with me. I am grateful to him for welcoming me at the airport

and took time to guide me.

I want to thanks all the members of my team for their help and the advice, to have teach

me a lot of things about Japanese culture. I would like to thank all of you for trying to

speak in English with me even if it was hard.

I wish to thanks Mss. Okamura Wakana, Mss. Hirano Yuri, M. Suwannarat Kamon and

M. Nanjyo Tsubasa to have spent time with me for lunch, for the advice they gave me

and for helping me to communicate with the team by translating.

I would like to thanks M. Chenevier who sent to my school the opportunity for student to

come in Japan and also for the welcome party he made for us and for having invite us to

European event.

I would like to thanks my french teacher Pr. Holger Klein who answered to my mails and

followed the proceedings of my internship.

I also want to thanks all the people off Global Partner and Kuwanoki dormitory to help

me as they could without English/Japanese translator.

Many thanks to L-Café who gave me the opportunity to meet a lot of new people and to

learn Japanese language, improve my English skills and help some student to learn

French.

I want to thanks all the student managers of my dormitory for their help for their time in

discussions with me and for organizing a lot of events to allow all the members of

dormitory to meet each other.

Thanks to all my new friends, met here in Japan.

ありがと ございます

3

Introduction:

For the end of my third year of studies and for my first year at Polytech Grenoble, I had

to make an internship of 12 weeks outside of France. Thanks to M. Chenevier and the

international relationship of my school I went into Japan, at Okayama University to do

this internship. My supervisors were Professor Ohkubo Takahiro into Japan and

Professor Holger Klein in France. The internship take place from 29th of May to 20th

august, the initial subject was “Fundamental characterization and application of porous

carbons”.

The first period of my 3-month internship consisted in reading scientific articles about the

initial subject, the latest study of the team and understanding the fundamental techniques

of characterization used for porous carbons. I learnt how to use Raman spectroscopy,

XRD, TG-DTA and Gas Adsorption. After the test of black powders identification, I start

to work on the subject of “Elucidation of structural effects to the specific reaction of

copper acetate adsorbed on porous carbons” by using porous carbon.

I. Internship presentation

＊ Okayama University:

At the beginning the Okayama University was a medical training place sponsored

by the lord of Okayama and founded in 1870. It has evolved to become an official

place to medicine school, the Okayama Medical College, in 1922. From this time,

new faculties had been built around the school. Okayama University became a

national university in 1949. Since 2004, Okayama University enjoys the reputation

of being one of Japan’s leading universities.

Okayama Tsushima campus is the main of the 3 campus of this university, it is

located near downtown Okayama City. The university have 271 different university

partnership in 40 different countries, especially into Asia. From 1870 to 2016, this

university received more than 600 international students.

＊ The internship takes place under the tutelage of Professor Takahiro Ohkubo, from

29th May to 20th August at Okayama University, in the department of inorganic

chemistry. The subject is “the fundamental characterization and application of porous

carbons”, the aim is to furnish some data which can be useful for the research project:

“Elucidation of structural effects to the specific reaction of metal complex adsorbed

on carbons”; it can help some other student in their research project. That mean, I

had to do the fundamental characterization of new kinds of porous carbons and to

4

try to make the specific reaction of metal complex adsorbed on these carbons. The

results should be used to work on the structural effects and especially on the pore

size on the reaction of metal complex adsorption.

II. Devices used for fundamental characterization

1) Raman spectroscopy

This type of spectroscopy is similar to IR spectroscopy but here we look for intensity

of an inelastic scattering of light. Raman spectroscopy identifies changes in the

polarizability of the molecule, which induce a change into the molecule dipole and so

into the cloud of electron around the atoms of the material molecules studied. The

phenomenon is illustrated on figure 1.

Figure 1: Illustration of change of polarizability for water molecule. [1]

For carbon material we can distinguish specifics bands:

RBM (Radial Breathing Mode)

It should be at a wavenumber inferior at 200 cm-1. It represents the movement of

carbon atom in radial direction which is the contraction and expansion of nanotube;

as you can see on figure 2. This peak is specific to nanotube; with this one we can

obtain the nanotube diameter with the following equations

For Single Walled Carbon Nanotube (SWNT): D = 248

𝜔 with D in nm and 𝜔 in cm-1

5

For Double Walled Carbon Nanotube (DWMT): D = 234

𝜔 + 10 with D in nm and 𝜔 in

cm-1; 10 represent the interaction between the tubes.

D Band

This peak represents the disorder in the system. It should be at around 1300 cm-1.

G band

This peak correspond to the carbon atoms which are moving in the plan (planar

vibration), so in opposite direction of the RBM vibration. That is similar to the vibration

of carbon atoms at the surface of the sample as shown on figure 2. This band can

be seen around 1600 cm-1.

D’/G’ band

It represents the second induced disorder at around 2600 cm-1.

Figure 2: Illustration of carbon atom movement on nanotube for

G and RBM band. [2]

A spectra obtain by Raman spectroscopy

on carbon nanotube seem like that:

Figure 3: Example of Raman spectroscopy on carbon nanotube. [3]

2) TG DTA

This device submits an inert reference and the studied materials under identical

predetermined thermal cycles. After the measurement we deduce the changes

measured on the reference at those of the sample measure. We obtain the variation of

temperature, DTA and TG with time. DTA represent the amount of energy consume by

the chemical reaction, TG represent the variation of relative mass of the sample

We can use those data to obtain the purity and humidity of the studied sample because

we can see all the reaction which take place on the sample as water boiling,

decomposition of impurity…

6

3) XRD

This method is used to make a primary analysis of crystalline structure. It sends a beam

of X ray which strikes a crystal, producing a scattering beams.

These X-rays are generated by a cathode ray tube, filtered to produce monochromatic

radiation, collimated to concentrate, and directed toward the sample. The interaction of

the incident rays with the sample produces constructive interference (and a diffracted

ray) when conditions satisfy Bragg's Law (nλ=2d sin θ), there is a peak.

The peak intensity is determined by the distribution of atoms within the lattice.

Consequently, the X-ray diffraction pattern is the fingerprint of the periodic atomic

arrangements in a given material that mean the crystalline structure.

We can use it to identify graphite because graphite had a specific peak at 2θ = 26.5

degree, but we can also use it to identified crystalline structure like Cu2O.

4) Gas Adsorption

On a porous sample it is possible to measure the porous surface, pore size, their

distribution and their volume, and the porosity of it; for that, we use the gas adsorption

spectroscopy.

The adsorption means the enrichment of molecules, atoms or ions in the vicinity of an

interface. Here we speak about a solid/gas interface which fill the micro, meso and macro

pores of solid sample.

This device is based on a measurement of gas pressure in a calibrated and known gas

volume at a known constant temperature. An amount of pure gas is confined in a volume

containing the adsorbent, as adsorption take place, the pressure in the confined volume

falls until equilibrium is established. The adsorption isotherm is constructed by

successive charges of gas adsorbent. Most of the time, the result of the measurement is

presented as the amount adsorbed in function of the equilibrium relative pressure P/P0

(where P0 is the saturation pressure measured throughout the entire analysis by a

pressure transducer). The IUPAC have grouped the physisorption isotherm into 6 types,

represented into figure 4.

7

Figure 4: Classification of physisorption isotherms according to IUPAC classification of 1985. [4]

The number I correspond to a microporous solid, II is a nonporous material or macro

porous adsorbent, III is a material where the interaction between adsorbent and

adsorbate are weak so it is no identifiable with this device, IV is a mesoporous adsorbent,

V is similar to the III with weak adsorbent/adsorbate interaction it is assimilate to

hydrophobic micro or mesoporous adsorbents, the VI is typical of am adsorption of layer

by layer on a non-porous surface

I will apply the ∝-s method, which can be used to determine the pore surface, volume

and size. The reference isotherm in this method is a plot of the amount of gas adsorbed,

normalized by the amount of gas adsorbed at a fixed relative pressure, versus P/P0. The

referenced relative pressure is usually P/P0=0.4, and the normalized term Vads/Vads0.4 is

∝-s. The ∝-s plot is obtained by plotting the volume of gas adsorbed by a test sample

versus ∝-s in the same way as one produces a “t plot”. The estimation of micropore

volume from an ∝-s plot involves extrapolation of the plots to the Y axis since the ∝-s

method does not assume any value for the thickness of an adsorbed layer; the

calculation of the surface area is accomplished by relating the slope of the ∝-s plot of

the test sample to the slope of the corresponding plot for a standard sample of known

surface area. An illustration of this method is given on figure 5.

8

0

0,2

0,4

0,6

0,8

100 600 1100 1600 2100 2600

Inte

nsi

ty (

a.u

)

Raman shift (cm^-1)

Raman sample 4

Figure 5: Illustration of ∝s method with extrapolation of the curve. [5]

5) Identification test, example of fundamental characterization

Here, in order to check my knowledge, the students give to me 6 samples with just

number on it and I had to discover what kind of “black powder” it was.

First I use Raman spectroscopy to know what kind of carbon it could be. In this way I find

the 2 SWCNT and 2 activated carbons. I use the gas adsorption spectroscopy to identify

the activated carbon. I found which one are A7 and A20. I use XRD to check if there was

graphite, I find one. After measurement I deduce the last one was MWCNT.

For example, on the following result, we can deduce that sample 3 is SWCNT and

sample 4 is AC because they had specific peaks (RBM for sample 3 for example).

Figure 6: Example of Raman analysis with typical peak of SWCNT (left) and AC (right).

III. Studying of structural effects to the specific reaction of

metal complex adsorbed on porous carbons

0

5

10

15

0 500 1000 1500 2000 2500 3000 3500

Inte

nsi

ty (

a.u

)

Raman shift (cm^-1)

Raman sample 3

9

Professor Ohkubo and his lab team reported the possibility to synthesize Cu2O

nanoparticles with the photoreduction process of copper acetate adsorbed on SWCNT

under visible light irradiated condition. This photoreduction could be initiated by the

distortion of copper acetate confined in the narrow pores of SWCNT, we could also use

other kind of microporous carbons like activated carbons. This proceed involve a new

notion which is the “carbon catalysis”. In this part I had to do some research about the

dependence of the pore structure and also the amount of surface functional group with

the photoreduction of copper acetate.

1) Fundamental characterization of W10 and W15

Here I had used the W10 and W15 which are new type of AC never used before into the

lab, usually they use microporous carbons. These ACs should be mesoporous ones, first

I had to do the fundamental characterization of these samples by using Raman

spectroscopy (to check if it is AC or graphite and deduce the crystallinity of sample by

using D/G ratio), gas adsorption spectroscopy, elemental analysis and TG-DTA.

I start with Raman analysis in order to check what kind of “black powder” can be the W10

and W15 samples. The spectroscopy results have typical peaks of activated carbon

materials (D and G bands), as you can see on figure 7.

Figure 7: Raman Analysis of W10 and W15 samples.

I made a TG-DTA analysis, done the same day than an elemental analysis. So, we have

the amount of surface functional groups and the average humidity of the sample. The

results obtained are presented on the tables above.

0,20,220,240,260,28

0,30,320,340,360,38

0,40,42

0 1000 2000 3000

Inte

nsi

ty(a

;u)

Raman shift (cm^-1)

W10

0,2

0,22

0,24

0,26

0,28

0,3

0,32

0,34

0 500 1000 1500 2000 2500

Inte

nsi

ty(a

;u)

Raman shift (cm^-1)

W15

10

C (%) H (%) N (%) O (%) Average humidity (%)

85.725 1.870 0 12.504 13.98

Table 1: Results of W10 elemental analysis and TG-DTA humidity obtained.

C% H% N% O% Average humidity (%)

86.065 1.695 0 12.240 14.75

Table 2: Results of W15 elemental analysis and TG-DTA humidity obtained.

As you can see, on the elemental analysis, the mesoporous sample have naturally

adsorbed a lot of oxygen, in addition to water.

I have done a gas adsorption analysis in order to characterize the porosity of this new

samples of porous carbons. The curve results has an unusual shape, very different from

the one of A7 or A20, so more difficult to analyze.

Figure 8 : Gaz adsorption αs analysis on W10 and W15.

The results of α-s analysis are presented on the table 3 for W10 and table 4 for W15.

Table 3: Results of αs analysis of gas adsorption spectroscopy for W10.

total micro meso

Surface (m^2 g^-1) 1024 759 265 W10 average pore size (m)

Volume (cm^3" g-1) 0.520 0.283 0.237 7.44319E-10

y = 548,3x

y = 231,02x + 216,24

050

100150200250300350400450500550600

0 0,5 1 1,5 2

amo

un

t ad

sorb

edm

g g

-1

αs

Gas adsorption on W15

y = 478.47x

y = 123,63x + 228,06

0

50

100

150

200

250

300

350

400

450

500

0 0,5 1 1,5 2

amo

un

t ad

sorb

edm

g g

-1

αs

Gas adsorption on W10

11

Table 4: Results of αs analysis of gas adsorption spectroscopy for W15.

If we compare these result with the one’s of A7 and A20 (Annex 2) we can see with total

surface and volume result that, the one with more porous surface is A20 and W15 is the

one with the more porous volume. Moreover, results exploitation with α-s method indicate

that the W samples have more meso surface and volume than A samples. W15 has twice

more meso surface and volume than W10. I obtain a pore size of 0.74 nm for W10 and

0.79 nm for W15. We also check the pore size distribution which are presented on Annex

1. The analysis of amount adsorbed with relative pressure confirm that samples are

typically mesoporous ones; because W10 and 15 show the IV shape of the classification

of physisorption isotherms according to IUPAC classification (figure 5).

These new AC have properties very different from the ones of A7 and A20, because A7

and A20 are micro porous AC, those ones are mesoporous ones. So these differences

can have an impact on the adsorption of copper and on the synthesis of Cu2O by using

carbon.

2) Study the effect of pore geometry and/or surface chemistry

Here the goal is to allow the students who are working on this subject to have more data

and to potentially open new horizon of study for Professor Ohkubo team.

The photoreduction process had been applied on W10 and W15, adsorbed with a

solution of copper acetate (0.26 mol/L), using vacuum line. The carbons obtained after

the process have been analyzed with XRD in order to check if W10 and W15 can be

used to obtain Cu2O. The results of XRD analysis are presented on the figure 10 and

compared to the ones obtained with A7 (result similar to A20 one).

On the left of figure 9, that is the global result of XRD analysis, on the right you can see

that all the samples have the specific peak of Cu2O, that confirm W10 and W15 can be

used to obtained Cu2O, as it has been done with A7 and A20. The peaks presented

aren’t present on W10, A7 and W15 without adsorption treatment (Annex 3).

total micro meso

Surface (m^2 g^-1) 1173 679 494 W15 average pore size (m)

Volume (cm^3" g-1) 0.738 0.268 0.470 7.89E-10

12

Figure 9: XRD analysis of adsorbed porous carbons after photoreduction process.

To check the adsorption capacity of the mesoporous carbons, I made an adsorption with

copper acetate and I titrate the amount of adsorbed copper adsorbed; with a solution of

2Na-EDTA and a colored indicator; on W10, W15, A7 and A20. The results obtained are

presented on the table 5.

Name Concentration

decreasing (mol/L)

Adsorbed copper

amount (mol)

Ratio adsorbed copper on

carbon mass(mol/g-1)

W10 9.23*10^-3 4.62*10^-5 0.895*10^-3

W15 14.04*10^-3 7.02*10^-5 1.304*10^-3

A7 10.92*10^-3 5.46*10^-5 1.06*10^-3

A20 18.72*10^-3 9.36*10^-5 1.78*10^-3

Table 5: Amount of adsorbed copper on W10, W15, A7 and A20.

Figure 10: Graphic of adsorbed amount of copper for carbon mass on porous carbon

0,0E+002,0E-044,0E-046,0E-048,0E-041,0E-031,2E-031,4E-031,6E-031,8E-032,0E-03

Ad

sorb

ed c

op

per

am

ou

nt

for

carb

on

mas

s (m

ol/

g)

Adsorbed amount of copper for carbon mass

on porous carbons

W10

W15

A7

A20

0

2000

4000

6000

8000

0 20 40 60 80

Inte

nsi

ty (

a.u

)

2θ (degree)

Photoreduction results

A7-

Cu2OW15-

Cu2OW10-

Cu2O

0

50

100

150

200

250

300

20 30 40 50

Inte

nsi

ty (

a;u

)

2θ (degree)

Photoreduction results

A7-

Cu2OW15-

Cu2OW10-

Cu2O

13

The W carbons have a capacity of adsorption very close from the one of A carbon,

instead of the difference of porosity. Globally, A20 is the best porous carbon to adsorb

copper. For me the porous surface influent the adsorption capacity because the capacity

of adsorption

IV. Feedbacks of internship

This internship allowed me to discover a new way of study, to discover how the Japanese

universities work and how does the students make experiments. I spoke with the

students about the safety into the lab and I saw that our notions about this were different

but finally I adapted my experimentation conditions to their laboratory.

I had some difficulties to understand clearly what was the aim of my internship and how

would the results be used.

I wished that I would be able to make several measurements in order to give average

results, obtained by making some statistics, but I had to considerer that my only result

reflect the fundamental properties of my sample, because I didn’t have enough time.

I also want to talk about the English speaking, the students don’t really want to speak

English because they are very shy or they believe they have bad English skills. But

everyone really tried to speak with me and, there are some students in the group who

translated from Japanese to English often for the rest of the team. But in general, people

understand me when I ask for somethings or if they can help me when I had problem.

All the Monday mornings the students made some presentations about scientific articles

or about their results. The problem was that those presentations were in Japanese,

sometime some students done them in English but the questions were in Japanese. Most

of the time I didn’t understand.

Conclusion:

The conclusion of the experiment is that, the type of porosity doesn’t seem to have a big

influence on the adsorption result and on the synthetize of Cu2O nanoparticles. But the

total porous surface or porous volume seem to have an influence on the result. Also the

difference observed on XRD analysis results is a field to explore because W10 show a

large area instead the other have very different profile.

This internship allowed me to discover some apparatus I didn’t know before. The

knowledge from my previous studies have been very useful for me.

14

This internship has been a good opportunity to test my English skills and improve it. By

travelling outside France and practicing my English, I get more confident in myself and

in my capacity. Thanks to that experience in Japan I really understand the importance of

the hierarchy and how to communicate with different “rank”.

Glossary:

SWCNT or SWNT: single walled carbon nanotube

DWCNT or DWNT: Double walled carbon nanotube

MWCNT or MWNT: Multi walled carbon nanotube

AC: activated carbon

W10, W15, A7, A20 sample reference

IUPAC International Union of Pure Applied Chemistry

DTA: Differential thermal analysis

TG: Thermogravimetric

XRD: X Ray Diffraction

Bibliography:

“Adsorption and diffusion in nanoporous materials” by Rolando M.A. Roque-Malherbe;

2007 on CRC Press Taylor and Francis Group. Support imprimé, livre

“Nanoporous materials: Science and engineering” by G.Q. Lu and X.S. Zhao; 2004 on

Imperial College Press (ICP). Support imprimé, livre.

“Characterization of porous solids and powders: surface area, pore size and density” by S.

Lowell, Joan E. Shields, Martin A. Thomas and Matthias Thommes; 2004 on Kluwer

Academic Publishers – Springer. Support, livre

” Physisorption of gases, with special reference to the evaluation area and pore size

distribution (IUPAC Technical Report)" by Matthias Thommes, Katsumi Kaneko, Alexander

V. Neimark, James P. Olivier, Francisco Rodrigez-Reinoso, Jean Rouquerol and Kenneth

S.W. Sing; 2015 on DE GRUYTER IUPAC Technical report.

“Nanospace-enhqnced photoreduction for the synthesis of copper(I) oxide nanoparticles

under visible-light irradiation” by Takahiro Ohkubo, Mitsushiro Ushio, Koki Urita, Isamu

Moriguchi, Bashir Ahmmad, Atsushi Itadani and Yasushige Kuroda; February 2014 on

Elsevier edition and science direct.

“Evaluating the characteristics of multiwall carbon nanotubes » by J.H.Lehman, M.

Terrones, E. Mansfield, K.E. Murst, V. Meunier; March 2011 on Elsevier edition and

Science Direct.

15

“Raman and TGA study of carbon nanotubes synthesized over Mo/Fe catalyst on

aluminum oxide, calcium carbonate and magnesium oxide support”, by Ezekiel Dixon Dikio,

Ntaote David Shooto, Force Tefo Thema and Abdullahi Mohamed Faral; February 2013 on

Chemical Science Transactions.

“Assymetric hydration structure around calcium ion restricted in micropores fabricated in

activated carbons” by Takahiro Ohkubo, Tomoko Kusudo and Yasushige Kuroda;

September 2016 on IOP Science publishing.

“Experimental information on the absorbed phase of water formed in the inner pore of

single walled carbon nanotube itself” by Masayasu Nishi, Takahiro Okhubo, Koki Urita,

Isamu Moriguchi and Yasushige Kuroda; 2016 on LANGMUIR.

“Highly compressed nanosolution restricted in cylindrical carbon nano spacest” by

Masayasu Nishi, Takahiro Ohkubo, Kazuma Tsurusaki, Atsushi Itadani, Bashir Ahmmad,

Koki Urita、Isamu Moriguchi, Shigeharu Kittaka and Yasushige Kuroda; 2013 on RSC

Publishing Nanoscale.

” Actual Structure of dissolved zinc ion restricted in less than 1 nanometer micropores of

carbon” by Takahiro Ohkubo, Masayasu Nishi, Yasushige Kuroda; 2011 in The journal of

Physical Chemistry.

“Water initiated ordering around a copperion of copper acetate confined in slit-shaped

carbon micropores” by Takahiro Ohkubo, Yutaro Tahehara, Yasushige Kuroda; 2011 on

Elsevier edition.

”Pratical group theory and Raman spectroscopy, Part I : Normal vivrational modes” by

David Tuschel; 2014 on Spectroscopy

“Characterization of carbon nanotubes by Raman Spectroscopy” by S. Costa, E. Borowiak-

Palen, M. Kruszynska, A. Bachmatiuk, R.J. Kalenczuk; 2008 on Material science.

“Novel adsorbent synthesis, diffusion in nanoporous materials, and adsorption system

optimization” by Thomas Grant Glover; 2008.

“Purity and defect characterization of Single alled Carbon Nanotubes using Raman

Spectroscopy”; Y. Miyata, K. Mizuro, H. Kataura; 2011.

Picture’s origins [1] https://www.slideshare.net/krishslide/raman-spectroscopy-39462565

[2] http://www.annualreviews.org/doi/pdf/10.1146/annurev-conmatphys-070909-103919

[3] https://en.wikipedia.org/wiki/Optical_properties_of_carbon_nanotubes

[4] https://www.researchgate.net/figure/263052423_fig8_Figure-11-Six-types-of-gas-

physisorption-isotherms-Reprinted-with-permission-from

16

[5] http://etd.library.vanderbilt.edu/available/etd-03282008-

110032/unrestricted/Glover_TG_Thesis.pdf#search=%272.14+gas+adsorption+alpha+s+metho

d%27

From figure 6 to 10 it is my own results.

Annexes :

Annex 1

Annex 2

0

0,01

0,02

0,03

0,04

0,05

0 2 4 6 8 10 12 14 16 18 20

Pro

bab

ilit

y

Pore size (A)

W15 pore size distribution

0

0,005

0,01

0,015

0,02

0,025

0,03

0,035

0,04

0,045

0 2 4 6 8 10 12 14 16 18 20 22

Pro

bab

ilit

y

Pore size (A)

W10 pore size distribution

17

0

200

400

600

800

20 25 30 35 40

Inte

nsi

ty (

a.u

)

2θ (degree)

W10 before and after

photoreduction

W10

W10-

Cu2O

Annex 3

A7 total micro meso

Surface 1027.542 1.02E+03 1.05E+01 pore size (m)

Volume 0.348017 0.33689 0.011127 6.62E-10

A20 total micro meso

Surface 1517.367 1.49E+03 3.03E+01 pore size (m)

Volume 0.610866 0.577621 0.033245 7.77E-10

0

1000

2000

3000

4000

5000

6000

0 20 40 60 80

Inte

nsi

ty (

a.u

)

2θ (degree)

W10 before and after

photoreduction

0

500

1000

1500

2000

2500

3000

0 20 40 60 80

Inte

nsi

ty (

a.u

)

2θ (degree)

W15 before and after

photoreduction

0

50

100

150

200

20 25 30 35 40

Inte

nsi

ty (

a.u

)

2θ(degree)

W15 before and after

photoreduction

W15

W15-

Cu2O

18

Student : LEJEUNE Eglantine MAT 3

2016-2017

Company: Okayama University

Address: 3-1-1 Tsushima-naka, Kita-ku,

Okayama 700-8530 Japan

Telephone : +81-86-252-1111

Internship tutor: Pr. Ohkubo Takahiro

Telephone : +81-(0)86-251-7843

Mail address: ohkubo@okayama-u.ac.jp

Referent teacher : Pr. Klein Holger

Telephone : +33 (0)4 76 88 79 41

Mail address: holger.klein@neel.cnrs.fr

Title: “Fundamental characterization and application of porous carbons “

Summary:

The internship take place into the inorganic chemistry lab from Science Department of

Okayama University. My teacher was Pr. Ohkubo Takahiro and my French tutor was Pr.

Holger Klein. It took place from 29th May to 20th august 2017. The subject was “the

fundamental characterization and application of porous carbon”. I learnt how to use the

apparatus for analysis and after I made fundamental characterization of mesoporous carbon,

W10 and W15, in order to compare the results obtained with the one of microporous carbon,

A7 and A20. I made the specific reaction of copper acetate adsorbed on porous carbons on

all of these porous carbons in order to deduce the structural effect of carbon on this reaction.

19

Étudiant : LEJEUNE Eglantine MAT 3

2016-2017

Entreprise : Okayama Université

Adresse : 3-1-1 Tsushima-naka, Kita-ku,

Okayama 700-8530 Japan

Telephone : +81-86-252-1111

Tuteur de stage : Pr. Ohkubo Takahiro

Téléphone : +81-(0)86-251-7843

Courriel: ohkubo@okayama-u.ac.jp

Enseignant-référent : Pr. Klein Holger

Téléphone : +33 (0)4 76 88 79 41

Courriel: holger.klein@neel.cnrs.fr

Titre: “Caractérisation fondamentale et application de carbones poreux”

Résumé:

Mon stage a eu lieu au sein du département de chimie inorganique de la faculté de science

de l’Université d’Okayama. Le stage était du 29 mai au 20 août 2017. Le sujet communiqué

initialement était « la caractérisation fondamentale et l’application du carbone poreux ».

J’ai appris à utiliser des appareils d’analyses de solide, puis j’ai fait de la caractérisation

fondamentale avec ces même appareils sur des carbones mesoporeux ; W10 et W15.

L’objectif étant de comparer les résultats obtenus avec ceux des carbones microporeux,

A7 et A20. J’ai appliqué la réaction d’adsorption de l’acétate de cuivre sur les carbones

poreux afin d’en déduire de possible effets de structure sur la synthèse de nanoparticules

de Cu2O.