Overview of

Carbon GroupResearch Program

Nano C

CARBON GROUP

-Rostam [Science Officer] -Zairy [Science

Officer]

-Norly [PhD student] -Imran [PhD

student] – Ali [PhD student]

-Rostam [science Officer] -Salamiah [Science

Officer]

-Azman [Science Officer]

NC200 Commercial AC KD Tech

NC100 - Local AC

Characterization

Acid Base Titration

Iodine / CCL4

NC100Objective

Achievement

• Succeed in producing activated carbon with low production cost.

• Succeed in producing of homogenous mesopores distribution but still shallow of pore features ( measured via pore volume) surface area 475m2/g, meso 0.04cc/g, total pore 0.2 cc/g.

• Low production cost of Activated carbon.• To get high mesopore distribution.

Solution vs weakness

An existance of Si and Fe and others inorganic compound will be removed by using Nitrate acid as an alternative .

Nitrate acid is helping breaking the micropores to mesopores features.

Flow Chart of NC100 Preparation Process ( For KD Replacement )

Palm kernel

Dry & wash

Deionized water by usingUltrasonic for 6 hours at 60oC

dried

Dry by using conventional oven at 60oc Overnight

carbonization

Gas CO2At 900C for 4 hours

Activation

Carbonized with N2 from room temp.

to 900C

Carbonized with N2 from room temp to

900oC

Soak with 17MNaOH /

12hrs/ dry 120oC 12hrs

NC100 – Preminalary Results

Element Weight% Atomic%C K 87.86 90.8O K 11.62 9.02Si K 0.29 0.13Fe K 0.22 0.05Totals 100

870 nm

737 nm

716 nm

816 nm

708 nm

I. Support modification

Objective : Oxidative treatment of activated carbon to obtain mesoporous carbon

II. Synthesis of CNT/CNF on AC supported Fe catalyst

Objective : to get high dispersion and homogeneous of nanocarbon on AC

NC200 – current work

Support Modification – Meso program

Raw AC-KD

475oC 500oC 525oC 550oC

Physisorption measurement

Heat 10K/min, hold 3hrs, synthetic air flow rate 25ml/min in UTP

575oC

Support Modification – Meso program

Raw-HT475 475 1568 0.502 0.557 0.055

Raw-HT500 500 1313 0.621 0.5389 0.0821

Raw-HT525 525 1217 0.5612 0.5264 0.0348

Raw-HT550 550 1203 0.5535 0.4855 0.068

Raw-HT575 575 1229 0.5859 0.5345 0.052

AC-Raw - 1124 0.441 0.399 0.042

Sample TOC SBET (m2g-1) Total pore V Vmicro (cc/g) Vmeso (cc/g)

0.0 0.2 0.4 0.6 0.8 1.0150

200

250

300

350

400

450

RAW HT475 HT500 HT525 HT550 HT575

cc /

g

P / Po0 5 10 15 20 25 30 35 40 45 50 55

-0.01

0.00

0.01

0.02

0.03

0.04

0.05

0.06

0.07

0.08

0.09

0.10RAW HT475 HT500 HT525 HT550 HT575

Dv/

Dr

(cm

3/g

A)

Pore radius A

isotherm BJH

mesopore

Support Modification – Meso program

Pre-treatment [heat 200oC, 2hrs, wash 5M HNO3 / 24hrs/ RT]

400oC 450oC 480oC 500oC

Physisorption measurement

5K/min, static air flow in small furnace

Raw AC-KD

Holds time : 1hrs, 3hrs, 5 hrs, 7hrs

0.0 0.2 0.4 0.6 0.8 1.0150

200

250

300

350

400

450

500

550

Vo

lum

e (

cc/g

)

Relative Pressure (P/Po)

RAWACAWA009_B ACAW5001HR_B ACAW4507HR_B ACAW4505HR_B ACAW4503HR_B ACAW4505HR20_B

0 10 20 30 40 50 60

0.00

0.02

0.04

0.06

0.08

0.10

Po

re V

olu

me

(cc

/A/g

)

Pore width (A)

Micropore Mesopore

isotherm

BJH

Sample TempTime

HoldRate/min

% Yield Decreased

Surface Area (m2/g)

Pore volume (cc/g)

Average pore width (nm)

Total Pore Volume (cc/g)

Pore volume [mesopore]

(cc/g)

ACAW50020HR 500 20 5 Ash X X X X X

ACAW60020HR 600 20 5 Ash X X X X X

ACAW5001HR 500 1 5 51.19 1224 0.6529 4.805 0.7538 0.1009

ACAW6001HR 600 1 5 Ash X X X X X

ACAW5003HR 500 3 5 Ash X X X X X

ACAW5005HR 500 5 5 Ash X X X X X

ACAW4001HR 400 1 5 6.19 1182 0.4889 3.749 0.5671 0.0782

ACAW4501HR 450 1 5 11.81 1372 0.6079 3.980 0.6786 0.0707

ACAW4003HR 400 3 5 8.75 1194 0.5023 3.873 0.5775 0.0752

ACAW4503HR 450 3 5 26.13 1280 0.5985 4.392 0.6982 0.0997

ACAW4005HR 400 5 5 7.93 1311 0.5617 3.900 0.6513 0.0896

ACAW4505HR 450 5 5 37.60 1340 0.6755 4.619 0.7955 0.1200

ACAW4507HR 450 7 5 63.52 1037 0.5600 4.728 0.6646 0.1046

ACAW4509HR 450 9 5 69.43

ACAW4505HR20 450 5 20 35.53 1299 0.6492 4.447 0.7614 0.1122

ACAW4505HR1 450 5 1 56.84

ACAW4801HR 480 1 5 27.41

ACAW4805HR 480 5 5

A009 Norly Ali

- - 1122 0.4598 3.469 0.5210 0.0612

Raw ACAW (A009)

- - 1234 0.5063 3.536 0.5827 0.0764

Future Plan

• Compare the highest mesopore volume method with UTP+synthetic air method– Rotating UTP – the burning process more

homogen

• The best method use to create a mesopore based substrate for impregnation process

Schematic diagram for mesoporous program

Raw AC-KD

450oC 475oC 500oC 525oC

Heat 10K/min, hold 3hrs, 5%O2 in N2 flow rate 100ml/min, ToC is based on Meso2

BET=Meso 1A

BET=Meso 1B

A009

Heat 10K/min, 5%O2 in N2 flow rate 100mil/min, ToC

Impregnate with Fe

BET = Meso2

BET=Meso 2A

1K/min 3K/min 5K/min

D080-1 D080-2 D080-3

Heat 10K/min, hold 3hrs, 5%O2 in N2 flow rate 100mil/min,

ToC is based on Meso1B [xxxOc]

BET = Meso 1C

Further Calcine 120C, 5%O2 in N2,Wash with 5M HNO3, RT, 24hrs

Heat 10K/min, hold 3hrs, 5%O2 in N2 flow rate 100mil/min

Synthesis CNF/CNT on AC/Fe

Big Raw AC Wash 5M HNO3 24hrs

Grain / seive <50µm

Wet impregnation 1wt% Fe-nitrate/Fe-acetate

Ultrasonification / 30min

Calcination

• 250oC

• Hold 1hrs

• 5%O2 in N2

Reduction

• 300oC

• Hold 1hrs

• 5%H2 in N2

Growth

• 700oC

• Hold 2hrs

• 200ml H2 / 30ml C2H4

SEM images – iron nitratecal250, red300, growth700

Element Weight% Atomic%C K 90.03 92.51O K 9.50 7.33Si K 0.23 0.10Fe K 0.24 0.05Totals 100.00 100.00

SEM images – iron acetate,

cal250, red300, growth700

Element Weight% Atomic%C K 85 88.52O K 14.39 11.25Si K 0.39 0.17K K 0.07 0.02Fe K 0.15 0.03Totals 100

Acknowledgement

Combicat & NanoC team

FHI team