Yasuki Kido, Kazuki Nakanishi,* and Kazuyoshi Kanamori Word -...

6
Suppl Sol- with Yasu Fig. S lines) obser and th PAAm PAAm cm -1 , Appe lementary Inf -Gel Syn h Well-D uki Kido, Ka S1 (a) TG-D ) and with P A rved in both s hose from 30 m. (b) FT -I m (solid line) N-H for 1,6 earance of new formation for nthesis o Defined M azuki Nakan DTA curves AAm (solid samples are a 00 ºC to 400 IR spectra of ). Dotted lin 604 cm -1 , 3, w bands and i r f Zinc F Macropo nishi,* and K for gel phas lines). Wei ascribed to cr 0 ºC observe f as-dried sa nes indicate a ,196 cm -1 , an intensity grow Ferrite-B ores Kazuyoshi K se of as-dried ight loss and rystallization d in sample amples prepar as following b nd 3,342 cm wth derived f Based Xe Kanamori d samples pr d exothermic n to ZnFe 2 O 4 prepared wit red without bondings: C-N m -1 , and C=O from PAAm a erogel M epared witho peaks from and decompo th PAAm is PAAm (dash N for 1,196 c O for 1,664 are observed. Monoliths out PAAm (d 200 ºC to 3 osition of gly the combust hed line) and cm -1 , CH 2 for cm -1 , respec s dashed 300 ºC ycerol, tion of d with r 1,420 ctively. Electronic Supplementary Material (ESI) for RSC Advances This journal is © The Royal Society of Chemistry 2013

Transcript of Yasuki Kido, Kazuki Nakanishi,* and Kazuyoshi Kanamori Word -...

Suppl

Sol-with

Yasu

Fig. S

lines)

obser

and th

PAAm

PAAm

cm-1,

Appe

lementary Inf

-Gel Synh Well-D

uki Kido, Ka

S1 (a) TG-D

) and with PA

rved in both s

hose from 30

m. (b) FT-I

m (solid line)

N-H for 1,6

earance of new

formation for

nthesis oDefined M

azuki Nakan

DTA curves

AAm (solid

samples are a

00 ºC to 400

IR spectra of

). Dotted lin

604 cm-1, 3,

w bands and i

r

f Zinc FMacropo

nishi,* and K

for gel phas

lines). Wei

ascribed to cr

0 ºC observe

f as-dried sa

nes indicate a

,196 cm-1, an

intensity grow

Ferrite-Bores

Kazuyoshi K

se of as-dried

ight loss and

rystallization

d in sample

amples prepar

as following b

nd 3,342 cm

wth derived f

Based Xe

Kanamori

d samples pr

d exothermic

n to ZnFe2O4

prepared wit

red without

bondings: C-N

m-1, and C=O

from PAAm a

erogel M

epared witho

peaks from

and decompo

th PAAm is

PAAm (dash

N for 1,196 c

O for 1,664

are observed.

Monoliths

out PAAm (d

200 ºC to 3

osition of gly

the combust

hed line) and

cm-1, CH2 for

cm-1, respec

s

dashed

300 ºC

ycerol,

tion of

d with

r 1,420

ctively.

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Fig. S

1.25/2

becom

Fig. S

witho

and th

S2 SEM im

2.75, and (c)

me finer.

S3 SEM im

out adding an

he aggregatio

mages of as-dr

1.00/3.00, re

mage of as-dr

ny iron(III) ch

on of spherica

ried samples

espectively.

ied sample s

hloride hexah

al particles les

with varied v

With increa

ynthesized fr

hydrate. No

ss than 1 m

volume ratio

ased the amou

rom only zin

o micrometer

was formed.

of VH2O/VGLY

unt of glycero

c chloride as

-ranged skele

Y; (a) 1.50/2.5

ol, macrostru

s a metal pre

eton was obs

50, (b)

uctures

cursor

served,

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Fig. S

Fe, R

ZnFe2

-Fe2

S4 XRD pa

R, from 0.20

2O4, and open

2O3 through Z

atterns of sam

to 2.00. Sy

n square is Z

ZnFe2O4 to Zn

mples heat-tre

ymbols indica

ZnO, respectiv

nO.

ated in air at

ate as follow

vely. With i

300 ºC for 4

s: open trian

increasing R,

h with varied

gle is -Fe2O

crystalline p

d the ratio of

O3, closed ci

phase changes

f Zn to

rcle is

s from

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Fig. S

S5 EDX analysis of sammples calcined

d under (a) air

r, and (b) Ar fflow at differrent temperatu

ure.

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Table S6. Caicination condition and the Zn/Fe ratio calculated from EDX analysis depicted in Fig.

S5. Under air heat-treatment, Zn/Fe is close to 0.50, which is starting composition, on the other

hand, Zn/Fe decreases to 0.08~0.22 under Ar heat-treatment, which results indicates there are few

zinc-based species at the surface.

Calcination Condition Zn/Fe

air 300 ºC, 4 h 0.42

Ar 300 ºC, 4 h (with continuous Ar flowing) 0.20

Ar 400 ºC, 4 h (with continuous Ar flowing) 0.22

Ar 500 ºC, 4 h (with continuous Ar flowing) 0.19

Ar 600 ºC, 4 h (with continuous Ar flowing) 0.08

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Fig. S

Mercu

sampl

sampl

shrink

S7 (a) SEM

ury intrusion

le (open circ

le also poss

kage of macro

M images of

n results indic

cle, solid lin

essed well-d

opore as well

(i) as-dried s

cate macropor

ne) and calcin

defined macr

l as reduction

sample and (

re size distrib

ned sample

ropore about

n of cumulativ

(ii) that of he

bution and cu

(open triang

533 nm. C

ve pore volum

eated under A

umulative por

le, dashed li

Compared to

me was obser

Ar at 600 ºC

re volume; as

ine). Heat-t

o as-dried sa

rved.

C. (b)

s-dried

treated

ample,

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