Cu en Opinion in Solid S a e and Ma e ials Science 27 (2023) 101122
A ailable online 16 No embe 2023
1359-0286/© 2023 The Au ho (s). Published by Else ie L d. This is an open access a icle unde he CC BY license (h p://c ea i ecommons.o g/licenses/by/4.0/).
On he ole o unc ionaliza ion in g aphene-mois u e in e ac ion
Zhijian Cao
a
, Xinyue Wen
a
, Vanesa Quin ano
a
,
b
,
*
, Rakesh Joshi
a
,
*
a
School o Ma e ials Science and Enginee ing, Uni e si y o New Sou h Wales, Sydney, NSW 2052, Aus alia
b
Ca alan Ins i u e o Nanoscience and Nano echnology (ICN2), CSIC and BIST, Campus UAB, Bella e a, 08193 Ba celona, Spain
ARTICLE INFO
Keywo ds:
G aphene oxide
Func ionaliza ion
Mois u e de ec ion
A mosphe ic wa e ha es ing
ABSTRACT
G aphene-based ma e ials such as g aphene oxide (GO) ha e demons a ed ex ao dina y sensi i i y owa ds
wa e molecules due o he hyd ophilic na u e. The hyd ophilici y o GO can be u he imp o ed ia addi ional
unc ionaliza ion. P e ious s udies sugges ha he in e ac ion be ween GO and wa e molecules esul s in he
o ma ion o a hyd ogen bond ne wo k and modi ies he in e laye s uc u e o GO lamina es. Based on he ecen
de elopmen s, we p esen ou opinion on he in e ac ion be ween mois u e and g aphene oxide and how his
in e ac ion can be u ilized o en i onmen al applica ions such as mois u e de ec ion and a mosphe ic wa e
ha es ing.
G aphene has been widely known as he i s disco e ed 2D ca bon-
based ma e ial [1,2], which is a omically hin and composed o sp
2
-
hyb idized ca bon a oms ha a e densely packed in he honeycomb
la ice [3–5], as shown in Fig. 1 (a). P is ine g aphene has g ea he mal
conduc i i y, heo e ical speci ic su ace a ea [6], adso p ion capaci y,
elec ical conduc i i y [7], and op ical anspa ency. G aphene can be
chemically modi ied by he a ached unc ional g oups on o he su ace.
Such a g aphene-based sys em, known as g aphene oxide, is widely used
in memb anes o sepa a ion and pu i ica ion [8,9] as well as o
chemical sensing [10,11].
As shown in Fig. 1 (b) [12], compa ed wi h g aphene, GO is
composed o sp
2
- and sp
3
-hyb idized ca bon a oms, wi h oxygen-
con aining unc ional g oups: hyd oxyl, epoxy, ca boxyl, and ke one
[13,14], p o iding he hyd ophilic na u e o g aphene oxide [15]. These
wa e -induced changes in g aphene oxide o e huge po en ial o
mois u e- ela ed en i onmen al applica ions such as humidi y senso s
[16–19], and a mosphe ic wa e ha es ing[20–25].
T adi ionally, he e ha e been se e al epo s on he a ious ypes o
humidi y senso s ha a e ab ica ed based on me al oxide nanopa icles
[26], ca bon nano ubes (CNTs)[27,28], ce amics, and polyme s[29].
Howe e , i has been demons a ed ha oxide-based humidi y senso s
equi e ex e nal hea ing o main ain hei sensi i i y [30,31], and CNTs-
based humidi y senso s a e commonly subjec o s ong es ic ions om
he low sensi i i y owa ds wa e molecules [32,33]. Mo eo e , GO
adso bs mois u e om he en i onmen like a adi ional desiccan
ma e ial [20]. Due o he s ong wa e adso p ion and deso p ion ki-
ne ics [34], GO can be used as a po en ial a mosphe ic wa e ha es ing
(AWH) applica ion [35]. AWH is de ined as a mois u e-cap u ing p o-
cess ha applies hyd ophilic ma e ials as ha es e s o induce spon a-
neous adso p ion o ap he wa e molecules in he o m o apou om
he ai and hen deso b as liquid wa e [36,37]. This opinion ocuses on
discussing how unc ionaliza ion imp o es he in e ac ion be ween
g aphene oxide and mois u e o imp o e he pe o mance in mois u e
de ec ion and AWH applica ions using hyd ophilic c osslinke s.
The lamina ed o m o GO has an in e laye s uc u e ha p o ides a
unique pa h o mass anspo [38] and ac s like a po ous ma e ial. The
in e laye egion o GO is gene ally di ided in o p is ine a oma ic e-
gions and oxidized non-a oma ic egions [8,39]. In con as , p is ine
egions e ain he a oma ici y owing o he sp
2
ca bon a oms-conjuga ed
sys ems. The oxidized egions o GO a e de ined as he hyd ophilic si es
o in e ac wi h he wa e molecules by o ming a hyd ogen bonds
ne wo k [40–43].
Fu he mo e, he hyd ophilic na u e o GO suppo s i s applicabili y
o wa e pu i ica ions [44–47] and ion sie ing [48]. Simila ly, in
mois u e de ec ion and AWH applica ions, he le el o hyd ophilici y
di ec ly de e mines he sensi i i y o he ma e ial owa ds he apou ,
indica ing how apidly he ma e ial could induce he in e ac ion wi h
wa e molecules [49]. Fu he mo e, i is wo h men ioning he e ha he
oxygen-con aining unc ional g oups no only con ibu e hyd ophilici y
o GO bu also p o ide s abili y o he lamina ed s uc u e, ha is, he
in e laye spacing (d-space). Hence, uning he unc ional g oups in GO
will di ec ly impac he in e laye space and he elec ical beha iou
[50]. In mois u e de ec ion applica ions, pa icula ly he sensing ma e-
ial should ini ially exhibi high elec ical esis ance in he d y s a e
* Co esponding au ho s a : School o Ma e ials Science and Enginee ing, Uni e si y o New Sou h Wales, Sydney, NSW 2052, Aus alia (V. Quin ano).
E-mail add esses: [email p o ec ed] (V. Quin ano), [email p o ec ed] (R. Joshi).
Con en s lis s a ailable a ScienceDi ec
Cu en Opinion in Solid S a e & Ma e ials Science
jou nal homepage: www.else ie .com/loca e/cossms
h ps://doi.o g/10.1016/j.cossms.2023.101122
Recei ed 26 Oc obe 2023; Recei ed in e ised o m 7 No embe 2023; Accep ed 9 No embe 2023
Cu en Opinion in Solid S a e & Ma e ials Science 27 (2023) 101122
2
[51]. A e wa ds, in he we s a e, he sensing ma e ial would be capable
o g adually al e ing he espec i e elec ical esis ance on in e ac ing
wi h wa e molecules[52–54]. The in e ac ion be ween hyd ophilic
ma e ial, GO in his case, and mois u e can be unde s ood in e ms o
adso p ion o abso p ion, depending on whe he he wa e molecules
pene a e he hyd ophilic ma e ial h ough he ac i e si es on i s su ace
o induce u he a ia ions in he chemical s uc u e[55,56].
A mosphe ic wa e ha es ing is a collec ing p ocess ha u ilizes he
in e ac ion be ween wa e and hyd ophilic ma e ials[57]. The key
mechanism o adso p ion and he associa ed physical deso p ion o GO
can be unde s ood by ailo ing he hyd ogen bonds ne wo k in he
p esence o wa e [34]. As he amoun o physically adso bed wa e
molecules inc eases, he ela i e humidi y (RH%) be ween he in e -
laye o GO lakes would ise[39,58]. A e wa ds, due o he e e s-
ibili y, he associa ed deso p ion esul s in he de achmen o wa e
molecules om he ac i e binding si es o GO.
Wang e al.[59] ecen ly epo ed a liquid-so ben a mosphe ic wa e
gene a o based on sal - esis an GO-based ae ogel, which e ains as
high as 66.9 % deso p ion e iciency wi h he inpu o sola ene gy. The
au ho s used 50 w % CaCl
2
solu ion as he so ben o adso b wa e
molecules om he apou in he ai hen p ocessed in e acial sola
hea ing on he GO-based ae ogels o deso b he wa e molecules om
he so ben ia e apo a ion. As a esul , Wang e al. demons a ed a 2.89
kgm
-2
day
−1
daily wa e gene a ion a 70 % RH le el[59]. As illus a ed
in Fig. 2 (a) o (c), he p ocedu e o AWH examined by he au ho s can
be summa ized in o h ee s eps: (i) open he lid, physically adso b he
wa e molecules om we ai by 50 w % CaCl
2
, (ii) close he lid,
e apo a e he cap u ed wa e ia he in e acial hea ing p o ided by
sunligh on he sal - esis an GO-based ae ogel, and (iii) condense he
e apo a ed wa e apou , calcium ca ions, and chlo ine anions back in o
eshwa e o collec .
Simila o he a mosphe ic wa e ha es ing (AWH) echnology, he
mechanism o GO-based humidi y sensing is also di ec ly based on he
physiso p ion o wa e molecules. Among he in insic cha ac e is ics o
GO discussed ea lie , he p esence o unc ional g oups on GO dis up s
he p o bi als on he join ed sp
2
hyb idized ca bon a oms[60], esul ing
in inc eased elec ical esis i i y in he d y s a e. Howe e , in he we
s a e, he in e ac ion be ween GO and wa e molecules gi es a ise in he
densi y o cha ge ca ie s, leading o a simul aneous dec ease in elec-
ical esis ance and an inc ease in capaci ance[61,62].
Based on he p e ious discussions, i is unde s ood ha in mois u e
de ec ion, he in insic hyd ophilici y o GO is a c ucial ac o . Highe
hyd ophilici y makes GO mo e sensi i e owa d wa e molecules; hence,
enhancing hyd ophilici y has been he p ima y means o imp o ing he
mois u e de ec ion pe o mance o GO in he pas decade[63–65]. The
unc ionaliza ion o GO has become a widely used modi ica ion
app oach o u he imp o ing he in insic cha ac e is ics o GO, which
in ol es he applica ion o eac i e c oss-linking eagen s o o m
chemical bonds wi h he oxygen-con aining unc ional g oups o GO
[66–70].
Func ionaliza ion o GO can be ca ego ized in o co alen and non-
co alen unc ionaliza ion[71,72]. The co alen unc ionaliza ion o
GO includes he in oduc ion o oxygen-con aining unc ional g oups on
GO such as ca boxyl, epoxy, hyd oxyl, and ke one[73,74], whe eas he
non-co alen unc ionaliza ion o GO elies on in e molecula in-
e ac ions be ween he ac i e si es o GO and he c oss-linking eagen s,
such as he
π
−
π
in e ac ion, pola i y-induced hyd ogen bonding, and
elec os a ic in e ac ions[75]. Consequen ly, i can be unde s ood ha
Fig. 1. (a) P is ine g aphene lamina e. (b) He e ocyclic chemical s uc u e and unc ional g oups dis ibu ion o g aphene oxide (GO). Ca boxyl, hyd oxyl, ke one,
and epoxy g oups a e highligh ed in ed, blue, g een, and pu ple, espec i ely. Fo he s uc u e o g aphene oxide shown in Fig. 1 (b), we e e o he Le -Klinowski
model[12].
Z. Cao e al.
Cu en Opinion in Solid S a e & Ma e ials Science 27 (2023) 101122
3
he co alen unc ionaliza ion o GO, by o ming o ganic co alen
bonding be ween unc ional g oups, ob ains signi ican ly g ea e s a-
bili y bu equi es mo e s ingen and complex eac ion condi ions and
ac i a ion p ocesses[76–79]. On he o he hand, he non-co alen
unc ionaliza ion o GO, while no as s able as co alen unc ionaliza-
ion does no equi e ex ensi e ac i a ion eagen s[79,80].
Among he mos used humidi y senso s a e he epoxy- ich, e hyl-
enediamine (EA) and polye hyleneimine unc ionalized GO-based sen-
so s. EA has wo amine g oups which ob ain he eac i i y owa d he
epoxy and ca boxy g oups on GO[81–83], dis ibu ed a bo h ends o i s
ca bon chain in one uni o EA molecule. The e o e, EA is commonly
applied as he amine-con aining c oss-linking agen in he ca boxyl
unc ionaliza ion o GO, whe e he amine g oups induce nucleophilic
subs i u ion o eac wi h he ac i a ed ca boxyl g oups o gene a e
amide linkages[84]. Howe e , because o he eac ion ene gy ba ie s
and s e ic hind ance e ec s[85–87], di ec c oss-linking h ough amine
g oups induced by ca boxyl unc ionaliza ion is no easible; hus, i is
ypically necessa y o apply ca bodiimide coupling eagen s o p e-
ac i a e he ca boxyl g oups on he edges o GO lakes[88–91], gene -
a ing highly eac i e in e media es o amida ion[92–94].
Ho e al.[95] epo ed an EA-deco a ed GO-based humidi y senso .
In hei wo k au ho s deposi ed he ca boxyl unc ionalized EA-GO on o
qua z c ys al mic obalance (QCM) elec odes, which shows a much
as e mois u e-de ec ing speed han he amine- ee GO/QCM-based
humidi y senso . Be o e es ing and compa ing he di e ences in mois-
u e de ec ion pe o mances, he au ho s measu ed he con ac angles o
bo h EA-GO and p is ine GO[95]. As shown in Fig. 3 (a) and (b), a e
he EA-induced amida ion eac ion be ween amine and ac i a ed
ca boxyl g oups, he con ac angle o EA-GO was ound o be 2 deg ees
smalle han ha o pu e GO[95], which di ec ly indica es ha he
success ul c oss-linking wi h EA has led o a signi ican imp o emen in
he hyd ophilici y o GO. Fig. 3 (c) illus a es he mois u e de ec ion
se ups in which he au ho s used di e en sal solu ions o adjus he
es ing RH% and deposi ed he EA-GO ilm on o QCM elec odes o
examine he mois u e-de ec ing pe o mance unde he con olled
ope a ing equency (15 MHz)[95]. Fig. 3 (d) clea ly demons a es ha ,
compa ed o pu e GO, al hough pu e GO exhibi s he abili y o adso b
mo e wa e molecules (75 RH%), EA-GO ilms display signi ican ly
sho e esponse and eco e y imes when in e ac ing wi h mois u e
unde 23 % RH.
In ano he s udy, Liu e al. p epa ed he epoxy-GO (EGO) samples ia
modi ied Humme ’s me hod[96]. Subsequen ly, hey deposi ed ilms by
spin-coa ing GO and EGO on o he elec odes. The au ho s employed
a ious sa u a ed sal solu ions in ai - igh essels o adjus di e en RH
% o examining he mois u e de ec ion pe o mances[96]. A e wa ds,
he au ho s es ed he esponse speed o epoxy- ich unc ionalized GO
samples, as shown in Fig. 4 (a), as he olume o added wa e inc eases,
he slope o he cu e di ec ly inc eases, which means he esponse ime
o senso s o eac becomes sho e . In Fig. 4 (a), he sample which was
unc ionalized wi h he la ges amoun o wa e du ing Humme ’s
me hod e ained he g ea es slope, he e o e i ob ained he highes
sensi i i y owa ds wa e molecules. Addi ionally, Liu e al. es ed ou
Fig. 2. Schema ic g aph o he ope a ing mechanism o in e acial sola -hea ing-assis ed a mosphe ic wa e gene a o based on GO-based ae ogel. (a) Vapou
so p ion by using 50 w % CaCl
2
. (b) Vapou deso p ion by e apo a ing he cap u ed wa e on GO-based ae ogel. (c) Wa e gene a ion by condensing he e apo a ed
apou . Figu es we e ep oduced wi h he pe missions om ( e .[59]). Copy igh (2019), wi h pe mission om John Wiley and Sons. Fo de ailed in o ma ion, we
e e o scheme 1 in he e .[59].
Z. Cao e al.
Cu en Opinion in Solid S a e & Ma e ials Science 27 (2023) 101122
4
samples wi h ixed RH le els wi hin 60 s[96]. As shown in Fig. 4 (b), as
he added wa e amoun inc eased, he esponse ime g adually
dec eased, and he EGO-W-5 sample exe ed an ex emely sha p
esponse cu e om 10 s o 30 s owa ds 32.8 % RH, which also p o ed
ha epoxy- ich unc ionalized GO would e ain highe hyd ophilici y
[96].
The ole o epoxy- ich unc ionaliza ion can be explained as
imp o ing he e ec i e su ace a ea o in e ac ion and modi ying he
hyd ophilici y by adding mo e ac i e si es[96,97]. Table 1 summa izes
he ole o unc ionaliza ion in g aphene-based mois u e de ec ion and
AWH applica ions. Fo de ailed in o ma ion abou he c oss-linke s,
ma e ials used and pe o mance we e e o he ci ed e e ences in
Table 1.
In summa y, he in insic cha ac e is ics o GO, such as in e laye
spacing and elec ical esis i i y, can be modi ied when i is exposed o
he mois u e en i onmen . This wa e -induced change can be u ilized
o humidi y sensing and a mosphe ic wa e gene a ion. Fu he mo e,
owing o he exis ence o oxygen-con aining unc ional g oups, GO is
Fig. 3. Con ac angles o (a) TCGO and (b) TCGO
EA
examined by Ho e al. (TCGO means he pu e GO ab ica ed unde con olled empe a u e, TCGO
EA
ep esen s
he unc ionalized GO). (c) Mois u e de ec ion se ups applied by Ho e al. on EA-GO and GO ilms. (d) Response and eco e y ime examina ions o EA-GO, pu e GO,
and QCM elec odes unde 23% RH o 75% RH. (RTGO means he esis i i y- ab ica ed GO). Figu es we e ep in ed wi h pe mission om ( e .[95]). Copy igh
(2020), wi h pe mission om Else ie . Fo de ailed in o ma ion, we e e o igu e 5 (a), igu e 5 (c), igu e 8 (a), and g aphical abs ac o e .[95].
Fig. 4. (a) S a ic esponse cu es o EGO samples unde inc easing RH%. (b) Dynamic esponse cu es o EGO samples in 32.8% RH. The igu es we e ep oduced
wi h pe mission om ( e .[96]). Copy igh (2020), wi h pe mission om Else ie . Fo de ailed in o ma ion, we e e o igu e 6 in e .[96].
Z. Cao e al.
Cu en Opinion in Solid S a e & Ma e ials Science 27 (2023) 101122
5
eac i e o a ious o ganic c oss-linking eagen s and, hence, a good
pla o m o unc ionaliza ion o enhance he applica ion po en ial. The
ole o unc ionaliza ion is o p o ide addi ional ac i e adso p ion si es
o su ace-dependen applica ions based on he o ma ion o he
hyd ogen bond ne wo k; hence, unc ionaliza ion s ill holds g ea po-
en ial in GO-based AWH and mois u e de ec ion applica ions.
Decla a ion o Compe ing In e es
The au ho s decla e ha hey ha e no known compe ing inancial
in e es s o pe sonal ela ionships ha could ha e appea ed o in luence
he wo k epo ed in his pape .
Da a a ailabili y
No da a was used o he esea ch desc ibed in he a icle.
Acknowledgemen
Vanesa Quin ano acknowledges he unding om he Eu opean
Union’s Ho izon 2020 esea ch and inno a ion p og amme unde he
Ma ie Skłodowska Cu ie G an Ag eemen No. 101066462. Zhijian Cao
hanks Dali Ji and Xiaojun Ren o he ui ul discussion.
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Table 1
Func ionalized g aphene-based AWH and mois u e sensing applica ions.
C oss-linke s Applica ions Func ionaliza ion Pe o mance S uc u e Re e ences
LiCl GO/PI oam-based AWH
π
-in e ac ion
unc ionaliza ion
Ha es ing capabili y:
1.15 gg
−1
(a 90 % RH)
GO/PI-Li
+
(ca ions-
π
in e ac ion) [23]
CaCl
2
Ca
2+
-GO ae ogel-based AWH
π
-in e ac ion
unc ionaliza ion
Adso p ion capaci y:
120 %
GO-Ca
2+
(ca ions-
π
in e ac ion) [35]
N/A Pu e GO/cellulose ae ogel-
based AWH
N/A Daily eshwa e p oduc ion:
2.89 kgm
-2
day
−1
(a 70 % RH)
Pu e GO [59]
Ni ic acid -c GO-based AWH No men ioned Wa e e apo a ion a e:
0.47 kgm
-2
h
−1
(a 1kWm
−2
sola in ensi y)
GO (mo e oxygen con aining
unc ional g oups)
[97]
Dopamine PDA-GO-based humidi y
senso
No men ioned 18 s/2s esponse/ eco e y ime (a 97 %
RH)
GO-amide-PDA [63]
E hylenediamine GO
EA
-based humidi y senso Ca boxyl-
unc ionaliza ion
10 s/11 s esponse/ eco e y ime ( om
23 % o 75 % RH)
GO-amide-EA [95]
N/A EGO-based humidi y senso Epoxy- ich
unc ionaliza ion
Sensi i i y:
40.1 % (a 32.8 % RH)
GO-mo e epoxy g oups [96]
1,6-
hexanediamine
HA-GO-based humidi y
senso
Ca boxyl-
unc ionaliza ion
52 s/72 s esponse/ eco e y ime ( om
20 % o 90 % RH)
GO-amide-HA [98]
Z. Cao e al.

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