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Eco-F iendly Liquid-Phase Syn hesis and Cha ac e iza ion o
G aphene Oxide Films o Chemical Senso Applica ions
Medina Uma 1*, Abdul D.A. Buba2, Akpa Ogbonaya Vic o 3, Ramalan
Abubaka 4
1,2,3,4Depa men o Physics, Uni e si y o Abuja, Abuja, Nige ia
Co esponding Au ho : medina.uma @uniabuja.edu.ng
ABSTRACT: The g ea demand o sus ainable ma e ial in Nano echnological indus ies has spa ked he
disco e y o wonde ma e ial known as g aphene and i s de i a i es (g aphene oxide, educed g aphene oxide)
because o i s unique p ope ies anging om s uc u al, elec ical and op ical p ope ies. Howe e , he
con en ional me hod has le chemical and high empe a u es ha a e haza dous o human heal h and he
en i onmen . This esea ch deals wi h an eco iendly me hod o syn hesis and deposi ion o g aphene oxide (GO)
using spin coa ing, achie ing hin ilms wi h uni o m s uc u al, op ical, and elec ical p ope ies. The Scanning
Elec on Mic oscope analysis a a magni ica ion o 1µm, e ealed a w inkled mo phology ypical o GO, while
Raman spec oscopy un eiled G band a ~1600 cm⁻¹ and D band a ~1350 cm⁻¹ which con i med he p esence o
g aphi ic domains and de ec s espec i ely. UV-V spec oscopy analysis e eals he abso p ion peak a 232 nm
while he shoulde appea s a ound 294 nm which e i ies he success ul oxida ion and ex olia ion o g aphi e in o
GO, wi h well-de ined op ical cha ac e is ics. Hence, he linea I-V cu e indica ed consis en elec ical beha io
ac oss he ilm. These indings demons a e he po en ial o i s eco- iendly GO ilms o senso s ia spin coa ing
o applica ions in ad anced ma e ials and nano echnology.
KEYWORDS: Eco- iendly Syn hesis, G aphene Oxide Film, G een Liquid-phase
I. INTRODUCTION
The g ea demand o sus ainable echnology has spa ked he disco e y o no el ma e ials and he modi ica ion o
exis ing ones o applica ion in a a ie y o sphe es o human endea ou , pa icula ly nano echnology. One o he
no el ma e ials disco e ed in 2004 by Manches e Uni e si y academics, No oselo and Geim, we e awa ded he
2010 Nobel P ize in Physics o hei pionee ing wo k on g ound-b eaking esea ch on g aphene, D esselhaus e
al., 2010. To add ess hese challenges, his esea ch has ocused on de eloping g een syn hesis me hods ha
minimize en i onmen al impac while main aining he desi ed p ope ies o g aphene oxide. One such app oach is
he liquid-phase ex olia ion o g aphi e using en i onmen ally iendly sol en s such as ace one and deionized
wa e , A o nyo & Ch ysikopoulos (2024) and He nandez e al. (2011). This me hod p o ides an e icien and
scalable ou e o p oducing high-quali y GO wi h con olled s uc u al p ope ies. Spin coa ing is a widely used
echnique o deposi ing hin ilms o GO on o subs a es such as glass slides, ensu ing uni o m dis ibu ion and
op imal unc ional p ope ies o senso applica ions (Kim e al., 2010). The cha ac e iza ion o hese ilms is c ucial
o e alua ing hei s uc u al in eg i y and pe o mance. Techniques such as scanning elec on mic oscopy (SEM),
Raman spec um, ou -poin p obe measu emen s, and UV- isible spec oscopy p o ide comp ehensi e insigh s
in o he mo phology, c ys allini y, elec ical conduc i i y, and op ical p ope ies o he syn hesized GO ilms
espec i ely (Zhou e al., 2011). On he soni ica ion me hod i has p o en o yield be e mechanical and
conduc i i y p ope ies. Soni ica ion slows he oxida ion o g aphi e by impeding he in e cala ion and educes he
unc ionaliza ion he g aphene basal plane. This s udy aims o explo e he eco- iendly syn hesis and
cha ac e iza ion o g aphene oxide hin ilms o senso applica ions. By op imizing he syn hesis p ocess and
sys ema ically analyzing he ma e ial p ope ies, his esea ch con ibu es o he g owing body o knowledge on
sus ainable nanoma e ial p oduc ion and i s p ac ical applica ions.
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II. RELATED WORKS
G aphene, a single laye o g aphi e wi h a 2D honeycomb-like la ice (sp² hyb idiza ion), possesses high-
demanding p ope ies like mechanical, elec ical, he mal, and op ical p ope ies ha a e c i ical o
nano echnological indus ies (Wo ku & Ayele, 2023). I is a semiconduc o wi h a ze o-band gap a he Di ac poin ,
exhibi ing e y high elec ical conduc i i y. The elec onic s a es o g aphene can be well desc ibed by he igh -
binding Hamil onian o π elec ons in ca bon a oms (Rajib e al., 2022). I s applica ion po en ial spans om
en i onmen al emedia ion (Abbas e al., 2022) o composi es (Pei & Cheng, 2012). Since i s i s isola ion ia
mechanical ex olia ion in 2004 (Mbayachi e al., 2021; Singh e al., 2011), i has been ecognized as a ca bon
allo ope wi h a plana shee o a oms a anged in hexagonal ings (Vee a, 2019; Ka snelson, 2007). The
de elopmen o sus ainable and eco- iendly ma e ials has gained signi ican a en ion in ecen yea s, pa icula ly
in he ield o nano echnology. G aphene oxide (GO), a de i a i e o g aphene, is an ad anced wo-dimensional
ma e ial known o i s excep ional elec ical, he mal, and mechanical p ope ies. GO has a simila hexagonal
ca bon s uc u e o g aphene bu is deco a ed wi h hyd oxyl (–OH), alkoxy (C–O–C), ca bonyl (C=O), ca boxylic
acid (–COOH) and o he oxygen-based unc ional g oups (Pendolino & A ma a, 2017). These unc ional g oups
a e no me ely s uc u al de ec s; hey a e ac i e si es ha acili a e u he chemical modi ica ion and enhance
dispe sibili y in a ious sol en s, which is c ucial o p ocessing and composi e o ma ion (Smi h e al., 2021). One
o he i al s eng hs o he unc ional g oups p esen in g aphene oxide is ha hei a ia ion can une he ma e ial's
elec ical, mechanical, he mal, and physical p ope ies (Sha ma e al., 2021).
GO holds g ea p omise o a a ie y o applica ions, including senso s, ene gy s o age de ices, and elec onic
componen s (Geim & No oselo , 2007). Howe e , adi ional syn hesis me hods, such as he Humme s' me hod
and i s modi ica ions, o en in ol e haza dous chemicals like concen a ed sul u ic acid (H₂SO₄), po assium
pe mangana e (KMnO₄), and hyd ogen pe oxide (H₂O₂), aising se ious en i onmen al and sa e y conce ns (Chen
e al., 2022; D eye e al., 2010). The en i onmen al oo p in o hese con en ional ou es has ca alyzed a pa adigm
shi owa ds mo e sus ainable p oduc ion echniques (Yada & Kuma , 2023). In esponse, he ield o g een
chemis y has been ac i ely applied o g aphene syn hesis. A p ominen s a egy in ol es using enewable biomass
as a p ecu so . Fo ins ance, Chua e al. (2022) demons a ed he syn hesis o g aphene oxide om suga cane
bagasse, an ag icul u al was e p oduc , highligh ing a ci cula economy app oach ha educes eliance on pu i ied
g aphi e. Simila ly, Lee & Pa k (2024) e iewed a ious plan -based ex ac s (e.g., om lea es and ui s) ha can
se e as educing and s abilizing agen s o p oducing GO and educed GO, minimizing he need o oxic
hyd azine. These bio-inspi ed me hods no only mi iga e en i onmen al impac bu also o en esul in GO wi h
unique mo phological p ope ies sui able o biomedical applica ions. The push o sus ainabili y ex ends beyond
syn hesis o he ma e ial's en i e li e cycle. A ecen li e-cycle assessmen (LCA) s udy by Fe nández e al. (2023)
compa ed he adi ional Humme s' me hod wi h a g een elec ochemical ex olia ion p ocess. Thei indings
con i med ha he g een ou e signi ican ly educes ene gy consump ion, ca bon emissions, and oxic was e
gene a ion, p o iding a quan i a i e a gumen o i s adop ion. Fu he mo e, he unc ional g oups on GO can be
le e aged o en i onmen al good, such as in wa e pu i ica ion. A s udy by Gup a e al. (2023) de eloped a GO-
based memb ane unc ionalized wi h speci ic ions o he highly e icien and selec i e emo al o hea y me als
om indus ial was ewa e , di ec ly add essing he pollu ion conce ns associa ed wi h i s own adi ional
p oduc ion.
III. RESULTS AND DISCUSSION
A. S udy Loca ion and Da a Collec ion
Me eo ological da a o his s udy, including empe a u e, humidi y, and sola i adiance, we e sou ced om he
headqua e s o he Nige ian Me eo ological Agency (NiMe ) in Abuja. The ci y ea u es a opical we and d y
clima e and is si ua ed a an a e age ele a ion o app oxima ely 455.89 me e s abo e sea le el (Nige ian
Me eo ological Agency [NiMe ], n.d.). I s geog aphic coo dina es a e 9.07°N la i ude and 7.60°E longi ude,
encompassing an a ea o 1,769 squa e kilome e s. The opog aphy immedia ely su ounding he ci y (wi hin a 3.2
km adius) is cha ac e ized by ela i ely modes ele a ion changes. The maximum ele a ion shi in his a ea is 143
me e s, wi h an a e age al i ude o 494.7 me e s abo e sea le el (NiMe , n.d.). In e ms o land co e , he ci y is
p edominan ly composed o a i icial su aces (77%) and c opland (22%). On a b oade scale, he landscapes wi hin
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16.1 km and 80.5 km o he ci y cen e a e la gely a mix o c opland and sh ubs, accoun ing o 37% and 43% o
he a ea, espec i ely.
Abuja expe iences annual empe a u es ha ypically luc ua e be ween a low o 16.6°C and a high o 33.9°C
(NiMe , n.d.). The ho es pe iod las s oughly 2.5 mon hs, du ing which a e age daily high empe a u es exceed
32.2°C. A coole season spans app oxima ely 3.5 mon hs, whe e a e age highs emain below 28.3°C. Decembe is
he coldes mon h, wi h a e age lows o 16.1°C and highs o 30.6°C.
The ci y's clea es wea he begins a ound No embe 7 h and las s o abou 3.6 mon hs, wi h Janua y s anding ou
as he clea es mon h. In con as , a cloudie pe iod s a s a ound Feb ua y 24 h and pe sis s o abou 8.4 mon hs,
eaching i s peak in May. The we season ex ends o 6.2 mon hs and ca ies a g ea e han 42% p obabili y o
p ecipi a ion on any gi en day. This is coun e balanced by a 5.8-mon h d y season; Decembe has he ewes
numbe o ainy days. Augus is he we es mon h, while Decembe is he d ies . Dayligh hou s in Abuja emain
ela i ely consis en yea - ound, a e aging abou 12 hou s wi h only mino a ia ion. Con e sely, humidi y le els
shi signi ican ly wi h he seasons. A muggy and o en uncom o able pe iod las s o abou nine mon hs, om la e
Feb ua y o la e No embe . Du ing his ime, condi ions a e humid o opp essi e o a leas 27% o he ime.
Augus is he mos humid mon h, wi h nea ly all 31 days classi ied as muggy o wo se (NiMe , n.d.).
B. MATERIALS
The ollowing ma e ials we e used in his s udy:
(a). P epa a ion o Sol en Mix u e: ace one and DI wa e we e mixed in a 7:3 a io (ace one: wa e ), ha is 70%
ace one and 30% DI wa e . This mix u e can e ec i ely dispe se g aphi e while balancing ex olia ion and
s abili y. The sol en mix u e was s i ed ho oughly o ensu e a homogeneous solu ion.
(b). G aphi e Dispe sion: The g aphi e powde was added o he ace one/DI wa e mix u e a a concen a ion o
a ound 5 mg/mL. Hence, he mix u e was s i ed wi h a magne ic s i e o 15 minu es o p e-dispe se he
g aphi e pa icles.
(c). Sonica ion P ocess: The mix u e was ans e ed o a sui able con aine ha i s he ul asonica o . The solu ion
was hen ul asonica ed in an ul asonic ba h o 2 hou s, o mode a e yield and good quali y o g aphene. I
was ensu ed ha he empe a u e o he mix u e did no exceed 40°C du ing sonica ion using an ice ba h, as
highe empe a u es can deg ade he g aphene quali y.
(d). Cen i uga ion: A e sonica ion, he mix u e was cen i uged a 3000 RPM o abou 40 minu es. This was
done o sepa a e la ge g aphi e pa icles and unex olia ed lakes om he ex olia ed g aphene. The abo e
condi ion was o di ide he mix u e in o wo (2) laye s: supe na an and sedimen . The supe na an (liquid pa )
will con ain he ex olia ed g aphene, while he sedimen will con ain non-ex olia ed g aphi e.
(e). Collec ion o G aphene Oxide: To collec he g aphene oxide, he supe na an was ca e ully decan ed in o a
clean con aine wi hou dis u bing he sedimen . This supe na an con ains he ew-laye o single-laye
g aphene oxide.
( ). Washing and Pu i ica ion: The deionized wa e was g adually added o he supe na an o emo e any esidual
ace one o impu i ies.
(g). Cleaning he Glass Slide: The glass slides we e washed ho oughly wi h soap and wa e o emo e any g ease
o di ha may al e he quali y o he g aphene. Hence, he slides esidue insed wi h ace one o emo e
o ganic esidue con en s. Subsequen ly, i was insed wi h deionized (DI) wa e o ensu e all cleaning agen s
we e emo ed. Finally, he glass slide was d ied by placing i on a ho pla e a a bi empe a u e (~60°C) o
emo e any emaining mois u e.
(h). Spin-Coa ing: The cleaned glass slide was secu ed on o he spin-coa e s age using a acuum and a pipe e was
used o deposi a small d ople (app oxima ely 200 µL) o he g aphene dispe sion on o he cen e o he glass
slide. Howe e , he spin-coa e was s a ed a a low speed (600 RPM) o 15 seconds o sp ead he liquid
e enly. I was u he inc eased he spin speed o a highe alue (4000 RPM) and main ained his speed o
abou 50 seconds. The high-speed o a ion helped o c ea e a uni o m hin ilm as he sol en e apo a ed
apidly.
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(i). Annealing he ilm: A e spin-coa ing, he glass slide was placed on a ho pla e se o a ound 70°C o 7 minu es
o ensu e comple e e apo a ion o he sol en and good ilm adhesion on he subs a e (glass slides). Figu e 1
demons a e he schema ic low o he deposi ion p ocess o he wo k.
Figu e 1: Schema ic low cha o he syn hesis and deposi ion p ocess
IV. RESULTS AND DISCUSSION
A a magni ica ion o 1 µm, pla e 1 shows he SEM image p o ides a de ailed iew o he g aphene oxide (GO)
ilm s uc u e, showcasing i s mic os uc u al a angemen a a ine scale. The image e eals a cha ac e is ic laye ed
and w inkled mo phology, which is a well-known ea u e o g aphene oxide ilms. These w inkles a e a ibu ed o
he d ying and se ling p ocesses du ing spin coa ing, as well as he in insic s uc u e o GO shee s, as p e iously
epo ed in he li e a u e (Pa k e al., 2009). Addi ionally, he con inui y o he GO laye , as obse ed in he image,
indica es a well-con olled spin-coa ing p ocess, which is c ucial o achie ing uni o m ilm deposi ion (Li e al.,
2011). This mo phology is pa icula ly ad an ageous o applica ions in senso s, anspa en conduc i e ilms, and
elec onic de ices, whe e he unique p ope ies o GO can be e ec i ely u ilized (Kim e al., 2010).
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Pla e 1: SEM images o g aphene Oxide ilm on a glass slide
Figu e 2: Raman Spec um o G aphene Oxide deposi ed on a Glass Slide
Raman spec um o he deposi ed ilm as shown in Figu e 2 shows he D band a ~1350 cm⁻¹ is a ibu ed o he
p esence o de ec s and diso de in he ca bon la ice. These de ec s a ise om s uc u al impe ec ions, oxygen-
con aining unc ional g oups in oduced du ing he oxida ion p ocess, and edge e ec s in g aphene oxide (Fe a i
e al., 2015). The G band a ~1600 cm⁻¹ co esponds o he in-plane ib a ions o sp²-hyb idized ca bon a oms
wi hin he g aphene la ice. This peak is indica i e o g aphi ic domains and is obse ed in bo h p is ine g aphene
and g aphene oxide (D esselhaus e al., 2010). The dis inc D and G peaks in he spec um indica e a uni o m
deposi ion o g aphene oxide on he glass subs a e. The well-de ined na u e o hese bands con i ms ha he spin-
coa ing p ocess has e ec i ely dis ibu ed he GO laye s ac oss he su ace (Zhou e al., 2011).
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Figu e 3: UV-Vis Spec oscopy o G aphene Oxide deposi ed on Glass Slide
The p ominen abso p ion peak obse ed a 232 nm in he UV-Vis spec um co esponds o he π-π* ansi ions o
a oma ic C=C bonds in g aphene oxide (GO) as displayed Figu e 3. This peak is a cha ac e is ic ea u e o he
conjuga ed elec onic s uc u e wi hin he g aphi ic domains o GO, e lec ing he e en ion o sp² hyb idized ca bon
a oms in he ma e ial's amewo k (Zhang e al., 2010). The shoulde appea ing a ound 294 nm is a ibu ed o n-
π* ansi ions in ol ing ca bonyl (C=O) o o he oxygen-con aining unc ional g oups. These unc ional g oups
a e in oduced du ing he oxida ion p ocess used o con e g aphi e in o g aphene oxide. Thei p esence dis up s
he ex ended π-conjuga ion o he g aphi ic s uc u e, in oducing localized de ec s a es wi hin he ma e ial (D eye
e al., 2010). The dis inc and well-de ined peaks in he spec um indica e ha he spin-coa ing p ocess success ully
p oduced a uni o m and consis en deposi ion o g aphene oxide on he glass subs a e. This ou come unde sco es
he e ec i eness o spin coa ing in c ea ing hin ilms wi h homogenous op ical and s uc u al p ope ies sui able
o u he applica ions (Hassanzadeh e al., 2014).
Figu e 4: I-V Cu e showing Shee Resis ance o G aphene Oxide deposi ed on a Glass Slide
Figu e 4 shows he I-V cu e exhibi s a linea ela ionship be ween cu en (mA) and po en ial (V), indica i e o
ohmic beha iou in g aphene oxide (GO) hin ilms deposi ed on a glass slide. Such beha iou is cha ac e is ic o
GO due o i s insula ing na u e, which esul s om oxygen-con aining unc ional g oups ha dis up he conduc i e
π-conjuga ed ne wo k wi hin he ma e ial (Pei and Cheng, 2012). The linea i y and smoo hness o he I-V cu e
sugges ha he spin-coa ing p ocess e ec i ely p oduced a uni o m and de ec - ee GO ilm. Uni o m deposi ion
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is essen ial o ensu ing consis en elec ical p ope ies ac oss he su ace, which is c ucial o applica ions equi ing
eliable conduc i i y and esis ance (Dubey e al., 2017).
V. CONCLUSION
The wo k op imized he syn hesis and deposi ion o g aphene oxide using spin coa ing, achie ing hin ilms wi h
uni o m s uc u al, op ical, and elec ical p ope ies. The SEM analysis e ealed a w inkled mo phology ypical o
GO, while Raman spec oscopy con i med he p esence o g aphi ic domains and de ec s. The UV-Vis
spec oscopy u he e i ied he success ul oxida ion and ex olia ion o g aphi e in o GO, wi h well-de ined op ical
cha ac e is ics. The linea I-V cu e indica ed consis en elec ical beha iou ac oss he ilm. These indings
demons a e he po en ial o spin-coa ed GO ilms o applica ions in senso s due o he p esence o i s unc ional
g oup like epoxides hyd oxyls and oxygen, hence can be a good gas senso and i s s abili y is s ill an open-ended
esea ch gap o be explo ed by physicis s, chemis s and biologis s. As he new wo ld e ol es a ound clima e and
eco- iendly ma e ials g aphene nano-senso s ha e a u u is ic applica ion in indus ial p oduc ion as well as
en i onmen al emedia ion due o hei bene i s in abso p ion, sensi i i y and selec i i y.
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