OPTICS AND OPTOELECTRONICS VOLUME: 16 |NUMBER: 2 |2018 |JUNE
Elec odeposi ion o Cup ous Oxide on Bo on
Doped Diamond Elec odes
Mi osla BEHUL1, Ma ian VOJS1, Ma ian MARTON1,
Pa ol MICHNIAK1, Ma io KURNIAWAN2, Ral PEIPMANN2,
Cod u a Au elia VLAIC2, And eas BUND2, Robe REDHAMMER1
1Ins i u e o Elec onics and Pho onics, Facul y o Elec ical Enginee ing and In o ma ion Technology,
Slo ak Uni e si y o Technology, Ilko ico a 3, 812 19 B a isla a, Slo ak Republic
2Ins i u ue We ks o echnik, FG Elek ochemie und Gal ano echnik, Fakul ae ue Elek o echnik und
In o ma ions echnik, Technische Uni e si ae Ilmenau, Ki chho -S . 6, 98693 Ilmenau, Ge many
mi osla .beh[email p o ec ed], ma ian. ojs@s uba.sk, [email p o ec ed], pa ol.mic[email p o ec ed],
ma io.ku niaw[email p o ec ed], al .p[email p o ec ed], co[email p o ec ed],
[email p o ec ed], ob[email p o ec ed]
DOI: 10.15598/aeee. 16i2.2778
Abs ac . Nowadays, Cu2O is e y p omising elec-
ode ma e ial o pho oelec ochemical applica ions. In
his pape , we epo on he con ollable syn hesis o
Cu2O single pa icles as well as compac laye s on
Bo on Doped Diamond (BDD) elec odes using po en-
ios a ic deposi ion in con inuous and pulse mode. The
BDD laye s we e p epa ed wi h di e en B/C a ios in
he gas phase in o de o in es iga e bo on doping le el
in luence on he Cu2O p ope ies. The e ec o elec-
odeposi ion condi ions such as deposi ion egime and
pulse du a ion was in es iga ed as well. The Cu2O co -
e ed BDD elec odes we e analysed by Scanning Elec-
on Mic oscopy (SEM) and Raman spec oscopy. Im-
p o emen in he homogenei y o he elec odeposi and
emo al o clus e s we e achie ed when he pulse po-
en ios a ic egime was used. Using he same pulse
elec odeposi ion pa ame e s, we con i med he possibil-
i y o con olling he deposi ion a e o Cu2O by a y-
ing he BDD conduc i i y. Finally, we we e able o
scale he size o Cu2O pa icles by changing he numbe
o deposi ion pulses. The ob ained esul s ha e shown
a g ea po en ial o con olling he mo phology, amoun ,
size and dis ibu ion o Cu2O ilms on BDD subs a es
by changing he bo on doping le el and elec odeposi ion
condi ions as well. The in es iga ions epo ed he ein
allowed us o be e unde s and he deposi ion mecha-
nism o Cu2O on BDD elec odes which could hen be
used o p epa a ion o ac i e laye s o elec ochemical
applica ions and in op oelec onic de ices such as sola
cells and pho ode ec o s.
Keywo ds
Bo on doped diamond, cup ic oxide, chemical
apo deposi ion, pulse pla ing.
1. In oduc ion
Diamond possesses many excep ional p ope ies such
as he highes ha dness and he mal conduc i i y,
excellen wea esis ance, chemical ine ness and
he lowes ic ion coe icien . The e o e, diamond
ilms g own by Chemical Vapo Deposi ion (CVD)
ound wide ange o applica ions in elec onics,
op ics, elec ochemis y and o he ields [1], [2],
[3] and [4]. In addi ion, con olled bo on doping
enables o adjus conduc i i y which has a posi i e
impac mainly on he sensi i i y and selec i i y o
BDD elec odes used o elec ochemical applica-
ions [5]. Elec ochemical eac ions pe o m mos ly
a he in e ace be ween elec oly e solu ions and
he elec odes su aces. The e o e, modi ica ion o
he elec ode su ace mo phology is a key ac o
o uning he elec ode pe o mance [6] and [7].
Elec odeposi ion o cup ous oxide (Cu2O) mic o-
c ys als may be used o con ol su ace p ope ies
o biosensing o bioca aly ic applica ions. Cu2O is
well known as one o he s able oxide o ms o coppe
which has a b ownish- ed colo and a bandgap o
c
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2.0–2.2 eV [8]. Cup ous oxide is an in e es ing subs i-
u e o noble me al ca alys s owing o i s signi ican
ca aly ic ac i i y [9]. O he ad an ages o Cu2O in-
clude he abundance o he p ecu so ma e ials, non-
oxic na u e and cos e ec i e syn hesis ou es. Cu2O
exhibi s se e al a ac i e cha ac e is ics o op oelec-
onic de ices such as sola cells, lase s and pho ode-
ec o s due o i s high abso p ion coe icien and good
majo i y ca ie mobili y [10] and [11]. BDD is e y
p omising candida e as a subs a e o Cu2O based
pho oelec odes due o chemical ine ness, mechanical
s abili y, and i suppo s he cha ge sepa a ion wi hin
he semiconduc o and acili a e he pho oca aly ic ac-
i i ies in gene al [12] and [13]. Cu2O hin ilms can
be p epa ed using a ious me hods including chemical
deposi ion, eac i e e apo a ion, Chemical Vapo De-
posi ion (CVD), he mal oxida ion and sol-gel [8]. In
con as o o he syn hesis p ocesses elec osyn hesis is
a ela i ely simple and e sa ile echnique ha is pe -
o med a a mosphe ic p essu e and does no equi e
high empe a u es. Mo eo e , i allows a good con-
ol o he p oduc s by con olling pa ame e s such as
po en ial, cu en densi ies, pH o p ecu so concen a-
ion in he elec oly e. This wo k is aimed o demon-
s a e he possibili y o elec odeposi ion o Cu2O pa -
icles and ull laye s on he BDD elec odes. Fo he
i s ime, he in luence o bo on doping le el on he
Cu2O mo phology is in es iga ed.
2. Expe imen al
Polyc ys alline BDD elec odes we e p epa ed by
plasma enhanced Ho Filamen Chemical Vapo De-
posi ion (HF CVD) [14]. Be o e he BDD deposi ion
he silicon subs a es we e seeded in an ul asonic ba h
in suspension o 50 mg nanodiamond powde (diame e
< 10 nm, CAS No. 7782–40–3, Sigma Ald ich) in 1 l o
demine alized wa e (18 MΩ) o 40 minu es. The BDD
laye s wi h hickness o 300±50 nm we e deposi ed o
2 hou s in a CH4/H2gas mix u e wi h an addi ion o
ime hylbo on a p ocess p essu e o 3 000 Pa. The
B/C concen a ion in he gas phase was se up o 0,
2 000, 4 000, 8 000, 10 000, 15 000 and 20 000 ppm
and he concen a ion o CH4in H2 o 1 %. The sub-
s a e holde empe a u e 700 ◦C was moni o ed du -
ing he g ow h p ocess by a he mocouple. Finally,
BDD samples we e ixed in o p in ed ci cui boa d sup-
po , elec ically connec ed by a sil e pas e and iso-
la ed by a polyme pas e (ESL 240-SB) (Fig. 1). So-
lu ion con aining 100 mM sodium ace a e, C2H3NaO2,
and 100 mM coppe (II) ace a e, Cu(CH3COO)2, wi h
pH o 5.6 was used o syn hesize he Cu2O. Elec ode-
posi ion o Cu2O pa icles was conduc ed in a glass
cell wi h a BDD wo king elec ode, pla inum coun e
elec ode and a sil e /sil e chlo ide e e ence elec ode
(Ag/AgCl 1 M sa u a ed KCl) using a BioLogic SP–
150 gal anos a /po en ios a . In he case o po en io-
s a ic deposi ion, a po en ial o −1V was applied o
10 s and in he case o po en ios a ic pulse elec odepo-
si ion, 5 pulses o −1V o 2 s wi h du y cycle o 50 %
we e applied. The po en ios a ic and pulsed po en io-
s a ic p o ocols we e chosen in o de o ha e simila o-
al cha ge o bo h elec odeposi ion p ocedu es. P e-
pa ed se ies o BDD laye s we e analyzed by scanning
elec on mic oscopy and Raman spec oscopy a oom
empe a u e. Scanning elec on mic og aphs o Cu2O
laye s we e ob ained using a JEOL 7500F ins umen
ope a ing a 10 kV. Mic o-Raman spec oscopy (Con-
ocal Raman mic oscopy MonoVis a CRS 750/BX51
manu ac u ed by S&I Spec oscopy) spec oscopy was
pe o med using an a gon lase (λ= 514.5 nm) as he
exci a ion sou ce. Each p esen ed spec um is an a e -
age o wen y con inuously acqui ed spec a wi h a col-
lec ion ime o 3 seconds each.
(a) (b) (c) (d)
Fig. 1: P ocess o ixa ion o BDD elec odes in o he elec ode
holde s – (a) elec ode holde , (b) connec ion o BDD
elec ode using conduc i e sil e pas e, (c) applying o
polyme isola ion pas e, (d) pho o o eal elec ode.
3. Resul s and Discussion
Fi s , we ha e in es iga ed he di e ence be ween pulse
and con inuous deposi ion. Fo his pu pose, he BDD
elec ode wi h concen a ion B/C = 10 000 ppm and
CH4/H2= 1 % was used (Fig. 3(a)). By applying
he pulse deposi ion (Fig. 2), Cu2O g ains doubled in
size compa ed o he no mal po en ios a ic deposi ion
we e ob ained along wi h he emo al o clus e s and
imp o ed homogenei y o he deposi (Fig. 3(c)). We
suppose ha i is because each o he pulses ini ia es
a new nuclea ion p ocesses on he su ace si e wi h he
c
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0 4 8 12 16 20
-10
-8
-6
-4
-2
0
2
4
J
(
m A /c m
2
)
Time (seconds)
Con inuous deposi ion
Pulse deposi ion
Fig. 2: E olu ion o he cu en densi y du ing he con inuous
and pulse elec odeposi ion o Cu2O.
Fig. 3: SEM mic og aphs showing (a) BDD subs a e be o e
Cu2O deposi ion, (b) Cu2O laye deposi ed by con in-
uous deposi ion (10 s) and (c) Cu2O laye deposi ed by
pulse deposi ion (5×2 s).
bes condi ions o elec odeposi ion which esul s in
a mo e uni o m deposi ion. This is i s ep esen ed by
he mo e conduc i e BDD laye and a e a homoge-
neous co e ing also by he o med Cu2O g ains. This
beha iou causes a mo e uni o m and as e deposi ion.
On he o he hand, in he case o con inuous deposi ion
sha pe Cu2O c ys als we e obse ed, which migh be
mo e a ou able o elec ochemical eac ions in some
cases (Fig. 3(b)).
The p epa ed samples o con inuously and pulse de-
posi ed Cu2O BDD laye s we e analyzed by Raman
spec oscopy (Fig. 4). The bo on doping is ep esen ed
in Raman spec a by wo b oad bands a app oxi-
ma ely 500 cm−1and 1220 cm−1, which a e associa ed
wi h inco po a ion o bo on in o he diamond la ice.
The 500 cm−1maximum is a ibu ed o he local i-
b a ional modes o he bo on pai s and he small shoul-
de a 1320 cm−1is associa ed wi h polyc ys alline di-
amond in highly bo on doped ilms [15] and [16]. Ra-
200 400 600 800 1000 1 200 1400 1600
B
In e ns i y ( a. u .)
G
D
B
Si
Cu
2
O
Si
Si
Cu
2
O
Cu
2
O
Con inuous deposi ion
Pulse deposi ion
Raman shi (cm
-1
)
Fig. 4: Raman spec a o Cu2O deposi ed on BDD elec odes
wi h B/C = 10 000 ppm and CH4/H2= 1 % using
po en ios a ic deposi ion and pulse po en ios a ic depo-
si ion.
0 4 8 12 16 20 24
-12
-8
-4
0
4
+ clus e s
Cu
2
O laye
Cu
2
O laye
Cu
2
O pa icles
B/C (ppm)
0
2 000
4 000
8 000
10 000
15 000
20 000
J
(
m A /c m
2
)
Time (seconds)
wi hou Cu
2
O
Fig. 5: E olu ion o he cu en densi ies du ing he pulse elec-
odeposi ion o Cu2O on BDD subs a es p epa ed by
di e en B/C a ios.
man peaks co esponding o Cu2O a e obse able a
152 cm−1, 216 cm−1and 630 cm−1[17]. The obse ed
Raman signals indica e he p esence o Cu2O while no
CuO peaks we e de ec ed. The de ec ed Raman peaks
a e in good ag eemen wi h li e a u e alues o Raman
modes o Cu2O nanos uc u es [8]. The b oad max-
imum a 303 cm−1, sha p peak a 521 cm−1and he
b oad one a 950 cm−1belong o he silicon subs a e
[8]. In compa ison wi h a con inuous deposi ion, he
pulse deposi ion exhibi s an inc ease o he Cu2O sig-
nals and a dec ease o he o he peaks which is mos
p obably caused by a hicke Cu2O laye .
In he nex pa , we in es iga e he in luence o
bo on doping le el on he elec odeposi ion o Cu2O.
Figu e 5 shows e olu ion o he deposi ion cu en den-
si ies du ing he pulse elec odeposi ion o Cu2O on he
BDD samples wi h a ious bo on doping le els. In ou
p e ious s udy, S o c e al epo ed a signi ican de-
c ease o shee esis ance wi h inc ease o bo on con en
c
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Fig. 6: SEM mic og aphs showing (a), (b) Cu2O c ys als, (c), (d) Cu2O laye , (e), ( ) Cu2O laye wi h clus e s.
in diamond [18]. Thus he inc ease o bo on concen-
a ion and ela ed highe elec ode conduc i i y and
highe amoun o su ace ac i e si es accele a ed he
elec odeposi ion o Cu2O on he BDD su ace. The
enhanced BDD conduc i i y enables an inc ease o he
o al elec ic cha ge passed h ough he subs ance and,
ollowing he Fa aday’s law, a consequen inc ease o
he mass deposi ed on he elec ode su ace. In he
case o ully co e ed BDD subs a es wi h Cu2O laye ,
8–11 % dec ease o cu en densi y was obse ed du -
ing he pulse deposi ion. This phenomenon is caused
by co e ing he mo e conduc i e BDD laye wi h he
less conduc i e Cu2O laye .
Figu e 6 shows he scanning elec on mic og aphs o
Cu2O c ys als deposi ed on BDD elec odes wi h a i-
ous bo on concen a ions a e pulse deposi ion shown
in Fig. 5. On he elec ode wi h B/C = 0 ppm no
deposi ed Cu2O was obse ed, which is p obably due
o e y low BDD conduc i i y and insu icien cha ge
ans e . On he su ace o elec odes wi h B/C =
2 000 ppm and 4 000 ppm, homogenously dis ibu ed
Cu2O c ys als wi h diame e s in he ange o 1–3 µm
we e obse ed. The elec odes wi h B/C = 8 000
and 10 000 ppm we e almos con inuously co e ed by
Cu2O laye , and on he elec odes wi h a io B/C =
15 000 ppm and highe , he co e ing was e en dense
and sphe ical clus e s on op o a compac Cu2O laye
we e obse ed in addi ion. These esul s indica e a di-
ec in luence o he elec ode conduc i i y de e mined
by bo on doping le el on he o al cu en densi y and
consequen mass anspo , hus in luencing densi y
and mo phology o Cu2O on he BDD su ace p o iding
an e ec i e ool o su ace p ope ies con olling. The
Raman spec a (Fig. 7) show inc eased Cu2O peaks a
152 cm−1and a 216 cm−1in he case o elec odes
wi h highe bo on doping le el [8].
This indica es he p esence o hicke laye s caused
by as e g ow h on mo e conduc i e BDD subs a e.
The inc ease in in ensi y o 500 cm−1and 1 220 cm−1
maxima ollows he inc ease in B/C a io in he gas
mix u e du ing deposi ion o BDD ilms e idencing
he inc easing doping le el. A peak a 1 332 cm−1
co esponding o he polyc ys alline diamond was also
eco ded in spec a o he ilms wi h lowe and no bo on
concen a ions [15].
200 400 600 800 1000 1200 1400 1600
B
In e n si y (a . u .)
Si
Cu
2
O
Cu
2
OB/C (ppm)
20 000
15 000
10 000
8 000
4 000
2 000
0
Raman shi (c m
-1
)
Si
Si
B
D
G
Fig. 7: Raman spec a o Cu2O deposi ed on BDD elec odes
wi h a ious B/C concen a ion and CH4/H2=1%
using pulse deposi ion.
Finally, we ied o con ol he size o he Cu2O
laye g ains by a ying he du a ion and num-
be o he pulses main aining he same cha ge.
Fo his pu pose, we choose he elec ode wi h
c
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B/C = 8 000 ppm whe e no Cu2O clus e s we e ob-
se ed. Th ee di e en deposi ions consis ing o (1)
i e pulses wi h a du a ion o 400 ms and du y cy-
cle o 10 % (Fig. 8(a)), (2) en pulses wi h a du a ion
o 200 ms and du y cycle o 5 % (Fig. 8(b)), and (3)
wen y pulses wi h a du a ion o 100 ms du y cycle o
2.5 % (Fig. 8(c)) we e pe o med. SEM mic og aphs
ha e shown ha he size o Cu2O g ains was success-
ully scaled down by applying highe numbe o pulses
wi h sho e du a ion. This phenomenon is caused by
a e mina ion o pa icle g ow h and nuclea ion o new
pa icles du ing nex pulse. Simila in luence o depo-
si ion pulses on size o Cu2O pa icles was epo ed by
Liau e al [19]. Based on he expe imen al esul s and
heo e ical knowledge we can assume ha he numbe
and size o g ains can be di ec ly a ec ed by he num-
be and du a ion o he pulses, which oge he wi h
he bo on doping le el gi e a g ea po en ial o con ol
he amoun , size and dis ibu ion o Cu2O on BDD
subs a e.
Fig. 8: Mo phology o Cu2O laye s deposi ed using di e en
pulses du a ions. The du a ion was se up o (a) 400 ms,
(b) 200 ms and (c) 100 ms.
4. Conclusion
In his s udy, we demons a ed he possibili y o con-
ollable elec odeposi ion o Cu2O pa icles as well as
compac laye s on he bo on doped diamond elec odes.
The BDD elec odes ab ica ed wi h a ious B/C con-
cen a ion in gas mix u e (0–20 000 ppm) we e used o
he deposi ions o Cu2O by po en ios a ic pulse elec-
odeposi ion. Compa ison o con inuous elec odepo-
si ion wi h pulse elec odeposi ion showed signi ican
enhancemen o he homogenei y using a pulse elec-
odeposi ion. The in es iga ions o bo on doping le el
in luence on he mo phology o Cu2O on BDD sub-
s a e has shown se e al in e es ing esul s. In he case
o non doped diamond, no Cu2O deposi ion was ob-
se ed. In he case o B/C = 2 000–4 000 ppm, he
Cu2O mic o pa icles we e obse ed and in he case o
B/C > 8 000 ppm he BDD he su ace was ully co -
e ed wi h a Cu2O laye . The ob ained esul s indica e
a signi ican in luence o he B/C a io on he deposi-
ion a e, densi y and he mo phology o Cu2O ilms
caused by di e en BDD conduc i i y and su ace-
ac i e si es dis ibu ion. Following he SEM in es i-
ga ion, we also ound ha he elec odeposi ed lay-
e s o Cu2O pa icles we e homogeneously dis ibu ed
o e he whole BDD subs a e. Finally, we success-
ully con olled he size o he Cu2O g ains by a ying
he numbe and du a ion o he deposi ion pulses. The
p esen ed in es iga ions ha e shown a g ea po en ial
o con olling he mo phology, amoun , size and dis-
ibu ion o Cu2O ilms on BDD subs a es h ough
he change o bo on doping le el and elec odeposi ion
condi ions as well.
Acknowledgmen
This wo k was inancially suppo ed by he Slo ak Re-
sea ch and De elopmen Agency unde he con ac
No. APVV-16-0124 and by he g an s o Slo ak Na-
ional G an Agency No. 1/0887/16 and 1/0558/17.
The au ho s a e also g a e ul o he suppo o he
DAAD o unding he coope a ion and o he sup-
po by he Thü inge G aduie en o de ung. This
wo k was pa ially suppo ed by he p ojec „Roz oj
yskumnej in as uk u y STU, p ojek c. 003STU-
2-3/2016“ by he Minis y o Educa ion, Science, Re-
sea ch and Spo o he Slo ak Republic. The au ho s
a e also g a e ul o he suppo o ITMS: 26240220084
(Uni e zi ny edecky pa k STU B a isla a). Ou
hanks also belong o Ja osla Ko ac J . o suppo
du ing Raman measu emen .
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Abou Au ho s
Mi osla BEHUL was bo n in B a isla a, Slo akia.
He ecei ed his M.Sc. om Mic oelec onics in 2014
and Ph.D. om Elec onics and pho onics in 2017.
His esea ch in e es s include ca bon ma e ials, hin
laye s deposi ion, elec ochemis y and elec onics.
Ma ian VOJS was bo n in Spisska No a Ves,
Slo akia. He ecei ed his M.Sc. om Elec onics in
2002 and his Ph.D. om Elec onics in 2009. His e-
sea ch in e es s include deposi ion o diamond, ca bon
s uc u es, DLC and cha ac e iza ion o mo phology,
elec ical and elec ochemical p ope ies and Raman
spec oscopy.
Ma ian MARTON was bo n in B a isla a,
Slo akia. He g adua ed in elec onics in 2004
and in 2008 he ecei ed his Ph.D. in elec on-
ics and acuum echnology, bo h a STU in
B a isla a. Cu en ly his esea ch deals wi h ca bon
nanoma e ials, e.g. diamond, CNTs, CNWs and DLC.
Pa ol MICHNIAK was bo n in T s ena, Slo-
akia. He ecei ed his Ph.D. om Elec onics and
Pho onics 2016. His esea ch in e es s include P epa-
a ion o Ca bon Thin Films (Diamond, Ca bon
Nanowalls) by Chemical Vapou Deposi ion.
Ma io KURNIAWAN was bo n in Pema ang
Sian a , Indonesia. He ecei ed his M.Sc. om
Mechanical Enginee ing a he Uni e si y o Tokyo,
Japan in 2013. His esea ch in e es s include nanoma-
e ials, elec odeposi ion, op oelec onics, and ene gy
con e sion.
Ral PEIPMANN was bo n in Ka lsbu g, Ge many.
He ecei ed his Ph.D. in Chemis y om Technical
Uni e si y D esden in 2012. His esea ch in e es s
include in insically conduc ing polyme s, co osion
and co osion p o ec ion and simula ion.
Cod u a Au elia VLAIC was bo n in Cluj-
Napoca, Romania. She ecei ed he Ph.D. om
Chemical Enginee ing in 2012. He esea ch in e es s
include co osion p o ec ion, li hium ion ba e ies and
elec odeposi ion om ionic liquids.
And eas BUND was bo n in Pue lingen, Ge -
many. He ecei ed his diploma om he Uni e si y
o Saa land in 1995. His esea ch in e es s include
undamen al and applied elec ochemis y.
Robe REDHAMMER was bo n in B a isla a,
Slo akia. He ecei ed his Ph.D. om elec onics and
acuum echnology in 1993. His esea ch in e es s
include nano echnology and nanoma e ials.
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2018 ADVANCES IN ELECTRICAL AND ELECTRONIC ENGINEERING 245