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E ec o Reac ion Condi ions on he Cop ecipi a ion o Ni(OH)2 o Li hium-Ion
Ba e ies
© 2023 he Au ho s
Published e sion
Tynjälä, Pekka; Laine, Pe e i; Välikangas, Juho; Kauppinen, Toni; Lassi, Ulla
Tynjälä, P., Laine, P., Välikangas, J., Kauppinen, T., & Lassi, U. (2023). E ec o Reac ion
Condi ions on he Cop ecipi a ion o Ni(OH)2 o Li hium-Ion Ba e ies. Chemical Enginee ing
and Technology, 46(11), 2279-2284. h ps://doi.o g/10.1002/cea .202300086
2023
E ec o Reac ion Condi ions on he
Cop ecipi a ion o Ni(OH)
2
o Li hium-Ion
Ba e ies
Elec ochemical pe o mance o ca hode ac i e ma e ials (CAMs) is dependen on
he p ope ies o cop ecipi a ed p ecu so s (pCAMs). This is a sensi i e p ocess
a ec ed by se e al eac ion pa ame e s such as empe a u e, pH, concen a ion o
eac an s, agi a ion a e, and esidence ime. In his pape , he e ec o pa ame e s
in luencing he pa icle size g ow h and he physical p ope ies, such as pa icle
mo phology and apped densi y, was s udied in he cop ecipi a ion o Ni(OH)
2
.
Fo ma ion o a homogeneous popula ion wi h na ow pa icle size dis ibu ion
was obse ed, ollowed by a mo e he e ogeneous popula ion o dense pa icles.
Ammonia concen a ion and esidence ime had signi ican e ec s on pa icle size
g ow h and mo phology, bu agi a ion a e also had an impac .
Keywo ds: Ba e y chemicals, Cop ecipi a ion o Ni(OH)
2
, Li hium-ion ba e ies, Nickel
hyd oxide
Recei ed: Feb ua y 05, 2023; e ised: Ma ch 25, 2023; accep ed: May 25, 2023
DOI: 10.1002/cea .202300086
1 In oduc ion
Li hium-ion ba e ies (LIBs) a e ex ensi ely used in po able
elec onics and elec ic ehicle (EV) applica ions due o hei
high ene gy, powe densi y, and enhanced cycle li e compa ed
o o he echa geable ba e ies, such as lead-acid o NiMH ba -
e ies [1]. Pu e LiNiO
2
(LNO) is a p omising candida e as a
ca hode ma e ial in Li-ion ba e ies, as i is Co- ee and has a
high heo e ical capaci y o 274 mAh g
–1
[2–5]. The elec o-
chemical p ope ies o ca hode ma e ials may be aylo ed du -
ing he cop ecipi a ion o p ecu so s by applying p ocedu es
such as, e.g., doping wi h a ying elemen s [6] and by cop eci-
pi a ion o p ecu so s ha ing concen a ion g adien s o ansi-
ion me als wi hin he seconda y pa icles [7].
Key LNO p ope ies a e ailo ed p io o li hia ion du ing
he cop ecipi a ion o p ecu so Ni(OH)
2
[4]. In addi ion o i s
chemical composi ion, hese include apped densi y (po osi y),
pa icle size, and seconda y pa icle size dis ibu ion. These
mo phological ea u es o he ac i e pa icles a e usually de e -
mined du ing he syn hesis o Ni(OH)
2
[8].
Se e al possibili ies a e a ailable o making LNO, such as
cop ecipi a ion, sol-gel syn hesis [9], and solid-s a e eac ions
a high empe a u e [10]. Cop ecipi a ion is he indus ially el-
e an me hod and is conside ed in his pape . Du ing he
cop ecipi a ion, se e al pa ame e s a e p esen simul aneously,
a ec ing he pa icle size g ow h and pa icle mo phology [11].
The op imiza ion o p ecipi a ion pa ame e s may be challeng-
ing and ime-consuming because some pa ame e s may in lu-
ence ano he . Fo example, changing he pH may al e he con-
cen a ion o ammonia and hus a ec ing he concen a ion o
ansi ion me al ammine complexes [12]. Also, he change o
agi a ion a e may al e he e ec i e olume o a eac o , hus
a ec ing he esidence ime o he p ocess. The e o e, op i-
mized cop ecipi a ion condi ions may be conside ed as a com-
p omise o se e al pa ame e s applied o a ce ain eac o
con igu a ion.
In his pape , he e ec o eac ion condi ions on he cop eci-
pi a ion o nickel hyd oxide ca hode p ecu so ma e ial was
s udied. In he se ies o cop ecipi a ion expe imen s, he impac
o p ocess a iables, such as eac an concen a ion, ammonia
concen a ion, esidence ime, and agi a ion a e, was s udied.
2 Expe imen al
2.1 Cop ecipi a ion o Ni(OH)
2
Sphe ical Ni(OH)
2
p ecu so s we e syn he ized using alkali
me al hyd oxide (NaOH) cop ecipi a ion in an ine gas (ni o-
gen) a mosphe e, acco ding o li e a u e e e ences [13, 14].
Ine gas was used o p e en he oxida ion o p ecu so . P e-
Chem. Eng. Technol. 2023,46, No. 00, 1–7 ª2023 The Au ho s. Chemical Enginee ing & Technology published by Wiley-VCH GmbH www.ce -jou nal.com
Pekka Tynja
¨la
¨
1,2,
*
Pe e i Laine
1,2
Juho Va
¨likangas
1,2
Toni Kauppinen
1,2
Ulla Lassi
1,2
This is an open access a icle unde
he e ms o he C ea i e Commons
A ibu ion-NonComme cial-
NoDe i s License, which pe mi s
use and dis ibu ion in any
medium, p o ided he o iginal
wo k is p ope ly ci ed, he use is
non-comme cial and no
modi ica ions o adap a ions a e
made.
–
1
D . Pekka Tynja
¨la
¨([email p o ec ed]), Pe e i Laine,
Juho Va
¨likangas, Toni Kauppinen, P o . Ulla Lassi
h ps://o cid.o g/0000-0001-5319-9525
Uni e si y o Oulu, Resea ch uni o Sus ainable Chemis y, Pen i
Kai e an ka u 1, 90570 Oulu, Finland.
2
D . Pekka Tynja
¨la
¨, Pe e i Laine, Juho Va
¨likangas, Toni Kauppinen,
P o . Ulla Lassi
Uni e si y o Jy askyla, Kokkola Uni e si y Conso ium Chydenius,
Talonpojanka u 2 B, 67100 Kokkola, Finland.
Resea ch A icle 1
These a e no he inal page numbe s! ((
cipi a ion was conduc ed in a con inuous- low s i ed- ank
eac o (CSTR) wi h a eac o olume o 3 L a empe a u es o
40, 50, o 60 °C unde igo ous agi a ion (Fig. 1) using di e en
agi a ion a es. The key pa ame e s du ing he cop ecipi a ion
included empe a u e, pH, agi a ion a e, esidence ime, as
well as hyd oxide, ammonia, and me al solu ion concen a-
ions.
The eac o was p eloaded wi h deionized wa e ; hen, aque-
ous solu ions o me al sul a e NiSO
4
6H
2
O, NaOH, and con-
cen a ed ammonia we e ed sepa a ely o he eac o using
pe is al ic pumps. The ammonia concen a ion in he solu ion
was measu ed equen ly du ing he p ecipi a ion and i was
adjus ed based on he a ge ammonia concen a ion du ing
he expe imen .
Pa icle size g ow h du ing Ni(OH)
2
cop ecipi a ion was ol-
lowed by de e mining he pa icle size dis ibu ion o he slu y
sampled om he eac o ’s o e low ubing. The solu ion was
hea ed o a p ecipi a ion empe a u e, and he pH was adjus ed
o a desi ed le el wi h NaOH solu ion. The eeding a es o
nickel sul a e, NaOH, and ammonia solu ions we e adjus ed o
main ain he desi ed esidence ime. A e cop ecipi a ion, he
p ecu so slu y was il e ed in a acuum, and he p ecipi a e
was ca e ully washed wi h a su icien amoun o wa m deio-
nized wa e . The syn he ized Ni(OH)
2
p ecu so s we e d ied
o e nigh a 60 °C in a acuum o en.
2.2 Cha ac e iza ion o Ni(OH)
2
The apped densi y was measu ed using an E weka SVM 222
apped densi y analyze acco ding o he ISO EN 787/11 s an-
da d. The e olu ion o pa icle size dis ibu ion du ing cop eci-
pi a ion was ollowed using a Mal e n Mas e size 3000. The
ammonia concen a ion o he mo he liquo was analyzed by
au oma ic i a ion using a 1 mol L
–1
HCl solu ion. Field emis-
sion scanning elec on mic oscopy (FESEM) images o he pa -
icle mic os uc u e we e ob ained on a Zeiss Sigma a he
Cen e o Ma e ial Analysis o he Uni e si y o Oulu, ope a -
ing a 5 kV.
3 Resul s and Discussion
3.1 E ec o Tempe a u e on P ecipi a ion
Cop ecipi a ion is ypically done a empe a u es o 40–80 °C.
The empe a u e is known o ha e a signi ican e ec on cop e-
cipi a ion kine ics o ansi ion me al hyd oxide ma e ials [15].
In his s udy, he impac o p ecipi a ion empe a u e was i s
s udied using empe a u es o 40–60 °C. The mo phology o
he p ecipi a ed Ni(OH)
2
pa icles was ollowed and is p e-
sen ed in Fig. 2.
Acco ding o FESEM imaging, he highe p ecipi a ion em-
pe a u e led o he o ma ion o mo e closely packed p ima y
pa icles. A he highes p ecipi a ion empe a u e, c acking o
he seconda y pa icles was obse ed. The ob ained pa icle
mo phology p esen ed in Fig. 2 is compa able o ha epo ed
ea lie by Yang e al. [11]. The de e mined apped densi y al-
ues o he p ecu so s p ecipi a ed a di e en empe a u es a e
gi en in Tab. 1. They we e consis en wi h isual obse a ions.
The mos homogeneous pa icle size dis ibu ion wi h ac-
cep able apped densi y was achie ed a a cop ecipi a ion em-
Chem. Eng. Technol. 2023,46, No. 00, 1–7 ª2023 The Au ho s. Chemical Enginee ing & Technology published by Wiley-VCH GmbH www.ce -jou nal.com
Figu e 1. Con inuous s i ed- ank eac o used o cop ecipi a-
ion.
Figu e 2. E ec o p ecipi a ion empe a u e on he mo phol-
ogy o p ecu so s.
Table 1. Tapped densi y alues o he Ni(OH)
2
p ecu so s p e-
cipi a ed a di e en empe a u es.
P ecipi a ion empe a u e [°C] Tapped densi y [g cm
–3
]
40 1.86
50 2.00
60 2.07
Resea ch A icle 2
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pe a u e o 40 °C. Highe empe a u es, especially 60 °C, e-
sul ed in he c acking o he seconda y pa icles. The e o e,
based on he obse a ions made in Fig. 2, he p ecipi a ion em-
pe a u e 40 °C was selec ed o u he s udies.
3.2 E ec o Cop ecipi a ion Condi ions on Pa icle
Size G ow h
Du ing he eac ion, Ni(OH)
2
p ecipi a ion occu ed as ol-
lows:
Me alammonia complex o ma ion:
Ni2þþnNH3fiNi NH3
ðÞ
n

2þ(1)
Me alhyd oxide p ecipi a ion eac ion:
Ni NH3
ðÞ
n

2þþ2OHfiNi OHðÞ
2þnNH3
(2)
The o ma ion o ansi ion me al hyd oxide p ecu so s
om a me al sul a e solu ion in ol es se e al physicochemical
phenomena. Due o hei high solubili y p oduc , ansi ion
me al sul a es eadily dissol e in wa e . I he pH o he solu ion
is inc eased by adding NaOH, ansi ion me al hyd oxides a e
p ecipi a ed. In he case o impu e solu ions, impu i y phases
may o m [16] in he p esence o ansi ion me als and g oup
II/III me als.
Pa icle size g ow h du ing Ni(OH)
2
cop ecipi a ion (Fig. 4)
a 40 °C was ollowed by de e mining he pa icle size dis ibu-
ion as desc ibed in Sec . 2.1. Du ing he i s s age o he p e-
cipi a ion p ocess, a pa icle popula ion wi h a homogeneous
size was o med. As he popula ion g ew, he pa icles appea ed
o be dense and sphe ical, esul ing in a na ow pa icle size
dis ibu ion. The g ow h o he i s pa icle popula ion is p e-
sen ed in Fig. 4 (cop ecipi a ion ime o 22 h) and in Fig. 5 (6 h,
12 h, and 18 h). A e a ce ain p ecipi a ion ime, depending
on he p ocess condi ions, a second popula ion o small pa -
icles is o med (Fig. 3, p ecipi a ion ime o 24 h; Fig. 5, 24 h).
The o ma ion o he second pa icle popula ion can also be
seen as a bimodal pa icle size dis ibu ion cu e (Fig. 3).
The g ow h o he i s popula ion subsequen ly slowed
down and inally ceased. Las ly, he sys em eached pa icle size
dis ibu ion equilib ium. Due o he con inuous nuclea ion and
o ma ion o p ima y pa icles, he sys em was composed o
small and highly po ous agglome a es, seconda y pa icles a
a ious g ow h s ages, and dense pa icles ha eached hei
maximum size, esul ing in a ai ly b oad pa icle size dis ibu-
ion. In his con inuous p ocess, he sys em eached a s eady
s a e (Fig. 5, p ecipi a ion imes o 30–33 h). A e 33 h o p e-
cipi a ion, he pa icles we e dense, wi h he apped densi y o
2.1 g cm
–3
.
The g ow h o he i s pa icle popula ion and he o ma ion
o a s eady-s a e pa icle size dis ibu ion in a con inuous co-
p ecipi a ion is p esen ed in Fig. 5. The obse ed pa icle
g ow h is in acco dance wi h esul s epo ed by Zheng e al.
[17].
Chem. Eng. Technol. 2023,46, No. 00, 1–7 ª2023 The Au ho s. Chemical Enginee ing & Technology published by Wiley-VCH GmbH www.ce -jou nal.com
Figu e 3. Bimodal pa icle size dis ibu ion a e 30 h o p ecipi-
a ion (D50: 5 mm; apped densi y: 2.1 g cm
–3
).
Figu e 4. E olu ion o Ni(OH)
2
pa icle size dis ibu ion as a
unc ion o p ecipi a ion ime a 40 °C.
Figu e 5. E olu ion o pa icle size dis ibu ion as a unc ion o
p ecipi a ion ime (6–33 h).
Resea ch A icle 3
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3.3 E ec o Ammonia Concen a ion
As illus a ed in Fig. 6, a highe ammonia concen a ion no a-
bly inc eased he g ow h a e o he seconda y pa icle popula-
ion. Unlike in he case o a lowe ammonia concen a ion, he
i s pa icle popula ion g ew con inuously wi hou he spon a-
neous o ma ion o a second popula ion. Due o he highe
ammonia concen a ion, small p ima y pa icles p obably
unde wen dissolu ion/ ep ecipi a ion eac ions simila ly as in
Os wald ipening. The o ma ion o he second pa icle popula-
ion was ini ia ed by dec easing he ammonia concen a ion in
he mo he liquo . Thus, in a CSTR p ecipi a ion p ocess, he
pa icle size and pa icle size dis ibu ion can be ailo ed by
ca e ully con olling he ammonia concen a ion and pH le el.
Addi ionally, he esidence ime also a ec s he p ima y pa i-
cle size g ow h. The sho e he esidence ime is, he highe is
he g ow h a e o seconda y pa icles. The inc eased g ow h
a e may be due o a highe nuclea ion a e, which p o ides
mo e building blocks o he g ow h o seconda y pa icles.
The g ow h o he i s pa icle popula ion s opped wi h a
dec easing ammonia concen a ion in he mo he liquo , which
is in line wi h Ba ai e al. [12].
3.4 E ec o Agi a ion Ra e
P ecu so p ope ies, i.e., o ming o he agg ega es and he
g ow h o he agg ega es, a e highly dependen on he agglom-
e a ion mechanism due o pa icle collisions aking place in he
eac o . The luid mo ion is de e mined by he eac o layou
and he ype and a e o applied agi a ion [18].
Homogeneous mixing is much easie o achie e in a labo a-
o y-scale eac o han in la ge -scale eac o s. The linea
eloci y o he luid mus be g ea e han he se ling eloci y o
he pa icles. O cou se, pa icle size and se ling eloci y o he
pa icles do no scale wi h he size o a eac o . High speci ic
powe inpu (high agi a ion speed) imp o es mixing and he
homogenei y o pa icle suspension in he eac o . Howe e ,
pa icle damage is an unwan ed e ec ha is ela ed o high
agi a ion a es. The e o e, mixing has o be a comp omise
be ween app op ia e homogenei y o he suspension (high agi-
a ion a e p e e ed) and a oidance o unad an ageous p o-
cesses like pa icle damages (low agi a ion a e p e e ed).
The e ec o applied agi a ion ene gy on he ap densi y
and speci ic capaci y has been epo ed by Pu e al. [19].
Inc eased agi a ion ene gy has a posi i e e ec on ap den-
si y, bu oo igo ous agi a ion esul s in dec eased speci ic
capaci y p ope ies. Agi a ion is one possible pa ame e o
con ol he pa icle g ow h and pa icle size dis ibu ion. By
aising he agi a ion ene gy, he pa icle size can be dec eased
when app oaching a s eady s a e in a con inuous cop ecipi a-
ion p ocess (Fig. 7).
3.5 E ec o Residence Time
In a cop ecipi a ion p ocess, p ecu so pa icles de elop om
an amo phous ma e ial o dense and sphe ical seconda y pa -
icles ha ing a mean pa icle size o se e al mic ome e s. Unde
app op ia e eac ion condi ions, he g ow h o seconda y pa -
icles ake place in adial di ec ion, hus esul ing in he p es-
ence o adially o ien a ed c ys alli es inside he pa icle [20]. A
adial g ow h o a seconda y pa icle obse ed in he p esen
s udy is p esen ed in a c oss-sec ional SEM image in Fig. 8.
A sho e esidence ime enhanced signi ican ly he g ow h
a e o he i s pa icle popula ion du ing he i s hou s o he
p ecipi a ion as demons a ed in Fig. 9. The inc eased g ow h
a e may be due o highe nuclea ion a e, hus p o iding mo e
‘‘building blocks’’ o he g ow h o seconda y pa icles.
Chem. Eng. Technol. 2023,46, No. 00, 1–7 ª2023 The Au ho s. Chemical Enginee ing & Technology published by Wiley-VCH GmbH www.ce -jou nal.com
Figu e 6. E ec o ammonia concen a ion on pa icle size
g ow h a e.
Figu e 7. E ec o agi a ion a e on he pa icle size g ow h.
Figu e 8. Radially o ien a ed c ys alli es in a seconda y pa icle.
Resea ch A icle 4
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In a con inuous cop ecipi a ion p ocess he esidence ime
has a signi ican e ec on he ap densi y and he mo phology
o p ecipi a ed seconda y pa icles (Fig. 10).
Unde he used cop ecipi a ion condi ions, esidence imes
ha a e sho e han 2.5 h esul ed in unwan ed p ope ies o
he p oduc . In such cases, he a e age esidence ime in he
eac o is oo sho o he seconda y pa icles o achie e he
desi ed physical p ope ies such as sphe ical mo phology and
high ap densi y.
4 Conclusions
The aim o he p esen pape was o s udy he e ec o eac ion
pa ame e s on he cop ecipi a ion o nickel hyd oxide ca hode
p ecu so ma e ials. In a se ies o cop ecipi a ion expe imen s,
he e ec o p ocess a iables, such as eac an concen a ion,
ammonia concen a ion, esidence ime, and agi a ion a e, was
s udied.
The main conclusions o his esea ch a e as ollows:
– A homogeneous pa icle popula ion wi h a na ow pa icle
size dis ibu ion is always o med be o e a s eady s a e. A
semi-ba ch ype cop ecipi a ion can be applied o p oduce
high-quali y p ecu so pa icles. In a s eady-s a e p ecipi a-
ion, a he e ogeneous pa icle popula ion was o med a y-
ing om small, po ous pa icles o la ge and dense pa icles,
hus esul ing in he b oadening o he pa icle size dis ibu-
ion.
– The concen a ion o ammonia had a signi ican e ec on
he g ow h a e o p ecu so pa icles. Fu he mo e, by ad-
jus ing he ammonia concen a ion o he mo he liquo he
o ma ion o a new pa icle popula ion can be con olled.
– The esidence ime has a no able impac on he physical
p ope ies o he p oduc pa icles. Sho ened esidence
imes esul ed in a p oduc wi h smalle pa icle size, bu
also signi ican ly dec eased ap densi y alues as well as e-
sul ed in poo e mo phology o he pa icles. In CSTR p e-
cipi a ion wi h sho esidence imes, a su icien concen a-
ion o ammonia is essen ial in o de o achie e p ope ap
densi y o he p oduc . The size o he p oduc pa icles can
also be a ec ed wi h an e icien agi a ion in he p ecipi a-
ion eac o .
Al hough knowing a well-known disad an age o ha ing
nume ous conjuga ed p ecipi a ion a iables ha a ec he
quali y o he p oduc , CSTR p ecipi a ion can be used o he
p oduc ion o p ecu so ma e ial wi h desi ed p ope ies by a
s ic con ol o he p ecipi a ion condi ions.
Acknowledgmen
The au ho s acknowledge Business Finland o esea ch und-
ing 2021–2024 (Uni e si y o Oulu, BATCi cle2.0, No. 44612/
31/2020). D . Tao Hu is acknowledged o FESEM analyses.
The au ho s ha e decla ed no con lic o in e es .
Symbols used
D10 [mm] 10 % o pa icles a e smalle han
he gi en D10 alue
D50 [mm] 50 % o pa icles a e smalle han
he gi en D50 alue
D90 [mm] 90 % o pa icles a e smalle han
he gi en D90 alue
Abb e ia ions
CAM ca hode ac i e ma e ial
CSTR con inuous s i ed- ank eac o
LIB li hium-ion ba e y
LNO li hium nickel oxide
pCAM p ecu so o ca hode ac i e ma e ial
SEM scanning elec on mic oscopy
Re e ences
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Figu e 9. E ec o esidence ime on he g ow h a e o he i s
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Resea ch A icle 6
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Chem. Eng. Technol. 2023,46, No. 00, 1–7 ª2023 The Au ho s. Chemical Enginee ing & Technology published by Wiley-VCH GmbH www.ce -jou nal.com
Resea ch A icle: A p ecu so
de e mines he p ope ies o ca hode
ac i e ma e ial in ba e ies. Physical
p ope ies like pa icle mo phology and
apped densi y can be con olled by
op imized p ecipi a ion condi ions. The
e ec o p ecipi a ion pa ame e s, i.e.,
empe a u e, pH, mola a ios o
eac an s, agi a ion a e, and esidence
ime, on he o ma ion o dense,
homogeneous, and sphe ical seconda y
pa icles is e alua ed.
E ec o Reac ion Condi ions on he
Cop ecipi a ion o Ni(OH)
2
o Li hium-
Ion Ba e ies
Pekka Tynja
¨la
¨*, Pe e i Laine,
Juho Va
¨likangas, Toni Kauppinen,
Ulla Lassi
Chem. Eng. Technol. 2023,46 (XX),
XXX KXXX
DOI: 10.1002/cea .202300086
Cop ecipi aon o Ni(OH)2
Cop ecipi aon condions
P ope es o Ni(OH)2
p ecu so
Resea ch A icle 7
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