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A o dable Au oma ed Modules o Lab-Scale
High-Th oughpu Syn hesis o Ino ganic Ma e ials
Icia Mon e ubio,[a,b]Joseba O i e,[a]Maha Ismail,[a,b]E a is o Cas illo,[a]Ja ie Ga cía,[a]
Ismael Redondo,[a]Jean-Luc Dau e gne,[a]Amaia Sa aciba ,[b]Ja ie Ca asco,[a,c]
Mon se Casas-Cabanas,[a,c]and Ma ine Reynaud*[a]
The de elopmen o sus ainable ad anced ma e ials is inc eas-
ingly d i en by he need o sus ainable, as e , scalable, and
mo e e icien esea ch wo k lows. Ad ancemen s in compu a-
ional sc eening, high- h oughpu expe imen a ion, and a i icial
in elligence (AI) a e accele a ing p og ess in ma e ials disco -
e y. To ully le e age he bene i s o hese complemen a y
app oaches, he implemen a ion o ma e ials accele a ion pla -
o ms (MAPs) and sel -d i ing labo a o ies (SDL) has eme ged
as a p omising s a egy. He e, we p esen he de elopmen
o a semi-au oma ed s a ion o he lab-scale high- h oughpu
syn hesis (HTS) o ino ganic ma e ials, as pa o he Ma e ials
Accele a ion and Inno a ion plaT o m o ENe gy Applica ions
(MAITENA). The sys em in eg a es wo in-house-designed liquid-
handling modules capable o pe o ming sol-gel, Pechini, solid-
s a e, and hyd o/sol o he mal syn heses. Each module enables
he p epa a ion o se e al dozen g am-scale samples pe week
wi h high ep oducibili y and minimal manual in e en ion.
The sys em’s capabili ies a e demons a ed h ough h ee case
s udies in ol ing Li-ion ba e y ma e ials. Resul s highligh he
module’s u iliza ion o e icien sc eening o composi ions and
syn hesis condi ions o a y ma e ials’ p ope ies. This acces-
sible and modula in as uc u e o e s a p ac ical ou e o
implemen ing high- h oughpu s a egies in ino ganic ma e ials
esea ch.
1. In oduc ion
Add essing he global challenges o clima e change and c i -
ical ma e ials sca ci y equi es accele a ing he de elopmen
o sus ainable ad anced ma e ials. While adi ional esea ch
app oaches ha e his o ically been e ec i e, hey ha e become
oo slow and esou ce-in ensi e o mee he u gen demands
o s a egic sec o s such as ene gy, ca alysis, o elec onics.[1–3]
In esponse, Ma e ials Accele a ion Pla o ms (MAPs) and Sel -
D i ing Labo a o ies (SDLs) ha e eme ged as pa adigm-shi ing
[a] I. Mon e ubio, J. O i e, M. Ismail, E. Cas illo, J. Ga cía, I. Redondo,
J.-L. Dau e gne, J. Ca asco, M. Casas-Cabanas, M. Reynaud
Cen e o Coope a i e Resea ch on Al e na i e Ene gies (CIC ene giGUNE),
Basque Resea ch and Technology Alliance (BRTA), Ala a Technology Pa k,
Albe Eins ein 48, Vi o ia-Gas eiz 01510, Spain
E-mail: m eynaud@cicene gigune.com
[b] I. Mon e ubio, M. Ismail, A. Sa aciba
Physical Chemis y Depa men , Pha macy Facul y, Basque Coun y
Uni e si y (UPV/EHU), Ála a, Vi o ia-Gas eiz 01006, Spain
[c] J. Ca asco, M. Casas-Cabanas
Ike basque, Basque Founda ion o Science, Plaza Euskadi 5, Bilbao 48009,
Spain
Suppo ing in o ma ion o his a icle is a ailable on he WWW unde
h ps://doi.o g/10.1002/chem.202502072
© 2025 The Au ho (s). Chemis y - A Eu opean Jou nal published by
Wiley-VCH GmbH. 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.
solu ions. These in eg a ed esea ch in as uc u es combine
au oma ion, high- h oughpu expe imen a ion, and A i icial
In elligence (AI)-d i en decision-making o enable as e and
mo e e icien ma e ials disco e y.[3–10]
Se e al di e en ini ia i es ha e been launched in ecen
yea s o accele a e ma e ials de elopmen including he Ma e-
ials P ojec (USA), BIG-MAP (EU), he Accele a ed Conso -
ium (Canada), and DIADEM (F ance). High- h oughpu heo e -
ical app oaches ha e been widely used o iden i y p omising
ad anced ma e ials. These app oaches include le e aging Den-
si y Func ional Theo y (DFT) calcula ions o p edic new ma e-
ials h ough combina o ial composi ions sc eenings,[11]as well
as mining ma e ials da abases o ind s uc u es wi h desi able
p ope ies using as e alua ion me hods like elec on densi y
analyses[12–14]and bond- alence si e ene gy calcula ions.[15–19]
Al hough compu a ional me hods a e esou ce-e icien al e -
na i es in e ms o ime, ma e ials, and in as uc u e,[20] hey
o en gene a e a la ge numbe o candida es ha equi e labou -
in ensi e expe imen al alida ion. To a oid any bo leneck a his
la e s age, high- h oughpu expe imen a ion becomes essen-
ial.
High-Th oughpu Syn hesis (HTS) allows o an e icien
p oduc ion and es ing o la ge lib a ies o ma e ials. The con-
cep was i s pionee ed in o ganic chemis y by Me i ield
and S ewa in he 1960s o au oma ed pep ide syn hesis,[21]
and has since been widely applied in combina o ial chemis y
and ma e ials science.[1,2,22–29]Howe e , al hough HTS is now
s anda d in ields such as d ug de elopmen , i s applica ion o
ino ganic ma e ials emains limi ed. In gene al, o ganic syn he-
ses a e mo e amenable o au oma ion because hey ypically
Chem. Eu . J. 2025,31, e02072 (1 o 10) © 2025 The Au ho (s). Chemis y - A Eu opean Jou nal published by Wiley-VCH GmbH
ChemEu J
Resea ch A icle
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ollow well-cha ac e ized and a ionalized eac ion pa hways
and a e usually pe o med in solu ions unde mild condi ions.
In con as , ino ganic syn heses in ol e a b oade ange o
elemen s, equen ly equi e he handling, mixing, and eac ing
o solid p ecu so s, and o en demand di e se eac ion con-
di ions including he use o au ogenous p essu e (e.g., hyd o-
and sol o he mal ou es) o high- empe a u e ea men s (e.g.,
solid-s a e ou es); all o which make au oma ion conside ably
mo e challenging.[30–32]When p oducing la ge se s o samples,
high- h oughpu cha ac e iza ions coupled wi h e icien da a
analysis me hodologies a e also essen ial o p e en bo h wo k-
low bo lenecks and misin e p e a ions (e.g., un eliable Rie eld
analysis[33]o o e looked ma e ials diso de [34]). Recen ully
au onomous pla o ms, such as he A-Lab p oposed by Cede
e al., ha e d awn a en ion o hese challenges, highligh ing he
impo ance o obus alida ion p o ocols in au oma ed disco -
e y wo k lows.[33,35]High- h oughpu cha ac e iza ion echniques
can include au oma ed sample p epa a ion and measu emen s
o X-Ray Di ac ion (XRD), elec ochemical p ope ies,[36,37]X- ay
luo escence (XRF) mic oscopy,[38]Scanning Elec on Mic oscopy
(SEM),[39]Raman mic oscopy,[40]e c. As o au oma ed da a
analysis, FullP o APP[41–43]was de eloped o ca y ou au oma ic
Rie eld e inemen s on la ge powde di ac ion da ase s,
PRISMA[44] o p ocessing chemical spec a, and Ba alyse o
p ocessing elec ochemical da ase s.[45]Mo eo e , he in eg a-
ion o AI, pa icula ly machine lea ning models, is inc easingly
enabling eal- ime da a in e p e a ion, anomaly de ec ion, and
p edic i e analysis, he eby enhancing decision-making wi hin
au onomous wo k lows.[46–48]
Ini ial HTS app oaches in ino ganic ma e ials elied on com-
bina o ial sc eening o ma e ials h ough hin- ilm me hods (e.g.,
ALD)[38,49]o d op-cas ing app oaches.[50,51]The eme gence o
mo e sophis ica ed da a-d i en pla o ms has ecen ly aken
high- h oughpu expe imen a ion a s ep u he . Examples o
MAPs include AMANDA[23](pe o ski es and o ganic ma e ials
o pho o ol aics), PANDA[22](elec odeposi ion o polyme ilms
o elec och omic de ices and op oelec onics), MEDUSA[29]
(solu ion-phase syn hesis and elec ochemical sc eening o
me al–ligand complexes), ASTRAL[52](me al oxides o in e ca-
la ion ba e ies), MINERVA[24]and AFION[53](nanoma e ials o
bioimaging, biomedical, and mic oelec onics). Comme cial lab
au oma ion solu ions o e ad an ages such as being eady-
o-use and bene i om echnical suppo , bu hey a e o en
expensi e, and ailo ed o speci ic asks, wi h limi ed lexibil-
i y o modi ica ions o upg ades, and in ol e elying on he
manu ac u e o supplies o eplacemen s. They ypically a ge
ei he mic og am-scale ( ypically o pha maceu ical esea ch) o
la ge-scale (indus ial applica ions) p oduc ions. Howe e , many
ma e ial science esea ch ields equi e in e media e quan i ies
(hund eds o millig ams o g ams), allowing all cha ac e iza-
ions o be conduc ed on a single ep esen a i e sample. This
imp o es eliabili y, as well as p o ides esul s ha be e sup-
po scalabili y de elopmen . In hese cases, in-house-de eloped
solu ions p o ide cos -e ec i e and cus omizable al e na i es.[54]
Such sys ems ha e o in eg a e ailo ed ha dwa e and so -
wa e, and obus quali y p o ocols (e.g., p ecision, calib a ion,
alida ion) o ensu e da a accu acy and eliabili y.
To add ess he limi a ions o exis ing solu ions, in his wo k
we p esen he de elopmen o an in-house s a ion o semi-
au oma ed high- h oughpu ino ganic syn hesis, pa o he
Ma e ials Accele a ion and Inno a ion plaT o m o ENe gy Appli-
ca ions (MAITENA) a CIC ene giGUNE. This s a ion in eg a es
wo unc ional modules ha enable p ecise handling and mixing
o p ecu so solu ions, and suppo a ious syn hesis ou es—
including solid-s a e, sol-gel, Pechini, and hyd o/sol o he mal—
while minimizing manual wo k. Each module can p oduce
up o 12 samples pe un. Typical isola ed yields a e in he
ange o 400 mg o 1 g am, depending on he eac ion condi-
ions, which enables comp ehensi e cha ac e iza ions on single
ba ches. They also o e p ecise mic os uc u e con ol, which
is key o uning ma e ial p ope ies. He ein, we desc ibe he
design and unc ionali y o hese modules and demons a e
hei capabili ies h ough h ee case s udies.
2. Resul s and Discussion
2.1. Desc ip ion o he Modules
The s a ion desc ibed he ein consis s o wo dis inc in-house-
designed au oma ed liquid-handling modules ( e e ed o as
Module-I and Module-II), each capable o syn hesizing 12 sam-
ples simul aneously. Module-I is dedica ed o he p epa a ion o
eac an mix u es o we syn heses, including sol-gel and Pechini
me hods, while Module-II ocuses on solu ion-based syn heses,
such as hyd o- and sol o he mal syn heses. The wo modules a e
shown in Figu e 1.
Bo h modules a e based on a obo ic sys em ha au o-
ma es liquid handling, dispensing, and mixing. This app oach
minimizes manual in e en ion, educes human e o , and con-
ibu es o he o e all p ocess op imiza ion. Ins ead o di ec ly
using solid eac an s, liquid-handling au oma ion enhances
ope a ional ease, allowing o e icien and p ecise handling
o he ma e ials. The ope a ion o he liquid-handling obo
in ol es dispensing he eac an s as uni o m solu ions, whe e
he solubili ies o he eac an s de e mine he concen a ion
ange used o he eac ions. In bo h modules, a se ies o pumps
a e used o dispense he eac an solu ions (A in Figu es 1a,b).
A las scien i ic p og ammable pumps we e i s selec ed as hey
enable accu a e dispensing o he quan i ies equi ed o he
chemical sys ems unde s udy, and hey a e also easy o calib a e
( ide in a). Howe e , hese pumps can be easily subs i u ed in
he sys em by o he ypes o pumps acco ding o he needs. To
mix he eac an s, a di e en app oach was adop ed o each o
he wo modules (Figu e SI1). In Module-I (Figu e 1a), he eac-
an solu ions a e combined and s i ed in a ound lask mixe
(B in Figu e 1a) be o e being in oduced in o he c ucibles (C
in Figu es 1a,andSI1a). This app oach o e s he possibili y o
add one eac an mix u e o ano he one ha has p e iously
been pumped in o he c ucibles. The mixe is au oma ically
cleaned h ee imes wi h dis illed wa e be ween each mix u e.
In Module-II (Figu e 1b), all solu ions a e sepa a ely pumped in o
he inal eac o s (B in Figu es 1b and SI1b). This a oids obs uc-
ion o he sys em in case a iscous solu ion is o med a e
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Figu e 1. Au oma ed liquid-handling modules designed o handle and mix p ecu so solu ions a sui able s oichiome ies o ino ganic syn heses: a)
Module-I o solid-s a e and we syn heses (e.g., sol-gel syn hesis) and b) Module-II o solu ion- ype syn heses (e.g., hyd o- and sol o he mal syn heses). The
main componen s o a) Module-I (A-F) and b) Module-II (A-H) a e indica ed.
mixing he eac an s, gene a es less was e, and esul s as e
compa ed o Module-I. The mixing in he eac o s is done ei he
wi h classical magne ic s i ing o using a e ical s i e (C in
Figu e 1b) o allow high-speed agi a ion when iscous solu ions
a e o med.
To dispense he solu ions in o he di e en eac o s, wo
op ions we e again conside ed: (i) a mul i-axis obo ic a m and
(ii) a wo-axes (x-y) Compu e Nume ical Con ol (CNC) able.
While a obo ic a m p o ides g ea e mo emen lexibili y, i
also in oduces mo e complexi y in e ms o p og amming,
calib a ion, and main enance. In con as , he CNC able (D in
Figu es 1a, b) p o ed o be a mo e accessible and obus al e -
na i e, less cos ly and echnically demanding. I is adap able o
he a ailable space dimensions and p o ed o be mo e p ecise
and eliable o e ime (design schemes a e shown in he Gi Hub
eposi o y ha can be ound in he Suppo ing In o ma ion). In
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he case o Module-II, a ube dis ibu o was coupled o he CNC
able o a oid con amina ion be ween ubes (E in Figu e 1b).
A pH me e (Lab G ade pH P obe Pa # ENV-40-pH om A las
Scien i ic) was also included on he mobile head o he CNC
able(FinFigu e1b), allowing he au oma ed measu emen o
he pH o he solu ion a any momen o he p ocess. Las ly, he
modules include a mul i-posi ion hea ing and mixing pla e (E
and G in Figu es 1a, b, espec i ely), placed below he CNC able,
which allows s i ing and hea ing he solu ions o conduc ing
eac ions and/o concen a ing he esul an mix u es.
In he case o solid-s a e and we syn heses, he sol en
ac ion is en i ely e apo a ed p io o he annealing s ep, o
which he eac o s con aining he mix u e o eac an s a e ans-
e ed o he mu le o ubula u naces using qua z ays (Figu e
SI2). These cus omized ays also ensu e consis en placemen
o he eac o s inside he u nace, which allows acking he
eac o posi ion in he u nace and e en ually co obo a e i
wi h he inal ma e ial’s ea u es (see Sec ion 4c). Bo h ypes o
u naces, used o pe o m syn heses unde ai and con olled
a mosphe es (i.e., A /H2,A ,O
2), espec i ely, a e equipped wi h
p og ammable empe a u e con olle s. These con olle s play a
ole in main aining p ecise con ol o e he hea ing and cooling
amps du ing he syn hesis p ocesses, ensu ing op imal ep o-
ducibili y o he expe imen s by acili a ing compa ison and
alida ion o esul s.
In he case o hyd o- and sol o he mal syn heses, once
he solu ion mix u es a e p epa ed in he bo osilica e eac o s,
hey a e ans e ed o he mic owa e o en (CEM Disco e 2.0)
equipped wi h a obo ic sample handle . This o en enables p e-
cise con ol o he empe a u e and p essu e du ing he eac ion,
hanks o an in a ed empe a u e senso (iWa e) and h ough
he au oma ed sealing and en ing o he au ogenous gases in
he eac o . The u iliza ion o mic owa e hea ing o e s signi i-
can ad an ages o e classical hyd o he mal syn hesis me hods
wi h con en ional hea ing u naces.[55,56]Oneo hemis he
educ ion in syn hesis imes ha enhances he o e all e iciency
o he p ocess enabling a as sc eening o chemical spaces and
syn hesis condi ions.
To ensu e sa e ope a ion, he syn hesis modules a e placed
on a con ainmen ay equipped wi h a pe o a ed uppe shel
ha di ec s any spills in o a lowe compa men . An in e nal en-
ila ion sys em wi hin he cabine emo es apo s du ing sol en
e apo a ion. Elec onic componen s a e loca ed ou side he ay
and kep unde d y condi ions.
2.2. Wo k low
The en i e ha dwa e sys em desc ibed abo e is con olled using
a mic ocon olle (F and H in Figu es 1a, b, espec i ely). He e,
an A duino Mega boa d was chosen; A duino being an open-
sou ce pla o m based on ee ha dwa e and so wa e ha allows
o de elop elec onic de ices and p ojec s in a use - iendly
mode.[57]The A duino Mega boa d is based on he ATmega2560
mic ocon olle , which is a high-pe o mance 8-bi AVR mic o-
con olle . I ope a es a a clock speed o 16 MHz and has 256 KB
o lash memo y o s o ing p og am code.
The expe imen al wo k low is o ches a ed by an in-house
code uploaded on o he A duino mic ocon olle . Figu e 2shows
examples o expe imen al wo k lows o sol-gel syn heses and
hyd o he mal syn heses, ou lining he sequence o ac ions nec-
essa y o ca y ou success ul syn hesis p ocesses using Module-I
and Module-II, espec i ely. An example o code o p epa ing a
se o wel e samples wi h he sol-gel me hod can be ound in
he Gi Hub eposi o y (Supplemen a y In o ma ion). Wo king in
A duino code ins ead o o he languages such as G-code, yp-
ically used when wo king wi h CNC ables,[58]was selec ed o
enable he use o his kind o mic ocon olle and o ensu e a
lexible con ol o e he en i e expe imen al wo k low including
pumps and senso s.
To conduc sol-gel syn heses, Module-I is ypically used o
p oduce a se ies o 12 samples consecu i ely (Figu e 2a). Fi s ,
he desi ed quan i ies o eac an s o sample N =1a eall
pumped in o he mixe om he di e en p ecu so solu ions.
Then, hey a e s i ed in he mixe o a speci ic du a ion. Sub-
sequen ly, he CNC able mo es o align wi h he i s eac o ,
in o which he eac an mix u e is ans e ed om he mixe .
Following his, he dispensing sys em unde goes a se ies o
washing s eps wi h dis illed wa e (DW). A e wa ds, he sys em
is eady o s a he p ocess again o he second sample. In a
ypical se ies o sample p epa a ions, his p ocess is epea ed
12 imes o 12 eac o s ha a e con inuously s i ed. Once all
samples a e p epa ed, hey a e le o s i o e nigh . Then, he
solu ions a e e apo a ed by hea ing a 80 °C un il a solid mix-
u e is ob ained. The A duino mic ocon olle manages he liquid
handling s eps, whe eas hea ing and s i ing a e independen ly
con igu ed be o e each expe imen . Once he e apo a ion s age
is comple e, he eac o s a e ans e ed in o a qua z ay, which
is di ec ly placed in a mu le o ubula u nace o ca y ou he
annealing s ep. A e he he mal ea men , 300–400 mg o each
sample a e ypically eco e ed.
To pe o m syn heses in solu ion (hyd o- o sol o he mal-
syn hesis), Module-II is designed o accommoda e up o 15 sam-
ples simul aneously. The sample p epa a ion consis s o di ec ly
pumping he di e en solu ions in o he indi idual eac o s (30-
mL bo osilica e ubes) h ough he dispense head o he CNC
able. Du ing he p epa a ion p ocess, an au oma ed mixing s ep
can be included using a e ical mixe ha homogenizes is-
cous solu ions h ough igo ous agi a ion (C in Figu e 1b). The
pH o he solu ion can also be measu ed, a any s ep o he
p ocess, using he elec ode a ached o he dispense head
o he CNC able (D in Figu e 1b). Once he p ocedu e in-
ishes, he eac o s a e ans e ed o he mic owa e equipmen
(CEM Disco e 2.0 mic owa e) equipped wi h a obo ic sample
handle o comple e he syn heses in an au onomous manne ,
whe ein di e en pa ame e s such as empe a u e, p essu e, and
ime can be a ied o each sample. A e he mic owa e ea -
men s, he samples a e washed and cen i uged oge he o
collec up o 900 mg o each sample and pe o m he equi ed
cha ac e iza ions.
In bo h cases, he inal amoun o he indi idual samples
allows o he execu ion o all he equi ed cha ac e iza ion
echniques on a single sample, ensu ing consis ency and ep e-
sen a i eness in he analysis.
Chem. Eu . J. 2025,31, e02072 (4 o 10) © 2025 The Au ho (s). Chemis y - A Eu opean Jou nal published by Wiley-VCH GmbH
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Figu e 2. Examples o p og am wo k lows o p oducing N samples by a) sol-gel and b) hyd o he mal syn heses using he au oma ed Modules I and II,
espec i ely.
2.3. Rep oducibili y Conside a ions
To ensu e accu acy and eliabili y o he samples p oduced, a
comp ehensi e p ocess o calib a ions, op imiza ion, and ep o-
ducibili y alida ion is conduc ed o e e y newly de eloped
syn hesis wo k low.
Fo op imal sol-gel syn heses, a ca e ul s udy o he he -
mal dis ibu ion o he hea ing pla e was conduc ed o ensu e
uni o m e apo a ion condi ions ac oss all c ucible posi ions. Ini-
ial esul s e ealed signi ican empe a u e a ia ions o up o
10 °C ac oss he wel e posi ions, which was iden i ied as being
caused by a high a iabili y in he con ac esis ances be ween
he c ucibles and he hea ing pla e. This issue was sol ed by
applying silicone oil o silicone g ease a he bo om o he
alumina eac o s, imp o ing he mal con ac be ween su aces
(Figu e SI3).
Regula calib a ion o he pumps and he u naces is also
pe o med o main ain p ecision and eliabili y. Typical solu ion
olumes pumped ange om 1.3 o 7.6 mL, wi h a ole ance limi
o 0.1 mL es ablished o minimize de ia ion in he sample com-
posi ions. To u he ensu e accu acy, he mola i y o solu ions
is p epa ed be ween 0.3 and 1 M, depending on he eagen .
Figu e SI4 shows ha all pumps ope a e consis en ly wi hin he
es ablished ole ance ange o e ime. The calib a ion esul s o
he mu le and ubula u naces a e p esen ed in Figu es SI5, SI6,
espec i ely. Fo each posi ion, he a e age empe a u e and he
s anda d de ia ion (based on h ee o mo e measu emen s) el-
a i e o each se poin empe a u e a e eco ded as me ada a o
each sample.
2.4. Case S udies
This sec ion p esen s h ee case s udies demons a ing he capa-
bili ies o he au oma ed modules o HTS and op imiza ion o
ino ganic ma e ials. The selec ed examples illus a e he ep o-
ducibili y o he modules and hei p ac ical applica ion o
explo e phase diag ams and mic os uc u al uning.
2.4.1. Rep oducibili y o he Sol-Gel Syn hesis o LiFe0.5Mn1.5O4
LiFe0.5Mn1.5O4(LFMO) is a spinel ma e ial, which equi es p e-
cise syn hesis con ol o p e en he o ma ion o Fe-Li an isi e
de ec s. Twel e samples o LFMO we e p epa ed wi h Module-I
using he sol-gel me hod unde iden ical condi ions (see Supple-
men a y In o ma ion). Figu e 3compa es he XRD pa e ns o he
12 syn hesized ma e ials. The XRD esul s con i m he o ma ion
o a pu e spinel phase o LFMO ac oss all module posi ions, wi h
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Figu e 3. Compa ison o he XRD pa e ns o he LiMn1.5Fe0.5O4spinel samples syn hesized in he 12 posi ions o he au oma ed module (labeled om A1
o C4). Enla gemen s a ound he di ac ion peaks (220) and (222) a e shown on he uppe pa o he igu e.
no signi ican change in ela i e in ensi y o peak b oadening.
No ably, he (220) and (222) e lec ions, known o be sensi i e o
Fe-Li de ec s, emain una ec ed, demons a ing he obus ness
and eliabili y o he au oma ed syn hesis.
The esul s o he Rie eld e inemen s o he 12 XRD pa e ns
a e p esen ed in Figu e SI7, and Table SI4 o Table SI6. The e ined
uni cell pa ame e s o he wel e samples ange om 8.297(2) o
8.307(2) Å, wi h an a e age alue o 8.301 Å. Despi e he mino
a ia ions in annealing empe a u e obse ed ac oss he di e -
en c ucible posi ions in he u nace, he s uc u al pa ame e s
emained consis en , demons a ing he ep oducibili y o he
syn hesis me hod.
2.4.2. Mapping o he Li-Ni-Mn Oxide Pseudo-Te na y Phase
Diag am h ough High-Th oughpu Sol-Gel Syn hesis
Module-I was used o explo e a subse o he pseudo- e na y
phase diag am o Li-Ni-Mn oxides, which ha e been widely
s udied o hei applica ion in ene gy s o age, ca alysis, and
elec onics. As de ailed in he Expe imen al Sec ion, 48 Li-Ni-
Mn oxide samples we e syn hesized ia he sol-gel p ocess
unde iden ical syn he ic condi ions, a ying solely he me al
s oichiome ies o each sample o illus a e he module’s capa-
bili ies o combina o ial syn hesis. The samples we e cha ac e -
ized by Synch o on XRD o iden i y and map he di e en phase
domains o he phase diag am, as shown in Figu e 4.Fo his
analysis, he p og am FullP o APP[41–43]was used o pe o m he
au oma ed phase iden i ica ion and pseudo-Rie eld e inemen
o he 48 XRD pa e ns. The esul s o he e inemen s o a selec-
ion o 4 samples a e ga he ed in Figu e SI8,TableSI7, and Table
SI8. The esul s e eal h ee dis inc egions wi hin he phase
diag am:
1. Region 1 (in yellow in Figu e 4), co esponding o nominal
composi ion LiNi0.5+xMn1.5-xO4(0 ≤x≤1). A ound x =0
(Figu e 5, Poin A), he spinel phase LiNi0.5Mn1.5O4p edom-
ina es. A seconda y phase inc eases as x ises. This phase,
indexed as a ock sal , has been ubiqui ously epo ed as a
seconda y phase in samples ha de ia e om he heo e ical
s oichiome y o LiNi0.5Mn1.5O4.[59]To accoun o he e lec-
ions appea ing a 10–25° (Figu e SI9), i is indexed wi h a
cell pa ame e o 8.28 Å, co esponding o a 2a2b2csupe cell
o he cubic cell commonly epo ed o ock sal phases.[60]
These esul s illus a e ha he spinel phase canno accom-
moda e addi ional NiII in subs i u ion o MnIV, esul ing in he
o ma ion o he ock sal phase as he Ni con en in he
sample inc eases. While bo h phases coexis h oughou his
egion, he spinel diminishes a highe Ni concen a ions.
2. Region 2 (in blue in Figu e 4), wi h nominal composi ion
Li1+2xNi0.5+xMn1.5-xO4(0 ≤x≤0.5). Fo x =0, he LiNi0.5Mn1.5O4
spinel is ob ained (Figu e 5, Poin A). As he Ni and Li con-
en s inc ease, a Li2MnO3(C2/m) laye ed oxide phase appea s,
compensa ing o li hium excess, while he ock sal phase
would balance he nickel excess, as obse ed in Region 1. The
cell pa ame e s o hese phases emain unchanged o e his
ange o composi ions, sugges ing he absence o solid solu-
ion domains o any o hese phases. Towa d he o he end
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Figu e 4. On he le , a pseudo- e na y phase diag am ob ained o he Li-Ni-Mn oxide sys em whe e he black poin s ep esen he nominal composi ions
o he samples, and he colo ed lines indica e he h ee dis inc phase egions iden i ied. A, B, C, and D poin s co espond o selec ed samples, whose
e ined XRD pa e ns a e shown in Figu e SI-8. On he igh , he di ac og ams ob ained o he 48 syn hesized samples. The a ows indica e he inc easing
amoun o Ni and Li in he a ge ed composi ion, and he ob ained phases a e indica ed as headings o each egion.
o his egion, a laye ed oxide (R-3m) eme ges a he expense
o he Li- ich phase, al hough pa e n simila i ies complica e
p ecise phase iden i ica ion.
3. Region 3 (in g een in Figu e 4), wi h nominal composi ion
Li1+2xNi0.5+xMn1.5-xO4(0.5 <x≤1). A single-phase solid-solu ion
domain o a laye ed oxide LiaNi0.5+bMn0.5-bO2(R-3m)isiden i-
ied o e his composi ion ange. Unlike Regions 1 and 2, no
ock sal phase is p esen in his egion.
This case s udy illus a es he module’s capabili y o acili a e
HTS o explo e complex composi ional sc eenings beyond his
Li-Ni-Mn pseudo- e na y phase diag am.
2.4.3. Mic owa e-Assis ed Sol o he mal Syn hesis o LiFePO4
The pe o mance o oli ine- ype LiFePO4(LFP), a s a e-o - he-
a ca hode ma e ial o Li-ion ba e ies, is known o be highly
dependen on i s mic os uc u e and pa icle size, which c i i-
cally in luence li hium-ion di usion and cha ge ans e kine ics.
Module-II was employed o p epa e he eac an s mix u e o he
syn hesis o nine dis inc samples o LFP ia mic owa e-assis ed
sol o he mal ea men , a ying he syn hesis pa ame e s o
modi y he mic os uc u e o he samples (Table SI9). All he syn-
hesized samples show simila XRD pa e ns, wi h la ge peak
b oadening when he samples a e syn hesized a lowe em-
pe a u es wi h sho e imes (Figu e SI10b). The esul s o he
Rie eld analysis o he XRD pa e ns con i med ha a pu e i-
phyli e phase o LiFePO4is ob ained (Figu e SI11,TableSI10,Table
SI11, and Table SI12), while di e ences in he uni cell pa ame e s,
s ains, and a e age c ys alli e sizes a e obse ed, as e lec ed
in Figu e 5A. A he lowes syn hesis empe a u e (160 °C), he
uni cell olume o LFP inc eases wi h syn hesis ime due o he
g ow h o he a and b cell pa ame e s. In con as , a highe em-
pe a u es (180 °C and 200 °C), all h ee cell pa ame e s exhibi
ela i ely s able alues ega dless o he eac ion ime. The s ain
shows a nea ly linea dec ease o e ime a all h ee empe -
a u es. This end sugges s an inc eased homogenei y o he
la ice pa ame e s as he hea ing p ocess ad ances, and could
be a ibu ed o c ys al g ow h ia he coalescence o adjacen
pa icles and pa ial elaxa ion o su aces. The appa en a e -
age c ys alli e sizes also inc ease wi h syn hesis ime a all h ee
empe a u es, anging in size om 42 o 74 nm, indica ing he
p og essi e g ow h o he c ys alline s uc u e h oughou he
hea ing ea men . SEM indeed e ealed a a ie y o pa icle
sizes and mo phologies ob ained om sligh modi ica ions o
he syn hesis pa ame e s (Figu e 5B). A he sho es syn hesis
imes (5 minu es) (Figu e 5B-a,d,andg), elonga ed pseudo-
hexagonal nanoshee s a e o med. A 160 °C (Figu e 5B-a,b,and
c), pa icle hickness and size inc ease wi h syn hesis ime, ansi-
ioning om agglome a es o independen pa icles (100-300 nm
in leng h and 40–60 nm in hickness). A he highes empe a-
u e (200 °C) (Figu e 5B-g, h, and i), pa icles s a hicke , o ming
la ge semi-welded s uc u es wi hin 15 minu es. F om his poin
onwa ds, c ys alline g ow h is igge ed and, e en ually, hese
s uc u es end up sin e ing in o much la ge pa icles (500 nm
o mic ons). A 180 °C (Figu e 5B-d, e, and ), pa icles e ol e in o
unique hollow nanop isms (Figu e SI12).
This case s udy illus a es he capabili y o he modules o
sys ema ically p epa e a se ies o samples o an au oma ed
sc eening o syn hesis condi ions, enabling an e icien assess-
men o hei impac on ma e ial p ope ies.
3. Conclusion
The HTS s a ion, de eloped wi hin he MAITENA Ma e ials Accel-
e a ion Pla o m, in eg a es wo in-house-designed modules ha
enable he p ecise and ep oducible p epa a ion o se ies o sam-
ples wi h a wide ange o ino ganic syn hesis ou es, including
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Figu e 5. A) E olu ion o he uni cell pa ame e s, c ys alli e size, and s ain alues as he syn hesis empe a u e and ime o he LFP samples inc ease.
S anda d de ia ions a e no clea ly isible in he igu e, as hey a e on he o de o 10−4, ende ing hem oo small o be disce ned. B) Pa icle mo phology
and size e olu ion wi h empe a u e, om 160 o 200 °C, and syn hesis ime, om 5 o 30 minu es o he LFP samples (160 °C, a-c; 180 °C, d- ; 200 °C, g-i)
moni o ed by SEM.
sol-gel, Pechini, solid-s a e, and hyd o/sol o he mal me hods.
The modula and lexible design, coupled wi h open-sou ce con-
ol and cus omizable ha dwa e, p o ides a cos -e ec i e al e -
na i e o comme cial au oma ion sys ems, speci ically adap ed
o mee he in e media e-scale needs o ma e ials science
esea ch.
The ep oducibili y and e sa ili y o he modules we e
demons a ed h ough h ee case s udies in ol ing he syn he-
sis o Li-ion elec ode ma e ials: (i) he consis en syn hesis o
12 LiFe0.5Mn1.5O4samples con i med he high ep oducibili y o
he au oma ed p ocess o sol-gel syn hesis; (ii) a combina o-
ial syn hesis o 48 Li-Ni-Mn oxide composi ions enabled he
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mapping o a pseudo- e na y phase diag am, showcasing he
sys em’s po en ial o accele a ed disco e y; and (iii) he sys em-
a ic a ia ion o syn hesis pa ame e s in he mic owa e-assis ed
hyd o he mal syn hesis o LiFePO4highligh ed he sys em’s
capaci y o mic os uc u al uning.
These modules enable an easy shi om adi ional lab-
scale expe imen a ion o high- h oughpu wo k lows. They allow
he p oduc ion o ma e ial quan i ies sui able o ho ough
cha ac e iza ion and u u e scalable de elopmen . T adi ionally,
he manual p epa a ion o ino ganic ma e ials ypically limi ed
esea che s o jus a hand ul o a couple dozen samples pe
week, depending on he complexi y o he syn hesis. In con-
as , he au oma ed modules p esen ed in his wo k consis en ly
deli e se e al dozen samples pe module wi hin he same ime-
ame; esul ing in a 5- o 10- old inc ease in h oughpu while
deli e ing consis en and eliable ou comes. We belie e his
accessible and adap able solu ion can help mo e owa d mo e
e icien ma e ials de elopmen wo k lows and ul ima ely accel-
e a e inno a ion and b eak h oughs in he ene gy sec o and
beyond.
Suppo ing In o ma ion
The au ho s ha e ci ed addi ional e e ences wi hin he Suppo -
ing In o ma ion.
Acknowledgmen s
The au ho s hank D . F ancisco Bonilla o he assis ance and
se ice o he SEM pla o m. The sXRD expe imen s we e pe -
o med a BL04-MSPD beamline a ALBA Synch o on wi h
he collabo a ion o F ançois Fau h. This wo k was ca ied
ou a CIC ene giGUNE (Spain) and was suppo ed h ough
unding om he Spanish Minis e io de Ciencia y Uni e -
sidades and Agencia Es a al de In es igación (MICIU/ AEI
/10.13039/501100011033), FSE in ie e en u u u o, and ERDF/EU
h ough he p ojec s ION-SELF ( e . PID2019-106519RB-I00) and
SMART ( e . PID2022-140823OB-I00) and h ough he PhD g an
PRE2020-092978, om he Basque Go e nmen h ough he PhD
g an PRE_2021_2_0160 and he p og am ELKARTEK CICe2025
( e . KK2025-00054), and om he Eu opean Commission’s Ho i-
zon 2020 esea ch and inno a ion p og amme h ough he
Fi s S akeholde Ini ia i e o he BIG-MAP p ojec , unde g an
ag eemen No 957189.
Con lic o In e es
The au ho s decla e no con lic o in e es .
Da a A ailabili y S a emen
The da a ha suppo he indings o his s udy a e openly a ail-
able in Gii hub and Zenodo a h ps://doi.o g/10.5281/zenodo.
15608412, e e ence numbe 15 608 412.
Keywo ds: au oma ed syn hesis modules •hyd o he mal syn-
hesis •ma e ials accele a ion pla o m •sel -d i en labo a o y
•sol-gel syn hesis
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