Towa ds inc eased s eng h and e ained duc ili y o Zn–Mg-(Ag) ma e ials
o medical de ices by adop ing powde me allu gy p ocessing ou es
Jiˇ
í Kub´
asek
a,*
, Selase To ko noo
b,**
, Da id Neˇ
cas
a
, Ing id McCa oll
b
,
Voj ˇ
ech Hyb´
aˇ
sek
a
, Bap is e Gaul
b,c
, E a Jablonsk´
a
d
, ˇ
C omi Donik
e
, I ena Paulin
e
,
Pe e Gogola
, Ma in Kusý
, Zdenˇ
ek Míchal
d
, Ja osla Foj
a
, Mi osla ˇ
Ca ojský
g
,
Jan Duchoˇ
n
h
, Ma k´
e a Ja oˇ
so ´
a
i
, Ja osla ˇ
Capek
a,h
a
Uni e si y o Chemis y and Technology P ague, Facul y o Chemical Technology, Depa men o Me als and Co osion Enginee ing, Technick´
a 5, 6 – Dej ice, 166 28,
P aha, Czech Republic
b
Depa men o Mic os uc u e Physics and Alloy Design, Max-Planck-Ins i u ü Nachhal ige Ma e ialien GmbH, Max-Planck-S aße 1, 40237, Düsseldo , Ge many
c
Depa men o Ma e ials, Impe ial College London, Royal School o Mines, Exhibi ion Road, London, SW7 2AZ, UK
d
Uni e si y o Chemis y and Technology P ague, Depa men o Biochemis y and Mic obiology, Technick´
a 5, 6 – Dej ice, 166 28, P aha, Czech Republic
e
Ins i u e o Me als and Technology, Lepi po 11, SI-1000, Ljubljana, Slo enia
Slo ak Uni e si y o Technology in B a isla a, Facul y o Ma e ials Science and Technology in T na a, Ulica J´
ana Bo u 2781/25, 91724, T na a, he Slo ak Republic
g
Ins i u e o Ma e ials and Machine Mechanics, Slo ak Academy o Sciences, Dúb a sk´
a ces a 9/6319, 845 13, B a isla a, he Slo ak Republic
h
FZU – Ins i u e o Physics o he Czech Academy o Sciences, Na Slo ance 1999/2, 8, P ague, 18200, Czech Republic
i
FZU – Ins i u e o Physics o he Czech Academy o Sciences, Cuk o a nick´
a 112/10, 6, P ague, 16200, Czech Republic
ARTICLE INFO
Keywo ds:
Zinc
Bioabso bable ma e ials
Mechanical alloying
Spa k plasma sin e ing
Mic os uc u e
ABSTRACT
The de elopmen o bioabso bable zinc-based alloys wi h ailo ed mechanical p ope ies and biocompa ibili y
holds g ea p omise o ad ancing medical implan echnology. In his s udy, Zn–Mg and Zn–Mg–Ag alloys we e
syn hesized using mechanical alloying (MA) ollowed by ex usion o achie e a combina ion o enhanced
s eng h, duc ili y, and co osion esis ance. MA o 4 h p oduced ul a ine-g ained powde s inco po a ing
Mg
2
Zn
11
in e me allic phases and oxide pa icles, which con ibu ed o mic os uc u e s abiliza ion du ing
subsequen p ocessing. Ex usion consolida ed hese powde s in o dense ma e ials wi h a uni o m g ain size o
~700 nm, exhibi ing ul ima e ensile s eng hs up o 435 MPa and elonga ion o ac u e o ~12 %, ep esen ing
a signi ican imp o emen o e con en ional p ocessing me hods. The addi ion o sil e u he enhanced he
an ibac e ial p ope ies, demons a ing no able e icacy agains S aphylococcus epide midis, while main aining
non-cy o oxic beha io in i o. Co osion a es emained low, wi h uni o m su ace deg ada ion and he o -
ma ion o p o ec i e co osion laye s. This wo k highligh s he e icacy o combining powde me allu gy ech-
niques o bioabso bable zinc-based alloys wi h excep ional mechanical pe o mance, co osion beha io and in
i o cy ocompa ibili y, p o iding a pa hway o nex -gene a ion biodeg adable medical de ices.
1. In oduc ion
Zn–Mg alloys a e conside ed pe spec i e ma e ials o applica ions in
biodeg adable s en s o o bone ixa ions, especially in maxillo acial
su ge y, due o hei easonable co osion a e and excellen biocom-
pa ibili y [1–3]. Thei unc ion is supposed o be ime-limi ed wi h
comple e eplacemen by newly healed issue [2,4], which helps o
p e en long- e m issues wi h in lamma ions leading, in some cases,
e en o he emo al o he implan as obse ed in o he sys ems
including Mg-based o Fe-based biodeg adable ma e ials. Localized
co osion leads o he p ema u e loss o mechanical in eg i y and
hyd ogen gas (H
2
) elease cas s doub s on he usabili y o Mg-based
ma e ials [2,4]. Fe-based ma e ials deg ade by o ming i on oxide-
s/hyd oxides, which a e no su icien ly soluble in he o ganism and
may cause se ious heal h issues [2,5]. Zinc and i s alloys, on he con-
a y, dissol e slowly in an o ganism, and he co osion eac ions do no
* Co esponding au ho .
** Co esponding au ho .
E-mail add esses: [email p o ec ed] (J. Kub´
asek), [email p o ec ed] (S. To ko noo).
Con en s lis s a ailable a ScienceDi ec
Jou nal o Ma e ials Resea ch and Technology
jou nal homepage: www.else ie .com/loca e/jm
h ps://doi.o g/10.1016/j.jm .2025.06.185
Recei ed 10 Ap il 2025; Recei ed in e ised o m 23 June 2025; Accep ed 24 June 2025
Jou nal o Ma e ials Resea ch and Technology 37 (2025) 4345–4361
A ailable online 8 July 2025
2238-7854/© 2025 The Au ho s. Published by Else ie B.V. This is an open access a icle unde he CC BY license ( h p://c ea i ecommons.o g/licenses/by/4.0/ ).
o m ha m ul by-p oduc s in he human body (no H- elease, biocom-
pa ible co osion p oduc s) [3,5].
Expanding he use o Zn as a bioabso bable ma e ial equi es im-
p o emen s in mechanical p ope ies, which can be achie ed h ough
alloying wi h sui able elemen s, including Ag, Cu, Li, Mg, Mn. Among
hem, Mg seems o be he bes candida e o imp o ing he ma e ial’s
s eng h, dec easing he modulus o elas ici y [1], and posi i ely
a ec ing bone mine aliza ion and o e all biocompa ibili y [6]. The
maximum solubili y o Mg in he Zn ma ix is nea 0.3 a .% a 364 ◦C and
dec eases o almos ze o a ambien empe a u e [2,7], leading o he
p ecipi a ion o in e me allic phases [8]. These include Mg
2
Zn
11
,
MgZn
2
, Mg
7
Zn
3
, Mg
2
Zn
3
and MgZn, which a e ha d and b i le, he eby
imp o ing s eng h bu dec easing duc ili y. Zn–Mg ma e ials howe e
gene ally exhibi a low biodeg ada ion a e.
Fu he imp o emen o he mechanical p ope ies can be achie ed
h ough mechanical alloying (MA). MA causes an in ensi e plas ic
de o ma ion du ing he p ocess, which leads o he o ma ion o alloy
powde s con aining me as able phases. These include o e sa u a ed
solid solu ions wi h ex emely small pa icles and g ains, eaching nano-
g ained ma e ials [9]. Howe e , MA is highly dependen on he p o-
cessing condi ions, including he milling media and essels, hei shape
and size, empe a u e and a mosphe e du ing p ocessing, and also
addi ional con ol agen s, such as s ea ic acid, which a e added o p e-
en excessi e cold welding [9,10]. Al hough MA echnology is capable
o p epa ing ul a ine-g ained ma e ials, he p ese ing o such mic o-
s uc u e du ing he consolida ion a inc eased empe a u es (>200 ◦C)
is challenging due o he low ec ys alliza ion empe a u e o pu e zinc
(<0 ◦C) [11], esul ing in he ma e ials’ ec ys alliza ion and coa s-
ening, especially when he milled powde is highly s essed.
Cold isos a ic p essing (CIP) and con en ional sin e ing o g een
compac s [12,13], ho isos a ic p essing (HIP) [13], spa k plasma sin-
e ing (SPS) [13] and ex usion (E) [13,14] a e gene ally conside ed o
Zn-based alloys compac ion. The esul ing ma e ials possess mic o-
s uc u es wi h ex ensi e po osi y, oxides and inhomogenei ies in
chemical and phase composi ion, signi ican ly de e io a ing mechanical
p ope ies. Classical sin e ing a an inc eased empe a u e usually akes
se e al hou s be o e su icien compac ion akes place, esul ing in
coa se-g ained mic os uc u es. A simila p oblem occu s du ing ho
isos a ic p essing, whe e ma e ials a e exposed o high empe a u es o
se e al hou s, a ec ing he mic os uc u e o phase composi ion
[15–17]. The ma e ials’ ec ys alliza ion and coa sening, may be, o
some ex en , p e en ed using compac ion by spa k plasma sin e ing
(SPS). SPS o e s he ad an age o a as compac ion echnique wi h
sho imes and low empe a u es o he p ocess (0.7 o he mel ing
empe a u e o he me al o be compac ed) [17,18]. In his echnique,
pulses o elec ic cu en low h ough he sample and gene a e hea a
he powde pa icle in e aces due o he local high esis ance. Besides,
he p ocess is accompanied by adjus able comp ession and can p oduce
ma e ials wi h a homogeneous nonpo ous s uc u e wi hou signi ican
g ain coa sening [18–20].
Zn-alloys ha e also been p epa ed by addi i e manu ac u ing
me hods such as lase powde bed usion (LPBF) [21–23]. Howe e ,
based on he alloy composi ion, he densi y o he p epa ed ma e ials
eached a maximum o 98 %. Fu he mo e, he eu ec ic mic os uc u e
was o med along g ain bounda ies, and a highe magnesium concen-
a ions (>7.7 a .%), he inhomogeneous mic os uc u e was gene a ed
due o local p ecipi a ion o he MgZn
2
phase. Those issues nega i ely
a ec mechanical p ope ies [21].
He e, we p epa ed ma e ials by combining MA, SPS and ex usion, o
de elop a ine-g ained mic os uc u e in Zn-based alloys. As a s a ing
ma e ial, we ha e selec ed Zn-2.6Mg (a .%) co esponding o he
Zn–1Mg in w .%, which epea edly showed, a e a con en ional way o
p oduc ion, a good comp omise be ween s eng h and duc ili y [3,24].
Due o he uniqueness o he ma e ials p epa a ion ou e, a main
emphasis was placed on he s udy o he mic os uc u e, which has
subsequen ly se ious impac on bo h mechanical and co osion
p ope ies. To p o ide mo phological, c ys allog aphic and composi-
ional in o ma ion om millime e s o nanome e s, we combined
scanning-elec on mic oscopy (SEM), ansmission elec on mic oscopy
(TEM) and a om p obe omog aphy (APT). In pa icula , APT p o ides
de ailed in o ma ion abou he ma e ial’s nanoscale composi ion in 3D,
hough se ing as a e y help ul complemen a y echnique o con en-
ional 2D imaging echniques such as elec on mic oscopy. Fu he mo e,
we in es iga ed how he addi ion o Ag a ec s he mic os uc u e, me-
chanical pe o mance and dissolu ion o he ma e ial. He e, we discuss
he de ails o he mic os uc u e-p ope y ela ionships in hese alloys
and demons a e hei high po en ial o di ec applica ion as bio-
abso bable me als.
2. Ma e ials and me hods
2.1. Ma e ials syn hesis
The Zn-2.6Mg and Zn-2.6Mg-0.6Ag alloys we e p epa ed by me-
chanical alloying (MA) o 4 h using 800 o a ion pe minu e (RPM) in a
Re ch E-max mill equipped wi h a wa e -cooling sys em capable o
main aining a empe a u e below 50 ◦C. The powde s used we e pu e Zn
(99.9 %, pa icle size <149
μ
m, Al a Aesa ), Mg (99.8 %, pa icle size
<44
μ
m, Al a Aesa ) and sil e (99.9 %, pa icle size <20
μ
m, Sa ina a.
s.). The ball- o-powde a io (B/P a io) was selec ed as 5:1. The
g inding p ocess was ca ied ou using zi conia balls in a 125 ml ellip-
ically designed essel wi h zi conia coa ing. To p e en powde
agglome a ion du ing he mechanical alloying, 0.03g s ea ic acid was
added o he powde mix u e be o e milling. Ma e ials we e mechani-
cally alloyed unde a p o ec i e A a mosphe e (99.96 %). The MA pa-
ame e s we e selec ed based on se e al expe imen s documen ing he
e ec o a ious pa ame e s on powde p ope ies. Two me hods o
compac ion o alloyed powde s we e selec ed. Fi s ly, he as compac-
ion me hod – spa k plasma sin e ing (SPS - FCT Sys eme HP-D 10) was
pe o med a 300 ◦C, 80 MPa p essu e o 10 min in g aphi e ools unde
a p o ec i e A a mosphe e (99.96 %). Secondly, he Zn–2.6Mg alloy
was compac ed by ho ex usion a 200 ◦C wi h an ex usion a io (ER)
equal o 25. Be o e ex usion, “g een compac ” om powde s we e
p oduced in he o m o cylinde s wi h 30 mm in diame e and 50 mm
high by acuum ho p essing (HVP) a 200 ◦C o 2 h. The designa ion o
he syn hesized ma e ials is shown in Table 1. The chemical composi ion
o he p epa ed powde s and compac ed ma e ials was e i ied by
a omic abso p ion spec ome y - AAS (Agilen 280 FS AA
spec ome e ).
2.2. Mic os uc u e
The p epa ed samples we e i s g ound on SiC pape s P400 – P2500,
hen polished on diamond pas e D2 (UR-Diaman ), and inally polished
on he Eposile NonD y suspension (QATM) o 20 min. The mic o-
s uc u e was cha ac e ized using an SEM (TESCAN VEGA 3 LMU) wi h
an EDS analyze (OXFORD Ins umen s AZ ec). Addi ionally, elec on
Table 1
The ma e ials designa ion and p ocessing condi ions.
Ma e ials
designa ion
Alloy
composi ion
[a . %]
Alloy
composi ion
[w . %]
Mechanical
alloying
Compac ion
me hod and
condi ions
Zn-
2.6Mg
(4h)
Zn-2.6Mg Zn–1Mg 800RPM, 4h,
BP =5:1
–
Zn-2.6Mg-
0.6Ag
(4h)
Zn-2.6Mg-
0.6Ag
Zn–1Mg–1Ag 800RPM, 4h,
BP =5:1
–
Zn-
2.6Mg
(4h)
+Ex
Zn-2.6Mg Zn–1Mg 800RPM, 4
h, BP =5:1
Ex usion,
200 ◦C, ER25
Zn-2.6Mg-
0.6Ag
(4h)
+Ex
Zn-2.6Mg-
0.6Ag
Zn–1Mg–1Ag 800RPM, 4 h Ex usion,
200 ◦C, ER25
J. Kub´
asek e al.
Jou nal o Ma e ials Resea ch and Technology 37 (2025) 4345–4361
4346
backsca e ed di ac ion (EBSD) analyses we e pe o med on an Ap eo
2 SEM using an accele a ion ol age o 15 kV wi h a p obe cu en o 13
nA a e inal polishing was pe o med using OPS o 20 min. EBSD
Kikuchi pa e ns we e measu ed wi h a Symme y S3 came a (Ox o d
ins umen s) using AZ ec so wa e. Samples we e il ed 70◦ o mea-
su emen s and an accele a ion ol age o 15 kV o used. The da a we e
p ocessed using AZ ecC ys al so wa e. Obse a ion and documen a ion
o he mic os uc u e a a nanoscale was pe o med using a FEI Tecnai
TF20 X- win ield emission gun ansmission elec on mic oscope (TEM)
ope a ed a 200 kV and equipped wi h an EDS de ec o . Pa icula ly,
scanning ansmission elec on mic oscopy (STEM) mode was used o
he mic os uc u e obse a ion. Fo STEM, Z-con as imaging was
pe o med using a high-angle annula da k ield (STEM–HAADF) de-
ec o . Samples o TEM analyses we e p epa ed using a JEOL ION
SLICER EM 09100 IS wi h a ol age o 5 kV and a cu en o 120
μ
A. The
phase composi ion was measu ed by X- ay di ac ion (X’Pe
3
Powde
ins umen in B agg-B en an geome y using a Cu anode (λ =1.5418, U
=40 kV, I =30 mA). Quan i a i e phase analysis was ca ied ou using
he whole pa e n Rie eld e inemen so wa e MAUD [25]. The heo-
e ical po osi y was calcula ed om he p epa ed samples’ weigh ,
olume, and densi y. Image analyses in ImageJ so wa e measu ed he
g ain size.
A 2.5
μ
m ×20
μ
m egion o he polished sample was coa ed wi h 1
μ
m o pla inum ca bon (P –C) using a gas-injec ion sys em inside a dual-
beam scanning elec on mic oscope/ ocused ion beam (SEM/Ga FIB)
(FEI Helios Nano-Lab 600i) (FEI Company, Hillsbo o, OR, USA) a 3.0 kV
and 1.4 nA. A ench was milled using a ol age o 30 kV and a cu en o
2.5 nA on each side o he P –C-coa ed lamella. Nex , 3
μ
m ×3
μ
m o he
lamella edge was milled a 30 kV and 0.23 nA o a ach he 2.5
μ
m ×20
μ
m lamella o he OmniP obe 200 Nanomanipula o (Ox o d In-
s umen s, Abingdon, UK) wi h P –C. Lamella (2.5
μ
m ×2
μ
m) we e
moun ed on o P esha pened Mic o ip™ Coupons (PSM M36) (CAMECA
Ins umen s, Madison, WI, USA) and sha pened in o needle-like shapes
wi h a diame e o 30–100 nm. The Zn–1Mg
(4h) +Ex
sample was
analyzed in he LEAP™ 5000 XR (CAMECA Ins umen s, Madison, WI,
USA using a lase pulse ene gy o 50 pJ, a base empe a u e o 50 K, and
a epe i ion a e o 125 kHz, and he de ec ion a e was ixed a 5 ions
de ec ed pe 1000 pulses on a e age. The Zn–1Mg
(8h) +Ex
sample was
analyzed in he LEAP™ 5000 XR (CAMECA Ins umen s, Madison, WI,
USA using a pulse ac ion o 20 %, a base empe a u e o 50 K, and a
epe i ion a e o 200 kHz, and he de ec ion a e was ixed a 5 ions
de ec ed pe 1000 pulses on a e age. The Zn–1Mg–1Ag
(4h) +Ex
sample
was analyzed in he LEAP™ 5000 XS (CAMECA Ins umen s, Madison,
WI, USA using a pulse ac ion o 20 %, a base empe a u e o 50 K, and a
epe i ion a e o 500 kHz, and he de ec ion a e was ixed a 5 ions
de ec ed pe 1000 pulses on a e age. The econs uc ion o all da ase s
and analysis we e pe o med in CAMECA Ins umen s APSUITE ( e sion
6.3.0.90).
2.3. Mechanical p ope ies
The mechanical p ope ies o he p epa ed alloys we e cha ac e ized
by Vicke s ha dness and ensile es s. HV1 was measu ed on a Fu u e-
Tech FM-100 a a load o 1 kg o 10 s. Tensile es s we e pe o med
using an Ins on 8802 ins umen on “dog bone” specimens (Fig. S1 –
supplemen a y ile), espec i ely, a a s ain a e o 0.003 s
−1
.
2.4. Co osion beha iou
To desc ibe he co osion p ope ies o he ma e ial, a 7-day expo-
su e was pe o med, ex ended by non-des uc i e elec ochemical
measu emen s: open ci cui po en ial (OCP), elec ochemical imped-
ance spec oscopy (EIS) and pola iza ion esis ance (R
P
). Measu emen
was pe o med in a complex body simula ion, i.e. in EMEM M7278 wi h
5 % FBS (Foe al Bo ine Se um, Sigma Ald ich) and he necessa y
addi ion o 1 % an ibio ics/an imyco ics (all Sigma Ald ich) a 37 ◦C.
Cylind ical samples 10 mm high and 4.3 mm in diame e we e g ound
( o FEPA P2500), washed wi h demi-wa e and deg eased in e hanol.
Samples we e u he , moun ed on a PTFE (Poly e a luo oe hylene)
holde immedia ely be o e measu emen . Subsequen ly, he samples,
oge he wi h glassy ca bon ods and a 75 ml polyme hylpen ene cell,
we e s e ilized using UV-C (ul a iole ligh in he wa eleng h ange o
100–280 nm (nm). A e wa ds, he measu ing cell was assembled and an
e hanol-washed sil e -chlo ide e e ence elec ode (SSCE - Sil e /Sil e
Chlo ide Elec ode, 3 mol/KCl) was added. Du ing he subsequen
exposu e, OCP was acqui ed, in e mi en ly by R
P
measu emen (+-15
mV/OCP, 0.125 mV/s) o EIS (60 kHz −0.01 Hz, 7 poin s pe decade,
E
AC
15 mV. ms, E
DC
=OCP). Measu emen s we e pe o med on a Gam y
Re e ence 600 po en ios a , he co ec ness o he impedance da a was
e i ied by K ame s-K onig ans o ma ion in Gam y Echem Analys
so wa e, and subsequen e alua ion was pe o med in ZView so wa e.
The ma e ial was also analyzed a e exposu e using SEM/EDS Tescan
Vega 3 and OXFORD Ins umen s AZ ec and a ligh mic oscope Olympus
SZX10 (LM).
2.5. In i o biological beha io
2.5.1. In i o cy o oxici y es - es on ex ac s
Human oe al os eoblas s hFOB 1.19 (ATCC® CRL-11372™) we e
main ained in DMEM/Ham’s F-12 (Sigma, D6434) medium wi h 10 %
FBS (Foe al bo ine se um - Sigma F7524), 2.5 mM L-glu amine in he
o m o s able dipep ide (Sigma, 8541) and selec ion eagen G418
(Sigma, G8168) a a pe missi e empe a u e o 34 ◦C, wi h 5 % CO
2
and
100 % ela i e humidi y. Cells we e passaged egula ly using a ypsin-
EDTA solu ion wi hou phenol ed (Gibco, 15400054). Cells we e used
om he 3 d passage a e hawing and only un il he 15 h passage.
On day 1, hFOB 1.19 cells we e ypsinized and esuspended in he
cul i a ion medium o ob ain a suspension wi h a concen a ion o 2⋅10
5
cells pe mL. Subsequen ly, 100
μ
l o he cell suspension was seeded in a
96-well pla e, which means he seeding densi y o 2⋅10
4
cells pe well.
Cylind ical samples (heigh 10 mm, diame e 4 mm) o he alloys
(Zn-2.6Mg
(4h) +Ex
and Zn-2.6Mg-0.6Ag
(4h) +Ex
) we e weighed, s e ilized
by 70 % e hanol (2 h) and by UV ligh (2 h). The ea e , samples we e
ans e ed o a cul i a ion medium L-15 (Leibo i z’s L-15 medium)
supplemen ed wi h educed concen a ion o FBS (5 %, as sugges ed by
ISO 10993-5 s anda d) wi hou G418 and agi a ed (130 RPM) a 37 ◦C in
closed essels o 24 h. The su ace- o- olume a io s a ed in he ISO
10993-12 (1.25 cm
2
mL
−1
) was adjus ed as ecommended o deg ad-
able me als [26] i.e. he olume was i e imes highe . Th ee eplica es
we e used o he alloys es ed.
On day wo, he medium in 96-well pla es was eplaced by he ex-
ac s p epa ed as desc ibed abo e. The ex ac s we e used undilu ed
(100 % ex ac s) and wice dilu ed (50 % ex ac s). Six echnical epli-
ca es we e used o each sample. Sole cul i a ion medium L-15 se ed as
nega i e (una ec ed) con ol. The concen a ion o eleased ions in he
ex ac s was measu ed by AAS.
On day h ee, a e 24 ±1 h o incuba ion wi h he ex ac s a 37 ◦C
wi hou CO
2
, he cell me abolic ac i i y was e alua ed by a esazu in
assay. Resazu in is me abolized o eso u in by li ing cells. The ex ac s
we e emo ed and a esazu in solu ion ( inal concen a ion 25
μ
g mL
−1
)
in Hank’s balanced sal solu ion (HBSS) was added. A e 2 h, luo es-
cence a 560/590 nm (exci a ion/emission) was measu ed (Fluo oskan
Ascen FL, The mo). Cy o oxici y o he ex ac s was calcula ed as a
pe cen age o he me abolic ac i i y o he nega i e con ol. Ex ac s
causing a dec ease below 70 % o he ac i i y o he nega i e con ol
we e conside ed cy o oxic, as desc ibed in he ISO 10993-5 s anda d.
2.5.2. An ibac e ial es s
An ibac e ial es s we e pe o med wi h Esche ichia coli (DBM 3138)
as a ep esen a i e o G am-nega i e bac e ia and S aphylococcus epi-
de midis (ATCC14998 CCM21245) ep esen ing G am-posi i e bac e ia.
The es condi ions we e adop ed om Re . [27].
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A bac e ial suspension was p epa ed he day be o e he es . The
bac e ia we e inocula ed in o he liquid Lu ia-Be ani (LB) medium
(Lennox) and incuba ed a 37 ◦C o e nigh . On he day o he expe i-
men , he bac e ial suspension was dilu ed wi h phospha e-bu e ed
saline (PBS) o a u bidi y o 1 McFa land s anda d (which co e-
sponds o app ox. 3⋅10
8
colony o ming uni s, CFU/mL o E. coli).
Subsequen ly, a se ial dilu ion was p epa ed; he six h decimal and
ou h decimal dilu ions we e used o E. coli and S. epide midis,
espec i ely. The specimens Zn-2.6Mg
(4h) +Ex
and Zn-2.6Mg-0.6Ag
(4h) +
Ex
(heigh 3 mm, diame e 4 mm) we e s e ilized in 70 % e hanol (2 h)
and unde UV ligh (2 h) and hen subme ged in 0.5 ml o bac e ial
suspension ( he su ace o olume a io was 1.25 cm
2
pe mL). The
samples we e incuba ed in bac e ial suspensions o 4 h a labo a o y
empe a u e. Th ee eplica es we e used o each ype o ma e ial.
Coppe was used as a posi i e (an ibac e ial) con ol. The nega i e
con ol (suspension wi hou samples) was used as a con ol o bac e ial
g ow h.
A e 4 h, he d ip es was pe o med by ans e ing 25
μ
L o sus-
pension in o each ield o Pe i dish (LB aga o E. coli and pla e coun
aga , PCA o S. epide midis) di ided in o wel e squa es. A Pe i dish
con ained ou d ops (o 25
μ
L) o each iplica e o one specimen. Thus,
e e y ype o sample was applied on one pla e. Blank (pu e PBS) and a
con ol dish (bac e ial suspension wi hou samples) we e p epa ed using
he same d ip me hod. Fu he mo e, a subsequen 1:1 dilu ion o each
suspension was pe o med wi h PBS o ensu e he coun abili y o he
colonies in he case o oo la ge numbe o colonies in he o iginal sus-
pensions. The pla es we e hen le a labo a o y empe a u e and, i
necessa y, he nex day ans e ed o 37 ◦C un il he colonies on he
con ol pla e we e isible and sui able o coun ing. Colonies on pla es
we e coun ed using he Schue Coun de ice. The colonies coun s we e
compa ed o he coun in he con ol dish. Fu he mo e, he same se o
samples was s e ilized and incuba ed o 4 h in he same olume o PBS
as o he an ibac e ial es . The concen a ion o eleased Zn was
measu ed by AAS.
3. Resul s
3.1. Mic os uc u e
3.1.1. P ocessing o powde s by mechanical alloying
Elec on mic og aphs o he supplied powde s a e displayed in
Fig. S2 (supplemen a y ile). These powde s we e combined in app o-
p ia e olumes in he milling essels o p oduce mechanically alloyed
powde s.
Fi s ly, we ha e s udied he e ec o long- e m high-ene gy MA on
he mic os uc u e de elopmen o he Zn-2.6Mg alloy, including phase
and chemical composi ion. Bo h MA powde s we e e y ine, wi hou
agglome a es, due o con olled milling pa ame e s and he addi ion o
s ea ic acid (Fig. 1). The powde pa icles we e u he cha ac e ized by
sha p edges and a laye ed s uc u e, which is caused by he epea ed
cold welding o he inpu pa icles and hei subsequen b eakage. The
indi idual pa icles we e up o 90
μ
m in size; howe e , he main ac ion
was 30 ±17
μ
m o Zn-2.6Mg
(4h)
and 24 ±12
μ
m o Zn-2.6Mg-
0.6Ag
(4h)
. The inal size o he alloy powde s is educed compa ed o he
inpu zinc powde . We expec ha his is a ec ed by wo main ac o s.
Fi s ly, p olonged exposu e o empe a u e-con olled MA c ushes he
powde by he impac o he g inding balls. Secondly, due o he low
magnesium solubili y in zinc, i is likely ha b i le in e me allic phases
p ecipi a e du ing he milling and suppo he disin eg a ion o la ge
pa icles. Such beha io is suppo ed by he iden i ica ion o he
Mg
2
Zn
11
phase in he milled powde by X- ay di ac ion (Table 2 and
Fig. 4).
Fu he mo e, he XRD esul s o MA powde s (Table 2, Fig. 2)
e ealed no MgZn
2
al hough me as able condi ions could lead o i s
o ma ion. Ou p e ious wo k has shown ha mechanical alloying a
800 RPM leads o he o ma ion o alloy in a sho e ime (4 h) han a
lowe RPM alues [28]. Inc easing he milling ime o 8 h led e en o he
dissolu ion o almos all he inpu magnesium in he Zn ma ix. Subse-
quen AAS analyses o he MA powde s con i med ha he composi ion
is as designed, p o ing he e we e no selec i e losses o Mg in he milling
essels du ing he p ocess.
3.1.2. Consolida ed ma e ials
Fig. 3 shows he phase composi ion o compac ed Zn–Mg-(Ag) ma-
e ials wi h he e alua ed esul s epo ed in Table 2. The compac ed Zn-
2.6Mg
(4h) +Ex
and Zn-2.6Mg-0.6Ag
(4h) +Ex
ma e ials exhibi ed compa-
able phase composi ion as he powde p ecu so s. The sligh inc ease in
he con en o Mg
2
Zn
11
in he ex uded p oduc s can be a ibu ed o he
u he p ecipi a ion o Mg
2
Zn
11
du ing he consolida ion p ocess. Be-
sides, aces o MgO we e obse ed by de ailed analyses in simila
amoun s in powde p ecu so s and compac ed ma e ials indica ing some
p e e en ial oxida ion o Mg. I is wo h men ioning ha MgO di ac ion
Fig. 1. Mechanically alloyed powde s: A) Zn-2.6Mg
(4h)
B) Zn-2.6Mg-0.6Ag
(4h)
.
Table 2
The phase composi ion o p epa ed MA powde s and compac ed p oduc s ac-
co ding o XRD.
Ma e ial condi ions Phase composi ion [w .%]
Zn Mg
2
Zn
11
Ag
0.12
Zn
0.88
MgO
Zn-2.6Mg
(4h)
Powde 93.0 6.2 –0.8
Zn-2.6Mg
(8h)
Powde 99.3 – – 0.7
Zn-2.6Mg-0.6Ag
(4h)
Powde 92.8 6.4 <0.1 0.7
Zn-2.6Mg
(4h) +Ex
Compac 91.9 6.9 –1.2
Zn-2.6Mg-0.6Ag
(4h) +Ex
Compac 92.2 7.0 <0.1 0.8
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peaks pa ially o e lap wi h he Mg
2
Zn
11
phase a 36.9 and 42.9 ◦2θ
posi ions, making hem di icul o obse e in XRD pa e ns. ZnO was no
de ec ed, al hough i s p esence unde he de ec ion limi canno be
excluded. I is wo h men ioning ha he alloy milled o 8 h su e ed
om ex ensi e c acking du ing ex usion. This happened e en wi h he
p ocessing empe a u e up o 400 ◦C. The e o e, Zn-2.6 Mg
(8h) +Ex
is no
u he s udied in he pape .
3.1.2.1. Mic os uc u e analyses using SEM wi h EDS and EBSD. As
shown in he scanning elec on mic og aphs in Fig. 4., bo h success ully
syn hesized (Zn-2.6Mg
(4h) +Ex
and Zn-2.6Mg-0.6Ag
(4h) +Ex
) ma e ials
p epa ed by ex usion ha e an ul a ine-g ained mic os uc u e wi h a
ypical a angemen o in e media e phases in he ows pa allel o he
ex usion di ec ion (Fig. 4a–d). Fu he igu es o mic os uc u e a e
shown in Fig. S3 – supplemen a y ile. Fi s ly, he mic os uc u e o bo h
ma e ials con ained phases en iched by Mg wi h a size in he ange o
0.3–1
μ
m (Fig. 4b and d). These phases we e analyzed using SEM-EDS
and con ained abou 14.6 a . % o Mg, which co esponds o he
Mg
2
Zn
11
phase. Due o he size o hese phases, hei a angemen and
con i ma ion o hei p esence in he powde p ecu so by XRD
(Table 2), i is belie ed ha hey we e o med du ing mechanical
alloying. Indeed, he es ima ed con en o Mg
2
Zn
11
in Zn–1Mg
(4h)
using
Rie eld analyses o XRD was 15.1 a .%. Simple ecalcula ion shows us
ha i co esponds o he 2.5 a .% o Mg in he alloy, indica ing ha Mg
would be dissol ed in he ma ix in a e y low concen a ion (≈0.1 a .
%), u he con i ming ha hese phases a e no o med du ing ex u-
sion. O he smalle phases we e obse ed in he mic os uc u e mainly
a he g ain bounda ies. Due o he exis ence o oxide shells on he
su ace o powde pa icles b eaking du ing MA, hese phases a e ex-
pec ed o be oxide pa icles inco po a ed inside he mic os uc u e
du ing ex usion. This will be u he discussed below.
The in-plane in e se pole igu e (IPF) maps (Fig. 5) ob ained by EBSD
e eal he g ain size and o ien a ion. Bo h ma e ials ha e compa able
g ain size dis ibu ion (Fig. 6) wi h he a e age g ain size o 0.74 and
0.72
μ
m o Zn-2.6Mg and Zn-2.6Mg-0.6Ag, espec i ely. Bo h ma e ials
ha e e y low ex u e s eng h wi h signs o (0110)and (1210) ibe
ex u e (Fig. 7) and wi h he p e e en ial o ien a ion o basal planes
pa allel o he ex usion di ec ion. Howe e , he ex u e is much weake
compa ed o he Zn-based alloys p epa ed by con en ional cas ing and
w ough echniques (eg. ho ex usion, olling, ECAP) [2,29,30]. Bo h,
he p esence o ul a- ine g ains and mo e andom dis ibu ion o c ys-
allog aphic o ien a ions a e belie ed o be a ec ed by he p esence o
in e media e phases in he size om en hs o hund eds o
μ
m. To
con i m his assump ion u he de ailed analyses o he mic os uc u e
using APT and TEM we e pe o med.
3.1.2.2. De ailed mic os uc u e analyses using APT and TEM. The esul s
o he APT analyses on he ex uded ma e ials a e shown in Fig. 8 and
Table 3. The Zn–1Mg
(4h) +Ex
sample con ains mainly he Zn ma ix and
inely dispe sed bu une enly dis ibu ed pa icles (Fig. 8a). The
composi ion (a . %) o he di e en phases was ob ained using p o iles
along a 5x5x4 nm cylinde wi h a bin size o 0.3 nm. Subsu ace in e -
me allic pa icles show a Zn/Mg a io consis en wi h he Mg
2
Zn
11
phase
as epo ed in Table 3. P ecipi a e I (Fig. 8b), which in e sec s he
specimen’s su ace is en iched in oxygen, mos ly in he o m o ZnO/Zn
(OH)
2
ions in he APT analysis. Due o su ace con amina ion du ing
sample p epa a ion and he p esence o esidual gas in he APT analysis
chambe , accu a e quan i ica ion o O and H is a known challenge and
con ibu es o he a ia ion o O and H on he su ace laye [31–33]. Ye ,
his en ichmen compa ed o he Zn phase, can be conside ed as indic-
a i e o p e e en ial oxida ion. The second in e me allic phase con-
aining mos ly Zn and Mg has Zn/Mg a io inconsis en wi h equilib ium
phases known in he Zn–Mg sys em and p obably co esponds o he
p esence o an in e media e me as able phase. Fig. 8c is a composi ion
p o ile using a 10x10x10 nm cylinde and a bin size o 0.3 nm showing a
clea inc ease in Mg composi ion. These could be he o ma ion o
Guinie -P es on (GP) zones o clus e s p ecu so o he in e me allic
phase.
The esul s o APT analysis o he Zn-2.6Mg-0.6Ag
(4h) +Ex
shown in
Fig. 8d indica e he p esence o a Zn phase and an in e me allic phase
wi h en hs o nm in size. The bulk composi ion (a %) o he phases was
ob ained by an analysis o a 5x5x4 nm cylinde and a 10x10x4 nm
cylinde . The in e me allic phase co esponding o p ecipi a e I-III
(Fig. 8d) con ains mos ly Zn and Ag. P ecipi a e III has a composi ion
consis en wi h he Ag
0.12
Zn
0.88
ε
-phase. No Ag-con aining in e me allic
phase was obse ed using XRD o he milled powde , whe eas he
p esence o he
ε
-phase was con i med by XRD in he ex uded ma e ial
indica ing he p ecipi a ion o hese phases du ing he ex usion. Fig. 8e
and Fig. , espec i ely sugges ha g ain bounda ies and disloca ions
(Fig. S4 - supplemen a y ile) a e a ac i e seg ega ion si es o Ag. The
g ain bounda ies en iched wi h Ag a e also deco a ed by clus e s o Mg.
The pa e n o med by he assembly o Ag-seg ega ed disloca ions can be
in e p e ed as a low-angle bounda y as e ealed by APT in o he alloy
sys ems [34–36].
TEM-EDS analyses o he Zn-2.6Mg
(4h) +Ex
e ealed ha nano-sized
pa icles bo h a g ain bounda ies and inside he g ains co espond o
he Mg
2
Zn
11
and/o magnesium o zinc-en iched oxides (Fig. 9). These
pa icles a e smalle han he hickness o he lamellae, he e o e he
alues o chemical composi ion es ima ed by EDS a e a ec ed by he
su ounding ma ix. Fo his eason, i is di icul o exac ly dis inguish
oxide pa icles and he Mg
2
Zn
11
phase wi h oxidized su ace as sug-
ges ed by se e al APT obse a ions. We belie e ha pa o hese pa -
icles come om he b eakage o he oxide shells (ZnO) loca ed a he
su ace o he powde p ecu so s. This can be po en ially he main
sou ce o obse ed ZnO inside he consolida ed ma e ials. XRD analyses
o MA powde p ecu so s (Table 2) also e ealed he p esence o MgO.
This he modynamically s able phase is p ese ed also in he consoli-
da ed ma e ials. Mg
2
Zn
11
was also obse ed in he MA powde p e-
cu so s, howe e , i s con en is sligh ly inc eased (Table 2) o
Fig. 2. XRD pa e ns o he Zn-2.6Mg-(0.6Ag) powde s p epa ed by MA.
Fig. 3. XRD pa e ns o he Zn-2.6Mg-(0.6Ag) ex uded ma e ials.
J. Kub´
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Jou nal o Ma e ials Resea ch and Technology 37 (2025) 4345–4361
4349
consolida ed ma e ials. This may indica e he in-si u p ecipi a ion o his
phase du ing he ex usion p ocess. These esul s a e suppo ed by
almos he ex emely low amoun o Mg dissol ed in he zinc ma ix
measu ed by APT (Table 3). We we e no able o dis inguish be ween he
oxides and in e me allic pa icles eliably, because o he image a e-
ac s, low con as di e ence and simila shape and size. In gene al, he
seconda y phases o m pa icles o a size anging be ween app oxi-
ma ely 10 and 30 nm. The TEM analyses also e ealed he Zn-based
ma ix con ained la ge numbe o ine g ains/subg ains wi h a size
anging be ween app oxima ely 50 and 150 nm. The pa icles and p e-
cipi a es help pin g ain bounda ies and, he e o e, p e en
mic os uc u e coa sening. Al hough he empe a u e o he p e-
consolida ion and ex usion p ocess was ela i ely high (200 ◦C), he
p esence o hese pa icles is belie ed o be he main eason o he low
a e age g ain size (below 1
μ
m) in he ex uded p oduc s.
3.2. Mechanical p ope ies
The mechanical p ope ies o he s udied ma e ials we e e alua ed
based on ensile es s. The ue s ess-s ain cu es a e plo ed in
Fig. 10a. Due o he simila i ies o measu emen s and o cla i ica ion,
only one measu emen om h ee is shown. Resul s conside ing a e age
Fig. 4. Mic os uc u e o he consolida ed ma e ials - SEM: a), b) Zn-2.6Mg
(4h) +Ex
; c), d) Zn-2.6Mg-0.6Ag
(4h) +Ex
; ed a ows indica e Mg
2
Zn
11
phase, blue egions
indica e he oxide pa icles pinning he g ain bounda ies.
Fig. 5. IPF maps o he compac ed ma e ials: a) Zn-2.6Mg
(4h) +Ex
, b) Zn-2.6Mg-0.6Ag
(4h) +Ex
, ex usion di ec ion is he e e ence di ec ion o map.
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4350
alues and s anda d de ia ions a e summa ized in Fig. 10b and also
supplemen a y da a (Table S1 – supplemen a y ile). Resul s o an
ex uded Zn-2.1Mg-1.15S alloy a e added o compa ison as an
example o a widely s udied alloy, wi h p ope ies ul illing e-
qui emen s o in eg a ion in medical de ices. This ma e ial was p e-
pa ed by a common op- o-bo om app oach (mel ing, homogeniza ion
annealing and ho ex usion), esul ing in Zn mean g ain size o
app oxima ely 2.5
μ
m [37,38]. Zn has a low mel ing empe a u e
(420 ◦C), making 37 ◦C a he high homologous empe a u e o es ing.
To show he e ec o empe a u e on mechanical p ope ies, ensile es s
a 37 ◦C ha e been pe o med o Zn-2.6Mg
(4h) +Ex
and also
Zn-2.1Mg-0.15S
Ex
as a e e ence alloy. Due o he limi ed quan i y o
ma e ial a ailable ollowing he p epa a ion p ocess, i was no possible
o conduc ensile mechanical p ope y measu emen s a 37 ◦C o he
Zn-2.6Mg-0.6Ag
(4h)+Ex
alloy. The alues o TYS (279 MPa) and UTS
(384 MPa) o he Zn-2.6Mg
(4h) +Ex
exceed he pe o mance o a ma-
jo i y o bina y Zn–Mg o mo e complex alloys p oduced by con en-
ional echniques like cas ing, ex usion, olling [3]. Fu he mo e, he
Zn-2.6Mg-0.6Ag
(4h) +Ex
alloy eached an 11 % highe alue o TYS and
13 % highe alue o UTS a almos simila elonga ion o ac u e (E).
Bo h Zn-2.6Mg
(4h) +Ex
and Zn-2.6Mg-0.6Ag
(4h) +Ex
showcase a signi -
ican inc ease in s eng h a he expense o hei duc ili y. Mino de-
ia ions we e obse ed among measu emen s o TYS, and UTS,
al hough he duc ili y o Zn-2.6Mg-(0.6Ag)
(4h) +Ex
luc ua ed mo e,
sugges ing ha he mic os uc u e o he p epa ed alloys was sligh ly
he e ogeneous and he seconda y phases we e locally concen a ed,
causing he inc ease in local in e nal s esses and dec eased duc ili y.
I is e iden om Table 2 and Fig. 10 ha all Zn-based ma e ials
es ed a 37 ◦C ins ead o labo a o y empe a u e lose in mechanical
pe o mance signi ican ly. The TYS and UTS alues o Zn-2.1Mg-
0.15S
Ex
ep esen ing he e e ence ma e ial a e dec eased o 222 and
276 MPa which is e en below he sugges ed ole able alues, while due
o he gene ally highe mechanical s eng h o Zn–1Mg, he measu ed
alues o TYS and UTS a 37 ◦C co espond o he 246 MPa and 329 MPa,
espec i ely. In summa y, he dec ease in mechanical s eng h is in bo h
cases ≈14 %.
Compa ing he shapes o he indi idual ensile cu es (Fig. 10a), one
can see ha he cu es o all powde me allu gical ma e ials a e o he
same shape. Fu he da a e alua ion conside ing he ue s ess – ue
s ain alues a e shown in Fig. S5 – supplemen a y ile. Ob ained esul s
sugges ha he de o ma ion is accommoda ed by he same de o ma ion
mechanisms independen on he chemical composi ion and es ing
empe a u e. The e e ence alloy shows a signi ican inc ease in duc ili y
a e he inc ease in he es ing empe a u e, while main aining he
gene al shape o he cu e. To ob ain mo e in o ma ion, we ea ed he
cu es acco ding o Re . [39] and e alua ed s ain ha dening coe icien
n, s ain ha dening a e and disloca ion s o age densi y (Eqs. (1) and
(2)).
σ
=K⋅
ε
n(1)
θ=d
σ
d
ε
(2)
In hese equa ions
σ
is no malized plas ic ue s ess,
ε
is no malized
plas ic ue s ain, n is s ain ha dening coe icien , K is s eng h cons an
and θ ha dening a e. The disloca ion s o age a e was e alua ed as he
slope o linea pa o he ha dening a e*no malized plas ic s ess s.
no malized plas ic s ess cu es [39]. The plo s showing a ious de-
pendencies o mechanical beha io a e shown in Fig. S4 (supplemen a y
ile) and he impo an alues e alua ed om hose cu es a e lis ed in
Table 4.
I is impo an o no e ha s eng hening pa o he cu es belonging
o powde me allu gical samples was e y sho and i was e y di icul
o dis inguish he elas o-plas ic and plas ic de o ma ion egion, which
could lead o he o e es ima ion o he alue o s ain ha dening
coe icien .
Fig. 6. The dis ibu ion o g ain size: a) Zn-2.6Mg
(4h) +Ex
, b) Zn-2.6Mg-
0.6Ag
(4h) +Ex
.
Fig. 7. The ex u e o s udied ma e ials p esen ed by IPFs: a) Zn-2.6Mg
(4h) +Ex
, b) Zn-2.6Mg-0.6Ag
(4h) +Ex
.
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Jou nal o Ma e ials Resea ch and Technology 37 (2025) 4345–4361
4351
3.3. Co osion
The co osion beha io o he Zn-2.6Mg
(4h) +Ex
and Zn-2.6Mg-
0.6Ag
(4h) +Ex
was s udied by pe o ming a one-week exposu e in an
EMEM - medium simula ing blood plasma, bo h in e ms o simila
ino ganic ion con en and biochemical componen p esence. A e
exposu e, he ma e ials we e analyzed by SEM/EDS, hen mechanical
emo al o bulk co osion p oduc s was pe o med, and ma e ials su -
ace again analyzed by SEM/EDS (Fig. 11) and by OM (Fig. S6 – sup-
plemen a y ile).
F om an o e all pe spec i e, he e is a no iceable di e ence be ween
he ma e ials. The Zn-2.6Mg
(4h) +Ex
alloy shows signi ican ly ewe
changes compa ed o he o iginal su ace, he main ones being long
ib ous deposi s occupying a small pa o he su ace. Thei shape in-
dica es hei p o ein o igin. Zn-2.6Mg
(4h) +Ex
su ace has obse able
u ows a e g inding o he ma e ial. Thei sligh ly blu ed con ou s,
oge he wi h he change in colo o he ma e ial o blue-g ey, indica e
he p esence o a hin ilm. Acco ding o he EDS, he hin ilm compo-
si ion can be es ima ed o be p edominan ly a mix u e o oxide and
ca bona e. Looking a he less abundan elemen s, apa om Mg wi h a
lowe abundance han in he bulk, he p esence o calcium and phos-
pho us in app oxima ely equia omic p opo ions can be obse ed. Long
ib ous deposi s a e also isible and hei shape indica es hei p o ein
o igin. A e mechanical emo al o he deposi s, a localized a ack si e is
obse ed wi h nume ous small sha p-edged c e ices and a la ge cen al
pi con aining co osion deposi s. He e again, pa ially sha p edges
e e ing o bo h ini ia ion and p opaga ion along he in e aces p esen
in he ma e ial a e obse able, i.e. p obably he Mg
2
Zn
11
phase su -
ounded by oxides. The composi ion o he co osion p oduc s in he pi
Fig. 8. De ailed analyses o ex uded ma e ials using APT: a) Zn-2.6Mg
(4h) +Ex
; b) isualiza ion o Mg
2
Zn
11
and Zn phase in e ace in Zn-2.6Mg
(4h) +Ex
; c) isu-
aliza ion o nano-size pa icle and Zn phase in e ace in Zn-2.6Mg
(4h) +Ex
d) Zn-2.6Mg-0.6Ag
(4h) +Ex
; e) isualiza ion o g ain bounda y (GB) in e ace wi h Zn-
2.6Mg-0.6Ag
(4h) +Ex
wi h a highe ac ion o Mg ions; ) isualiza ion o low-angle g ain bounda ies (LAGB) in e ace wi hin Zn-2.6Mg-0.6Ag
(4h) +Ex
ma ix wi h a
highe ac ion o Ag ions.
Table 3
Bulk composi ional (a %) analysis ob ained by APT measu emen s o Zn-
2.6Mg
(4h) +Ex
and Zn-2.6Mg-0.6Ag
(4h) +Ex
.
Zn Mg Ag O H
Zn-2.6Mg
(4h) þEx
Bulk Zn 99.13 0.04 0.52 0.30
P ecipi a e I 57.80 12.48 19.00 10.72
P ecipi a e II 73.60 5.50 11.72 9.16
P ecipi a e III 94.81 2.10 1.74 1.35
Zn-2.6Mg-0.6Ag
(4h) þEx
Bulk Zn I 99.10 0.90
Bulk Zn II 99.09 0.92
Bulk Zn III 99.61 0.01 0.37 0.02
P ecipi a e I 97.09 0.03 2.79 0.09 0.01
P ecipi a e II 98.14 1.93 0.03
P ecipi a e III 88.81 0.05 11.13 0.01
P ecipi a e IV 97.92 0.98 1.02 0.04
P ecipi a e V 97.44 1.04 1.15 0.29 0.08
P ecipi a e VI 98.05 0.96 0.99
J. Kub´
asek e al.
Jou nal o Ma e ials Resea ch and Technology 37 (2025) 4345–4361
4352
Fig. 9. Zn-2.6Mg
(4h) +Ex
mic os uc u e analysis and p o ile o chemical composi ion along he o ange line – STEM-EDS: a, b) loca ion 1 and b, c) loca ion 2.
Fig. 10. Mechanical p ope ies o ma e ials: a) Tensile enginee ing s ess – enginee ing s ain cu es a labo a o y empe a u e and 37 ◦C (ma ked by *), b) e alua ed
p ope ies o s udied ma e ials.
J. Kub´
asek e al.
Jou nal o Ma e ials Resea ch and Technology 37 (2025) 4345–4361
4353
7) Sil e p esence in alloy suppo s he an ibac e ial e ec owa ds
S. epide midis.
Au ho con ibu ions
Jiˇ
í Kub´
asek – da a analyses, mechanical es s, w i ing, e iew,
edi ing, Selase To ko noo – APT analyses, w i ing, e iew, edi ing,
Da id Neˇ
cas – ma e ials p epa a ion using SPS, mic os uc u e analyses
using OM, Ing id McCa oll – APT analyses, Voj ˇ
ech Hyb´
aˇ
sek – co osion
es s, Bap is e Gaul – APT da a analysis, e iew, edi ing, E a Jablonsk´
a
– in- i o biological es s, w i ing, ˇ
C omi Donik – EBSD analyses, I ena
Paulin – mic os uc u e analyses using SEM, Pe e Gogola – XRD ana-
lyses, Ma in Kusý – XRD analyses, Zdenˇ
ek Míchal – in- i o biological
es s, Ja osla Foj – co osion es s, Mi osla ˇ
Ca ojský – ma e ials
p epa a ion by ex usion, Jan Duchoˇ
n – TEM analyses and hei e alu-
a ion, Ma k´
e a Ja oˇ
so ´
a – EDX, WDX analyses, Ja osla ˇ
Capek – p o-
cessing and in e p e a ion o TEM da a, e iew, edi ing.
Decla a ion o compe ing in e es
The au ho s decla e he ollowing inancial in e es s/pe sonal e-
la ionships which may be conside ed as po en ial compe ing in e es s:
Ji i Kubasek, Da id Necas, Voj ech Hybasek, E a Jablonska, Ja osla
Foj , Ja osla Capek epo s inancial suppo was p o ided by Czech
Science Founda ion. C omi Donik, I ena Paulin epo s inancial sup-
po was p o ided by Slo enian Resea ch and Inno a ion Agency. Mi -
osla Ca ojsky epo s inancial suppo was p o ided by Minis y o
Educa ion Science Resea ch and Spo o he Slo ak Republic. Ji i
Kubasek, E a Jablonska, Ja osla Foj epo s inancial suppo was
p o ided by Minis y o Educa ion You h and Spo s o he Czech Re-
public. I he e a e o he au ho s, hey 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 .
Acknowledgemen
This esea ch was suppo ed by he Czech Science Founda ion
(p ojec no. 21–11439K) and by he p ojec "Mechanical Enginee ing o
Biological and Bio-inspi ed Sys ems", unded as p ojec No.
CZ.02.01.01/00/22_008/0004634 by P og amme Johannes Amos
Comenius, call Excellen Resea ch. Fu he mo e, his wo k was ca ied
ou wi hin he amewo k o he Slo enian Resea ch Agency ARIS
p ojec N2-0182 ‘‘De elopmen o ad anced bioabso bable Zn-based
ma e ials by powde me allu gy echniques. ‘‘and ARIS p og am P2
0132 ‘‘Physics and Chemis y o Me als‘‘. Bap is e Gaul , Ing id McCa -
oll and Selase To ko noo a e g a e ul o he Deu sche Fo -
schungsgemeinscha (DFG) o unding h ough Bap is e Gaul ’s
Leibniz Awa d. The Slo ak au ho s would like o hank he Vega 1/
0531/22 p ojec unded by he Minis y o Educa ion, Science, Resea ch
and Spo o he Slo ak Republic o he inancial suppo and Cos ac-
ion CA22147 (EU4MOFs).
Appendix A. Supplemen a y da a
Supplemen a y da a o his a icle can be ound online a h ps://doi.
o g/10.1016/j.jm .2025.06.185.
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