V ol. 15　 N o .

4 　　　　　　　　　　　　 CHIN ESE JO U RN A L OF A ERO N A U TICS 　　　　　　　　　　　　 N ovember 2002

Inf l uence of Ambient -Temperature Corrosion

on the Oxidation Behavior of Al -Si Coatings
1 1 2 1
ZHANG Qi , SONG F u-bin , WANG Hua -g e , L UO Jun-hua
( 1. School of M at erials Science and E ngineering, Beij ing University of A eronaut ics and A st ronautics,
Beij ing　100083, China)
( 2. Sheny ang A eronautics Engine Research and Design Instit ute, Shengy ang 　110015, China)

Abstract: 　 T he high-temper atur e ox idat ion behavior of A l-Si coating s on the N i-base super allo y
DZ125, w ith and w ithout the ambient-temper atur e corr osio n test, was inv estig ated. T he r esults
show that the iso ther mal oxidation behavior of the cor roded coating changes, w hich has the higher
mass g ain than that of the o rig inal co at ing during the initial ox idation stag e. M oreov er , the cyclic ox -
idat ion resistance of the co rro ded coating decreases severely . T he ox ide scale w as primar ily co mposed
of A l2 O 3 , cont aminated with T iO2 that was due to the incr ease of T i content after the ro om -temper a-
tur e cor rosion test .
Key words: 　ambient-temper atur e cor rosion; o xidatio n; A l-Si coating
常温腐 蚀对 Al -Si 涂层氧化 行为的影响. 张琦, 宋 复斌, 王华 阁, 骆军华. 中国航 空学报( 英文版) ,
2002, 15( 4) : 244- 249.
摘　要: 研究了未经/ 经常温腐蚀的 D Z125镍基合金表面 Al -Si 涂层的高温氧化 行为。
结果 表明, 经
腐蚀的涂层等温氧化行为发 生变化。
在 初始阶段, 经 腐蚀的试样增重大 于未经腐蚀的试样, 而且经
腐蚀的试样的耐高温性能明显下降。氧化皮中主要是 A l2 O 3 及少量的 T iO 2 .
关键词: 常温腐蚀; 氧化; A l -Si 涂 层
文章编号: 1000-9361( 2002) 04-0244-06　　　中图分类号: T G172　　　文献标识码: A

　　Ni-base superalloys are widely used as turbine
blade mat erial f or advanced engines that are re-
quired t o be operat ed at elevated t emperat ures.
Deg radat ion by hig h-t emperat ure ox idat ion is one
of t he main f ailure modes of gas t urbine blades.
T herefore, som e protect ive coat ings are applied to
im prove t he hig h-t emperature ox idat ion resistance
of the superalloy s. T o some ext ent, t he useful lif e
of the superalloy components depends on t he quali-
ty of the coat ings. T hus, t he ox idat ion behavior is
very import ant f or t he high -temperat ure coatings.
Alt hough there are dif ferent coatings developed in
recent years, t he Al-Si coating is st ill used w idely
[ 1, 2]
for its low cost and st able performance . It has
been report ed that t he addition of Si can decrease
the ox idat ion rat e and improve the isothermal and
[ 3-6]
cyclic ox idat ion resist ance of superalloy s .
It is w ell know n t hat the aero -engines do not
w ork under high-temperat ure condit ions cont inu-
ously . It is ev en longer f or them to st ay at t he
fields than t o work in t he sky . T herefore, the am-
bient-t emperat ure corrosion behavior of t he coat-
ings should be invest igat ed, especially , the ox ida-
tion behavior of t he coat ings t hat had been corrod-
ed at t he am bient -t emperat ure. How ever , no e-
noug h eff ort has been paid t o study t he influence of
t he at mospheric corrosion t o t he protect ive coat-
ings.
In t he present work , t he const ant im mersion
t est f or the Al-Si coat ing at t he ambient tempera-
ture w as carried out prior to t he high t em perature
oxidation test in order t o examine t he eff ect of t he
corrosion on t he coat ing. T hen, special at t ention
w as given to t he com parison bet ween t he oxidation

Received dat e: 2002-06-26; R evision received dat e: 2002-09-29

Foundation item: A eronaut ical Science Foundat ion of Ch ina( 01I51006)
A rt icle U RL: ht t p: / / ww w . hkx b. n et . cn/ cja/ 2002/ 04/ 0244/
© 1994-2010 China Academic Journal Electronic Publishing House. Open access under CC BY-NC-ND license. http://www.cnki.net
 Inf luence of A mbient-T emperat ure Corrosionp
N ovember 2002 ・ 245・
on t he O xidat ion Behavior of A l-Si Coatings

behavior of t he original coat ing and that of t he cor- coating show ed t hat the roughness ( R a ) was in-
roded coating . creased by t he immersion , e . g . t he R a of t he sam-
ple bef ore corrosion w as 0. 32 m , while aft er 5
1　Experiments
days im mersion t he R a becam e 0. 40 m . In addi-
1. 1　Material s and coating tion, t he t hickness of -NiAl phase lay er of t he
T he nominal composit ion of DZ125 alloy used corroded coating had been reduced . On the ot her
is listed in T able 1. T he procedure for producing hand, T able 1 indicates that t he surf ace com posi-
the Al-Si coat ing is as follow s: t he slurry w as ap- tion of the corroded coating had been chang ed in
plied to t he sample surface, then 970℃× 40min contrast to the original coating . T he Al cont ent in
deposit ion , thereaf ter 870℃× 2h dif fusion under t he surf ace layer of t he corroded coating decreased
the condit ions of Ar protect ion . obviously and t he content s of Cr, Si and T i in-
1. 2　Ambient-temperature immersion test creased correspondingly .
A solut ion of 5% NaCl, 0. 5% Na 2SO4 and Table 1　 Contents of elements on the surface
0. 5 m ol/ L CH 3COOH w as used for t he ex peri- of the coating( at. % )
Al Si Cr Ti C Co Ni
ment . T he coated samples w ere ex posed to t he so-
original coating 43. 04 3. 21 0. 20 - 7. 42 4. 24 Bal.
lution for 500 h . At the end of the test, t he sam- corroded coat ing 22. 76 12. 19 4. 56 4. 87 10. 46 6. 86 Bal.
ples were taken f rom the corrosive m edium , and
2. 2　Oxidation kinetics
cleaned in running w at er .
T he oxidation kinetics of t he orig inal and cor-
1. 3　Oxidation test
roded coating s are illustrated in F ig . 1. It can be
Bot h t he isot hermal and cy clic ox idat ion t est s
seen that both coat ings ox idized under isot hermal
w ere perf ormed at 1050℃ in air. T he isot hermal
oxidation condit ions were in accordance to t he
oxidation test w as carried out in a vert ical alumina
tube react or wit h continuous mass measurement ,
using a thermal gravimetry m icrobalance ( to an ac-
curacy of ±0. 1m g) . T he cy clic ox idat ion t est was
perf ormed using a v ertical t ube furnace w it h 55-
min heating / 5-min cooling . T he samples were
quickly placed in the preheat ed furnace and t aken
out aft er each run for up t o 200h. T he w eight
change was measured discont inuously using an
electrobalance wit h a sensit ivity of 0. 1 mg .
1. 4　Metal l ographic examinations
T he t est ed sam ples w ere analyzed by X-ray
diff raction( XRD) w ith Cu-K radiation at 40 kV
and 30 mA. T he surf ace morphologies and cross-
sectional m icrost ruct ures of t he t est ed coat ings
w ere observed and analyzed w ith t he JSM-5800
scanning electron microscopy( SEM ) and an energy
dispersive X-ray analyzer .

2　Results
2. 1 　 Ambient-temperature corrosion of Al -Si
F ig . 1　 T he isotherm al ( a) and cyclic ( b) ox idation
coating
curv es of the orig inal and cor roded coating
T he surface morpholog ies of corroded Al-Si
© 1994-2010 China Academic Journal Electronic Publishing House. Open access under CC BY-NC-ND license. http://www.cnki.net
 ・ 246・ ZHA N G Qi, SO N G Fu-bin, W A N G Hua-ge, LU O J un-hua
parabolic law. At t he initial ox idat ion periods, t he
corroded coat ing show ed rat her quick mass gain
compared t o t he original coat ing, w hich could be
at t ributed to the increase of surface roughness and
the f ormation of T iO 2 ( this w ill be ex plained
lat er ) . With the progress of ox idat ion , t he ox ida-
tion rat e of t he corroded coating reduced. At about
40 hours, t he weig ht gain of the original coat be-
came less t han t hat of t he orig inal coating . Fig . 1
( b) shows cyclic ox idat ion kinetics of t he tw o coat-
ings. Contrary to isot hermal ox idat ion, it can be
found that t he corrosion decreased t he cy clic ox ida-
tion resistance of t he Al-Si coating remarkably .
T he obvious w eight loss was found for the corrod-
ed coat ing, w hich sug gest ed t hat the spallat ion of
the corroded coating w as m ore severe t han t hat of
the orig inal one during t he cy clic oxidation.
2. 3　Metal l ographic examinations
Fig. 2 illust rat es the cross-sectional morpholo-
gies and m icrost ruct ures of t he corroded and orig i-
nal coatings af t er 100h of isot hermal oxidation at
1050℃. T he m orphologies show ed t hat t here was
a continuous and relative smoot h Al2O 3 scale on t he
Fig . 2　T he SEM microg raphs of the samples w hich
had been isothermally ox idized for 100h
( a ) cross-section o f the o rig inal coating ;
( b ) cro ss -section of the corr oded coat ing
© 1994-2010 China Academic Journal Electronic Publishing House. Open access under CC BY-NC-ND license. http://www.cnki.net
CJA
orig inal coating , w hich prov ided good prot ection
for t he subst rate . However , t here w as an uneven
Al2O3 scale and some obvious spallat ions on t he
corroded coat ing . According t o t he results ob-
tained f rom the EDS analysis, it w as f ound that
besides some !′ -Ni3Al phases formed nearby t he
int erface betw een the -NiAl phase lay er and t he
Si-rich carbide barrier, t here was a complete lay er
of !′
-Ni3 Al phases beneath the Al2O3 scale f or t he
corroded coat ing. By comparison, t here w ere som e
!′-Ni3Al phases formed mainly adjacent t o the in-
terface betw een the -NiAl phase layer and the Si-
rich carbide barrier in t he original coat ing, sug-
gest ing t hat t he prot ect ive ef fect of the corroded
coating w as not as g ood as t hat of the orig inal coat-
ing, i. e. the corrosion w orsened t he qualit y of t he
coating .
Aft er the t hermal ox idat ion test f or 150 cycles
at 1050℃, !′ -Ni3 Al phases had been f ormed in
bot h coatings. It can be f ound t hat t he -NiAl
phases decreased obviously and the !′-Ni3 Al phases
increased considerably in the out er lay er of t he
coating s( Fig. 3 ( c) , ( d) ) as compared t o that ob-
served in t he 50 cy cle samples( Fig. 3 ( a) , ( b) ) .
T he amount and size of !′ - phase in t he corroded
coating w ere larger t han t hose in t he original coat-
ing. T his reduced t he lif e of the coat ing because of
 Inf luence of A mbient-T emperat ure Corrosionp
N ovember 2002
on t he O xidat ion Behavior of A l-Si Coatings
F ig . 3　Cr oss-section micr ogr aphs of
Al-Si coating after ox idation
( a) o rig inal coating ( 50 h ) ; ( b ) corr oded co ating( 50 h ) ;
( c) or iginal coat ing( 150 h ) ; ( d ) corr oded coating( 150 h )
the w eaker oxidation resist ance of !′
[ 7, 8]
- phase .
Cont rary t o t he corroded coat ing the !′
, - phases in
the orig inal coat ing were disperse and m ainly
formed adjacent t o t he int erf ace bet w een t he -
NiAl phase layer and the Si-rich carbide barrier.
3　Discussion
T he Al-Si coating is of typical inw ard-diff u-
sion type, w hich consist ed of t he -NiAl phase in
it s out er layer , depositing a small amount of t he
secondary phase particles along t he grain bound-
aries, such as MC ( M w as T i primarily ) , M 23 C 6
( M w as Cr primarily ) , ∀ and ( W , Mo ) observed
in Fig. 4[ 9] . During the immersion t est , the int er-
granular corrosion took place on t he surface of t he
Al-Si coat ing . A likely cause of t he degradat ion is
that t he secondary phases are preferentially corrod-
ed in the corrosiv e medium . T hen, some -NiAl
cryst al grains becam e loosely at tached and then
desquamat ed f rom t he surface w hen the corroded
sam ples w ere cleaned by running w ater, and t here-
fore t he corresponding holes can be observed( Fig.
5 ) . T hus, t he thickness of -phase layer de-
© 1994-2010 China Academic Journal Electronic Publishing House. Open access under CC BY-NC-ND license. http://www.cnki.net
・ 247・
creased. On t he ot her hand, af ter t he am bient -
t emperat ure corrosion , t he Al cont ent of t he sur-
face layer w as reduced obviously and the cont ent s
of ot her element s were increased correspondingly,
w hich w as due to t he f act that Al element was
more active t han ot her elements in the Al-Si coat-
ing. Hence it w as pref erent ially corroded. Conse-
quent ly , t his result ed in t he decrease of Al cont ent
in the coat ing before the initiat ion of t he oxidation
t est .
Fig . 4　T he secondary phases depositing along the
gr ain boundar ies of the sample surface
F ig . 5　Surface mor pholo gy o f the A l-Si coating
after ambient -temperature cor rosion
During t he initial stage of the isot hermal ox i-
dation, t he oxidation rate of t he coat ing w as con-
trolled by t he air/ coating int erf ace react ion. T he
Al element could be selectively ox idized t o form a
layer of prot ect ive Al2O 3 scale. It can be seen f rom
t he micrograph of t he sample surf ace t hat t he
Al2O3 scale f ormed on t he corroded coat ing was
very rough, w hich sug gest ed t he f act that t he real
area of t he corroded coat ing was greater than that
of t he orig inal coating . As a consequence , more Al
of the surface layer w as consumed t o f orm Al2O 3
scale and the w eig ht gain of t he corroded coat ing
 ・ 248・ ZHA N G Qi, SO N G Fu-bin, W A N G Hua-ge, LU O J un-hua
w as quicker t han t he original one. With t he
progress of oxidation, t he controlling step becam e
the diff usion gradually . T hat means, t he oxidat ion
process changed from the original directive react ion
betw een the coat ing and air int o the diff usion reac-
tion t hrough t he oxide scale and t he outw ard-diff u-
sion of t he Al elem ent. At t his t im e, since a larg e
am ount of Al beneath t he ox ide scale had been de-
plet ed in t he corroded coat ing , it could be consid-
ered t hat the grow t h rate of t he Al2 O3 was rest rict-
ed. How ever, owing t o no ef fect of am bient -tem-
perature corrosion on t he original coating , a suff i-
cient amount of Al was retained in it . T hus, t he
oxide scale on the original coating grew g radually
w it h t he progress of ox idat ion. T his induced that
the mass gain of the original coat ing w as close to
that of the corroded coating at t he init ial st age and
ex ceeded it at about 40 cycles.
Because the -phase can be transf ormed to t he
!′-phase in the lack of Al[ 10-12] , it could be f ound
from Fig. 2 ( a ) , ( b ) t hat t here w ere som e
!′
-Ni3Al phases f orm ed adjacent to t he int erf ace
betw een the -NiAl phase lay er and Si-rich carbide
barrier in bot h t he original and corroded coatings,
w hich w as due to considerable out ward dif fusion of
Al nearby t he interface area to form t he prot ect ive
scale. M oreover, owing t o t he deplet ion of Al in
the surf ace layer of t he corroded coating prior to
the oxidat ion , w it h process of ox idat ion , there was
a lay er of !′
-Ni3Al phases f orm ed beneat h t he ox-
ide scale.
T he failure of the prot ect ive oxide scale result s
mainly f rom t he t hermal expansion coef ficient m is-
match bet w een t he scale and the outer lay er of t he
coating . T hus, t he ox ide scale will be subject ed to
therm al st ress generat ed during t he cyclic oxidat ion
process. Moreover, owing to t he increase of t he
surf ace roughness af ter the ambient -t em perature
corrosion test in t he present st udy , t he stress had
also been generat ed wit h t he g row t h of t he ox ide
scale on t he corroded surf ace. T he spallat ion can
be induced by t he st resses, w hich result ed in a
great er w eight loss of the corroded coat ing under
cyclic oxidation conditions. In addition, as men-
© 1994-2010 China Academic Journal Electronic Publishing House. Open access under CC BY-NC-ND license. http://www.cnki.net
CJA
tioned previously, it should be not ed t hat T iO 2
could be f ound on the corroded coat ing caused by
t he sim ilar free energies of the formation of T iO 2
and Al2 O3 [ 13, 14] . T iO 2 is an oxide wit h productivit y
much weaker t han Al2 O3 [ 14] . M oreover , because
T iO2 could dest roy the continuit y of the prot ect ive
oxide scale, t he compound ox ide scale consisting of
T iO2 and Al2 O3 had large inner stress and w as easy
t o crack and spall. As a result, the w eight gain of
t he corroded coating was much less t han t hat of
t he orig inal coat ing during the cyclic oxidation
t est , and t he cy clic oxidation resist ance had been
reduced severely by the am bient -t emperat ure cor-
rosion .
A layer of !′
-Ni3Al phases could be found be-
neat h t he Al2O 3 scale in the corroded coat ing aft er
50 cycles at 1050℃, w hich w as t he same reason as
t hat of isot hermal oxidation mentioned previously.
How ever, there w ere not !′ -Ni3Al phases observed
in t he original coating at the same t ime . T his re-
veals t hat the suff icient Al content was rem ained in
t he coat ing. Aft er 150h cyclic ox idat ion, larg e
numbers of Al adjacent to t he int erface bet w een
t he -NiAl phase layer and the Si-rich carbide bar-
rier had diff used outw ardly t o heal the spalled ox-
ide scale. T his induced t hat a mass of -NiAl phas-
es transformed to !′ -Ni3Al phases in t he
zone
[ 15, 16]
. Especially , t he !′
-Ni3Al phases in t he
corroded coating almost dispersed t hrough the en-
tire outer layer. T o sum up, ow ing t o prev ious de-
crease of t he t hickness of t he -NiAl phase lay er
and t he Al content within the surf ace layer aft er
t he am bient -t emperat ure corrosion, it induced that
t he cy clic oxidation resist ance of Al-Si coat ing was
w orsened severely .
4　Conclusions
T he Al-Si coating specimens w it h / wit hout
im mersion test w ere oxidized cyclically w it h t he
t emperat ure varying betw een ambient -t em perature
and 1050℃ in air . T he isotherm al ox idat ion t est
w as also perf ormed f or short periods. Depending
on t he experiment al result s, the follow ing main
point s w ere att ained.
 Inf luence of A mbient-T emperat ure Corrosionp
N ovember 2002
on t he O xidat ion Behavior of A l-Si Coatings
( 1) Ambient -temperat ure corrosion decreased
the useful life of t he Al-Si coat ing obviously .
( 2) T he surf ace roughness of the Al-Si coat-
ing increased obviously and the Al cont ent of t he
surf ace layer decreased severely , ow ing t o t he am-
bient -t emperat ure immersion corrosion .
( 3 ) T he ox ide scale consists primarily of
Al2O3 contaminated w ith T iO 2 and the isot hermal
oxidation behavior chang ed aft er the am bient -tem-
perature corrosion.
( 4) T he cyclic ox idat ion resistance decreased
severely caused by t he ambient -temperat ure corro-
sion.
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Biography:
ZHANG Qi　Bo rn in 1945, P rofessor .
She graduated fr om Beijing U niv er sit y
of A er onautics and Astronautics in
1969, and g ot her P hD at U M IST U .
K . in 1990, and did the post-doctorial
resear ch at CN RS, F rance in 1991. She
has been major ing in failure analy sis,
corr osio n control, protection methods, co mputer simula-
tion of the corr osion behav ior , the ex per t system etc, about
the aeronaut ical and astro nautical materials, including high
str eng th alum inum alloys, N i-based alloy s and their high
temper atur e protective coatings, carbon/ epo xy composites
etc. She has published mor e than 50 papers in the above a-
cademic field in recent y ear s. T el: ( 010) 82316841.