ú{à®wï æ 66 ª æ 7 †(2002)784_791
½ž«nËÉæ邻¨±qªU`^“A‹~iChî
¡‡çŒÌì»
¯ R N m1,Þ
O î G a2
º 㠒 ™3
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1Ö¼åwåw@Hw¤†È
2Ö¼åwHw”Þ¿HwÈ
3åãåwYÆÈw¤†Š
J. Japan Inst. Metals, Vol. 66, No. 7 (2002), pp. 784_
791
Ý 2002 The Japan Institute of Metals
Titanium Aluminide_Based Composite Deposits with Dispersed Nitride Particles Produced
by Reactive Thermal Spraying
Yasuhiro Hoshiyama1,Þ
, Hidekazu Miyake2, Kenji Murakami3 and Hideo Nakajima3
1Graduate
School of Engineering, Kansai University, Suita 564_
0073
2Department
3The
of Materials Science and Engineering, Faculty of Engineering, Kansai University, Suita 564_
0073
Institute of Scientific and Industrial Research, Osaka University, Ibaraki 567_
0047
A composite powder is produced by ball_milling of elemental titanium, aluminum and aluminum nitride powders in an argon
atmosphere, and is plasma_
sprayed in an argon atmosphere, yielding titanium aluminide_
based deposits. The constituents of
sprayed deposit results in the formation of
the as_
sprayed deposit are Ti3Al (a2), TiAl (g) and Ti2N. Heat treatment of the as_
Ti2Al(C, N). The carbon in Ti2Al(C, N) is incorporated into the composite powder during ball_milling due to decomposition of
methanol which is used as process controlling agent. There is little difference in hardness between the as_
sprayed deposit and the
deposits heat_
treated at temperatures up to 1473 K. Hardness of the as_
sprayed deposit and the heat_
treated deposits are higher
than that of the cast titanium_aluminum binary alloy whose titanium and aluminum contents are similar to those of the sprayed
deposit.
(Received March 1, 2002; Accepted May 30, 2002)
Keywords: titanium aluminides, ball_
milling, reactive plasma spraying, composite powder, nitride
½žMÉæèn˱qªÇÁÁM³êé½ßC½žðºíÈ
1.

¾
¢ÊíÌv‰Y}nËÌê‡Éä×ÄîÞÉÕ˵½²–±
qÌG½»ª£i³êCæèk§ÅG½±qÔª­Åɋ‡
ßNCà®Ô»‡¨ª‚·Þ¿ÆµÄÚ³êĨèC»
µ½Þ¿Ì컪úÒÅ«é3)D±Ì½ž«v‰Y}nË@
ÌêÂÉ`^“A‹~iChà®Ô»‡¨ª éD`^“A
ÉÍC2 íÞÌû@ª éD1 Âͽž«Ì év‰Y}K
‹~iChÍCyÊł·­xÆÏ_»«ªDêÄ¢é½
XÆnËÞ¿Æ𽞳¹éû@Å èCठ1 ÂÍCÝ
ßCqóEFˆpâ©®ÔpG“W“”iÈÇÉgp·éŸ
¢É½žðN±·´¿©ç¡‡²–ð컵C±êðnË·
¢ãÌyÊÏM޿ƵÄúÒ³êÄ¢é1)Dµ©µC`^
éû@Å éDãÒÌáƵÄCºãçÍ`^“²–CA‹
“A‹~iChÍí·tßÅ̄«ªá¢½ßÉC]ˆÌ³
~jE€²–¨æÑ{“²–𢱵½¡‡²–ð¸³v
„@ÅÍÁHÅ«È¢ïÁH«Þ¿Å éD±êÜÅCA‹
‰Y}n˵C÷×È TiB2 ±qðªUµ½`^“A‹~i
~jE€ÜLÊ̲®âæO³fÌYÁÉæÁĄ«â‚·
Ch޿ð컵Ģé4)D
­xÉDê½`^“A‹~iChð¾éŽÝ2)ªÈ³êÄ«
`^“A‹~iChÌÏNŠ[vÁ«ðüP·é½ßÉC
½ªC³çÉVµ¢`^“A‹~iChÌ»¢vZXðm
d¿ÅÏM«Ì é TiB2 ±qð`^“A‹~iCh}gŠ
§·éKv«ª©ÎêÄ¢éD±Ìæ¤ÈvZXÌêÂ
bNX†Én»@ŪU³¹éŽÝªÈ³êÄ¢é5_11) D
ÉCÞ¿ðv‰Y}WFbgÉæÁÄÁMCnZCÁ¬µî
Hyman ç6)Í{“ð 0.1 mass÷ðÜÞ`^“_A‹~jE
ÞãÉçŒðì»·év‰Y}nË@ª èC±êÍo‹N
€‡àòð컵C10`20 mm ÌubNóÌ TiB2 ±qª
ÞðìéXvŒ[tH[~“OÉàgíêÄ¢éDÁÉ»¡
‰»ÆµÄ`¬³êÄ¢é±ÆðñµÄ¢éDܽCXD
[¢ÌÍCnËÞ¿†Ì»w½žÉæÁÄ»‡¨ð‡¬·é
vZXÅͽž¶¬µ½ 1 mm ÈãÌ TiB2 ±qª`^“
½ž«v‰Y}nË@Å éD½ž«v‰Y}nË@ÅÍC
A‹~iChɪUµÄ¢é10,11)D±êç̱qÌ嫳É
ä×Cºãç̤†Å`^“A‹~iCh޿ɪU
ÞÖ¼åwåw@¶(Graduate Student, Kansai University)
µ½ TiB2 ±qÍC‡àÌ{“ÜLʪ 2 mass÷Ƃ¢É
7
æ
†
785
½ž«nËÉæ邻¨±qªU`^“A‹~iChçŒÌì»
à©©íç¸ÉßÄ÷×Å é4) D½ž«v‰Y}nËÅ
̬‡ðÍCTi_Al_N Ì 3 ³nóÔ}17)©çC®( 1 )Ì
ÍCîÂÉÕ˵½tHÌâp¬xªÉßÄå«¢Ì
½žÉæÁÄCTi3Al(a2 Š)¨æÑ TiAl(g Š)©çÈé}g
Å12) C½ž«v‰Y}nËÍC»Ì궬µ½÷×ÈZ‰
ŠbNX†É Ti2AlN ±qðªU³¹½çŒª¾çêéð
~bNX±qð`^“A‹~iCh}gŠbNX†ÉªU³
Ƶ½D·Èí¿Cì»·éçŒÌ}gŠbNXg¬ª`^
¹½¡‡Þ¿ðì»·é£ÍIÈvZXÅ éD
“ 67 mass÷CA‹~jE€ 33 mass÷Å èC‚fÜLÊ
‚fÍ`^“¨æÑA‹~jE€Æ½žµÄd¢‚»¨ð
ª 1 mass÷ÆÈéæ¤z‡µ½DTi_Al_N ¡‡²–ðnË
¶¬·éD˜ÒçÍC`^“¨æÑA‹~jE€²–ð‚f
µ½ÛCA‹~jE€ª‚·xÌv‰Y}tŒ[€†Åê”
µÍC†Å{[‹~Š“OµÄ¾½¡‡²–(ȺCTi_Al_
ö­µCçŒÌA‹~jE€ÜLʪ²–Ì»êÉä׸­
N ¡‡²–ÆÌ·)ðv‰Y}n˵C`^“A‹~iCh
µ½13) D{À±ÅÍC±ÌA‹~jE€Ì¸­ðl¶µC
îÌú¢¡‡çŒð컵½13) DçŒðì»·éÛCnË
¡‡²–Ì컞Éz‡Êð]ªÉ 7 mass÷½­µ½DÜ
†Ì猷xÌᢪ컵½çŒÌgD¨æÑÁ«ÉyÚ
½C¡‡²–ðì»·éÛC~Š“O•ÜƵÄp¢½^
·e¿ðŸ¢·é½ßCîÂͼڅâ·éê‡ÆÔÚIÉ
m[‹ªªðµ²–†Éæè±ÜêéYfÌe¿Íl¶µÄ
…â·éê‡Ì 2 íÞƵ½D¼Ú…âµ½îÂãÉì»
¢È¢D컵½¡‡²–ð Ti_Al_AlN ¡‡²–ÆÌ·D
µ½çŒÌ\¬ŠÍnËvZXÉÁ¥IÈ}âÃÅÉæÁ
Table 1 É{[‹~Š“Oðð¦·D¾ç꽡‡²–ð
Ăf¨æÑYfªßOaÉÅnµ½ Ti3Al Å èC±ÌÞ
32`53 mm ÉÓ颪¯µCX üñÜ(CuKa ü)ÉæéŠÌ
¿ðMˆ·éÆ TiAlCTi2N ¨æÑ Ti2AlC ª¶¬µ½D
¯è¨æÑ SEM ÉæéÏ@ðsÁ½D
çŒÉÜÜêéYfÍC~Š“O•ÜƵÄp¢½^m[
‹ªªðµ²–†Éæè±Üê½àÌÅ é14_16) DÔÚI
2.2
½ž«v‰Y}nË
Ʌ⵽îÂãÉ컵½çŒÌ\¬ŠÍ Ti3AlCTiAl
A‹~iÅOŠbgu‰Xgµ½ 8 ‡Ìc 50 mm~¡ 60
¨æÑ Ti2N Å Á½D±êç컵½çŒÌ\¬Šðl¶
mm ~ ú ³ 3 mm Ì SS400 î  ð ñ ] V ƒ t g É æ è t
µC¡‡²–Ì‚fÜLÊðÁ³¹ÄCn˵½ÜÜÌó
¯CeR 7MT ^v‰Y}K“ðp¢ÄC40 kPa ÌA‹
ÔÅ Ti2AlN ðªU³¹½`^“A‹~iChçŒð
S“µÍC†Å¡‡²–ð¸³v‰Y}n˵½D±ÌÛC
ì»·é±ÆðŽÝ½D
K“ÍÅèµ½ÜÜÅ èCîÂðæ诽Vƒtgðñ
˜Òç13) ªì»µ½ Ti_Al_N ¡‡²–Ì‚fÜLÊÍ
]³¹½Dºãç18_21)C¨æÑ Hoshiyama ç13)̤†Éæ
0.1 mass÷Å Á½D»±ÅC`^“¨æÑA‹~jE€²
éÆCnˆÌ猷xðK–È‚·ÉÛÂÆCE¦ªá
–ð‚fµÍC†Å 75.6~103 s ~Š“OµCÄxCeíà
­Cܽ÷×ÈÍo±qª½­ªUµ½çŒðì»·é±Æ
ɂfKXð±üµ~Š“O·éÆ¢¤Höð 4 ñ(‡v
ªÅ«éDµ½ªÁÄ{¤†É¨¢ÄàCnˆÉîÂÌâ
302.4~103 s)JèÔµC¡‡²–†Ì‚fÜLÊðÁ³
pðsÁĢȢDTable 2 Év‰Y}nËðð¦·Dn
¹é±ÆðŽÝ½Dµ©µC»Ìê‡Åà‚fÜLÊÍ 0.1
mass÷ÆÏíçÈ©Á½D±Ìæ¤ÉC‚fÜLʪϻ
µÈ©Á½½ßC{¤†ÅÍC‚f̟‹¹ÆµÄ‚fKX
Table 1
Ball_
milling conditions.
æèࡇ²–Ì‚fÜLÊðeÕɲ߷é±ÆªÂ\È
Milling vial
AlN ²–ðp¢½DAlN ÍC¡‡²–ðì»·éÛ̳f
Ball pestle
Cr steel, 12.7 mm dia, 7 kg
Starting powders
Ti(100.5~10|3 kg){Al(64.1~10|3 kg)
{AlN(4.4~10|3 kg)
Rotation speed of vial
1.5 s|1
Milling time
3.02~105 s
Process control agent
methanol, 3.0~10|6 m3
Atmosphere
Ar
²–Å éA‹~jE€Ì‚»¨Å é½ßC²–¨æÑç
ŒÌg¬Ée¿ðyڳȢD`^“CA‹~jE€¨æÑ
AlN ²–©ç컵½¡‡²–ðp¢Äv‰Y}n˵C
6Ti{2Al{AlN¨Ti3Al{TiAl{Ti2AlN
(1)
̽žð˜pµ¡‡çŒÌì»ðŽÝ½D·Èí¿CAlN
ªnˆÉZðµA‹~jE€¨æтfɪðµC`^“
SUS304, 2.6~10|3 m3
¨æÑA‹~jE€Æ‹‡·é±ÆÉæÁĶ¬·é
Ti2AlN ±qðªU³¹½`^“A‹~iChçŒÌ
gDÆÁ«ð]¿µ½D
2.
À
2.1
±
û @
¡‡²–Ìì»
ƒx 99.4 mass÷űa 45 mm ȺÌ`^“²–(100.5~
10|3 kgjCƒx 99.9 mass÷űa 45 mm ȺÌA‹~jE
€²–(64.1~10|3 kg)¨æѱa 1 mm ÈºÌ AlN ²–
(4.4~10|3 kg)ðA‹S“µÍC†Å{[‹~Š“OµC¡
‡²–ð컵½D±ÌÛC~Š“O•ÜƵā^m[‹
(3.0~10|6 m3)ðÁ¦½D¡‡²–ðì»·éÛÌ´¿²–
Table 2
Plasma spraying conditions.
Plasma gases
Primary gas, Ar
4.9~10|4 m3/s
Secondary gas, H2
1.5~10|4 m3/s
Voltage_current
60 V_500 A
Chamber
Gas
Ar
Pressure
40 kPa
Spraying distance
0.3 m
Substrate rotation
1 s|1
Spraying time
90 s, 150 s~3
786
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ˆÌ猷xÌᢪG½±qÔ̧…ÍâÍo±q̶
­©¦éA‹~jE€ªwó\¢ðȵĢéDAlN Íñ
¬ÉyÚ·e¿ðŸ¢·é½ßCn˞Ôð 90 s ¨æÑ
íÉ÷×Ȳ–Å é½ß Fig. 1 ÅÍ©çêÈ¢D
450 s Ì 2 íÞƵ½D»ê¼êÌn˞ÔÅ컵½çŒ
ðCçŒ A ¨æÑçŒ B Æ»ê¼êÌµC»ê¼êÌ
3.2
¡‡²–©ç컵½çŒ
as_
sprayed çŒðçŒ A0 ¨æÑ B0 ÆÌ·DçŒ B Ìê‡C
Table 3 ÉçŒ B0 Ì»wg¬ð¦·DçŒÌA‹~jE
450 s ÔA±ÅnËðs¤ÆCîªÔMóÔÉÈèc£·
€ÜLÊÍ¡‡²–Æä×Äñ 8.4 mass÷á¢D±êÍC
é±ÆÉæÁÄçŒÉžÍªW†µ„ꪶ¶éÂ\«ª ¡‡²–ª‚·xÌv‰Y}tŒ[€†ðòsµÄ¢éÔ
é½ßC150 s n˵ 300 s âp·éÆ¢¤Höð 3 ñs
ÉCA‹~jE€ªê”ö­µ½½ßÅ éÆl¦çêéD
¢C‡vn˞Ôð 450 s Ƶ½DçŒ A0 Ìú³Íñ 400
Fig. 2 Æ Fig. 3 ÉçŒ A ¨æÑçŒ B Ì X üñÜ}`ð»
mm Å èCçŒ B0 Ìú³Íñ 2000 mm Å éDîÂðæ
ê¼ê¦·DçŒ A0CB0 ÆàÉC\¬ŠÍ Ti3Al(a2 ŠjC
诽Vƒtgªñ]·éÌÅnˆÉMdÎÅî·x
TiAl(g Š)¨æÑ Ti2N ŠÅ éDçŒ A0CB0 ÆàÉ 873
ðªè·é±ÆªÅ«È¢D»±ÅCî Ê̆›”ªÉ
`1473 K ÅMˆ·é±ÆÉæÁÄCTi2Al(C, N)ÌñÜ
¼a 7.0 mmC[³ 1.0 mm ̊ð 4 –Š ¯C»±ÉZ_
s[NªŸo³ê½D±±ÅCTi2AlC ¨æÑ Ti2AlN ͋
ÌÙÈéà®Ðð»ê¼ê•UãCîÂ\ÊÉv‰Y}nË
»\¢ª¯¶Åiqè”àÉßÄߢÌÅñÜpªÝ¢ÉÙ
µCeà®ÐÌnZÉæé`óÏ»©çî·xðªèµ
Ú¯¶Å é±ÆC¨æÑãq·é EPMA ªÍÅÍo¨©
½DçŒ B ðì»·éÛÌłî·xÍñ 873 K Å éD
2.3
çYfƂfª¯žÉŸo³ê½±Æ©çCãLÌñÜs[
Nð Ti2AlC ÌYfÌê”ð‚fªu··é±ÆÉæÁĶ
çŒÌ]¿
¬·é Ti2Al(C, N)22) Å éƵ½DFig. 2 Æ Fig. 3 Ì X
çŒðî©ç@BIɪ£µCÎpÇÉ^ó•üµC
üñÜ}`ɨ¢ÄCMˆ·xÌã¸ÆÆàÉ a2 ŠÌ„
873 K, 1073 K, 1273 K é¢Í 1473 K Å 7.2 ks ۝ãC
‡ª¸­µCg ŠÌ„‡ªÁµÄ¢éD±êÍCnËÉÁ
Fâµ½DçŒ A0 ð±êçÌ·xÅMˆµ½çŒð»ê
¥IÈ}âÃÅÅ`¬³ê½€ÀèÈ a2 ŠªMˆð{·
¼êçŒ A1, A2, A3, A4 Æ̵CçŒ B0 ð±êçÌ·x
±ÆÉæÁÄꔪðµÄ g Šª¶¬·é23,24)½ßÅ éD
ÅM ˆ µ ½ç Œð » ê¼ ê B1, B2, B3, B4 ÆÌ · DÜ
çŒ A0 ¨æÑçŒ B0 ÆàÉCv‰Y}tŒ[€†ÈçÑ
½CçŒ B0 ð 1473 K Å 216 ks ۝ãCFâµ½çŒðç
ÉçŒÌ}âÃÅɺ¤ñ½tóÔºÅCTi2N Šª`¬µ
Œ B5 ÆÌ·DçŒfÊð¤ãCtb»…f_(3.0~10|6
½Æl¦çêéDµ½ªÁÄC®( 1 )ÌEÓÍȺÌæ¤
m3 ){É_(2.0~10|5 m3 ){…(7.7~10|5 m3 )̅Htðp
ɦ³êéD
¢Äº·Å 1`3 s ԅHµCSEM Ï@¨æÑ EPMA ªÍ
ðsÁ½DܽCX üñÜ(CuKa ü)Ŋ̯èðs¢C}
¨Ti3Al{TiAl{Ti2N{N{C
(2)
±±ÅC®( 2 )Ì N ¨æÑ C ÍCn蠃 a2 Š¨æÑ g
gŠbNX†ÌÍo¨É墀 TEM Ï@ðs¢CçŒfÊ
Š©çÈé}gŠbNX†É­§Ån³ê½‚f¨æÑYf
ãÅ 2.94 N Ì×dðp¢Ä}CNrbJ[Xd³ðªè
Å éD®( 2 )Ŧ³êé as_sprayed çŒðMˆ·éÆ
a2 ŠÌê”Í g ŠÉªðµC}gŠbNX†É­§Ån³
µ½D
꽂f¨æÑYfª`^“¨æÑA‹~jE€Æ‹‡µC
3.
‹ Ê Æ l @
3.1
®( 3 )ɦ·æ¤É Ti2Al(C, N)ª¶¬µ½Æl¦çêéD
¨Ti3Al{TiAl{Ti2N{Ti2Al(C, N)
¡‡²–
(3)
Table 3 É¡‡²–Ì»wg¬ð¦·D‚f̟‹¹Æµ
Ä AlN ²–ðp¢½±ÆÅCŸ‹¹ÆµÄ‚fKXðp¢
½ê‡Ì‚fÜLÊ(0.1 mass÷)13) æè 0.99 mass÷Ƃ
¢DȨCYfÌÜLÊÍ 0.61 mass÷Å éD±ÌYf
ÍC~Š“OÌÛC•ÜƵÄp¢½^m[‹ªªðµÄ
²–†ÉæèžÜê½àÌÅ é14_16)DFig. 1 Ì SEM Ê^
ɦ·æ¤ÉC¡‡²–ÌfÊÉ;魩¦é`^“ÆÃ
Table 3 Chemical compositions of the composite powder and
the deposit B0.
(mass÷)
Composite powder
Deposit B0
Ti
59.1
67.4
Al
39.3
30.9
N
0.99
1.0
C
0.61
0.70
Fig. 1 Scanning electron micrograph of cross_section of com­
posite powder.
æ
7
†
½ž«nËÉæ邻¨±qªU`^“A‹~iChçŒÌì»
787
ȨCçŒ ACçŒ B ÆàÉCas_sprayed çŒÉÍ Ti2N
æéàÌÅ éDYfÌÅnÀÍC1023 K Å 0.3 mass÷Å
Šª¶¬µCTi2Al(C, N)Ͷ¬µÄ¢È¢D±êÍCa2 Š
è‚fæèà‚¢17,25)D»Ì½ßCYf͂fæèà a2
¨æÑ g Š©ç¬éÌæÉηé‚fÆYfÌÅnÀÌ·É
Š¨æÑ g Š©ç¬é}gŠbNXÉÅnµâ·¢DæÁÄC
Fig. 2 X_ray diffraction patterns of deposit A.
(a) deposit A0; (b) deposit A1; (c) deposit A2; (d) deposit A3;
(e) deposit A4.
Fig. 3 X_ray diffraction patterns of deposit B.
(a) deposit B0; (b) deposit B1; (c) deposit B2; (d) deposit B3;
(e) deposit B4; (f) deposit B5.
Fig. 4 Scanning electron micrographs of cross_sections of
deposit A.
(a) deposit A0; (b) deposit A1; (c) deposit A2; (d) deposit A3;
(e) deposit A4.
788
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66
ª
Fig. 5 Scanning electron micrographs of cross_sections of
deposit B.
(a) deposit B0; (b) deposit B1; (c) deposit B2; (d) deposit B3;
(e) deposit B4.
as_sprayed çŒÉÍ Ti2Al(C, N)Ͷ¬µÄ¢È¢Æl¦ç
2 mm Ìeåȱqª¬ÝµÄ¢éDçŒ A4 ¨æÑçŒ B4
êéD
ÆàÉÍo±qª½¢ÌæÆ­È¢Ìæª éD±êÍCç
Fig. 4 Æ Fig. 5 ÉçŒ A ¨æÑçŒ B ÌfÊÌ SEM Ê
ŒðMˆ·éÆ Ti2Al(C, N)ª`^“Zx̂¢Ìæɽ
^ð¦·DçŒ A0 ÅÍñ 0.1 mm Æñ 0.5 mm ÌÍo±qª
­¶¬·é17,22,25)½ßÅ éD®( 2 )Æ®( 3 )̽žÉæÁ
¬ÝµCçŒ B0 ÅÍñ 0.5 mm ÌÍo±qª©çêéD±
ÄCas_sprayed çŒ é¢ÍMˆçŒÅ Ti2N Š¨æÑ
êçÌÍo±qÍCFig. 2 Æ Fig. 3 É»ê¼ê¦µ½ X ü
Ti2Al(C, N)ª¶¬µ½±Æ©çC‚f̟‹¹ÆµÄp¢
ñ܋ʩç Ti2N ŠÅ éDçŒ A0 ¨æÑçŒ B0 Æà
½ AlN ÍnˆÉZðµC‚fÍ`^“Æ‹‡µÄ Ti2N Š
ÉCSEM Ê^ɨ¢ÄC}gŠbNXɾ魩¦éÌæ
𶬷éC൭Í}âÃÅÉæÁÄçŒÌ}gŠbNX
(G½±q)Æí©¦éÌæª èC¾é­©¦éÌæÉ
†É­§Ån³êéÆl¦çêéD±ÌçŒðMˆ·é±
Ti2N Šª½­¶¬µÄ¢éD±êÍçŒàÌg¬ÌsÏê
ÆÉæÁÄ Ti2AlC ÌYfÌꔪ‚fÆu·µ½ Ti2Al(C,
«ÉæéàÌÅ éDçŒàÌg¬ÌsÏê«ÍC¡‡²–
N)ª¶¬·éDçŒ A ÆçŒ B ðär·éÆCçŒ A Ì
Ìg¬ÌsÏꫪe¿µÄ¢éD³çÉv‰Y}tŒ[€
ûª÷×ÈÍo±qª½¢D±êÍCçŒ B0 ÌûªçŒ
†Å̲–ÌòsoHÌᢩçCÂX̲–±qŬª³
A0 æèànˆÌ猷xª‚·Å é½ßÅ éD
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Fig. 7 TEM micrographs of deposit B.
(a) deposit B0; (b) deposit B4.
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