• 검색 결과가 없습니다.

Òò~B–5 wÏö®ÚBºÒ W

N/A
N/A
Protected

Academic year: 2024

Share "Òò~B–5 wÏö®ÚBºÒ W"

Copied!
6
0
0

로드 중.... (전체 텍스트 보기)

전체 글

(1)

Ni-Fe  . «¶ ªÖ Al

2

O

3

¾ž Ò ò ~ ^– ç 5 ß W

ΧCÁ;Ò'ÁJßçÁšÒWÁšsÒ*Á;'"*

‚·&v .³Òò"

*ºëVFö ¾ž²Ò&

Microstructure and Properties of Nano-Sized Ni-Fe Alloy Dispersed Al

2

O

3

Composites

Seok Namkung, Jae-Young Jeong, Sung-Tag Oh, Jai-Sung Lee, Hong-Jae Lee* and Young-Keun Jeong*

Dept. of Metallurgy and Materials Science, Hanyang University, Ansan 425-791, Korea

*Nano Materials Lab., Korea Institute of Ceramic Engineering and Technology, 233-5 Gasan-Dong, Seoul 153-023, Korea

(Received 23 April 2002 ; Accepted form 4 June 2002)

Abstract - Processing and properties of Al2O3 composites with Ni-Fe content of 10 and 15 wt% were investigated.

Homogeneous powder mixtures of Al2O3/Ni-Fe alloy were prepared by the solution-chemistry route using Al2O3, Ni(NO3)2Á6H2O and Fe(NO3)3Á9H2O powders. Microstructural observation of composite powder revealed that Ni-Fe alloy particles with a size of 20 nm were homogeneously dispersed on Al2O3 powder surfaces. Hot-pressed composites showed enhanced fracture toughness and magnetic response. The properties are discussed based on the observed microstructural characteristics.

Keywords : Nanocomposite, Chemical processing, Fracture toughness, Magnetic property

1. B †

¾ž’V~ .³«¶¢ ^¢ VæÚö ªÖÎ

¾žÒòº ^¢Òò~ £‚ ÏÏW" Ô f &Wj ~² >–, ‚’V~ ªÖç j <º ¢>'ž Òòf jv~ ;ê 5

žW, Ò Ö>‚ NßWj B–† > ®º 6öB ôf ’~ &çš > ®.1-3) š‚ ^

¢/.³ ¾žÒòº ËçB Vê' ßW" Ž þ VËW .³«¶~ ªÖj Û~ î‚Ú ßWj

<º .æ Òò‚~ wϚ &Ë~. .¢ Ú, Al2O3/W,4) Al2O3/Ni5) 5 Al2O3/Ni-Co6) ~ Al2O3/.³ ¾žÒòº 1 GPa šç~ ;êf Ã&B žW8j ¾æÚ–, Ni 6º Ni-Co çj Î

&‚ ãÖ ë߂ ¶V' ßW 5 wKb ~ .æ VËW j &.

¾ š‚ Ë6öê ®’~ VËW ¾ž

Òò~ B– 5 wÏö ®ÚBº ÒW~ ^Bö ò jî¢, ;&‚ ^–ç BÚ 5 n;‚ ßW’

* ö ôf ÚJæš ®.7,8) šº VËW ¾ž

’V .³«¶~ ªÖj ۂ ^¢Ú~ VË zö &‚ æ.ræ~ ’& V.*çö &‚ Úê 'ž šC, ¯ ªöWV’, ^–ç B";" ö

ž ö &‚ ;{‚ šš ìš ãþ'ž O»b‚

ò B–>Ú ·‚ êö &‚ B–;~ ‚' zf ;&‚ ^–ç 5 ßWBÚ& Ú[V r^š

. V¢B ^¢/.³ ¾žÒò~ ë߂ . æVËWj ò—ÊV *šBº B–;ö &NB .³ªÖ«¶~ WV’, ‚'~ Î&ï 5 ‚« ²

’z ";ö ššVræ~ ^–ç B";" ~

&z–ÿö &‚ ;ï'ž šCš º’B.

‚"ö &¶f .³Özb~ >²~ö 5

(2)

*&{²Öj Û~ Ã&B Vê' 5 ¶V' ßW j <º Al2O3/10 wt% Ni-Fe ¾žÒò~ B–

ö &~ ‚ : ®.9)¾ š‚ ¾ž

Òò¢ º’ WËö ¦~º VËW Òò‚~ w Ïj *šBº ¾ž’V .³ªÖç~ Î&ïš ‚

« ^–ç 5 ßWö ~º 'Ëj ;ï'š Ú ê'b‚ šC~º ’& jº~. 6‚ š‚ Ö

"¢ V.‚, º’>º ²ÖÚ~ ßW ö ¦~º ''~ ¾žªö~ Jê 5 B–;~ ‚'z

& &Ë~. V¢B ’öBº Al2O3 Væçö Ni-Fe . ªÖçj '' 10 wt% 5 15 wt% Î&

~ ‚« ²ÖÚ~ ^–ç" Vê' 5 ¶V' ß Wö ~º ªÖç~ 'Ëö &~ –Ò‚ ê, º

’>º ßWö ¦~º ‚'~ ªöW ;j B

~¶ ‚.

2. þ O»

þö Òς ÂBöòº, High Purity Chemetals Lab. (Japan) B®~ Fe(NO3)3Á9H2O, Ni(NO3)2Á6H2O

" α-Al2O3 (99.99%, 0.2µm, Sumitomo Chem.

Co., Japan) š. ªÖçf ÂBöòž v .³îÖ

"j ‚« Z²j& Ni0.5-Fe0.5 .š >êƒ “ï

~ öêR 200 ml f Žþ 2¢Ê’ö I, 6 öB 40oC‚ &~ j*® ϚV. ϚB .

³"ö α-Al2O3 ªö 5 200 ml~ Ïê ¦b¢ <

º Al2O3 " (çã 5 mm, 99.5%)j Òö2 Ï Vö Žþ IÚ 3Nö bVöB 24* ÿn Û

&ç ~&. šr, Al2O3ªö~ ·f ²Ö ê ‚«

–Wš '' Al2O3/10 wt% Ni-Fe" Al2O3/15 wt%

Ni-Fe Ú& >êƒ Î&~&. Û&çö ~š

bB ªöf ÃBV¢ ÒÏ~ j*® š–¢ ~ , 400oC, &V 7öB 2* ÿn ~²¢ Û~

.³"j .³Özb ç‚ æ~~&. ~²B ª öf w÷ç~ ‚²zf î‚ bj *~ ? f –šb‚ Û&çj ¯‚ ê, çã 10 mm~

Al2O3 "j šÏ~ 24* ÿn š&ç ~&.

²Öf *&{²ÖV (hot-press)¢ šÏ~,

ªöj wšö If ê ²Ö‚ö Ë«~

700oC 5 1100oCöB '' 1* 5 30ª ÿn >

² ~ö‚ ê, 곚B jšb‚ ª*V¢ æ~~

1450oCöB 1* ÿn ²Ö~&. &{f 30

MPa~ {Kb‚ 1N >²~öš ƒ¾º Nêž

700oC¦V ¯~&b–, ßN³êº 20oC/min‚ ¢;

~² Fæ~& ²Öš ƒÂ êº žïj ~&

. jvÞb‚º B>‚ Al2O3 ªöj ÒÏ~

ÿ¢‚ –šb‚ ²Ö~&.

ªöbÚ~ ~ö–ÿf îïªCV(TG) Úö ªöj Ë«‚ ê, ßN³ê 10oC/min‚ &~–

>²ª*VöB Z²æz¢ G;~ ªC~&. "

Ò*¶*ã(SEM) 5 R"*¶*ã(TEM)j šÏ

~ ^–çj &V~&b–, ç ªCj *~ X- F ².ªC(XRD)j >¯~&. ²ÖÚ~ &êº toluene χ Úö Þj If ê Archi-medesöÒ

¢ šÏ~ êÖ~&. 2ZžW 5 ãêº Indentation Fracture(IF) O»10)b‚ Vickers ãêê

¢ šÏ~ ~7 10 kg, Fæ* 15 s~ –šb‚

G;~&. ¶V' ßWf vibrating sample magnetometer(VSM)j ÒÏ~ ‚& 10 kOe~ ¶ ê¢ ž&~ G;~&.

3. Ö" 5 V

'' 10 wt% 5 15 wt% Ni-Fe~ Î&ïj <º Al2O3 ªöbÚ¢ &ç 5 ~²¾Ò‚ ê TG¢

šÏ~ >²~ö –ÿj ªC‚ Ö"¢ â 1ö

¾æÚî. ~² ê Al2O3/.³Özb ç‚ šÒ

~&~ ªöf >²ª*VöB &, ÞÚ

~ H2O 6º FV®Bb~ ÃBö Vž~ £ 300oCræ 6ê'b‚ Z²& 6²‚. 300oC š çb‚ ßN~š, £ 400oCræ /ς Þ~ Z

² 6²& &V>º:, šº Fe- 5 Ni-Özb~ >

²~ö ";b‚ W>º H2O~ ÃBö Vž‚ © b‚ J«B.11) ê³'ž &‚ ªöbÚ~ Z

²º 6²~¾ Nê& 600oCö ššš –~ ¢;‚

8j Fæ~ >wš jò>îrj r > ®. š

‚ –ÿf 10 wt% 5 15 wt% Ni-Fe~ Î&ïj

<º Al2O3 ªöbÚöB ÿ¢~¾ â 1ö ¾æ Þ :f ?š .ç Î&ïö V¢ Z²6²·f N

𢠾æÚ ®. V¢B þ–šöB Al2O3/ .³Özb ªöbÚº 600oCšçöB >²~ö ö ~~ Î .³ªÖç~ Özbš .³b‚

~öB 6B. *~ Ö"¢ Û~ Al2O3/Fe- 5 Ni-Özb bÚ~ >²~ö –šj 700oC, 1

(3)

*b‚ ;~, ~öB bªö~ ßWj XRDf TEMj šÏ~ ï&~&.

â 2º >²~ö ¾Ò‚ ªö~ XRD ªCÖ"

‚B Î&ïö &êìš ''~ Þf Al2O3ç"

γ-Ni-Fe .çòb‚ šÒ~– ž >wçš ; W>æ p~rj ¾æÞ. â 3f ~ö‚ Al2O3/ 10 wt% Ni-Fe ªö~ TEM ^–çÒêb‚B Al2O3ªö‚šö £ 20 nm ’V~ Ni-Fe .«¶

& ¢~² ªÖ>Ú ¾žªöj ;W~&rj r > ®. VB γ-Ni-Fe ¾ž.ç~ ç7'ž

;W ¯, >²~ö¾Ò êö .³Özbš B>‚ .

³ Fe 5 Ni‚ ~ö>æ p .çb‚ šÒ~º

©š &V>º: šº Lee12)ö ~š B ÿ

.z (in-situ alloying) *çö ~‚ ©b‚ šCB . ß®, š‚ ÿ.z *çf ¾ž’V‚~ «

¶^zf ªö*~ bê& Ã&Žö V¢ z×

«{~² ¾æ¾º ©b‚ rJ^ ®.13) V¢B, ’öB Òς .³îÖ"j šÏ‚ W»f

¾ž.«¶& ¢~² ªÖB Al2O3 Væ ¾ž

ªö B–ö ®ÚB ‚'~ O»b‚ 6B.

â 4~ (a)f (b)º ~²‚ ªöj 700oC 5 1100oCöB '' 1* 5 30ªÿn >² ~ö

‚ ê, 곚B ²Ö‚Ú~ ª*V¢ jšb‚ æ

~~ 1450oCöB 1* ÿn 30 MPa~ {Kb‚

²Ö‚ Þ~ XRD ªCÖ"š. G;B ' Þ Fig. 1. Thermogravimetry curves for hydrogen reduction

of the calcined powder mixture with 10 wt% Ni-Fe and 15 wt% Ni-Fe in the final composite during heat up to 700oC at a rate of 10oC/min.

Fig. 2. XRD profiles for powder mixtures of (a) Al2O3/10 wt% Ni-Fe and (b) Al2O3/15 wt% Ni-Fe, reduced by hydrogen at 700oC for 1 h ((::) Al2O3, (00) γ-Ni-Fe).

Fig. 3. TEM micrograph of hydrogen-reduced powder mixture.

Fig. 4. XRD profiles of (a) Al2O3/10 wt% Ni-Fe and (b) Al2O3/15 wt% Ni-Fe composites, hot-pressed at 1450oC and 30 MPa for 1 h ((::) Al2O3, (00) γ-Ni-Fe, (55) FeAl2O4).

(4)

~ ç&&êº 98% šç~ ~&z¢ ¾æÚî.

XRD ªCöBº >²~ö‚ ªö~ ãÖf (â 2

^) Ò ²Ö‚ v ÒòöBº Al2O3ç"

Ni-Fe .ç šžö >wçb‚B FeAl2O4~ spinelçš ;W>îrj r > ®. š‚ >wç f .çb‚¦V ªšB Fe ö²¾, 6º .çj

;W~æ p ®î~ ¢¦ º~ Feö²š Al2O3 ç" ²Ö7 ç^ >w~ ;WB ©b‚ šC>Ú ê. ‚Þ, â 4~ XRDÖ"‚¦V r > ®š

Al2O3/15 wt% Ni-Fe²ÖÚ~ ãÖ Al2O3/10 wt%

Ni-Fef jv~ ç&'b‚ ¸f spinelç~

intensity¢ {ž† > ®. š¢ *Úç~ peak intensityö &‚ FeAl2O4ç intensity~ j‚ >~

z~š '' 0.193" 0.088‚B 15 wt% Ni-Fe š Î&B ÒòöB z ôf ·~ FeAl2O4çš ; W>îrj r > ®. š‚ Ö"º ç&'b‚

ôf ·~ Ni-Feš Al2O3Væçö Î&>îV r^

b‚ šC>– ¶^‚ >wV’ö &šBº *Ò

’¢ ê¯ 7š.

â 5~ SEM Òêf 1450oCöB 1* ÿn

&{²Ö‚ Þ~ ^–çb‚B, â (a)º B>

‚ Al2O3, (b)f (c)º '' 10 wt% 5 15 wt%

Ni-Feš Î&B Òò~ 2šš. B>‚

Al2O3²ÖÚ~ «¶f jv~ Al2O3/10 wt% Ni- Fe Òò~ Væç «¶’Vº £ 2~3µm‚Ž –

~ ÿ¢‚ 8j ¾æÚ–, 15 wt% Ni-Fe& Î&B

Òò~ ãÖº £* ^zB «¶’V¢

&. ¢>'b‚ ÒòöBº ªÖçö ~‚ V æç «ê~ OÎ" (pinning effect)14) r^ö çêf jv~ ^‚ «ê¢ ¾æÞ. ¾

’Ö"öB 10 wt% Ni-Fe& Î&B Òò~ V æç ^zº &V>æ pb–, 15 wt% Ni-Fe& Î

&B ãÖöBò Â]‚ ^z& &VB. š‚

*çf ªÖç Î&ö ~‚ «ê OÎ"f Žþ >

wç~ ;Wš Væç «¶WËö 'Ëj "îV r

^b‚ 6>– šö &‚ ’Ú'ž ’& º’B . ‚Þ, Al2O3/Ni-Fe ÒòöB~ ªÖçf ( â 5b 5 c) £ 600 nm ’V‚ Al2O3 «êf â 76ö ¢~² ªÖ>Ú ®Ú š*‚ ^–çj

<º Òò& B–>îrj ¾æÞ.

^–ç" Vê' ßW*~ &ê¢ šC~¶ B

>‚ Al2O3f Òò~ 2ZžW j G;~ ‚

1ö ¾æÚî. ‚öB "º :f ?š Al2O3/ 10 wt% Ni-Fe Òò~ ãÖ B>‚ Al2O3f j v~ Ã&B 2ZžWj ¾æÚ– Al2O3/15 wt%

Ni-Fef 5.26 MPaÁm1/2 ‚B £ 1.7V ¸f 8j

&. ¢>'b‚, ^¢öB~ žWÃ&V’º crack bowing, crack deflection, crack bridging 5 microcrackingb‚ J«† > ®.15) ß®, ductile‚ ªÖçš Î&B Òò ê, .¢ Ú Fig. 5. Fracture surface of the hot-pressed specimens observed in SEM; (a) monolithic Al2O3, (b) Al2O3/10 wt%

Ni-Fe and (c) Al2O3/15 wt% Ni-Fe composite.

(5)

^¢/.³ ÒòöBº crack bridging 5 crack deflection~ V’& 2ZžW Ã&ö V~º © b‚ >î. þ ê~ ãÖ, crack*2¢

&V‚ SEM –çÒê (â 6)öB š‚ *çš

&V> ®. V¢B ªÖç Ni-Fe~ Î&ïö V

¢ Ã&B 2ZžWf crack bridging 5 crack deflection~ V’ö ~‚ ©b‚ šCB. 6‚, Al2O3f .ç*~ 皂 ccê>‚¦V Vž

‚ º~wK 5 .ç ¶Úö ~‚ ;z ê ¢¦

º žWÃ&ö V~º ©b‚ 6B.16) â 7" ‚ 2ö 10 wt% 5 15 wt% Ni-Fe Î

&ïj <º Òòö &šB VSMj ۚ G;‚

¶VšKF" êÖB z¶z 5 ¶K 8j ¾ æÚî. v Òòº *;'ž ferromagnetism~

ßWj "–, G;B z¶z 8" ¶Kf B

>‚ Ni-Fe.ö &‚ Vš~ ’ Ö"f F҂

8j ¾æÞ.17,18) ¾, v Òò¢ jv†

r Al2O3/15 wt% Ni-Fe~ ²ÖÚ& Al2O3/10 wt%

Ni-Fe z Ôf z¶z 5 ¶K 8j

&. V¢B, ;{‚ šCj *šBº >wçž

FeAl2O4 ~ ¶V'ßW" ²ÖB ÒòöB >w çš ¶V' ßWö ~º 'Ë 5 Ni-Fe.«¶

’Vf ¶K*~ &ê19) ~ ’& ê³ >Ú^

¢ † ©š.

4. Ö †

Ni-Fe.š ªÖB Al2O3V ¾žªö B–¢

*‚ ‚'~ W;j B~ 6‚ B> Al2O3

²ÖÚf Ni-Fe .ªÖç~ ·j 10 wt%f 15 wt%‚ –.‚ ²ÖÚ~ Vê' ßW" ¶V' ßW j ï&~ jv~&. .³îÖ"~ ~² 5 >²

~ö ;j Û~ £ 20 nm ’V~ Ni-Fe.çj

W~&, Al2O3 Væç «¶ö ¢~² ªB

¾žªöj B–~&. *&{ ²Ö»b‚

98% šç~ ç&&ê¢ ¾æÚº ²ÖÚ¢ B–~&

. ²ÖÚº Al2O3ç" Ni-Fe .ç šžö >w çž FeAl2O4& ;W>îb–, ªÖçj ôš Î&

‚ ²ÖÚöB z ôf >wçš ¾æÒ. 2ZžW f B>‚ Al2O3f jv~ ÒòöB ªÖçš

ôjî>ƒ Ã&B 8j ¾æÚî, žWÃ&V’º crack bridging 5 crack deflectionb‚ J«~&

. Ã&B 2ZžW" Žþ Î&B Ni-Fe çö Vž

Table 1. Fracture toughness for Al2O3 and Al2O/Ni-Fe composites.

MPaÁm1/2

Monolithic Al2O3 3.32±0.18

Al2O3/10 wt% Ni-Fe 3.87±0.23 Al2O3/15 wt% Ni-Fe 5.26±0.79

Fig. 6. SEM microstructure of Al2O3/15 wt% Ni-Fe com- posite. Crack introduced by indentation.

Fig. 7. Room-temperature magnetization versus applied magnetic-field curve for hot-pressed composites.

Table 2. Magnetic saturation and coercive force for each hot-pressed specimens and pure Fe-Ni.

Saturation Magnetization Coercive Force Al2O3/10 wt% Ni-Fe 138 emu/g of alloy 16.82 Oe Al2O3/15 wt% Ni-Fe 109 emu/g of alloy 6.94 Oe γ-Ni-Fe alloy 140~180 emu/g of alloy 0.1~200 Oe

(6)

~ Òòº *;'ž ;¶W ßWj ¾æÚ

®b–, V¢B þöB Òς ªöW ;f î‚Ú .æ VËW Òò~ B–ö wÏ&˂ O

»b‚ 6B.

6Ò~ &

’º "VF¦~ 2001j “&æ;’Ò ëæöö ~~ >¯>îb– šö 6Òãî.

^^ò

1. K. Niihara: J. Ceram. Soc. Jpn., 99 (1991) 974.

2. T. Sekino and K. Niihara: Nanostr. Mater., 6 (1995) 663.

3. S. -T. Oh, T. Sekino and K. Niihara: J. Eur. Ceram. Soc., 18 (1998) 31.

4. T. Sekino and K. Niihara: J. Mater. Sci., 32 (1997) 3943.

5. T. Sekino, T. Nakajima, S. Ueda and K. Niihara: J. Am.

Ceram. Soc., 80 (1997) 1139.

6. S. -T. Oh, M. Sando and K. Niihara: J. Am. Ceram.

Soc., 81 (1998) 3013.

7. S. -T. Oh, T. Sekino and K. Niihara: Nanostr. Mater., 10

(1998) 327.

8. Y. K. Jeong, A. Nakahira: P. E. D. Morgan and K.

Niihara, J. Am. Ceram. Soc., 80 (1997) 1307.

9.ΧC, Jßç, šÒW, ;'", f;S : ‚“Òò

²æ, 11 (2001) 986.

10. K. Niihara, R. Morena and D. P. H. Hasselman: J.

Mater. Sci. Lett., 1 (1982) 13.

11. S. -T. Oh, S. Namkung and J. S. Lee: J. Mater. Sci. Lett., 21 (2002) 275.

12. J. S. Lee, T. H. Kim, J. H. Yu and S. W. Chung: Nanostr.

Mater., 9 (1997) 153.

13. P. Knorr, B. S. Kim and J. S. Lee: Mat. Res. Symp.

Proc., 577 (1999) 409.

14. C. S. Smith: Trans. Metall. Soc. AIME, 175 (1948) 15.

15. A. G. Evans: J. Am. Ceram. Soc., 73 (1990) 187.

16. B. Budiansky, J. C. Amazigo and A. G. Evans: J. Mech.

Phys. Solids., 36 (1988) 167.

17. B. D. Cullity: Introduction to Magnetic Materials, Addison-Wesley, Massachusetts (1972) 525.

18. X. Y. Qin, J. G. Kim and J. S. Lee: Nanostr. Mater., 11 (1999) 259.

19. X. Y. Qin, J. S. Lee and J. G. Kim: J. Appl. Phys., 86 (1999) 2146.

참조

관련 문서

Division of Gastroenterology, Department of Internal Medicine, Hanyang University College of Medicine, 22-2 Wangsimni-ro, Seongdong-gu, Seoul 133-791, Korea Tel: +82-2-2290-8379, Fax:

Synthesis and Luminescent Properties of YAs, Nb, P, VO4:Eu3+ Red Phosphors by Combinatorial Chemistry Method Il Woon Zeon*, Kee-Sun Sohn†, Hee Dong Park, and Seung Kon Ryu‡

Department of Animal Resources Sci- ence, Dankook University, Cheonan 330-714, Korea, 1 Abson BioChemica Lab, Ansan 425-220, Korea, 2 EASY BIO System, Inc, Cheonan 330-811, Korea

Mary’s Hospital, Seoul 150-822, Korea; 11 Department of Radiology, Dong-A University Medical Center, Busan 602-715, Korea; 12 Department of Radiology, Hanyang University

Center for Spintronics Research, Korea Institute Science and Technology, Seoul 136-791, Korea Department of Materials Science and Engineering, Korea University, Seoul