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1 Jurnal f the Krean Ceramic Sciety Vl., N. 1, pp. 53~57, Effect f MgB Additin n Synthesis f Hexagnal Brn Nitride Dae-Jin Lee*, **, Mi-Jung Jee*, Byung-Hyun Chi*, Mi-Jai Lee*, Nam-Hee Ch**, and Mi-Sun Cha*** *Electrnic Materials Labratry, Krea Institute f Ceramic Engineering & Technlgy, Seul , Krea **Schl f Materials Science and Engineering, Inha University, Inchn , Krea ***Large Industry, Daegu , Krea (Received Octber 28, 2008; Accepted December 5, 2008) Hexagnal Brn Nitride w MgB ƒ z *, **Á *Á x* Á *Á û **Á *** *» q ** w w œw *** ( ; ) ABSTRACT The h-bn pwder was synthesized by amrphus B 2 O 3 and activated carbn at 1550 C in nitrgen atmsphere, whse prperties were examined accrding t MgB additin. Amunt f MgB additin was varied in the range f 0 ~10 wt% f the initial mixture. It was bserved that MgB additin led t an increase in the amunt and the grain size f h-bn and decrease in the amunt f B C frming. When MgB added 5 wt%, the amunt and crystallinity f h-bn increased as the hlding time at the synthesis temperature was prlnged. It was als cnfirmed that the regularity f three-dimensinal rdering f h-bn increases. Key wrds : Hexagnal brn nitride, Rhmbhedral brn nitride, MgB, B C, Grain size 1. White graphite Hexagnal brn nitride( w h-bn) graphite q x š. w w, x p» w h-bn y wš, e w j,,» w p y t,, y w y š. w v p yww q jš, ƒ j p w j. 1) Hasan Erdem Çamurlu šw h-bn w, B 2 O 3, C, N w carbthermic B 2 O 3 (l) +3C(s)+N 2 (g) f w BN w š šw ù N 2 gas w gas y Bƒ C w B Cƒ ùkù» h-bn x wš, w x B C h-bn y j k š šw. 2-) Crrespnding authr : Byung-Hyun Chi Tel : Fax : B C h-bn w ƒ Ca yw, Li yw šw. Ca Li h-bn w 2,5) w B C x wš N 2 CO w h-bn ƒ jù Ca j» ƒ š 1µm w w w. 2) w Li ƒ brn nitride w 1300 C 1100 C¾ û š, hexagnal ³e w ù h-bn j» 1µm w. 5) 1µm w j» h-bn y j w. j» ƒ 5~10µm j y t, q c-bn w j» j»ƒ j h-bn w w v ƒ. Mgƒ y p w h-bn j» g MgB ƒw h-bn w e w w. amrphus B 2 O 3 activated C y w w MgB ƒ, MgB ƒw w h-bn, j» y w w w. 53

2 5 Á Á xá Á û Á Fig. 1. Methd f analysis fr determinatin f the quantities f the cnstituent f the reactin prducts. 2. x h-bn w w amrphus B 2 O 3 activated carbn 1: 3 wš, MgB ƒ ƒ 0, 5, 10 wt% ƒw z yww. yw k ƒ š N 2»w 1550 C 1~10 w w. w z w š š y wš Fig. 1 œ HCl:H 2 O 1:1( v ) yww 90 C 1 leaching ww z filtering w. w filtering B Cù C w» w air» 700 C 1 zy w. B C B 2 O 3 y û wš leaching ww. w BN sƒ XRD (D/max 2200V/PC, Rigaku, Japan), XRF (ZSX primus, Rigaku, Japan), j» x SEM (JSM-380, JEOL, Japan) w. 3. š Fig. 2 carbthermic w w w X- z ww z pattern ùkü. ƒƒ w MgB ƒ ƒ B C peakƒ w ùkû ù, MgB 5wt% 10 wt% ƒw B C peak ùkù ù MgB 10 wt% ƒw Mgyw peakƒ. yw yww Brn w» sx k h-bn w B C w brn w Fig. 2. X-ray diffractin patterns f the prducts (a) after synthesis fr 10 h at 1550 C and (b) after leaching. w wz

3 Hexagnal Brn Nitride의 합성에 있어서 MgB 첨가의 효과 55 B C의 합성을 제한하게 된다. 합성 시 촉매제로 사용된 Mg는 산화환원 반응을 통해 고열을 발생하며 Mg 주변에 micrmetric drplet을 형성하여 brn의 melting을 빠르게 이끌어냄으로써 용융된 brn이 쉽게 가스화하여 N gas 와의 반응을 촉진하므로 h-bn 형성에 Mg가 촉매로 작용 하여 B C의 생성을 제어하게 됨을 확인하였다. 불순물 제거의 효과를 확인하기 위하여 XRF를 통하여 Mg의 함량을 조사하였다. 그 결과 Fig. 1의 W1과 W의 결정성분의 강도가 5.7에서 0.09로 크게 감소하였다. 불 순물의 제거를 위해 Fig. 1과 같이 진행한 후 XRD pattern(fig. 2(b))을 확인하였을 때, 시료 BN-0에서 나타났 던 B C는 거의 제거되었고, MgB 를 10 wt% 참가한 경우 Mg화합물이 다량 남아 있었다. 반면 MgB 를 5 wt% 첨가 한 경우 h-bn peak만이 나타났다. Mg의 적당량 첨가는 B C의 형성을 제어해주는 효과가 있으나 과량을 첨가하 게 되면 제 2상이 다시 생성되어 h-bn을 얻기가 어려워 진다. 따라서 촉매제로서 MgB 의 첨가량은 5 wt%일 때 가 적당하였다. MgB 의 첨가에 따른 입자 성장의 효과를 보기 위해 미 세구조를 측정하여 Fig. 3에 나타내었다. Carbthermic법으 로 합성 시 출발물질만으로는 h-bn의 입자크기가 1~2 µm 이상 성장시키는 것이 어렵다는 연구결과가 있었으나, 미세구조로 보아 MgB 를 첨가하지 않은 경우에 비하여 MgB 가 5 wt%, 10 wt%를 첨가한 경우의 입자가 크게 성 장한 것을 확인할 수 있었다. 이는 Mg의 화학적 특성이 2 ) 2) 크게 작용하는 것으로 촉매제 외에 발화제의 역할도 하 며 연소에 의해 Mg가 발생시키는 고열이 주변 반응물을 급속하게 가열시킴으로써 동일한 실험조건하에 MgB 를 첨가하지 않은 시료에 비하여 MgB 의 5 wt%, 10 wt%의 첨가가 고열에 의한 B의 가스화를 촉진시켜 h-bn의 입 자를 성장시키는데 작용하였기 때문이다. BN의 입자크기 는 온도가 높아질수록 B의 가스화 비율이 증가되어 성장 하는 경향을 보이며 Mg의 발화에 의한 고열이 입자 성 장을 촉진한다. Fig. 는 MgB 5 wt%를 첨가한 시료를 1550 C에서 1시 간부터 10시간까지 합성유지시간을 달리하여 합성을 행 한 후 BN 생성량과 불순물 생성량을 산출하여 나타낸 것 이다. 5 wt%의 MgB 가 첨가된 시료를 합성유지시간을 변 화하였을 때 유지시간이 길어짐에 따라 h-bn의 생성량이 증가하는 것을 확인하였으나 시간 이상의 합성은 생성 량에 큰 변화가 없었다. 또한 각각 시료 5 wt%의 MgB 가 첨가된 시료를 1시간, 2시간 3시간 동안 합성을 진행 한 각각의 시료는 반응에 참여하지 못한 C와 B O 의 양 이 많았으며 시료 시간, 10시간 합성한 시료와 비교하여 B C의 양이 다량인 것을 확인할 수 있었다. MgB 를 5 wt% 첨가한 후 10시간 합성한 경우 첨가제를 첨가하지 않은 경우보다 h-bn의 생성량이 20% 정도 증가하였고 Fig. 3. SEM images f the h-bn frmed frm (a) 0, (b) 5, and (c) 10 wt% MgB added mixture at 1550C fr 10 h. 3), 2 3 Fig.. Chang in the amunt f h-bn, B2O3, BC and C in the prducts f the experiments cnducted at 1550C fr 1, 2, 3, and 10 h. 제 권 제 1호(2009)

4 5 Á Á xá Á û Á B C w. B C sx k system h-bn wì w ù d w N 2» w h-bn w y w. ) B C k œ h-bn y» w w BN w w w w w v w. MgB 5wt% ƒw z w w z w X- z wwš Fig. 5 ùkü. h-bn ƒw 2Θ=2 (10) z ql (100), (101) peak, 2Θ=50 w (102) peak ƒ ùkû. 1 w (10) peakƒ 2 rhmbhedral peak 1.5 hexagnal peak š 50 (102) peak x. w rhmbhedral peak w 3 ¾ w ù z ùk ù. w 3 ³e w (102) peak w 2 z l ùkùš ¼ sharpw š ƒw. ABC stack w r-bn ƒ w» w ùkù ƒ w ¼ brn nitrideƒ AB stack w h-bn yw. w x»w w y h-bn ww» w w r-bn x w» h-bn w w w œ w. wr w ¼ Mg yw B C peak y w h- BN w w w r-bn peak û š peak j ƒ w. Fig. 1 œ w w X- z ww Fig. 5(a) w ùkû Mg 2 B 2 O 5 B C peakƒ Fig. 5(b) x ùkù. Fig. 1 œ BN prduct û. Fig. 5 (a) (b)ƒ 5 r-bn peak ƒ w y w BN xk». h-bn 3 ³e üš G.I(Graphitizatin Index) d w Fig. ùkü. ƒw G.I w 3 z l 10 ¾ 3 w û w w ùkþ. Hexagnal ³e m y G.I t w, G.I Area[ ( 100) + ( 101) ] G.I = Area( 102) Fig. 5. X-ray diffractin patterns f the prducts (a) after synthesis at 1550 C fr 1, 2, 3, and 10 h and (b) after leaching that. Fig.. Graphitizatin Index f h-bn synthesized with hlding time. w wz

5 Hexagnal Brn Nitride w MgB ƒ z 57. (101) (102) peak ³e w w hexagnal G.I 1. j ƒ ƒ ùkü. 7) 1 G.I 8. y w w ù küš 10 w w G.I 2.2 w ƒ š 3 ³ e ƒ hexagnal.. h-bn w w» w amrphus B 2 O 3 C MgB ƒw z carbthermic 1500 C 1~10 w w. (1) MgB 5wt% ƒw B C š h-bn j» j ƒ g. 5 wt% MgB ƒw Mg yw. (2) Carbthermic w w HCl H 2 O yw leachingw, w w B 2 O 3 C, w w 2 B C Mgyw g. (3) 5 wt% MgB ƒw 1550 C w 3 w rhmbhedral hexagnal ƒ y BN š, w w hexagnal BN w B C Cƒ. w ¼ 3 ³e ƒw. REFERENCES 1. Kempfer, L., The Many Faces f Brn Nitride, Mater. Eng., 107, 1- (1990). 2. Hasan Erdem Çamurlu, Naci Sevinç, and Yavuz Tpkaya, Effect f Calcium Carbnate Additin n Carbthermic Frmatin f Hexagnal Brn Nitride, J. Eur. Ceram. Sc., 28 [3] (2008). 3. Ayd gdu, A. and Sevinc, N., Carbthermic Frmatin f Brn Nitride, J. Eur. Ceram. Sc., (2003).. Jn, S. J. and Jha, A. A., Vapur-Phase Reductin and the Synthesis f Brn-Based Ceramic Phases, J. Mat. Sci., (1995). 5. T.S. Bartniskaya, A.V. Kurdyumv, V.I. Lyashenk, N.F. Ostrvskaya, and I.G. Rgvaya, Catalytic Synthesis f Graphite-like Brn Nitride, Pwder Metallurgy and Metal Ceramics, 35 [5-] (199).. Hwang, Chyi-Ching and Chung, Shyan-Lung, Cmbustin Synthesis f Brn Nitride Pwder, J. Mater. Res., 13 [3] 80-8 (1998). 7. H. Lrenz and I. Orgzall, Influence f the Initial Crystallinity n the High Pressure-High Temperature Phase Transitin in Brn Nitride, Acta Mater., (200). «1y(2009)

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