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1 47 5 Vol.47, No RARE METAL MATERIALS AND ENGINEERING My B 1,3 1,4,3 ( ) ( ) ( ) ( ) B 14B B X (XRD) (TEM) X (EDS) (DSC) (VSM) 14B B 3O 4 B B 8 B O 3 B O 3 O 3 α- CH B O 3 51 B 678 O 3 O 3 α- H 895 B H α- 14B 14B TQ586.1 A 1-185X(18) B [1-3] B ( ) [3] B 786 ka/m 557 ka/m B B [4,5] 14 B [6,7] 3 µm Une [8] B 1 µm - [9-16] Swminthn [9] - CH - B Hik [17] B Zhng [18] BN 3 nm ka/m Dong [19] - - CO 1 µm 14 B 14 B 14 B 14 B (514113, ) , E-mil: youjunhu168@163.com

1644 47 B 14 B 1 (cc) 3 ( 99.9 %) (cc) 3 ( 99%) (C H 5 ) 3 NBH 3 ( 97%) ( 8% ~ 9%) ( 98%) ( 99.

B B 14 B Ar+5 %H 5 /min 8 1 min CH Ar+5 %H 5 /min 95 1 min CO C 14 B JEOL JEM-1 (TEM) X (EDS) Netzch DSC 44F3

54 nm 3 O 4 (311) (STEM) B TEM EDS c EDS 3 O 4 B B EDS B 3 XRD 3 O 4 B XRD B B 3 O 4 B.

2 B 14 B 1 (cc) 3 ( 99.9 %) (cc) 3 ( 99%) (C H 5 ) 3 NBH 3 ( 97%) ( 8% ~ 9%) ( 98%) ( 99.7%) CH ( 95%) B : Ar 3 mmol (cc) 3 6 mmol (cc) 3 3 ml 1 9 min 1 mmol (C H 5 ) 3 NBH min V /V =3/1 1 min 3 14 B B 14 B Ar+5 %H 5 /min 8 1 min CH Ar+5 %H 5 /min 95 1 min CO C 14 B JEOL JEM-1 (TEM) X (EDS) Netzch DSC 44F3 (DSC) SmrtL X (XRD) EZ9 (VSM) 14 B PDF 3 O 4 3 O 4 (311) (511) (44) 1 (HRTEM) nm 3 O 4 (311) (STEM) B TEM EDS c EDS 3 O 4 B B EDS B 3 XRD 3 O 4 B XRD B B 3 O 4 B. B B ~ min XRD 4 ~ 4 3 O 4 5 O 6 O (511) (311) (44) 3O4 prticle B element lignd 5 nm d=.99 nm d=.54 nm (311).1 B TEM B 1 TEM B 1 Fig.1 1 nm 1 B TEM HRTEM TEM () nd HRTEM () imges of B intermedite

5 14B 1645 c 5 nm Intensity/cps 1 8 6 4 B O Element t% O 79.56 19.51.9 4 6 8 1 Energy/keV 1 8 6 4 B O Element t% O 8.61 4.6 15.3 4 6 8 1 Energy/keV c Fig.

3 5 14B 1645 c 5 nm Intensity/cps B O Element t% O Energy/keV B O Element t% O Energy/keV c Fig. B TEM EDS TEM imge () nd EDS nlysis of zone () nd zone c (c) in Fig.1 for B intermedite.3 14 B Intensity/.u. (311) (4) (4) (511) (4) (533) DSC ( 5 ) min XRD XRD O 3 Fig.4 Intensity/.u θ/( ) 3 B XRD Fig.3 XRD pttern of B intermedite 3O4, O O3 BO3 α- O3 * BO θ/( ) 4 XRD XRD ptterns of the first-step reduction nneling process O 3 7 O 3 BO 3 α- 8 O 3 α- BO 3 O 3 B O 3 3 O 4 B O 3 B O 3 O 3 α- 8 C 7 C 6 C 5 C 4 C 3 C C O 3 α- 678 α- H CO 895 α- H 14 B DSC XRD 51 B O 3 CH B B B ( B 18 [] ) B XRD B O 3 O 3 CH. Het Flow/mW mg o C 895 o C o C Temperture/ o C 5 DSC Fig.5 DSC curve of second-step reduction nneling process

1646 47 Fig.6 Intensity/.u. O3 O3 α- H CO B 95 C 895 C 678 C 51 C 3 4 5 6 7 8 θ/( ) 6 XRD XRD ptterns of the second-step reduction nneling process d=.54 nm (31) 1 nm d=.

965-4.45-311.968 kj/mol 678 G 75.813-44.731-443.343-383.

4 Fig.6 Intensity/.u. O3 O3 α- H CO B 95 C 895 C 678 C 51 C θ/( ) 6 XRD XRD ptterns of the second-step reduction nneling process d=.54 nm (31) 1 nm d=.3 nm (1) N d O 3 + 3CH N d + 3CO + 3H (1) O 3 + 3CH H + 3CO + H () O3 + 3CH H + + 3CO + H (3) O 3 + 3CH + + 3CO + 3H (4) O 3 O 3 CH α- H CO HSC Chemistry (1) ~ (4) G (1) ~ (4) 51 G kj/mol 678 G kj/mol (1) XRD (4) () (3) G () (3) 678 Swminthn [9] CH O 3 O 3 H α- CO 895 B H α- 14 B 51 B O 3 + 3CH B + 3CO + 3H (5) 678 O 3 + 3CH H + 3CO + H () O3 + 3CH H + + 3CO + H (3) 895 H B 14B + H (6) 7 14 B TEM 7 14 B HRTEM.54.3 nm 14 B (31) (1) 8 C CO Fig.7 Fig.8 kg -1 Moment/Mss/A m 7 14B TEM HRTEM TEM nd () HRTEM () imges of 14B mgnetic powder Applied Field/ 79.6 A m B Mgnetic hysteresis loops of 14B mgnetic powder VSM ka/m nm

5 5 14B B (1) B 3 O 4 B () 8 O 3 B O 3 O 3 α- (3) 14 B 3 B O 3 51 B 678 O 3 O 3 α- H 895 B H α- 14 B References [1] Lio Hengcheng( ), M Liqun( ), Yun Hoyng( ). Rre Metl Mterils nd Engineering( )[J], 1999, 8(): 65 [] Coey J M D. Journl of Mgnetism nd Mgnetic Mterils[J], 1, 6(1): 17 [3] Tkehis M. Resource Geology[J], 8, 58(4): 414 [4] Song Xioping( ), Wng Xiotin( ). Rre Metl Mterils nd Engineering( )[J], 1994, 3(3): 1 [5] Yue Ming( ), Liu Xuo( ), Xio Yofu( ) et l. Rre Metl Mterils nd Engineering( )[J], 3, 3(7): 49 [6] Hung Zhohu( ), Li Qing( ), Zhng Shiyn( ) et l. Rre Metl Mterils nd Engineering( )[J], 9, 38(): 47 [7] Yu Linqing( ), Yn Mi( ). Rre Metl Mterils nd Engineering( )[J], 8, 37(9): 1681 [8] Une Y, Sgw M. Jpn Inst Metls[J], 1, 76(1): 1 [9] Swminthn V, Deheri P K, Bhme S D et l. Chemistry of Mterils [J], 1, (4): 659 [1] Deheri P K, Shukl S, Rmnujn R V. Journl of Solid Stte Chemistry[J], 1, 186(): 4 [11] Bhme S D, Swminthn V, Deheri P K et l. Advnced Science Letters[J], 1, 3(): 174 [1] Rhimi H, Ghsemi A, Mozffrini R. Journl of Super conduct-ivity nd Novel Mgnetism[J], 16, 9(8): 41 [13] Rhimi H, Ghsemi A, Mozffrini R et l. Journl of Mgnetism nd Mgnetic Mterils[J], 17, 444(15): 111 [14] Jdhv A P, Hussin A, Lee J H et l. New Journl of Chemistry[J], 1, 36(11): 45 [15] Hussin A, Jdhv A P, Bek Y K et l. Journl of Nnoscience nd Nnotechnology[J], 13, 13(11): 7717 [16] M H X, Kim C W, Kim D S et l. Nnoscle[J], 15, 7(17): 816 [17] Hik Y, Chtterjee J, Chen C J. Journl of Nnoprticle Reserch[J], 5, 7(6): 675 [18] Zhng Q, Jing Z, Yn B. Inorgnic Chemistry Frontiers[J], 14, 1(5): 384 [19] Dong X L, Kim B K, Choi C J et l. Journl of Mterils Reserch[J], 1, 16(4): 183 [] Boulnger J L, Autissier D. Journl de Physique IV[J], 1993, 3(C7): 135 Preprtion nd Rection Process of 14 B Mgnetic Powder Synthesized y Chemicl Method You Junhu 1, Zho Dong,3, Guo Yozu 1, Wu Chun,4, Pei Wenli,3 (1. Shenyng University of Technology, Shenyng 1187, Chin) (. Northestern University, Shenyng 11819, Chin) (3. Key Lortory for Anisotropy nd Texture of Mterils, Ministry of Eduction, Shenyng 11819, Chin) (4. Key Lortory of Ministry of Eduction for Electromgnetic Processing of Mterils, Shenyng 11819, Chin) Astrct: B intermedites were prepred y chemicl method nd then B mgnetic powder with min phse of 14B ws otined y two-step reduction nneling. Phse, microstructure, phse trnsformtion t different tempertures nd mgnetic properties of the smples were nlyzed y XRD, TEM, DSC, VSM nd so on. The formtion mechnism of 14B mgnetic powder ws discussed. The results show tht the nno-sized B intermedites with good dispersion, which re composed of sphericl 3O 4 prticle nd flocculent orgnic lignds of nd B elements, cn e synthesized y the chemicl method. In order to otin B mgnetic powder, the intermedite should e sujected to two-step reduction nneling. In the first-step reduction nneling process t 8 C, the B intermedites re converted into O 3, B O 3, O 3 nd α- phses. The second-step nneling is performed with the id of CH, nd the rection process is s follows: firstly, B O 3 is reduced into B phse t 51 C, then O 3 nd O 3 re reduced into H nd α- phses t 678 C, nd finlly, B, H nd α- re lloyed to form 14B mgnetic powder t 895 C. Key words: chemicl method; lignd; reduction nneling; 14B; mgnetic powder Corresponding uthor: Pei Wenli, Ph. D., Associte Professor, Key Lortory for Anisotropy nd Texture of Mterils, Ministry of Eduction, Northestern University, Shenyng 11819, P. R. Chin, E-mil: peiwl@tm.neu.edu.cn

Microsoft Word - 101944.doc

Microsoft Word - 101944.doc 2010 年第 30 卷有机化学 Vol. 30, 2010 第 12 期, 1944~1948 Chinese Journl of Orgnic Chemistry No. 12, 1944~1948 研究简报 Lewis 酸催化下苯乙酮型苯并吡喃的合成齐小燕伍林 *,,b 王建国易德莲刘敏彭功名 ( 武汉科技大学