V o l. 26 N o. 4 2 0 0 5 4 CH EM ICAL JOU RNAL O F CH IN ESE UN IV ERS IT IES 623 627 1, 2, 1, 2, 1, 1 1, 1, 1, 2 (1., 116023; 2., 100039),, 10 20 nm, 20 40 nm 40 60 nm,,,.,,.,, ; Χ Α, Χ.. ; ; ; ; O 641 A 025120790 (2005) 0420623205,,., [1, 2 ]., [3 ]., (, ), [4, 5 ]., [3 ] [6 ],,., [7 ] [8 ] [9 ]. [10 ] 20 80,,,.,,, [11 ].. [12 17 ], :. 2 (, ),,,,. 1 1. 1 ( ) ; (, ) ; (, ). R igaku D gm A X2ΒB X (Cu K Α, ) ; A SA P 2010 (M icrom eritics) ; JEM 22000EX ( JEOL ) ; PH (ph S225 : 2004204223. : ( : 20325620) ( : 20303017). : (1963 ),,,,. E2m ail: taozhang@dicp. ac. cn
6 24 V o l. 26, E22012C ). 1. 2 1. 2. 1 (1) (homo) : 012 mo lgl, 1 12,, 90. 6 8 h, ph,,.,,, 120 12 h, 350 4 h,. (2) (N H 3) : 012 mo lgl, 112 mo lgl. ph,,.,, 120 12 h, 350 4 h,. (3) A (so l2gel2a) : 110 mo lgl, 1 2, 90,, 120 12 h,. 550 2 h,,. (4) B (so l2gel2b) : [ 15 ], 110 mo lgl g [V ( ) gv ( ) = 7g10 ],. g, 1 215.,,,. 200 12 h,, 350 4 h,. 1. 2. 2, 20 40,,, 8 000 h - 1. 30 m in 300, 1 gm in 500, 2 h,., O 2gN 2 [V (O 2) gv (N 2) = 1% ], 300 h - 1, 10 h,. 2 2. 1 1 XRD., 4. B ( so l2gel2 b) Χ2, Α2, 3 Α2. 1, XRD, A (so l2gel2a),. 550,. 1 4, (so l2gel2a) 1717 m 2 g, 3 F ig. 1 XRD pattern s for iron ox ides a. (homo), b. (N H 3), c. (so l2gel2a), d. (so l2gel2b).
N o. 4 : 625 60 90 m 2 g. Samp le Table 1 Spec if ic surface areas(bet) of nano- iron ox ide and iron n itr ide (homo) (N H 3) ( so l2gel2a) ( so l2gel2b) (homo) (N H 3) ( so l2gel2a) ( so l2gel2b) Specific surface area (m 2 g) 9015 7211 1717 6112 1813 819 1015 215 2, 2, 10 100 nm.,, 40 60 nm [ 2 (A ) ],., 10 20 nm, [ 2 (B ) ],., 20 40 nm [ 2 (C), (D ) ]. (so l2gel2a) (so l2gel2b),,, Α Χ. 2. 2 F ig. 2 TEM images of nano- iron ox ide (A ) (homo) ; (B) (N H 3) ; (C) (so l2gel2a) ; (D ) (so l2gel2b). [18 ],, 350.,,, 450., 500, 3 X, Φ2. 1., 2 20 m 2 g,,,., F ig. 3 XRD pattern s for iron n itr ide a. (homo) ; b. (N H 3) ; c. (so l2gel2a) ; d. ( so l2gel2b). (homo) 1813 m 2 g, 3, (homo). ( 4), (homo), 3 100 nm, (so l2gel2b)..,
6 26 V o l. 26, (N H 3). (N H 3) 10 20 nm, 100 nm, 5 10., (homo) 40 60 nm,,,, 40 80 nm,. F ig. 4 TEM images of iron n itr ide (A ) (homo) ; (B) (N H 3) ; (C) (so l2gel2a) ; (D ) (so l2gel2b). (so l2gel2b), (so l2gel2a), 20 40 nm,,. Χ. Χ2, Α2,..,, (so l2gel2b) ;,. [ 1 ] Kappaganthu S. R., Sun Y.. Surf. Coaṫ T echno l. [J ], 2003, 167 (2 3) : 165_ 169 [ 2 ] Tong W. P., T ao N. R., W ang Z. B. et a l.. Science[J ], 2003, 299: 686_ 688 [ 3 ] Garg V. K., O liveira A. C., A zevedo R. B. et a l.. J. M agn. M agn. M ater. [J ], 2004, 272_ 276 (3) : 2326_ 2327 [ 4 ] A nderson R. B.. Catal. Rev. Sci. Eng. [J ], 1980, 21 (1) : 53_ 71 [ 5 ] Eastrup B.. J. Catal. [J ], 1994, 150: 345_ 355 [ 6 ] Zhuge L. J., Yao W. G., W u X. M.. J. M agn. M agn. M ater. [J ], 2003, 257 (1) : 95_ 99 [ 7 ] L i D., Cho i C. J., Kim B. K. et a l.. J. M agn. M agn. M ater. [J ], 2004, 277 (1_ 2) : 64_ 70 [ 8 ] Gup ta M., Gup ta A., Bhattacharya P. et a l.. J. A lloys Compd., 2001, 326 (1_ 2) : 265_ 269 [ 9 ] Q ian X. F., Zhang X. M., W ang C. et a l.. M ater. Res. Bull. [J ], 1999, 34 (3) : 433_ 436 [ 10 ] V o lpe L., Boudart M.. J. So lid State Chem. [J ], 1985, 59: 332_ 347 [ 11 ] L I J ing2guo ( ), GAO L ian ( ), ZHAN G Q ing2hong ( ) et al.. J. Ino rg. M ater. ( ) [J ], 2003, 18 (4) : 765_ 771 [ 12 ] N IU X in2shu ( ), XU Hong ( ), TAN G J ia2q iang ( ). Function M ater. ( ) [J ], 2001, 32 (6) : 649-650 [ 13 ] L IN Yan2Hong ( ), WAN G D e2jun ( ), ZHAO Q i2dong ( ) et al.. Chem. J. Ch inese U niversities( ) [J ], 2003, 24 (11) : 2077_ 2079 [ 14 ] ZHAN G L i2d e ( ), M OU J i2m ei( ). Science of N anom eter M aterial( ) [M ], Shenyang: L iaoning Science and Techno logy P ress, 1994: 76_ 88 [ 15 ] Dong W. T., W u S. X., Chen D. P. et a l.. Chem. L etṫ [J ], 2000: 496_ 497 [ 16 ] CU I Zheng2Gang ( ), Y IN Fu2Shan ( ). T echno logy and A pp lication of M icrom ulsions ( ) [M ], Beijing: L ight Industry P ress, 1999: 407-417 [ 17 ] YAN G Q ing2l in ( ), ZHA IJ in ( ), SON G Yan2L in ( ) et al.. Chem. J. Ch inese U niversities(
N o. 4 : 627 ) [J ], 2003, 24 (12) : 2290_ 2292 [ 18 ] ZH EN G M ing2yuan ( ), CH EN X iao2w ei( ), CH EN G Rui2H ua ( ) et al.. Petrochem. T echno l. ( ) [J ], 2004, 33: 1205_ 1207 Preparation of Nano- iron N itr ide by Tem perature-programm ed Reaction from Nano- iron Ox ides ZH EN G M ing2yuan 1, 2, CH EN G R u i2h ua 1, 2, CH EN X iao2w ei 1, L IN ing 1, CON G Yu 1, W AN G X iao2dong 1 1, 23, ZHAN G T ao (1. D alian Institu te of Chem ical P hy sics, Ch inese A cad em y of S ciences, D alian 116023, Ch ina; 2. G rad uate S chool of Ch inese A cad em y of S ciences, B eij ing 100039, Ch ina) Abstract A series of nano2iron ox ides w ith differen t particle sizes o r bu lk phases w ere firstly p repared from cheap ino rgan ic iron salts by p recip itation o r so l2gel m ethods. T hen, the nano2iron n itride samp les w ere p repared from the as2syn thesized nano2iron ox ides by temperatu re2p rogramm ed reaction (T PR ) m ethod under ammon ia atmo sphere. T he characterization s of X2ray diffraction and tran sm ission electron m icro scope demon strate that nano2iron n itride can be p roduced from the nano2 iron ox ides by T PR m ethod. T here a re app a ren t d ifferences in the p a rt icle sizes of iron n it ride p repared from differen t p recu rso rṡ W ith in som e range of sizes, sm aller iron ox ide p recu rso r leads to larger iron n itride particles. Fo r the Χphase and Αphase iron ox ides w ith sim ilar particle sizes, the fo rm er is mo re likely to agglom erate du ring the n itridation. T he iron n itride particles retain the mo rpho logy of the ox ide p recu rso rṡ Keywords P recip itation m ethod; So l2gel m ethod; T emperatu re2p rogramm ed reaction m ethod; N ano2 iron ox ide; N ano2iron n itride (Ed. : M, G) 3 ( ) 1 16 31 46 2 17 32 47 3 18 33 48 4 19 34 49 5 20 35 50 6 21 36 51 7 22 37 52 8 23 38 53 9 24 39 54 10 25 40 55 11 26 41 56 12 27 42 57 13 28 43 ( ) 58 14 29 44 59 15 ( ) 30 45 60 3, 2005 2 22.
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