Precursor structural influences on the final ZnO nanoparticle morphology from a novel family of structurally characterized zinc alkoxy alkyl precursors

被引:91
作者
Boyle, TJ [1 ]
Bunge, SD [1 ]
Andrews, NL [1 ]
Matzen, LE [1 ]
Sieg, K [1 ]
Rodriguez, MA [1 ]
Headley, TJ [1 ]
机构
[1] Sandia Natl Labs, Adv Mat Lab, Albuquerque, NM 87106 USA
关键词
D O I
10.1021/cm0493997
中图分类号
O64 [物理化学(理论化学)、化学物理学];
学科分类号
070304 ; 081704 ;
摘要
We have synthesized a variety of structurally diverse "Zn(OR)(Et)(solv)" and "Zn(OR)(2)(solv)(2)" where Et = CH2CH3 and solv = no bound solvent, pyridine (py), tetrahydrofuran (THF), or 1-methyl imidazole (Melm). The ligand OR represents the following: neo-pentoxide (ONep = OCH2CMe3) tert-butoxide (OBut = OCMe3), cycloalkane-substituted methoxide [(OCH2C(CH2)(n), n = 2, OCH2Prc; n = 3, OCH2Buc], cyclopentoxide [OCH(CH2)(4) = OPe(c)], tetrahydrofurfurylalkoxide [OCH2CH(CH2)(3)O] = OTHF], and several aryloxides [OAr = 2,6-dimethyl phenoxide (DMP), 2,6-di-isopropyl phenoxide (DIP), and 2,6-di-tert-butyl phenoxide (DBP)]. These compounds were characterized by single-crystal X-ray diffraction as [Zn(OR)(Et)(py)](2) [OR = ONep (1), OBut (2)], [Zn(mu(3)-OPe(c))(Et)](4) (3), Zn[Zn-3(mu(3)-OCH2Prc)(4)(Et)(3)](2) (4), [Zn(mu(3)-OCH2Buc)(Et)](4) (5), [Zn(mu(3)-OPe(c))(Et)](4) (6), Zn(OAr)(Et)(solv)(2) where OAr = DMP: solv = py (7), DIP: solv = py (8), MeIm (8a); DBP: solv = py (9) and [Zn(DBP)(mu-Et)](2) (9a), Zn(OAr)(2)(solv)(2) where OAr = DMP: solv = py (10), MeIm (10a), py/MeIm (10b), DIP: solv = py (11), Melm (11a), DBP: solv = py (12), Melm (12a), [Zn(mu(3)-OTHF)(Et)](4) (13). The solution state behavior of these compounds was explored by multinuclear NMR spectroscopy. In an effort to determine the effect of nuclearity on the final nanoparticle morphology and size, four representative nuclearities mono- (8), di- (1), tetra- (13), and hepta- (4) nuclear were chosen and used to generate nanoparticles of ZnO. The mononuclear compound formed polydispersed spherical nanoparticles of wurtzite, whereas the nanoparticles generated from the other samples were nanorods. A relationship between the precursors central core and the final morphological properties of the nanorods was proffered to explain the variations noted.
引用
收藏
页码:3279 / 3288
页数:10
相关论文
共 38 条
[1]  
BOLM C, 1992, CHEM BER, V125, P1
[2]   Structural diversity in solvated lithium aryloxides.: Syntheses, characterization, and structures of [Li(OAr)(THF)x]n and [Li(OAr)(py)x]2 complexes where OAr=OC6H5, OC6H4(2-Me), OC6H3(2,6-(Me))2, OC6H4(2-Pri), OC6H3(2,6-(Pri))2, OC6H4(2-But), OC6H3(2,6-(But))2 [J].
Boyle, TJ ;
Pedrotty, DM ;
Alam, TM ;
Vick, SC ;
Rodriguez, MA .
INORGANIC CHEMISTRY, 2000, 39 (22) :5133-5146
[3]   A novel family of structurally characterized lithium cobalt double aryloxides and the nanoparticles and thin films generated therefrom [J].
Boyle, TJ ;
Rodriguez, MA ;
Ingersoll, D ;
Headley, TJ ;
Bunge, SD ;
Pedrotty, DM ;
De'Angeli, SM ;
Vick, SC ;
Fan, HY .
CHEMISTRY OF MATERIALS, 2003, 15 (20) :3903-3912
[4]   Structural variations of potassium aryloxides [J].
Boyle, TJ ;
Andrews, NL ;
Rodriguez, MA ;
Campana, C ;
Yiu, T .
INORGANIC CHEMISTRY, 2003, 42 (17) :5357-5366
[5]   From clusters to ionic complexes: Structurally characterized thallium titanium double alkoxides [J].
Boyle, TJ ;
Zechmann, CA ;
Alam, TM ;
Rodriguez, MA ;
Hijar, CA ;
Scott, BL .
INORGANIC CHEMISTRY, 2002, 41 (04) :946-957
[6]   Hetero-alkoxide group (IV) and (V) neo-pentoxide compounds.: Syntheses, characterizations, and X-ray structures of [Zr(μ-OCHMe2)(OCH2CMe3)3(HOCH2CMe3)]2 and [Ta(μ-OCH2Me)(OCH2CMe3)4]2 [J].
Boyle, TJ ;
Gallegos, JJ ;
Pedrotty, DM ;
Mechenbier, ER ;
Scott, BL .
JOURNAL OF COORDINATION CHEMISTRY, 1999, 47 (01) :155-171
[7]   Structural diversity of lithium neopentoxide compounds [J].
Boyle, TJ ;
Alam, TM ;
Peters, KP ;
Rodriguez, MA .
INORGANIC CHEMISTRY, 2001, 40 (24) :6281-6286
[8]   Titanium(IV) neopentoxides. X-ray structures of Ti-3(mu(3)-Cl)(mu-OCH2CMe3)(3)(OCH2CMe3)(6) and [Ti(mu-OCH2CMe3)(OCH2CMe3)(3)](2) [J].
Boyle, TJ ;
Alam, TM ;
Mechenbier, ER ;
Scott, BL ;
Ziller, JW .
INORGANIC CHEMISTRY, 1997, 36 (15) :3293-3300
[9]   Niobium(V) alkoxides.: Synthesis, structure, and characterization of [Nb(μ-OCH2CH3)(OCH2C(CH3)3)4]2, {[H3CC(CH2O)(CH2-μ-O)(C(O)2)]Nb2(μ-O)(OCH2CH3)5}2, and {[H3CC(CH2O)2(CH2-μ-O)]Nb(OCH2CH3)2}2 for production of mixed metal oxide thin films [J].
Boyle, TJ ;
Alam, TM ;
Dimos, D ;
Moore, GJ ;
Buchheit, CD ;
Al-Shareef, HN ;
Mechenbier, ER ;
Bear, BR ;
Ziller, JW .
CHEMISTRY OF MATERIALS, 1997, 9 (12) :3187-3198
[10]   Bismuth(III) coordination compounds.: Synthesis, characterization, and X-ray structures of [Bi(Cl)(μ-Cl)2(THF)2]∞, Bi(O2CMe)3(Solv)x (Solv = py, x = 2 or MeIm, x = 4) [1], and [Bi(μ-O CH2CMe3)(OCH2CMe3)2(Solv)]2 (Solv = HOCH2CMe3 or py) [J].
Boyle, TJ ;
Pedrotty, DM ;
Scott, B ;
Ziller, JW .
POLYHEDRON, 1998, 17 (11-12) :1959-1974