Thermal stabilities of diethylaluminum azide were studied by means of theoretical analysis and expriments.The results have shown that diethylaluminum and azid be heated to vigorous refluxing under vacuum(400 Pa) at te...Thermal stabilities of diethylaluminum azide were studied by means of theoretical analysis and expriments.The results have shown that diethylaluminum and azid be heated to vigorous refluxing under vacuum(400 Pa) at temperature as high as 420℃ without incident of explosion and decomposes smoothly during 460 ～580℃ to form nanometric particles of aluminum nitride in the aerosol synthesis reactor. A new way of preparing nanometric parties of aluminum nitrideis found.展开更多
Diethylaluminum azide (DEAA) is an important compound in organoaluminum andes. But the synthesis and property of DEAA were reported a little. The DEAA is a liquid compound in literature that was synthesed by the react...Diethylaluminum azide (DEAA) is an important compound in organoaluminum andes. But the synthesis and property of DEAA were reported a little. The DEAA is a liquid compound in literature that was synthesed by the reaction of diethyl aluminum chloride (DEAC) and sodium azide. The solid product as a colorless crystal was first obtained by the reaction of DEAC and sodium azide in our work. The solid product was characterized as DEAA by IR spectrum and H NMR spectrum. The yield of crystal DEAA was increased as NaN3/DEAC (mol/mol) increased. When NaN3/DEAC = 1. 3 the yield of DEAA is increased from 74% in literature to 83%. The melting point of DEAA is 28 - 29℃ that was determined with two methods in the work. The DEAA containing trace DEAC (about 0. 2% of DEAC) is liquid which has been full proved by varied tests in this paper. The melting point of DEAA is - 130℃ in literature because the DEAA is not pure that may contain DEAC. The - 130℃ may be eutectic point of eutectic mixture forming of DEAA and DEAC. 27,Al NMR of DEAA is determined. At δ = 6. 4 there is a peak that 1/2 of the peak is 834Hz. The structure of crystal DEAA is inferred from 27Al NMR.展开更多
文摘Thermal stabilities of diethylaluminum azide were studied by means of theoretical analysis and expriments.The results have shown that diethylaluminum and azid be heated to vigorous refluxing under vacuum(400 Pa) at temperature as high as 420℃ without incident of explosion and decomposes smoothly during 460 ～580℃ to form nanometric particles of aluminum nitride in the aerosol synthesis reactor. A new way of preparing nanometric parties of aluminum nitrideis found.
文摘Diethylaluminum azide (DEAA) is an important compound in organoaluminum andes. But the synthesis and property of DEAA were reported a little. The DEAA is a liquid compound in literature that was synthesed by the reaction of diethyl aluminum chloride (DEAC) and sodium azide. The solid product as a colorless crystal was first obtained by the reaction of DEAC and sodium azide in our work. The solid product was characterized as DEAA by IR spectrum and H NMR spectrum. The yield of crystal DEAA was increased as NaN3/DEAC (mol/mol) increased. When NaN3/DEAC = 1. 3 the yield of DEAA is increased from 74% in literature to 83%. The melting point of DEAA is 28 - 29℃ that was determined with two methods in the work. The DEAA containing trace DEAC (about 0. 2% of DEAC) is liquid which has been full proved by varied tests in this paper. The melting point of DEAA is - 130℃ in literature because the DEAA is not pure that may contain DEAC. The - 130℃ may be eutectic point of eutectic mixture forming of DEAA and DEAC. 27,Al NMR of DEAA is determined. At δ = 6. 4 there is a peak that 1/2 of the peak is 834Hz. The structure of crystal DEAA is inferred from 27Al NMR.
