Aluminum Trihydride‐diethyl etherate ( Etherated Alane )

Abstract

Methods for the preparation of aluminum trihydride-diethyl etherate, AlH, -0.3 [ (C, H5 )2 01 ,$ have been published,'S2 but the absence of complete experimental details makes duplication difficult. The following procedure is a modification of that reported by Finholt, Bond, and Schlesinger.' Problems inherent in previous methods, such as premature precipitation, decomposition of the alane, and lithium chloride contamination, are avoided.Premature precipitation is controlled by maintaining a low temperature (-5'C.) in the reaction mixture. Purified reactants, as well as minimal exposure to light and higher temperatures, *The Dow Chemical Company, Midland, Mich. 48640. This work was supported by +Ohio State University, Columbus, Ohio 43210. SEbdiometric molecular weight determinations obtained in diethyl ether (concentration range, 0.25-1.0 M ) indicates molecular weights only slightly higher than 30. This is consistent with studies reported by Wiberg and U~o n .~ It must be assumed that in solution, AM, exists essentially as the monomeric form.ARPA and the Air Force under contracts AF 33(616)-6149 and AF 04(611)-7554.

Spectroscopic and structural investigations of α‐, β‐, and γ‐AlH3 phases

“…[3] Furthermore, it has been predicted that replacing aluminum with aluminum hydride (alane) will result in a 10% gain in specific impulse for about 20 s over currently used aluminum propellants. [2,3] Such an increase in optimum performance is possible because of this metal hydride fuel's low-ignition temperature of 1450 K and low-combustion temperature of 3391 K. Indeed, alane has a higher initial burning rate as compared with that of pure aluminum, which ignites at around the alumina melting point and combusts at 3716 K. [2] On the other hand, use of aluminum hydride presents several disadvantages: (1) the colorless solid material reacts violently with water and atmospheric moisture, [4] (2) it has low chemical and thermal stability, and (3) it is sensitive to friction. [2] The decomposition of alane as well as its reactivity with air [5] generates excessive amounts of hydrogen gas during storage.…”

A printed aluminum cathode with low sintering temperature for organic light-emitting diodes

“…We found the ink based on isopropyl ether (O(C 3 H 7 ) 2 ) to be particularly effective in achieving compact Al lms at relatively low temperature, and this ether is safer in use than the more familiar diethyl ether (O(C 2 H 5 ) 2 ), which is highly ammable even at À5 C, as mentioned by Schmidt et al 16 In addition, Al lms prepared using AlH 3 [O(C 4 H 9 ) 2 ] can be successfully formed at 110-150 C. 14,15 On the other hand, this temperature is still too high for some exible substrates and organic active layers, as mentioned above, and we therefore adopted the highly volatile but easily manipulated solvent O(C 3 H 7 ) 2 for printing the Al cathode, giving a sintering temperature of 80 C.…”

“…The Al precursor ink was typically prepared by reaction of aluminum chloride (AlCl 3 ) with lithium aluminum hydride (LiAlH 4 ) in an anhydrous ether such as diethyl ether (O(C 2 H 5 ) 2 ), 16 isopropyl ether (O(C 3 H 7 ) 2 ), or butyl ether (O(C 4 H 9 ) 2 ), 14,15 as shown in eqn (1). [14][15][16][17][18]…”

A Universally Applicable Methodology for the Gram-Scale Synthesis of Primary, Secondary, and Tertiary Phosphines

“…A solution of AlH 3 was prepared in situ by dropwise addition of a solution of LiAlH 4 to a solution of AlCl 3 (3:1 LiAlH 4 /AlCl 3 ) in glyme (ca. 0.2 M AlH 3 ) . The mixture was stirred for 30 min at room temperature.…”