Laser Emission from a Europium Benzoylacetonate Alcohol Solution1
Laser Emission from a Europium Benzoylacetonate Alcohol Solution1
复制标题
苯甲酰丙酮铕醇溶液的激光发射1
DOI：
10.1021/j100788a037
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发表时间：
1964
期刊：
影响因子：
--
通讯作者：
M. Weinberg
中科院分区：
文献类型：
--
作者：
M. L. Bhaumik;P. Fletcher;L. Nugent;S. M. Lee;S. Higa;C. Telk;M. Weinberg
6130 A受激发射的观测Lempicki和Samelson 2以及Schimit-schek报道了从苯甲酰丙酮铕的醇溶液中分离的方法。[3]前一位作者将铕螯合物命名为三配体化合物Eu（B）s，但没有给出制备方法或熔点;后一位作者没有给出化学组成和熔点，但指出该化合物是通过Whan和克罗斯比的哌啶法制备的。4 5然而，Whan和克罗斯比没有报道使用哌啶法制备苯甲酰丙酮铕;他们报道了制备稀土二苯甲酰甲基化物的方法，并给出了另一种在水溶液中制备稀土苯甲酰丙酮化物的方法。这意味着所报道的苯甲酰丙酮铕的激光发射是从一种基本上未被表征的螯合物中获得的。本文报道了苯甲酰丙酮铕的制备、熔点、溶质的化学组成和某些能产生激光发射的发射线的波长。苯甲酰丙酮铕激光材料的特性的重要性变得明显时，样品的熔点，水化度，配位数，化学组成，和发射波长的广泛变化，取决于制备方法和纯化技术。例如，从溶液中重结晶得到熔点在90 - 180之间变化的产物，这取决于溶剂、所取馏分、溶液温度和沉淀前溶液静置的时间。更重要的是，激光发射只从一种特殊的苯甲酰乙酸铕产物中观察到，这种产物是通过修改Whan和克罗斯比的哌啶方法得到的。4苯甲酰丙酮铕的制备和表征通过Whan和Crosby 4以及Sacconi和Ercoli 6描述的水溶液法制备苯甲酰丙酮铕得到二水合物。该材料在各种低温和浓度的乙醇溶液中反复测试时没有显示出激光振荡的证据。在同一篇论文中，Whan和克罗斯比描述了另一种制备稀土三苯甲酰甲基化物的非水方法，我们称之为哌啶法。在哌啶法中，产物在125 - 150 ℃下真空干燥，以除去第四摩尔螯合剂。但将此方法用于苯甲酰丙酮铕的合成时，产物的熔点发生了变化
Observation of stimulated emission of 6130 A. from an alcohol solution of europium benzoylacetonate was reported by Lempicki and Samelson2 and by Schimit-schek. 3 The former authors designate the europium chelate as the three-ligand compound Eu (B) s but give no method of preparation or melting point; the latter author gives no indication of thechemical composition and no melting point but states that the compound was prepared by the piperidine method of Whan and Crosby. 4 5However, Whan and Crosby did not report the use of the piperidine method for the preparation of europium benzoylacetonate; they report this method for the preparation of the rare earth dibenzoylmethides and give another method, in aqueous solution, for the preparation of the rare earth benzoylacetonates. This means that the reported europium benzoylacetonate laser emission has been obtained from a chelate which is essentially uncharacterized. The purpose of this paper is to report the preparation, the melting point, the chemical composition of the solute, and the wave lengths of some of the emission lines for the europium benzoylacetonate which yields laser emission. The importance of the characterization of the euro-pium benzoylacetonate laser material became apparent when samples of widely varying melting point, degree of hydration, coordination number, chemical composi-tion, and emission wave lengths were obtained, depend-ing upon the method of preparation and the technique of purification employed. For example, recrystalliza-tion from solution gave products varying in melting point from 90 to 180, depending upon the solvent, the fraction taken, the solution temperature, and the time the solution stands before precipitation. Of more consequence is the fact that laser emission has been observed only from a particular europium benzoylace-tonate product obtained by a modification of Whan and Crosby’s piperidine method. 4Preparation and Characterization Preparation of europium benzoylacetonate by the aqueous method described by Whan and Crosby4 and by Sacconi and Ercoli6 gives the dihydrate. This material showed no evidence for laser oscillation when repeatedly tested under various conditions of low temperature and concentration in alcohol solution. In the same paper Whan and Crosby describe another nonaqueous method, which we call the piperidine method, for the preparation of rare earth trisdibenzoyl-methides. In the piperidine method the product is vacuum-dried at 125 to 150 in orderto remove a fourth mole of chelating agent. However, when this method was applied in the synthesis of europium ben-zoylacetonate, the products were of varying melting