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  Preparation of high nitrogen compound and materials therefromUSPTO Application #: 20060211565Title: Preparation of high nitrogen compound and materials therefrom Abstract: was prepared. Pyrolysis of the compound yields carbon nitrides C2N3 and C3N5. The carbon nitrides vary in their density, texture, and morphology. The high-nitrogen compound of the formula (end of abstract) Agent: Los Alamos National Security, LLC - Los Alamos, NM, US Inventors: My Hang V. Huynh, Michael A. Hiskey USPTO Applicaton #: 20060211565 - Class: 501099000 (USPTO) Related Patent Categories: Compositions: Ceramic, Ceramic Compositions, Refractory, Elemental Carbon Containing The Patent Description & Claims data below is from USPTO Patent Application 20060211565. Brief Patent Description - Full Patent Description - Patent Application Claims
FIELD OF THE INVENTION [0002] The present invention relates generally to high-nitrogen compounds and more particularly to the preparation of the high-nitrogen compound 4,4',6,6'-tetra(azido)azo-1,3,5-triazine (TAAT), and carbon nitrides from the high-nitrogen compound. BACKGROUND OF THE INVENTION [0003] Carbon nitrides have interesting mechanical, optical, and tribological properties. These super-hard diamond-like materials have low densities, are extremely wear resistant, and are generally chemically inert. Carbon nitrides are used in biocompatible coatings for medical implants, battery electrodes, gas separation systems, corrosive protection, humidity and gas sensors, and other applications. The applications for carbon nitrides generally depend on particle size and texture and on the relative nitrogen content of the carbon nitride. [0004] An extensive effort has been focused on the synthesis of precursors and the development of methods to control the size, regulate the texture, and increase the nitrogen content in carbon nitrides. [0005] There have been recent reports describing the use of energetic "high-nitrogen" compounds for preparing carbon nitrides. High-nitrogen compounds are a relatively new class of energetic compounds whose energy is largely derived from their very high positive heats of formation that result from the large number of energetic N--N and C--N bonds in these compounds. SCHEME 1 shows the formulas of three high-nitrogen compounds (DAAT: 3,3'-azobis(6-amino-1,2,4,5-tetrazine); BTATz: 3,6-bis-(1H-1,2,3,4-tetrazol-5-ylamino)-1,2,4,5-tetrazine; and TAG-AT: triaminoguanidinium 5,5'-azobis(1H-tetrazolate)) and their associated heats of formation. [0006] High-nitrogen compounds that contain polyazido groups possess even higher heats of formation. In general, however, compounds with polyazido groups are extremely sensitive to spark, friction, and impact (H.sub.50) and generally exhibit poor thermal stability. Therefore, applications for these types of compounds tend to be limited. Gillan, however, has reported the preparation of carbon nitrides C.sub.3N.sub.4 and C.sub.3N.sub.5 from 2,4,6-tri(azido)-1,3,5-triazine [1]. The formulas of 2,4,6-tri(azido)-1,3,5-triazine and another high-nitrogen compound having polyazido groups are shown in SCHEME 2 below, along with some data related to their melting points, decomposition temperatures, heats of formation, and sensitivities to spark, friction, and impact. [0007] Other reported preparations of carbon nitrides using other types of precursors generally involve applied pressure, high temperature and/or shock compression, and the products obtained are often nitrogen poor materials that are occasionally contaminated with hydrogen-containing by-products [2-8]. [0008] High-nitrogen compounds with better thermal stability and less sensitivity to spark, friction, and/or impact than known precursors would be better precursor materials for carbon nitrides. [0009] There remains a need for better precursor materials for carbon nitrides. [0010] Accordingly, an object of the present invention is to provide better high-nitrogen compound precursor materials for preparing carbon nitrides. [0011] Another object of the present invention is to provide a method for preparing carbon nitrides from high-nitrogen compounds. [0012] Additional objects, advantages and novel features of the invention will be set forth in part in the description which follows, and in part will become apparent to those skilled in the art upon examination of the following or may be learned by practice of the invention. The objects and advantages of the invention may be realized and attained by means of the instrumentalities and combinations particularly pointed out in the appended claims. SUMMARY OF THE INVENTION [0013] In accordance with the purposes of the present invention, as embodied and broadly described herein, the present invention includes a chemical compound of the formula wherein Z is selected from --N.sub.3 and --NHNH.sub.2; and wherein -Q-Q- is selected from --NH--NH-- and --N.dbd.N--. [0014] The invention also includes a method for preparing carbon nitrides that involves heating a compound of the formula to a temperature sufficiently high to melt but not substantially decompose the compound, and then heating the melted compound to a temperature sufficiently high to decompose the compound and form carbon nitrides. BRIEF DESCRIPTION OF THE DRAWINGS [0015] The accompanying drawings, which are incorporated in and form a part of the specification, illustrate the embodiment(s) of the present invention and, together with the description, serve to explain the principles of the invention. In the drawings: [0016] FIG. 1 shows a scanning electron microscope (SEM) image of the carbon nitride C.sub.2N.sub.3 prepared according to the invention. [0017] FIG. 2 shows an SEM image of a low-density C.sub.3N.sub.5 carbon nitride prepared according to the invention; and [0018] FIG. 3 shows an SEM image of C.sub.3N.sub.5 carbon nitride having a nanodendritic morphology and prepared according to the invention. DETAILED DESCRIPTION [0019] This invention is concerned with the preparation high-nitrogen compounds and with the preparation of carbon nitrides from high-nitrogen compounds. The invention is particularly concerned with the preparation of the high nitrogen compound 4,4',6,6'-tetra(azido)hydrazo-1,3,5-triazine and the conversion of this compound to 4,4',6,6'-tetra(azido)azo-1,3,5-triazine (TAAT), and also with the conversion of TAAT to carbon nitrides. [0020] An exemplary sequence of chemical reactions used for synthesizing TAAT is shown in SCHEME 3 below. Briefly, 4,4',6,6'-tetra(chloro)hydrazo-1,3,5-triazine (1) [9] reacts rapidly with an excess of hydrazine monohydrate in acetonitrile to give 4,4',6,6'-tetra(hydrazino)-hydrazo-1,3,5-triazine (2). Compound (2) undergoes diazotization to yield 4,4',6,6'-5 tetra(azido)hydrazo-1,3,5-triazine (3). A suspension of (3) in 1:2 (v/v) H.sub.2O:CHCl.sub.3 solution reacts with chlorine gas at room temperature to provide 4,4',6,6'-tetra(azido)azo-1,3,5-triazine (4, TAAT). Continue reading... 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