This work presents a study of the structural properties of thin films of the compound Cu2ZnSnSe4 varying both mass (MX) and the substrate temperature which was evaporated (Ts) ZnSe binary compound. All samples were deposited by co-evaporation method in three phases keeping all other parameters constant. From measurements of X-ray diffraction it was possible to establish Ts increasing the presence of associated binary phase’s quaternary compound during the 1 Licenciado en Matematicas y Fisica Universidad de la Amazonia; Especialista en Ciencias Fisicas Universidad Nacional de Colombia; Mg. en Ciencias Fisicas Universidad Nacional de Colombia y PhD. en Fisica Universidad Nacional de Rosario, Argentina. Docente Universidad Nacional de Colombia, Grupo de Materiales Nanoestructurados, Departamento de Fisica Universidad Nacional de Colombia, sede Bogota, Colombia. 2 Fisica Univesidad Nacional de Colombia; estudiante de Maestria Universidad Nacional de Colombia; Grupo de Materiales Nanoestructurados, Departamento de Fisica Universidad Nacional de Colombia, sede Bogota, Colombia. 3 Fisico Universidad de Cordoba; estudiante de Maestria en la Universidad Nacional de Colombia; Grupo de Materiales Nanoestructurados, Departamento de Fisica Universidad Nacional de Colombia, sede Bogota, Colombia. Revista EIA, ISSN 1794-1237 / Ano XI / Volumen 11 / Edicion especial N.1 / Mayo 2014 / pp. E25-E29 Publicacion semestral de caracter tecnico-cientifico / Escuela de Ingenieria de Antioquia —EIA—, Envigado (Colombia) Autor de correspondencia Quiroz-Gaitan, H.P.: Calle 5 N° 1C-39 int. 6, Chia Cundinamarca. Codigo Postal: 250001 Telefono: (57 1) 862 00 62. Correo electronico: hpquirozg@unal.edu.co e26 IdentIfIcacIon de una nueva fase en la estructura crIstalIna del compuesto cuaternarIo cu2Znsnse4 Revista EIA Rev.EIA.Esc.Ing.Antioq / Publicacion semestral Escuela de Ingenieria de Antioquia —EIA— growth process of the material. It was found that around the main peak, 2Θ = 27,1°, predominantly binary phases and the presence of ZnSe which is formed during the subsequent step of selenization of the material. A sort of fork in the main peak (2Θ = 27,1°) was observed for the transition between MZnSe = 0,153 g to 0,171 g. X-Ray diffraction measurements were made at binary compound pure, observing a correspondence with the peaks found around the main peak of the compound. A study by Raman spectroscopy, Raman shifts associated evidenced binary compounds observed by XRD. From the Scherrer equation it was found that crystallite sizes range between 80 and 90 nm.