METAL NANOparticleS HAVE MUCH ATTENTION IN THE FIELDS OF PHYSICS, CHEMISTRY, ELECTRONICS AND BIOLOGY BECAUSE OF THEIR UNIQUE ELECTRICAL CHEMICAL, OPTICAL, AND PHOTO-ELECTROCHEMICAL PROPERTIES, WHICH ARE STRONGLY DEPENDENT ON THE size AND SHAPES OF METAL NANOparticleS [1,2].IT IS KNOWN THAT THE MAGNETIZATION BEHAVIOR OF A MAGNETIC MATERIAL IS HIGHLY size DEPENDENT. DESPITE THE ENDLESS NUMBER OF REPORTS ON MAGNETIC STUDIES OF MAGNETIC NANOparticleS THE INFLUENCE OF particle size ON THE MAGNETIC PROPERTIES HAS NOT BEEN SYSTEMATICALLY STUDIED [3]. THE METALLIC NICKEL NANOparticleS SHOW MAGNETIC PARAMETERS SUCH AS SATURATION MAGNETIZATION AND COERCIVITY THAT VARY WITH particle size, USUALLY IN A NON-LINEAR FASHION [4]. IT IS ENVISAGED THAT THE APPLICATION OF NI NANOparticleS CAN BE EXPANDED ONCE THE INTRIGUE RELATIONSHIP BETWEEN MAGNETIC PROPERTIES AND particle size OF NI CAN BE DELINEATED. THE LARGE MAGNETIC particle CONTAINS MOBILE WALLS WHEN THE size OF THE particle DECREASES BELOW A CRITICAL size, THE DOMAIN WALLS DISAPPEARS AND THE particleS BECOME SINGLE DOMAIN. MAGNETIC particleS IN THE NANOMETER-size RANGE ARE NECESSARILY SINGLE-MAGNETIC-DOMAIN STRUCTURES. THE CRITICAL size DEPENDS ON THE SATURATED MAGNETIZATION, ANISOTROPY ENERGY AND EXCHANGE INTERACTION BETWEEN INDIVIDUAL SPIN [5]. IT IS ESTIMATED THAT THE CRITICAL size BELOW WHICH A SPHERICAL particle EXISTS AS A SINGLE-MAGNETIC DOMAIN IN THIS PROCEDURE, NICKEL NANOparticleS WERE PREPARED FROM NICKEL AZIDE COMPLEXES IN SOLID STATE BY INTRAMOLECULAR OXIDATION AND REDUCTION REACTION IN PRESENCE OF APPROPRIATE BASES. THE COERCIVITY OF METALLIC NICKEL SAMPLES ARE FOUND TO BE 162.46, 146.22 AND 154.34 OE FOR NI1-NI3 RESPECTIVELY. THUS ESTIMATED SINGLE DOMAINS ARE 17.27, 16.08 AND 18.08 FOR NI1-NI3 RESPECTIVELY. THE COERCIVITY OF FERROMAGNETIC NANOparticleS IS DEPENDENT ON particle size. AS THE particle size INCREASES THE COERCIVITY INCREASES INITIALLY AND THEN DECREASES AFTER SOME CRITICAL particle size. THIS MEANS THAT COERCIVITY OF NICKEL particle HAS A PEAK AROUND THIS CRITICAL size WHERE THE particleS UNDERGO TRANSITION FROM SINGLE-DOMAIN TO THE MULTIDOMAIN NATURE. THEN particle size IS CALCULATED BY USING OF SATURATION MAGNETIZATION. WHEREAS MAGNETIZATION OF METALLIC NICKEL SAMPLES ARE FOUNDED 41.97, 40.40 AND 47.43 EMU/G FOR NI1-NI3 RESPECTIVELY. ALL NICKEL NANOparticleS HAVE particle size DISTRIBUTION RANGING FROM 15.32, 16.53 AND12.00 NM. THE NICKEL NANOparticleS WERE CHARACTERIZED USING XRD, SEM, VSM ANALYSES.