La 2 O 2 CN 2 :Er 3+ and La 2 O 2 CN 2 :Er 3+ /Yb 3+ upconversion (UC) luminescence nanofibers were successfully fabricated via cyanamidation of the respective relevant La 2 O 3 :Er 3+ and La 2 O 3 :Er 3+ / Yb 3+ nanofibers which were obtained by calcining the electrospun composite nanofibers. The morphologies, structures, and properties of the nanofibers are investigated. The mean diameters of La 2 O 2 CN 2 :Er 3+ and La 2 O 2 CN 2 :Er 3+ /Yb 3+ nanofibers are 179.46 AE 12.58 nm and 198.85 AE 17.07 nm, respectively. It is found that intense green and weak red emissions around 524, 542, and 658 nm corresponding to the 2 H 11/2 ? 4 I 15/2 , 4 S 3/2 ? 4 I 15/2 , and 4 F 9/2 ? 4 I l5/2 energy levels transitions of Er 3+ ions are observed for La 2 O 2 CN 2 :Er 3+ and La 2 O 2 CN 2 :Er 3+ /Yb 3+ nanofibers under the excitation of a 980-nm diode laser. Moreover, the emitting colors of La 2 O 2 CN 2 :Er 3+ and La 2 O 2 CN 2 :Er 3+ /Yb 3+ nanofibers are all located in the green region. The upconversion luminescent mechanism and formation mechanism of the nanofibers are also proposed.(2) Fabrication of La 2 O 2 CN 2 :Er 3+ nanofibers La 2 O 2 CN 2 :x%Er 3+ [x = 1, 3, 5, and 7, x stands for molar percentage of Er 3+ to (Er 3+ +La 3+ )] nanofibers were prepared by calcinating the electrospun PVP/[La(NO 3 ) 3 +Er (NO 3 ) 3 ] composites followed by cyanamidation. In the typical procedure of preparing representative La 2 O 2 CN 2 :5%Er 3+ nanofibers, 0.9513 g of La 2 O 3 and 0.0581 g of Er 2 O 3 were dissolved in dilute HNO 3 (1:1, volume ratio) at elevated J. Ballato-contributing editor Manuscript No. 35368.