Herein the photoluminescence spectra of nanosized cubic Y 2 O 3 :Tb 3+ having Tb 3+ concentrations varying between 0.1 and 10 Mol% are described. Low temperature cathodoluminescence spectra from these materials recorded in a scanning transmission electron microscope are presented and discussed. By studying the photoluminescence-spectra recorded at room temperature and focused on the 5 D 4 → 7 F 5 (C 2 ) and 5 D 4 → 7 F 5 (C 3i ) transitions, at 542.8 and 544.4 nm respectively, it was found that the critical distance for energy transfer from Tb 3+ ions at C 3i lattice sites to Tb 3+ ions at C 2 lattice sites was 1.7 nm; at distances >1.7 nm, which prevail at low Tb 3+ concentration, this energy transfer virtually stops. The gradual change of the excitation spectra upon increasing the Tb 3+ concentration is also explained in terms of energy transfer from Tb 3+ at C 3i sites to Tb 3+ at C 2 sites. Cathodoluminescence spectra recorded at low temperatures with the scanning transmission electron microscope provided additional evidence for this radiationless energy transfer. Recently we published a study on the cathodoluminescence (CL) of nanosized cubic Y 2 O 3 :Tb 3+ particles; 1 reference to this work will be made as Part 1. We identified a few peaks in the CL spectra that are related to Tb 3+ at C 3i sites in cubic Y 2 O 3 (the structure is that of the mineral bixbyite). In Part 1, we have indicated the C 3i sites by S 6 . The vast majority of the spectral lines in the CL spectra of Y 2 O 3 :Tb 3+ arise from C 2 type transitions. We also found evidence that the two strongest emission lines in the 5 D 4 → 7 F 5 transition cluster at 542.8 nm and 544.4 nm are split when recorded at low temperature. These spectral data provided insight into the energy flow from Tb 3+ ions at C 3i lattice sites to Tb 3+ ions at C 2 lattice sites: the critical distance between a Tb 3+ (C 3i ) donor ion and Tb 3+ (C 2 ) acceptor ion was found to be 1.7 nm, which is about 5 times larger than the shortest distance between a cation at a C 3i site and a cation at a C 2 site.1,2 It is the objective of the work described herein to gain more insight into the studies reported in Part 1 by measuring the photoluminescence (PL) spectra at room temperature and the CL spectra in a scanning transmission electron microscope (STEM) at low temperatures.Many authors have reported on the PL spectrum of Y 2 O 3 :Tb 3+ ; here we shall mention only the most relevant publications on the spectroscopic characteristics of Y 2 O 3 :Tb 3+ . An important result in Part 1 was the doublet structure of the 542 nm and 544 nm lines, which became noticeable at a temperature of 103 K. A similar result was reported by Song and Wang, 3 who also found 4 lines between 541 and 545 nm at 83 K. At 274 K these lines coalesced into two peaks, in which the 542 nm peak still showed a shoulder. Najafov et al. 4 showed the doublet structure of the 542 nm and 544 nm lines in the PL spectra of Y 2 O 3 :Tb 3+ with various Tb 3+ concentrations at room temperature. In the spectrum presented...