One can observe that the sample 0F as prepared (Red curve, Fig.1.

) presented majority
phase of YF3, with relatively broad peaks possibly related to the presence of small size
particles due the low temperature about 120 in the synthesis process, where the
growth process of the single-crystals it was not efficient. The secondary phase present in
this sample (Rhombus filled in green.) could not be identified, but can be that this
corresponding to layers of NH4Y2F7 connected to YF3 through the NH4+ cations forming
a weak N-H-F bond. Nevertheless, it has been successfully removed after heating
treatment at 400 C [1] (Blue curve, Fig.1.), such that for this sample single crystalline
phase of YF3 was obtained. No change in the structure was noticed due to the presence
of dopants.
The XRD and EDX measurements show that as the amount of fluorine increases, layers
of NH4Y2F7 connect to YF3 through the NH4+ cations forming a weak N-H-F bond. As
can be seen Figure 5, we tuned the crystal phase by varying the Y3+/NHF4 ratio, this
tuning is very abrupt varying from 0 to 30% in excess of fluorine, , nevertheless, from
30 to 60 % the structure keeps itself stable. The increase in nitrogen with increasing
amount of NH4F reported in table.1 confirms the formation of layers of NH4Y2F7 with
increasing amount of NH4F in the synthesis of the crystals.
Furthemore, an analysis of the samples with heating treatment varying from 0 to 60%
in excess of the ammonium fluoride precursor ( NH4F) made in this moment Fig.6, the
samples with heating treatment show no appreciable differences in crystalline structure,
all them crystalize to orthorhombic YF3 structure. This can be explained by the
decomposition
of reaction:
The heating treatment
in 400 is used to break N-H-F bond (i.e., to destroy the
NH4Y2F7 2YF3 + NH3(g) + HF(g)
in the treatment temperature.
The heating treatment in 400 is used to break N-H-F bond (i.e., to destroy the
layer structure by liberating NH3 gas), thereby the structure of NH4Y2F7 would
collapse due to decomposition of interweaving layers of NH4+ cations
in the treatment temperature.
The heating treatment in 4000 is used to break N-H-F bond (i.e., to destroy the
layer structure by liberating NH3 gas), thereby the structure of NH4Y2F7 would collapse
due to decomposition of interweaving layers of NH4+ cations in the treatment
temperature.
The figures 1 and 2 show that the samples as prepared
According to Rajeshwar and Secco [2]the NH4 Y2F7 structure may be visualized as
layers of YF6 octahedra (built up by mutual sharing of cornerand edges) with interlaying
layers of NH4+ cations, therefore, we can explain the secondary phase present in the
sample (Rhombus filled in green. Fig. 1.) and formed structure not identified (Fig. 2.)
as the process of formation of layers NH4 Y2F7 not finished.
one change of structure is seen when increasing the quantity of the ammonium fluoride
precursor although this change is very abrupt varying from 0 to 30% in excess of
fluorine, nevertheless, from 30 to 60 % the structure keeps itself stable.

The measures FTIR ( red curve of the fig. 8 to 10, and 11) show the peak located at
1427 cm-1 which correspond to the NH4+ cation of NH4 Y2F7, however, after heating
treatment this peak disappear. Also, to compare the nitrogen quantities between the
tables. 1. and 2., we can see one reduction with the heating treatment. This results
confirm the decompostion of NH4 Y2F7 structure to orthorhombic YF3 structure.
Besides the broad band in the region of 3000-3600 cm-1 is due to water O-H stretching
vibrations, and it suffers a strong reduction with the heating treatment.
As the amount of excess of fluorine used increased, the luminescence emissions
becomes smaller (Figure.7). In all cases, transition lines are attributed to levels of Nd3+.
The results suggest that with increasing the excess of fluorine favours the
formation of structure of NH4 Y2F7 where the formation is finished at 30% ,
nevertheless, from 30 to 60 % the structure keeps itself stable. After heating treatment in
all samples, the structure NH4 Y2F7 decomposes itself to orthorhombic YF3 structure.

[1] P. Ghosh, A. Patra, "Tuning of crystal phase and luminescence

properties of Eu3+ doped sodium yttrium fluoride nanocrystals", Journal of
Physical Chemistry C, 112 (2008) 3223-3231.
[2]