Briefly, FeCl36H2O (0.

125 mol L1) were dissolved in ethylene glycol (80

mL),followed by the addition of NaAc (1.1 mol L1) and polyethylene glycol
4000 (25 mg mL1) into the system. The mixture was stirred vigorously for 60
min and then transferred into a Teflon-lined stainless-steel autoclave (100 mL).The
autoclave was heated at 200 oC for 12 h and cooled at room temperature to form
the black products. The products were washed several times with deionized water
and ethanol and then dried at 60 oC for 12 h in vacuum
FeCl3_6H2O (3 mmol), succinic acid (1 mmol) and urea (30 mmol) were
completely dissolved in ethylene glycol (30 mL) or 1,2-propylene glycol (30 mL)
by vigorous mechanical stirring. The solution was sealed in a Teflon lined
stainlesssteel autoclave (50 mL capacity) and then heated at 200 1C for several
hours to fortnight. After cooling down to room temperature, the black sediments
were separated magnetically and washed with ethanol and deionized water for
several times to eliminate organic and inorganic impurities, and then dried
in vacuum at 60 1C for 6 h. New J. Chem., 2011, 35, 10721079

The chemical reagents used in the work were ferrous chloride (FeCl2_4H2O),
sodium hydroxide (NaOH), and diamine hydrate (H4N2_H2O, 50% water). All the
chemicals were of analytical grade. Distilled water, degassed with N2 gas for half
an hour, was used for the preparation of an aqueous solution of Fe2 ions (0.2
mol/l). 30.0 ml Fe2 solution was put into a Teflon-lined stainless autoclave, sodium
hydroxide (0.6 g) was dissolved into 5.0 ml H4N2_H2O and then the mixture was
slowly dropped into the Teflon-lined stainless autoclave. Green precipitate
immediately appeared in aqueous solution of Fe(II) ions. During the experiment,
N2 was kept passing through the solution to prevent the oxidation of Fe2 in the

system. Then, the autoclave was put into oven, kept at certain temperatures for 6 h,
then cooled to room temperature naturally. The products were filtered and washed
several times with distilled water and absolute ethanol, and finally dried in vacuum
oven at 25 8C for 12 h. The samples, which were recorded at a scanning rate of
0.058/s with the 2y range from 10 to 708, were characterized by XRD using an Xray diffractometer with high-intensity Cu Ka radiation (l 1:5418 A ).
Materials Research Bulletin 38 (2003) 11131118