Materials Science s a nd Applications, 2011, 2, 1578-1583
doi:10.4236/msa.2011.211211 Published Online November 2011 (http://www.SciRP.org/journal/msa)
Synthesis and Pigmental Properties of Nickel
Phosphates by the Substitution with Tetravalent
Cerium Cation
Hiroaki Onoda, Takeshi Sakumura
Department of Informatics and Environmental Sciences, Faculty of Life and Environmental Sciences, Kyoto Prefectural University,
Kyoto, Japan.
Received August 15th, 2011; revised September 27th, 2011; accepted October 12th, 2011.
ABSTRACT
In this paper, we report the preparation of nickel phosphate in aqueous solution and its use as inorganic pigment. Be-
cause cerium phosphate is insoluble in acidic and basic solution, the addition of cerium was tried to improve the acid
and base resistance of nickel phosphate pigment. The cerium substituted nickel phosphates were prepared from phos-
phoric acid, nickel nitrate, and ammonium cerium nitrate solution. The additional effects of tetravalent cerium cation
were studied on the chemical composition, particle shape and size distribution, specific surface area, color, acid and
base resistance of the precipitates and their thermal products.
Keywords: Inorganic Compounds, Chemical Synthesis, Precipitation, X-Ray Diffraction, Optical Properties
1. Introduction
Phosphates have been used for ceramic materials, cataly-
sts, fluorescent materials, dielectric substances, metal sur-
face treatment, detergent, food additives, fuel cells, pig-
ments, etc. [1-3]. Especially, as a pigment, these ma-
terials have good anticorrosion properties for oxidation
reaction and suitable for coating [4-7]. However, there is
a weak point that is a certain degree of solubility for aci-
dic and basic solution.
It is well known that rare earth phosphates are insolu-
ble for acidic and basic solution in the groups of phos-
phate materials. In general, the addition of rare earth ele-
ments gives higher functional properties to the material
[8]. Consequently, the addition of rare earth cation had
the anticipation to improve the acid and base resistance
of inorganic phosphate pigments and pigmental proper-
ties [9-11].
The substitution with lanthanum in nickel and cobalt
phosphate materials was studied on the chemical com-
position, powder condition, color, acid and base resis-
tance in previous works [12,13]. Specific surface area of
phosphates increased and particle size became larger by
the substitution with lanthanum. The substitution with lan-
thanum was effective on acid and base resistance for de-
sign of inorganic phosphate pigment. However, the color
of phosphate materials was whitened by the sub- stitution
with lanthanum.
Cerium cation is also one of rare earth cation. The di-
fferent phenomena are expected with lanthanum cation,
because cerium cation has stable tri- and tetra-valent sta-
tes [14]. Generally, tetravalent cerium cation forms the
yellow materials. Therefore, the substitution with tetra—
valent cerium cation is suitable to improve the acid and
base resistance of yellow pigments. In this work, nickel-
cerium (+IV) phosp hates were synthesized in aqueous
solution. The obtained products were estimated from their
particle shape and size distribution, specific surface area,
color, acid and base resistance.
2. Experimental Procedure
The 0.1 mol/L of nickel nitrate, Ni(NO3)2, solution was
mixed with 0.1 mol/L of phosphoric acid solution in the
molar ratio of Ni/P = 3/2. This ratio is settled from the
chemical composition of nickel orthophosphate, Ni3(PO4)2.
The certain part of nickel nitrate was substituted with
ammonium cerium nitrate, (NH4)2Ce(NO 3)6, in the molar
ratio of Ni/Ce = 10/0, 9/1, 8/2, 5/5, 2/8, and 0/10 [12,13].
For the valence balance, two nickel cations were replaced
with one cerium cation. Finally, the solutions were mixed
in the molar ratio of Ce/P = 3/4. This ratio is corres-

Synthesis and Pigmental Properties of Nickel Phosphates by the Substitution with Tetravalent Cerium Cation1579

ponding to Ce3(PO4)4. Then, the mixed solution was ad-
justed to pH 7 by ammonia solution. The precipitate was
filtered off and dried in air condition. All chemicals were
of guaranteed reagents from Wako Chemical Industries
Ltd. (Osaka, Japan) without further purification.
A part of the precipitates was dissolved in hydro-
chloric acid solution. The ratios of phosphorus and ce-
rium in the precipitates were also calculated from ICP re-
sults of these solutions, using SPS1500VR, Seiko Ins-
truments Inc. The thermal behavior of these materials was
analyzed by TG-DTA and XRD. TG and DTA curves
were measured with a Shimadzu DTG-60H at a heating
rate of 10˚C/min under air. XRD patterns were recorded
on a Rigaku Denki RINT 1200 M X-Ray diffractometer
using monochromated CuKα radiation.
The powder properties of thermal products at 200˚C,
400˚C, 600˚C, and 800˚C were characterized by particle
shape, particle size distribution, specific surface area, and
their color. Particle shapes were observed by scanning
electron micrographs (SEM) using JGM-5510LV, JEOL
Ltd. Particle size distribution was measured with laser
diffraction/scattering particle size distribution HORIBA
LA-910. Specific surface areas of phosphates were cal-
culated from the amount of nitrogen gas adsorbed at the
temperature of liquid nitrogen by BET method with
Belsorp mini from BEL JAPAN, INC. The color of phos-
phate pigments was estimated by ultraviolet—visible (UV-
Vis) reflectance spectra with a Shimadzu UV2550.
Furthermore, the acid and base resistance of materials
was estimated in following method. The 0.1 g of thermal
products was allowed to stand in 100 ml of 0.1 wt%
sulphuric acid or 0.1 wt% sodium hydroxide solution for
1 day. Then, solid was removed off by filtration, the
solution was dilute with nitric acid for ICP measurement.
The concentrations of phosphorus, nickel, cerium cation
were calculated by ICP results. As a resistance estimation,
the solubility (%) of target elements was calculated to
divide by the concentration that thermal products were
completely dissolved by hot hydrochloric acid.
3. Results and Discussion
3.1. Chemical Composition of Nickel—Cerium
Phosphates
Table 1 shows ICP results of samples synthesized in Ni/Ce
ratios. From the valence of nickel, cerium cations, and pho-
sphate anion, hydrogen ratio was calculated in the follo-
wing equation.


zhydrogen rafio
32xnichel ratio4ycerium ratio  (1)
The negative value of z means the existence of hydro-
xide anion. Sample prepared in Ni/Ce = 10/0 had the near
ratio with nickel hydrogenphosphate, NiHPO4. On the
other hand, cerium ratio was enough high at samples pre-
pared in Ni/Ce = 0/10. Cerium orthophosphate was con-
sidered to form with cerium hydroxide in this condition.
In the middle Ni/Ce ratios, cerium ratio was lower than
that in preparation process. In previous works [12,13],
rare earth ratio in precipitates was higher than that in pre-
paration conditions. This phenomenon was caused from
that rare earth phosphates have smaller solubility than
transition metal phosphates. In the case of tetravalent ce-
rium phosphate, this tendency was not appeared. How-
ever, it is not clear why the ratio of cerium became lower
than preparation condition.
Figure 1 shows DTA curves of nickel—cerium phos-
phates prepared in various Ni/Ce ratios. DTA curves of
sample prepared in Ni/Ce = 10/0 had large endo- thermic
peak at 100˚C, small endothermic peak at 250˚C, and
small exothermic peak at 770˚C (Figure 1(a)). These
peaks were due to the volatilization of water, dehy- dration
condensation of phosphate, and crystallization of nickel
phosphate, respectively [12]. Nickel hydrogenphosphate
was condensed to nickel pyrophosphate in following re-
action at 250˚C.
2NiHPO4 → Ni2P2O7 + H2O (2)
The substitution with cerium produced the exothermic
peaks at the range from 260˚C to 330˚C (Figures 1(b)-
(f)). These peaks were related with the reduction of ce-
rium cation [15]. Figure 2 shows TG curves of samples
prepared in various Ni/Ce ratios. Samples prepared in
Ni/Ce = 10/0 had large weight loss over 50%. Nickel
hydrogenphosphate had large amount of adsorbed and
crystalline water. By the substitution with cerium cation,
this weight loss became small.
Figure 1. DTA curves of samples prepared in various Ni/Ce
ratios, (a) 10/0; (b) 9/1; (c) 8/2; (d) 5/5; (e) 2/8; and (f) 0/10.

Synthesis and Pigmental Properties of Nickel Phosphates by the Substitution with Tetravalent Cerium Cation 1580
Figure 2. TG curves of samples prepared in various Ni/Ce
ratios, (a) 10/0; (b) 9/1; (c) 8/2; (d) 5/5; (e) 2/8; and (f) 0/10.
Samples prepared in Ni/Ce = 10/0 - 5/5 indicated XRD
peaks of NH4H2PO4. Samples heated at 200˚C - 600˚C
were amorphous phase in XRD analyses except for sample
prepared in Ni/Ce = 0/10 and then heated at 600˚C. This
exceptional sample had the peaks of Monazite-type
CePO4. Figure 3 shows XRD patterns of samples synthe-
sized in various Ni/Ce ratios and then heated at 800˚C.
Sample prepared in Ni/Ce = 10/0 had strong peaks of
nickel pyrophosphate, Ni2P2O7. The peaks of Monazite-
type CePO4 were observed in XRD patterns of cerium-
substituted samples. Tetravalent cerium phosphate changed
to trivalent cerium compound by heating.
We considered that the following reaction occurred in
sample prepared at Ni/Ce = 0/10.
Ce3(PO4)4 + Ce(OH)4 → 4CePO4 + H2O + O2 (3)
The starting materials, the mixture of cerium phos-
phate and hydroxide, was suited to the Ce/P ratio (=0.986)
in Table 1. Sample heated at 800˚C indicated XRD
peaks of CePO4 (Figure 3(f)). TG curves of cerium-
substituted samples had weight loss at the range from
260˚C to 330˚C corresponding with exothermic peak in
DTA curves (Figures 1, 2). These weight losses were cau-
sed from the volatilization of water and oxygen. The co-
lor of sample prepared in Ni/Ce = 0/10 changed from ye-
llow to white by heating at 400˚C. Tetravalent cerium
phosphate was yellow powder and trivalent one was whi-
te powder.
3.2. Powder Properties of Nickel—Cerium
Phosphates
Figure 4 shows SEM images of samples synthesized in
various Ni/Ce ratios. Sample prepared in Ni/Ce = 10/0
consisted of small particles. On the other hand, samples
prepared at high cerium ratios had large particles. The
Table 1. Chemical composition, NixCeyHzPO4, of precipi-
tates from ICP measurements.
Ni/Ce* x y z Ni/Ce**
10/0 1.064 0 0.872 10/0
9/1 0.786 0.027 1.320 9/0.31
8/2 0.915 0.179 0.454 8/1.57
5/5 0.668 0.401 0.060 5/3.00
2/8 0.267 0.687 –0.015 2/5.15
0/10 0 0.986 –0.944 0/10
*: preparation condition; **: in precipitates.
10 20 30 40 50 60
Intensity
2 /deg.θ
(a)
(f)
(c)
(b)
(d)
(e)
●●●
●
●
●●
◇◇
◇◇◇
◇
◇
◇◇
Figure 3. XRD patterns of samples prepared in various
Ni/Ce ratios and then heated at 800˚C, (a) 10/0; (b) 9/1; (c)
8/2; (d) 5/5; (e) 2/8; and (f) 0/10, ●; Ni2P2O7 and ◇; CePO4.
specified shape like pillar was observed in samples pre-
pared at Ni/Ce = 9/1 and 5/5. Samples prepared in Ni/Ce
= 2/8 and 0/10 had large particles.
Figure 5 shows the particle size distribution of sam-
ples synthesized in various Ni/Ce ratios. The main part of
particle of sample prepared in Ni/Ce = 10/0 was from
100 to 10 µm in size. Samples prepared in Ni/Ce = 9/1
and 8/2 had smaller particle size than sample prepared in
Ni/Ce = 10/0. In contrast, samples prepared in Ni/Ce =
2/8 and 0/10 had much larger particles. Particle size
distribution of samples prepared in this work was less
affected by heating temperature.
Table 2 shows the specific surface area of samples
synthesized in various Ni/Ce ratios. Specific surface area
as well as particle size has influence on color, and so-
lubility of phosphate materials [16-19]. Sample prepar-
ed in Ni/Ce = 8/2 had large specific surface area. On the
other hand, sample prepared in Ni/Ce = 2/8 had small
specific surface area. The change of specific surface area

Synthesis and Pigmental Properties of Nickel Phosphates by the Substitution with Tetravalent Cerium Cation1581
10μm 10μm
(a) (b)
10μm 10μm
(c) (d)
10μm 10μm
(e) (f)
Figure 4. SEM images of samples prepared in various Ni/Ce
ratios, (a) 10/0; (b) 9/1; (c) 8/2; (d) 5/5; (e) 2/8; and (f) 0/10.
Table 2. Specific surface area of nickel—cerium phosphates
/m2·g–1.
Temp. Ni/Ce
/˚C 10/0 9/1 8/2 5/5 2/8 0/10
200 42.83 43.63 62.4322.43 1.13 29.99
400 34.58 34.38 35.6415.88 14.8013.33
600 26.54 24.64 28.4011.33 21.3438.12
800 3.11 4.80 5.72 2.10 4.65 6.08
was not proportional to the Ni/Ce ratio. Samples pre-
pared in all Ni/Ce ratios had smaller specific surface area
by heating at 800˚C.
3.3. Pigmental Properties of Phosphates
The color of samples without heating changed from light
green to yellow with the increase of cerium ratio. By
heating, light green of nickel hydrogenphosphate trans-
formed to dark yellow powder of nickel pyrophosphate.
The yellow powder of tetravalent cerium phosphate chan-
ged to the white powder of trivalent cerium phosphate by
heating over 400˚C. Figure 6 shows UV-Vis reflectance
Figure 5. Particle size distribution of samples prepared in
various Ni/Ce ratios, (a) 10/0; (b) 9/1; (c) 8/2; (d) 5/5; (e) 2/8;
and (f) 0/10.
Figure 6. UV-Vis reflectance spectra of samples prepared in
various Ni/Ce ratios and then heated at 800˚C, (a) 10/0; (b)
9/1; (c) 8/2; (d) 5/5; (e) 2/8; and (f) 0/10.
spectra of samples synthesized in various Ni/Ce ratios
and then heated at 800˚C. Sample in Ni/Ce = 10/0 had
strong reflectance at 350 and 640 nm and weak reflec-
tance at 430 nm. By the substitution with cerium, the
adsorption at 430 nm became smaller. The optical band
gap energy of thermal products at 800 decreased from
5.17 eV to 4.43 eV [20]. The color of materials changed
from yellow to white (Figure 7) [21].
Figure 8 shows acid resistance of samples synthesized
in various Ni/Ce ratios. The small number of solubility
means high acid resistance. The eluted ratio of phos-
phorus changed from 100 to 28% with the increase of
cerium ratio [22]. Formation of cerium phosphate inhi-
bited the elution of phosphate materials. The elution ratio
of nickel cation changed a little smaller by the sub-
stitution with cerium to Ni/Ce = 5/5. Sample prepared in

Synthesis and Pigmental Properties of Nickel Phosphates by the Substitution with Tetravalent Cerium Cation 1582
N
i/Ce
R.T.
200˚C
400˚C
600˚C
800˚C
10/0 9/1 8/2 5/5 2/8 0/10
Figure 7. Photographs of samples prepared in various Ni/Ce
ratios.
Figure 8. Acid resistance of samples prepared in various
Ni/Ce ratios, (a) phosphorus; (b) nickel; and (c) cerium.
Table 3. Elution ratio of phosphorus in basic solution/%.
Temp. Ni/Ce
/˚C 10/0 9/1 8/2 5/5 2/8 0/10
R.T. 87.47 93.67 90.5475.00 48.4340.23
200 67.96 83.20 67.7164.49 4.14 22.12
400 62.70 52.26 47.505.13 2.05 16.16
600 46.59 38.85 40.658.41 4.84 15.71
800 0 1.01 0.05 0 8.28 0
Ni/Ce = 5/5 indicated small elution ratio of cerium ca-
tion.
In basic solution, all samples indicated no elution of
nickel and cerium cations, because of the formation of
their hydroxides. Table 3 shows the solubility of phos-
phorus in sodium hydroxide solution. The eluted ratio of
phosphorus had the tendency to decrease with the increase
of cerium ratio. Samples had high base resistance by hea-
ting at high temperature.
4. Conclusions
In summary, nickel-cerium phosphates were prepared in
aqueous solution. The obtained products were estimated
for design of functional materials. The cerium ratio in
precipitates was lower than that in preparation process.
By the substitution of cerium cation, samples changed the
mixture of nickel phosphate and cerium phosphate. The
color of nickel phosphate was changed from light green
to dark yellow by the substitution with cerium. The ce-
rium substituted nickel phosphate changed to yellow pow-
der by heating. The acid and base resistance of nickel pho-
sphate materials improved by the substitution with cerium.
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