Production of a stable and homogeneous colloid dispersion of nano CoAl2O4 pigment for ceramic...

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ARTICLE IN PRESS+ModelECS-9593; No. of Pages 8

Available online at www.sciencedirect.com

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Journal of the European Ceramic Society xxx (2014) xxx–xxx

roduction of a stable and homogeneous colloid dispersion of nano CoAl2O4

pigment for ceramic ink-jet ink

Masoud Peymannia a, Atasheh Soleimani-Gorgani a,∗, Mehdi Ghahari b, Farhood Najafi c

a Department of Printing Science and Technology, Institute for Color Science and Technology, PO Box 16765654, Tehran, Iranb Department of Nanomaterials & Nanocoatings, Institute for Color Science and Technology, PO Box 16765654, Tehran, Iran

c Department of Resin and Additives, Institute for Color Science and Technology, PO Box 16765654, Tehran, Iran

Received 23 November 2013; received in revised form 15 March 2014; accepted 21 March 2014

bstract

ifferent types of nano-CoAl2O4 pigments were prepared by controlling concentration of cetyltrimethylammonium bromide (CTAB) and polyvinylyrrolidone (PVP) as double capping agents in a co-precipitation process. The prepared nano-CoAl2O4 pigments were characterized by TGA,V spectroscopy, and XRD. The optimum synthesized nano pigment was well dispersed into de-ionized water to form the ink. Rheology, surface

ension and DLS of the prepared ink were examined. The prepared ink was printed onto a ceramic substrate. The printing process was repeated 1, and 5 times in order to evaluate variations in the optical properties by changing thicknesses of the printed film. Appearance of the printed image
nd morphology of the prepared nano-pigments were observed by SEM. Moreover, shape and size of the nano-particles in the prepared ink werenvestigated by TEM. The obtained results revealed that the ink-jet printing method can be used to produce a nano-film of pigments on the ceramic.
2014 Elsevier Ltd. All rights reserved.

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eywords: Ink-jet printing; Nano-CoAl2O4; Blue pigment; Ceramic; Ink

. Introduction

Pigments of cobalt aluminate (CoAl2O4) are agents witheramic characteristics and widely employed as a blue pigments.oAl2O4 is a composite oxide which is made up of two metallicompounds in a spinel structure, where Co2+ ions are locatedn tetrahedral positions, and Al3+ ions are located in octahedralositions. This pigment not only has unique optical character-stics but also is a highly stable with excellent resistance toight and weather. Therefore, it has found a widespread use as aeramic pigment.1,2 Pigments of CoAl2O4 are typically synthe-ized in solid-phase reactions, in which chemical composition

Please cite this article in press as: Peymannia M, et al. Production of a stafor ceramic ink-jet ink. J Eur Ceram Soc (2014), http://dx.doi.org/10.1016

nd particle size of the resulting pigment are not uniform withevel of its impurities being rather high.3 Recently, wet-chemicalechniques have been applied to prepare the CoAl2O4 spinelncluding chemical co-precipitation,4 sol–gel,5–7polymeric

∗ Corresponding author. Tel.: +98 21 22969771; fax: +98 21 22947537.E-mail addresses: [email protected], [email protected]

A. Soleimani-Gorgani).

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ttp://dx.doi.org/10.1016/j.jeurceramsoc.2014.03.022955-2219/© 2014 Elsevier Ltd. All rights reserved.

recursor,8 and hydrothermal treatment.9,10 They have led toevelopment of the CoAl2O4 spinels which are characterizedy a fine particle size and uniform distribution. However, mostf these processes are expensive, difficult in their operation andresent low productivity.

Nano-pigment are typically fabricated onto ceramic sub-trates by various methods such as stereo-lithography,11

elective laser sintering,12 laminated object manufacturing,13

-D printing,14–16 dip coating,17 and ink-jet printing.18–21 Thenk-jet printing method, which is the subject of study in thisaper, is one of the most potential techniques for printing imagesnto ceramics without any patterning or etching processes. Ink-et printing is known as a non-contact process which deposits aesired amount of various functional materials directly from themages designed by computer onto a selected area of the sub-trates without any contamination.22 In ceramic ink-jet printing,eramic ink, which contains well dispersed ceramic pigments in

liquid carrier, passes through the printer nozzles (40–100 �m

ble and homogeneous colloid dispersion of nano CoAl2O4 pigment/j.jeurceramsoc.2014.03.022

n diameter) at high speeds.23,24 Droplets of the ceramic ink areprayed on the substrate where they spread on impact to produce

layer of less than 1 mm thickness.13

dx.doi.org/10.1016/j.jeurceramsoc.2014.03.022

http://www.sciencedirect.com/science/journal/09552219


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ARTICLE IN PRESS+ModelJECS-9593; No. of Pages 8

2 ropean Ceramic Society xxx (2014) xxx–xxx

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Table 1Concentration of PVP and CTAB to produce different nano-CoAl2O4 pigment.

Pigment (nano-CoAl2O4) PVP (wt%) CTAB (wt%)

1 0 02 2 03 0 1.724 2 0.435 2 0.856

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M. Peymannia et al. / Journal of the Eu

Despite all advantages of the ink-jet printing technology,ozzle clogging is one major problem in all of them. Sincehe inks used for inkjet printing contain insoluble micro orometimes nano-particles that can be agglomerated and pre-ipitated during the printing process. Therefore, preparing thenk-jet inks is very challenging for the researchers. Agglomer-tion is usually attributed to the attractive interactions betweenhe particles to reduce the surface energy. According to theerjiaguin, Landau, Verwey and Overbeek (DLVO) theory,

he potential energies of attraction and repulsion are summedo provide a total interaction potential energy between theolloidal particles. Therefore, a stable colloidal dispersion ofano-CoAl2O4 pigments can be prepared by an electrostaticr steric stabilization method. This is expected to form aepulsive layer, which suppresses the coagulation of the nano-oAl2O4 particles and stabilizes the nano-CoAl2O4 particles.onsequently, stability and homogeneity of an ink are the key

equirements, while their physicochemical properties are fur-her needed to meet the requirements of the commerciallyvailable printers. In order to prevent agglomeration of theano-particles in ink formulation, a stable and homogeneousolloid of the CoAl2O4 ceramic nano-pigment with differentorphologies was prepared. The homogeneous nano-CoAl2O4

articles were produced in a co-precipitation process, withhe particles size being controlled by changing the amountf cetyltrimethylammonium bromide (CTAB). Concentrationf polyvinyl pyrrolidone (PVP) in CTAB was either zero oronstant in (2 wt%) and all the other parameters such as start-ng materials, pH value, reaction temperature and calcinationrocess were kept constant. Then an optimally synthesized nano-olloid of CoAl2O4 with an average size of 45 nm and cyanolor were properly dispersed by itaconic acid-co-acrylic acidispersant into the de-ionized water uniformly to form the ink.ano-CoAl2O4 ink-jet ink was tried to be fabricated onto the

eramic substrate in order to see whether the nano-CoAl2O4 par-icle is feasible for the ink-jet printing or not. Rheology, surfaceension and DLS of the prepared ink were also examined. Therint was set to 1, 3 and 5 runs in order to evaluate variationsn the optical properties by varying thicknesses of the printedlm.

. Experimental

.1. Materials

Cobalt nitrate [Co (NO3)3·9H2O] and aluminum nitrate [AlNO3)3·9H2O], were provided by Sigma–Aldrich Company.he polyethylene glycol 200, isopropyl alcohol, citric acid,mmonium solution and 2-pyrrolidone were supplied by Merck,


ermany. All the other chemicals used in this work were cho-en from laboratory grade as received from Merck Company,K. The substrate used here was ceramic slide. The itaconic

cid-co-acrylic acid as a dispersing agent was synthesized bycrylic/itaconic acids copolymer (2:1) according to the proce-ure described in references.25

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2 3.42

.2. Equipment and instrumentation

The prepared ceramic ink was filtered through a 0.45 �mnd 0.2 �m Sartorius Minisart filter (Göttingen, Germany). Therepared ceramic slides were ink-jet printed using an Epson Sty-us Photo P50 printer in 1, 3 and 5 runs. The printed ceramiclides were subsequently dried and heat-treated in an Azar250 furnace at 1100 ◦C. The values of CIE-L*a*b* were com-uted under a D65 illuminant and CIE 1964 (10◦) standardbserver. In this method, L* is the lightness axis [black (0)hite (100)], a* represents the green (−) to red (+) axis, while* represents the blue (−) to yellow (+) axis. The values ofH, surface tension and viscosity of the prepared ink werebtained using 827 pH Metrohm, Tensiometer K100MK2 andheometer MCR 300 devices, respectively. Morphology of therepared nano-CoAl2O4 particles was determined through usef a Scanning Electron Microscope (SEM). Shape and sizef nano-CoAl2O4 ink was determined using TEM. The nano-oAl2O4 particles were examined with an X-ray diffractometer

XRD) (MXP3; Bruker AXS K.K.) at a CuK radiation to evalu-te the mineral composition. To address the lowest temperatureor burning the organic components out of ink, thermal behaviorsf the formulated ink were analyzed by using Thermo Gravime-ry/Differential Thermal Analyzer (Seiko Exstar 6000, TG/DTA100) in nitrogen atmosphere at a heating rate of 10 ◦C/min.

.3. Preparation of nano-CoAl2O4 ceramic pigments

The nano-CoAl2O4 pigments were prepared by theo-precipitation method. In this method, cobalt nitrateCo (NO3)3·9H2O] (0.1 mol, 29.1 g) and aluminum nitrateAl(NO3)3·9H2O] (0.2 mol, 75.01 g) were used as sources ofobalt and aluminum, respectively. Cobalt nitrate and aluminumitrate in the molar concentration ratio of Co:Al = 1:2 were dis-olved into the de-ionized water. Then PVP and CTAB weredded to the solution at different concentrations (Table 1). Theixture was stirred for 30 min, and then slowly titrated with

M sodium hydroxide at room temperature until the pH becamelkaline. The suspensions were then stirred for 2 h at room tem-erature, and pH values of the suspensions were measured. Thenal pH of the suspensions was adjusted to 12. Determinationf these pH values were done based on pH values at which alu-inum hydroxide and cobalt hydroxide were precipitated from


l and Co ions in the solution, respectively.21 The reaction prod-cts were collected using a centrifugal separator, washed morehan five times with the de-ionized water to remove Na+ and



ropean Ceramic Society xxx (2014) xxx–xxx 3

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O3− ions and other impurities, and then dried at 100 ◦C for

4 h to remove the moisture. Then, the resulted pigments werealcinated at 1100 ◦C at a rate of 10 ◦C per minutes. Meanwhile,he total soaking time was one hour, after which the pigmentsere cooled down to the room temperature.

.4. Preparation of ceramic ink

In order to provide a stable and homogeneous nano-CoAl2O4nk, the optimal nano CoAl2O4 pigments (Pigment 4) with anverage size of 45 nm and optimum cyan color were dispersedith a small amount of the disperse agent in the de-ionized water,iethylene glycol (DEG) and ethanol within a ball-milling pro-ess of 72 h. Concentration of nano-CoAl2O4 particles in thenk was controlled to be 8 mass%. At last, rheology, surface ten-ion and DLS of the prepared ink were evaluated, while physicalroperties of the printed ceramic were examined.

.5. Ink-jet printing of nano-CoAl2O4 ink

The ink-jet printing was carried out with Epson Stylus Photo50 printer at 1200 dpi resolution using the prepared nano-oAl2O4 ink onto the ceramic slides. This printer operates byse of a piezoelectric squeeze mode print head that squirts inkroplets through a nozzle with a 65 �m opening. Prior to eachun, the printer was flushed through with the nano-CoAl2O4 inkn order to remove any contamination from the previous prints.ll the substrates were cleaned with isopropanol, acetone, andethanol, and finally boiled in isopropanol inside an ultrasonic

ath. The pH of ink was adjusted to 7–7.5 by buffer solutiono prevent damaging of the print-head and cartridge. The printsere set to 1, 3 and 5 runs by a computer program to evaluate

he variation in the optical properties by changing thickness ofhe printed film. After printing, the ink-jet printed CoAl2O4 thinlms were annealed at 1100 ◦C temperature at a rate of 10 ◦C perinute, while total infusing time was half an hour after which itas cooled down to the room temperature.

. Results and discussion

.1. Characterization of nano-CoAl2O4 ceramic pigments

Fig. 1 shows XRD patterns of the synthesized nano-CoAl2O4eramic pigment with different surfactants. All the pigmentsere annealed at 1100 ◦C for 1 h. Several diffraction peaks arebserved in the patterns and the position of these peaks closelyesembles that of cubic CoAl2O4 according to JCPD Card No.0-458.26 One weak peak appears at about 2θ = 49◦ (331) in allamples specially in the XRD pattern of Pigments 2 and 4, thatonfirms presence of a spinel phase. This peak is characteristicor the CoAl2O4 phase and the related pattern was investigated in

◦

Please cite this article in press as: Peymannia M, et al. Production of a stable and homogeneous colloid dispersion of nano CoAl2O4 pigmentfor ceramic ink-jet ink. J Eur Ceram Soc (2014), http://dx.doi.org/10.1016/j.jeurceramsoc.2014.03.022

ore details at 2θ = 65 . It was recognized that all the pigmentsxcept Pigment 4 have a clear shoulder beside the main peakshich indicates that there is some Co3O4 as the minor phase in

hose Pigments. There is also a shift peak at 2θ = 37◦ in Pigments

Fig. 1. The XRD patterns of the nano-CoAl2O4 particles.



4 M. Peymannia et al. / Journal of the European Ceramic Society xxx (2014) xxx–xxx

Fig. 2. The thermogravimetric and differential thermogravimetr

Table 2Average grain size of the nano-CoAl2O4 crystals.

Nano-(CoAl2O4) pigment Size XRD (nm)

1 552 503 504 465 456

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cAtLwith more negative values corresponding to the bluer one. The

40

, 5 and 6, which are imply that those pigments contain theo3O4 phase.


Intensity of the diffraction peaks decrease with increasingoncentration of CTAB. This observation is associated witheduction in crystallinity. Moreover, as can be seen in Table 2,

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Fig. 3. Optical images of synthesiz

ic analysis of the CoAl2O4 Pigment 4 before calcination.

he primary crystallite size decreases with increasing the CTABoncentration. Size of the crystals was calculated by the meansf Scherer formula.

The TG/DTG curves for the Pigment 4 before calcination isepicted in Fig. 2. The endothermic peak at 201 ◦C may be dueo decomposition of the nitrates and PVP, accompanied by aignificant weight loss. The exothermic peak at 300 ◦C may beorresponded to decomposition of CTAB.

Table 3 and Fig. 3 show the colorimetric data and opti-al images of the produced nano-CoAl2O4 pigments (1 to 6).ccording to the values of L* a* b* in this table, increasing

he concentration of CTAB and PVP, reduces the values of*. The blue color is mainly governed by the parameter b*,


alue of b* was optimum when the CTAB concentration was.43 wt%. These results indicated that CTAB concentration had

ed nano-CoAl2O4 pigments.



M. Peymannia et al. / Journal of the Europea

Table 3CIE-L*a*b* values of synthesized nano-CoAl2O4 pigments.

Pigment (nano-CoAl2O4) L* a* b*

1 43.79 −21.24 −22.252 34.81 −25.87 −7.843 35.57 −25.67 −8.224 48.11 −19.31 −31.175 21.12 −7.78 −0.116 19.81 −3.98 0.48

Table 4CIE-L*a*b* values of printed nano ceramic ink (Pigment 4).

Printing run L* a* b*

1 75.55 −0.33 −2.553 73.01 −0.42 −4.065

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71.03 −0.48 −6.46

significant effect on color tone of the resulting product, andt was suggested that bluer image could be obtained throughhe Pigment 4, in which the nano-particles of cobalt alumi-ate (CoAl2O4) ceramic, was synthesized with PVP (2 wt%)nd CTAB (0.43 wt%). The color of the Pigments 5 and 6 wasear black; however the color of Pigments 2 and 3 were reallylose to the green.

Table 4 and Fig. 4 summarize colorimetric data and opticalmages of the printed nano-CoAl2O4 ink, which was formulatedith Pigment 4. According the values of L* a* b* in this table,

ncreasing the number of the printing runs, reduces the L* valuesnd increases the b* value. Therefore, a bluer image could beielded within five printing runs.

.2. Effect of PVP and CTAB on nano-cobalt aluminateCoAl2O4) ceramic pigment

Based on XRD and SEM images, PVP affects size andhape of the nano-CoAl2O4 pigments. The particle size of nano-oAl2O4 pigment, which was synthesized without adding PVPnd CTAB, was measured to be 55 nm. When the amount of


VP was increased to 2 wt%, the particle size was also changedo 50 nm. At pH = 12 the ions of Co2+ and Al3+ were generatedn the mixed solution. PVP contains hydrophilic polar groups

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Fig. 4. Optical images of printed na

n Ceramic Society xxx (2014) xxx–xxx 5

O and N) that will preferentially interact on the crystal viahemical adsorption, which can slow down growth rate of therystals and yield smaller nano-pigments.

To study the effect of CTAB content on structure and size ofhe CoAl2O4 nanopigments, the nanoparticles of CoAl2O4 wereroduced in different concentrations of CTAB with morpholo-ies of the particles being examined by SEM. The results of XRDnd SEM showed that the particle size of Pigment 1 was 55 nm.n the other hand, when the amount of CTAB was increased to.7 g, the particle size decreased to 50 nm. As a common sur-actant, CTAB usually acts as a powerful protective agent andtabilizer for synthesis of the nano-metal particles. Being anlectron deficient, ammonium nitrogen of the CTAB coordinatedith the nano-CoAl2O4 particles. Both XRD results and SEM

mages of the nano-CoAl2O4 pigments synthesized by control-ing the CTAB concentration in 2 wt% PVP by co-precipitation

ethod proved that increasing the CTAB concentration willeduce size of nano-CoAl2O4 pigments continuously.

It is suggested that PVP interacts with Co2+ and Al3+ ions on or C O with their lone electron pairs. In addition, after form-

ng the nano-particles, steric effect of the PVP would restrictrowth of the nano-particles and thus inhibit agglomeration ofhe nano-particles. As a cationic surfactant, the CTAB easilyoordinates with the nano-CoAl2O4 particles by the ammo-ium nitrogen. CTAB also forms a similar double-layer structureround the nano-CoAl2O4 particle, which not only separates theano-particles of CoAl2O4 by electrostatic forces, but also byteric effect. It is the coupling interaction between the two surfac-ants that makes the nano-particle well suspended in the solution,nd prevents further agglomeration of the nano-CoAl2O4 par-icles. SEM photographs of the synthesized nano-CoAl2O4igments (1–6) are illustrated in Fig. 5.

.3. Rheological behavior of prepared nano-CoAl2O4 ink

Viscosity of the ceramic ink mainly affects the rheologicalharacteristics through capillary nozzles of the printer. A highiscosity could lead to an insufficient jet of ink, whereas a signif-


hich makes the ink drop crescent shaped, resulting in dampedscillation the result being that the ink-jet velocity decreases.ig. 6 shows the variation of viscosities with shear rate for

no ceramic ink (Pigment 4).



6 M. Peymannia et al. / Journal of the European Ceramic Society xxx (2014) xxx–xxx

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Fig. 5. SEM image of synthesized nano-C

ano-CoAl2O4 ceramic ink on a logarithmic scale. It is evi-ent that when viscosity of the ceramic ink was reduced to.17 mPas by increasing the shear rate to 1000 S−1, the preparednk behaves as non-Newtonian fluids. This observation is con-istent with the shear thinning behavior represented by severalther ceramic inks.27

.4. Surface tension of prepared nano-CoAl2O4 ink

Surface tension of the ceramic ink mainly affects two mainarts of the printing process. Firstly, decomposition into finerops of the ceramic ink efflux through capillary tube of therinter nozzle; and secondly, wettability of the ceramic ink ontohe forming carrier. The water, as a major phase in the ink formu-ation, had a predominant role in controlling the surface tension.xistence of the disperse agent further contributed to reduce

he surface tension. The surface tension of the ceramic ink was


ound to be 37.2 mN m−1, placing it within a normal range of thealues for commercial ink-jet inks of the ceramic printing.28,29

Fig. 6. Variation of viscosity with shear rate.

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O4 Pigments 1–6. Scale bars are 500 nm.

.5. DLS of prepared nano-CoAl2O4 ink

Size of the nano-CoAl2O4 particles which were dispersed inn itaconic acid-co-acrylic acid dispersant was determined byynamic light scattering method.

The distribution obtained from the prepared ink was mono-odal with one narrow peak that was about 45 nm (Fig. 7),hich proved a well dispersion of nano-CoAl2O4 particles in

nk formulation and agglomeration of non-appearance particles.

.6. Morphology of nano-CoAl2O4 ink by TEM

TEM image of the nano-CoAl2O4 pigment (Pigment 4) inhe ceramic ink is shown in Fig. 8, which clearly demonstratesell dispersed particles with minimal size variation (10–50 nm)

n the ink. No agglomerate was found and the particles werelmost completely spherical. The PVP and CTAB formed a shellround surfaces of the particles protecting them against collision.herefore, they are stable, uniform and separated in the ink.


he TEM image of the nano-CoAl2O4 pigment (Pigment 1) ineramic ink is depicted in Fig. 9, which is associated with angglomeration phenomenon.

Fig. 7. Size distribution by volume (Pigment 4).



M. Peymannia et al. / Journal of the Europea

Fig. 8. TEM image of nano-CoAl2O4 particle (Pigment 4) in the ceramic ink.

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ig. 9. TEM image of nano-CoAl2O4 particle (Pigment 1) in the ceramic ink.

. Conclusions

In this study, nano-CoAl2O4 pigments were produced by ao-precipitation method, while the size and distribution of thearticles have been controlled by varying the amount of CTABnd PVP. Two kinds of surfactant were used in the reaction,ncluding CTAB, and PVP. Change of the surfactant materialsnfluencing the shape, size and optical properties of the synthe-


ized nano-pigments. Either CTAB as the only protective agentithout adding PVP is used or PVP as the only protective sol-ent, the reaction has generated green nanopigments of CoAl2O4

1

n Ceramic Society xxx (2014) xxx–xxx 7

ith an average size of 50 nm that is of no interest. Cyan pre-ipitations could be seen clearly only when CTAB and PVP aresed together.

Homogeneous and stable cyan ink, without any visiblearticles were obtained with dispersion of the produced nano-oAl2O4 particles by an itaconic acid-co-acrylic acid dispersant.hen the prepared ink was printed using an Epson Stylus Photo50 printer onto ceramic slides. The printing was carried outy using a computer program in 1, 3 and 5 runs. A bluer imageould be obtained through increasing the printing runs. Surfaceension of the prepared ink at pH = 7.5 was 37.2 mN m−1, whileiscosities of this ink were reduced to 2.7 mPas by increasing thehear rate up to 1000 S−1. Therefore, the obtained ink behaveds non-Newtonian fluids. The values of surface tension and vis-osity in the prepared ceramic ink fell into the range required bydrop on demand” ink-jet printers, making the inks compatibleith the commercially available printers. DLS of the prepared

nk was mono-modal with one narrow peak, which was about09 nm. TEM images proved well dispersed particles with theinimal size variation (10–50 nm) in the ink. In conclusion the

esults of this work show that the direct ceramic ink-jet prin-ing (DCIJP) method can be used to produce used to produce aano-film of pigments on the ceramic.

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Production of a stable and homogeneous colloid dispersion of nano CoAl2O4 pigment for ceramic...

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